# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry. # This journal is © The Royal Society of Chemistry 2018 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_I _database_code_depnum_ccdc_archive 'CCDC 1875539' _audit_update_record ; 2018-10-26 deposited with the CCDC. 2018-12-12 downloaded from the CCDC. ; _chemical_name_systematic ? _chemical_name_common 4'-(4-nitrophenyl)spiro[indene-2,5'-[1,4,2]oxathiazol]-1(3H)-one-4'-oxide _chemical_formula_moiety 'C16 H10 N2 O5 S' _chemical_formula_sum 'C16 H10 N2 O5 S' _chemical_formula_iupac ? _chemical_formula_weight 342.32 _chemical_melting_point ? _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5520(11) _cell_length_b 8.2283(11) _cell_length_c 12.8010(18) _cell_angle_alpha 74.726(4) _cell_angle_beta 86.674(5) _cell_angle_gamma 72.819(4) _cell_volume 732.95(18) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5153 _cell_measurement_theta_min 2.6782 _cell_measurement_theta_max 26.1366 _cell_measurement_temperature 300.(2) _exptl_crystal_description PLATE _exptl_crystal_colour 'clear colourless' _exptl_crystal_size_max 0.498 _exptl_crystal_size_mid 0.385 _exptl_crystal_size_min 0.184 _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 352 _exptl_absorpt_coefficient_mu 0.252 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/4 (Bruker AXS Inc.)' _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.95 _exptl_special_details ; ; _diffrn_ambient_temperature 300.(2) _diffrn_source 'micro-focus sealed tube' _diffrn_source_type 'Bruker X2S' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'doubly curved silicon crystal' _diffrn_measurement_device_type 'Bruker SMART X2S' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3330 _diffrn_reflns_number 15211 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_unetI/netI 0.0329 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 26.40 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _refine_special_details ; ; _reflns_number_total 2960 _reflns_number_gt 2275 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_gt 0.1583 _refine_ls_wR_factor_ref 0.1729 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.057 _refine_ls_number_reflns 2960 _refine_ls_number_parameters 217 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1207P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.358 _refine_diff_density_min -0.405 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ? _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.6826(2) 0.9498(2) 0.24895(15) 0.0595(5) Uani d . . . 1 . . S S2 0.72499(8) 0.79147(9) 0.18484(5) 0.0538(3) Uani d U . . 1 . . C C3 0.4974(3) 0.7564(3) 0.22754(17) 0.0400(5) Uani d . . . 1 . . C C4 0.4596(3) 0.8320(3) 0.32380(17) 0.0400(5) Uani d . . . 1 . . N N5 0.5520(3) 0.9351(3) 0.33477(16) 0.0511(5) Uani d . . . 1 . . O O6 0.8669(2) 0.6377(3) 0.24525(16) 0.0704(6) Uani d U . . 1 . . C C7 0.3576(3) 0.8677(3) 0.13117(17) 0.0416(5) Uani d . . . 1 . . C C8 0.3056(3) 0.7421(3) 0.08614(16) 0.0373(5) Uani d . . . 1 . . C C9 0.1919(3) 0.7767(3) -0.00449(18) 0.0463(5) Uani d . . . 1 . . H H9 0.1358 0.8916 -0.044 0.056 Uiso calc U . R 1 . . C C10 0.1657(3) 0.6358(4) -0.0333(2) 0.0534(6) Uani d . . . 1 . . H H10 0.0931 0.6553 -0.0941 0.064 Uiso calc U . R 1 . . C C11 0.2462(3) 0.4651(3) 0.0272(2) 0.0515(6) Uani d . . . 1 . . H H11 0.2251 0.372 0.0067 0.062 Uiso calc U . R 1 . . C C12 0.3568(3) 0.4300(3) 0.11721(18) 0.0435(5) Uani d . . . 1 . . H H12 0.4101 0.3149 0.1573 0.052 Uiso calc U . R 1 . . C C13 0.3867(3) 0.5708(3) 0.14647(17) 0.0365(5) Uani d . . . 1 . . C C14 0.5030(3) 0.5641(3) 0.24007(17) 0.0408(5) Uani d . . . 1 . . H H14A 0.6291 0.4914 0.2364 0.049 Uiso calc U . R 1 . . H H14B 0.4514 0.5172 0.3086 0.049 Uiso calc U . R 1 . . O O15 0.3132(3) 1.0254(2) 0.10213(15) 0.0681(5) Uani d . . . 1 . . C C16 0.3173(3) 0.8013(3) 0.40496(17) 0.0395(5) Uani d . . . 1 . . C C17 0.1681(3) 0.7490(3) 0.38056(18) 0.0457(5) Uani d . . . 1 . . H H17 0.1591 0.73 0.3128 0.055 Uiso calc U . R 1 . . C C18 0.0338(3) 0.7252(3) 0.45640(19) 0.0455(5) Uani d . . . 1 . . H H18 -0.0641 0.6876 0.4409 0.055 Uiso calc U . R 1 . . C C19 0.0474(3) 0.7579(3) 0.55508(18) 0.0415(5) Uani d . . . 1 . . C C20 0.1923(3) 0.8121(3) 0.58168(17) 0.0421(5) Uani d . . . 1 . . H H20 0.1976 0.8347 0.6487 0.05 Uiso calc U . R 1 . . C C21 0.3278(3) 0.8316(3) 0.50721(17) 0.0405(5) Uani d . . . 1 . . H H21 0.4274 0.8651 0.5245 0.049 Uiso calc U . R 1 . . N N22 -0.0990(3) 0.7381(3) 0.63478(16) 0.0512(5) Uani d . . . 1 . . O O23 -0.0893(3) 0.7781(3) 0.71925(15) 0.0705(5) Uani d . . . 1 . . O O24 -0.2223(2) 0.6847(3) 0.61144(17) 0.0702(5) Uani d . . . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0716(10) 0.0691(11) 0.0592(11) -0.0483(9) 0.0172(8) -0.0245(9) S2 0.0597(4) 0.0696(5) 0.0463(4) -0.0362(3) 0.0127(3) -0.0216(3) C3 0.0465(11) 0.0415(11) 0.0362(11) -0.0196(9) 0.0018(8) -0.0096(9) C4 0.0456(11) 0.0414(12) 0.0372(11) -0.0177(9) -0.0035(9) -0.0107(9) N5 0.0609(11) 0.0608(13) 0.0473(11) -0.0356(10) 0.0108(9) -0.0222(10) O6 0.0450(9) 0.0844(13) 0.0858(15) -0.0156(9) -0.0026(9) -0.0315(11) C7 0.0557(12) 0.0338(11) 0.0358(11) -0.0154(9) -0.0009(9) -0.0069(9) C8 0.0408(10) 0.0405(11) 0.0331(10) -0.0152(9) 0.0020(8) -0.0101(9) C9 0.0420(11) 0.0568(14) 0.0394(12) -0.0153(10) -0.0016(9) -0.0093(10) C10 0.0474(12) 0.0816(18) 0.0455(13) -0.0335(12) 0.0037(10) -0.0247(13) C11 0.0569(13) 0.0620(15) 0.0555(14) -0.0354(11) 0.0139(11) -0.0309(12) C12 0.0468(11) 0.0422(12) 0.0495(13) -0.0223(9) 0.0140(9) -0.0175(10) C13 0.0358(10) 0.0374(11) 0.0404(11) -0.0157(8) 0.0091(8) -0.0130(9) C14 0.0453(11) 0.0372(11) 0.0410(12) -0.0148(9) 0.0029(9) -0.0093(9) O15 0.1066(14) 0.0338(10) 0.0596(12) -0.0144(9) -0.0161(10) -0.0074(8) C16 0.0442(11) 0.0379(11) 0.0386(11) -0.0153(9) -0.0012(9) -0.0094(9) C17 0.0503(12) 0.0546(13) 0.0404(12) -0.0235(10) 0.0009(9) -0.0168(10) C18 0.0421(11) 0.0481(13) 0.0498(13) -0.0185(10) -0.0013(9) -0.0120(10) C19 0.0443(11) 0.0345(11) 0.0416(12) -0.0099(9) 0.0030(9) -0.0051(9) C20 0.0533(12) 0.0388(11) 0.0333(11) -0.0121(9) -0.0028(9) -0.0084(9) C21 0.0447(11) 0.0405(11) 0.0390(11) -0.0163(9) -0.0038(9) -0.0096(9) N22 0.0512(11) 0.0476(11) 0.0481(12) -0.0122(9) 0.0053(9) -0.0046(9) O23 0.0791(12) 0.0845(14) 0.0508(11) -0.0280(10) 0.0193(9) -0.0212(10) O24 0.0552(10) 0.0878(14) 0.0742(13) -0.0343(10) 0.0127(9) -0.0193(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 N5 . 1.439(2) ? O1 S2 . 1.6610(19) ? S2 O6 . 1.458(2) ? S2 C3 . 1.854(2) ? C3 C4 . 1.499(3) ? C3 C14 . 1.535(3) ? C3 C7 . 1.568(3) ? C4 N5 . 1.284(3) ? C4 C16 . 1.480(3) ? C7 O15 . 1.199(3) ? C7 C8 . 1.461(3) ? C8 C13 . 1.389(3) ? C8 C9 . 1.401(3) ? C9 C10 . 1.374(3) ? C9 H9 . 0.93 ? C10 C11 . 1.385(4) ? C10 H10 . 0.93 ? C11 C12 . 1.379(3) ? C11 H11 . 0.93 ? C12 C13 . 1.388(3) ? C12 H12 . 0.93 ? C13 C14 . 1.506(3) ? C14 H14A . 0.97 ? C14 H14B . 0.97 ? C16 C17 . 1.396(3) ? C16 C21 . 1.406(3) ? C17 C18 . 1.383(3) ? C17 H17 . 0.93 ? C18 C19 . 1.375(3) ? C18 H18 . 0.93 ? C19 C20 . 1.387(3) ? C19 N22 . 1.476(3) ? C20 C21 . 1.373(3) ? C20 H20 . 0.93 ? C21 H21 . 0.93 ? N22 O24 . 1.222(2) ? N22 O23 . 1.222(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N5 O1 S2 . . 114.08(12) ? O6 S2 O1 . . 109.17(10) ? O6 S2 C3 . . 106.93(10) ? O1 S2 C3 . . 89.61(8) ? C4 C3 C14 . . 119.84(17) ? C4 C3 C7 . . 111.99(17) ? C14 C3 C7 . . 105.57(16) ? C4 C3 S2 . . 101.54(13) ? C14 C3 S2 . . 110.94(14) ? C7 C3 S2 . . 106.31(13) ? N5 C4 C16 . . 117.70(19) ? N5 C4 C3 . . 118.04(18) ? C16 C4 C3 . . 124.21(17) ? C4 N5 O1 . . 109.98(17) ? O15 C7 C8 . . 129.7(2) ? O15 C7 C3 . . 123.61(19) ? C8 C7 C3 . . 106.63(17) ? C13 C8 C9 . . 121.1(2) ? C13 C8 C7 . . 110.56(18) ? C9 C8 C7 . . 128.3(2) ? C10 C9 C8 . . 118.0(2) ? C10 C9 H9 . . 121.0 ? C8 C9 H9 . . 121.0 ? C9 C10 C11 . . 120.8(2) ? C9 C10 H10 . . 119.6 ? C11 C10 H10 . . 119.6 ? C12 C11 C10 . . 121.6(2) ? C12 C11 H11 . . 119.2 ? C10 C11 H11 . . 119.2 ? C11 C12 C13 . . 118.3(2) ? C11 C12 H12 . . 120.8 ? C13 C12 H12 . . 120.8 ? C12 C13 C8 . . 120.2(2) ? C12 C13 C14 . . 127.6(2) ? C8 C13 C14 . . 112.23(17) ? C13 C14 C3 . . 104.65(16) ? C13 C14 H14A . . 110.8 ? C3 C14 H14A . . 110.8 ? C13 C14 H14B . . 110.8 ? C3 C14 H14B . . 110.8 ? H14A C14 H14B . . 108.9 ? C17 C16 C21 . . 119.1(2) ? C17 C16 C4 . . 121.19(19) ? C21 C16 C4 . . 119.67(18) ? C18 C17 C16 . . 120.5(2) ? C18 C17 H17 . . 119.8 ? C16 C17 H17 . . 119.8 ? C19 C18 C17 . . 118.84(19) ? C19 C18 H18 . . 120.6 ? C17 C18 H18 . . 120.6 ? C18 C19 C20 . . 122.28(19) ? C18 C19 N22 . . 118.92(19) ? C20 C19 N22 . . 118.8(2) ? C21 C20 C19 . . 118.7(2) ? C21 C20 H20 . . 120.6 ? C19 C20 H20 . . 120.6 ? C20 C21 C16 . . 120.54(19) ? C20 C21 H21 . . 119.7 ? C16 C21 H21 . . 119.7 ? O24 N22 O23 . . 124.6(2) ? O24 N22 C19 . . 117.9(2) ? O23 N22 C19 . . 117.55(19) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N5 O1 S2 O6 . . . . -83.98(17) ? N5 O1 S2 C3 . . . . 23.84(16) ? O6 S2 C3 C4 . . . . 88.02(15) ? O1 S2 C3 C4 . . . . -21.93(14) ? O6 S2 C3 C14 . . . . -40.44(18) ? O1 S2 C3 C14 . . . . -150.38(16) ? O6 S2 C3 C7 . . . . -154.72(14) ? O1 S2 C3 C7 . . . . 95.33(14) ? C14 C3 C4 N5 . . . . 140.2(2) ? C7 C3 C4 N5 . . . . -95.4(2) ? S2 C3 C4 N5 . . . . 17.7(2) ? C14 C3 C4 C16 . . . . -42.3(3) ? C7 C3 C4 C16 . . . . 82.1(2) ? S2 C3 C4 C16 . . . . -164.87(17) ? C16 C4 N5 O1 . . . . -179.77(17) ? C3 C4 N5 O1 . . . . -2.1(3) ? S2 O1 N5 C4 . . . . -17.6(2) ? C4 C3 C7 O15 . . . . 44.5(3) ? C14 C3 C7 O15 . . . . 176.6(2) ? S2 C3 C7 O15 . . . . -65.5(2) ? C4 C3 C7 C8 . . . . -137.79(17) ? C14 C3 C7 C8 . . . . -5.8(2) ? S2 C3 C7 C8 . . . . 112.15(15) ? O15 C7 C8 C13 . . . . -179.0(2) ? C3 C7 C8 C13 . . . . 3.6(2) ? O15 C7 C8 C9 . . . . 1.2(4) ? C3 C7 C8 C9 . . . . -176.27(19) ? C13 C8 C9 C10 . . . . -1.2(3) ? C7 C8 C9 C10 . . . . 178.6(2) ? C8 C9 C10 C11 . . . . 1.5(3) ? C9 C10 C11 C12 . . . . -0.8(3) ? C10 C11 C12 C13 . . . . 0.0(3) ? C11 C12 C13 C8 . . . . 0.3(3) ? C11 C12 C13 C14 . . . . -179.31(18) ? C9 C8 C13 C12 . . . . 0.4(3) ? C7 C8 C13 C12 . . . . -179.45(18) ? C9 C8 C13 C14 . . . . -179.97(17) ? C7 C8 C13 C14 . . . . 0.2(2) ? C12 C13 C14 C3 . . . . 175.72(19) ? C8 C13 C14 C3 . . . . -3.9(2) ? C4 C3 C14 C13 . . . . 133.13(18) ? C7 C3 C14 C13 . . . . 5.7(2) ? S2 C3 C14 C13 . . . . -109.06(15) ? N5 C4 C16 C17 . . . . 156.1(2) ? C3 C4 C16 C17 . . . . -21.4(3) ? N5 C4 C16 C21 . . . . -21.5(3) ? C3 C4 C16 C21 . . . . 161.0(2) ? C21 C16 C17 C18 . . . . -0.8(3) ? C4 C16 C17 C18 . . . . -178.36(19) ? C16 C17 C18 C19 . . . . 1.5(3) ? C17 C18 C19 C20 . . . . -0.8(3) ? C17 C18 C19 N22 . . . . 178.06(18) ? C18 C19 C20 C21 . . . . -0.8(3) ? N22 C19 C20 C21 . . . . -179.59(17) ? C19 C20 C21 C16 . . . . 1.5(3) ? C17 C16 C21 C20 . . . . -0.8(3) ? C4 C16 C21 C20 . . . . 176.84(18) ? C18 C19 N22 O24 . . . . 3.5(3) ? C20 C19 N22 O24 . . . . -177.6(2) ? C18 C19 N22 O23 . . . . -175.7(2) ? C20 C19 N22 O23 . . . . 3.1(3) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C14 H14A O6 . 0.97 2.46 2.992(3) 114.1 ? _shelx_res_file ; TITL ARM_UK_PMC_2829_a.res in P-1 CELL 0.71073 7.5520 8.2283 12.8010 74.726 86.674 72.819 ZERR 2.000 0.0011 0.0011 0.0018 0.004 0.005 0.004 LATT 1 SFAC C H N O S UNIT 32 20 4 10 2 OMIT 0 0 1 L.S. 5 ACTA BOND $H FMAP 2 PLAN 5 HTAB C14 O6 SIZE 0.184 0.385 0.498 HTAB DELU 0.002 S2 O6 CONF TEMP 27.000 WGHT 0.120700 FVAR 1.11270 O1 4 0.682641 0.949776 0.248950 11.00000 0.07163 0.06910 = 0.05920 -0.02452 0.01721 -0.04832 S2 5 0.724993 0.791474 0.184843 11.00000 0.05968 0.06962 = 0.04634 -0.02159 0.01275 -0.03619 C3 1 0.497408 0.756353 0.227537 11.00000 0.04651 0.04146 = 0.03624 -0.00959 0.00175 -0.01962 C4 1 0.459642 0.832009 0.323805 11.00000 0.04559 0.04140 = 0.03718 -0.01068 -0.00345 -0.01774 N5 3 0.552007 0.935075 0.334768 11.00000 0.06087 0.06079 = 0.04730 -0.02215 0.01077 -0.03563 O6 4 0.866919 0.637738 0.245254 11.00000 0.04505 0.08435 = 0.08579 -0.03146 -0.00264 -0.01559 C7 1 0.357594 0.867651 0.131173 11.00000 0.05571 0.03384 = 0.03581 -0.00693 -0.00085 -0.01542 C8 1 0.305610 0.742078 0.086140 11.00000 0.04080 0.04052 = 0.03310 -0.01007 0.00204 -0.01521 C9 1 0.191880 0.776716 -0.004494 11.00000 0.04195 0.05681 = 0.03936 -0.00932 -0.00163 -0.01532 AFIX 43 H9 2 0.135785 0.891580 -0.043989 11.00000 -1.20000 AFIX 0 C10 1 0.165729 0.635824 -0.033263 11.00000 0.04740 0.08162 = 0.04555 -0.02468 0.00373 -0.03349 AFIX 43 H10 2 0.093103 0.655285 -0.094099 11.00000 -1.20000 AFIX 0 C11 1 0.246185 0.465148 0.027214 11.00000 0.05691 0.06203 = 0.05546 -0.03089 0.01389 -0.03537 AFIX 43 H11 2 0.225095 0.372031 0.006653 11.00000 -1.20000 AFIX 0 C12 1 0.356845 0.429997 0.117209 11.00000 0.04682 0.04216 = 0.04948 -0.01748 0.01400 -0.02231 AFIX 43 H12 2 0.410113 0.314876 0.157260 11.00000 -1.20000 AFIX 0 C13 1 0.386668 0.570849 0.146468 11.00000 0.03584 0.03744 = 0.04044 -0.01302 0.00910 -0.01566 C14 1 0.502967 0.564113 0.240070 11.00000 0.04526 0.03723 = 0.04097 -0.00930 0.00289 -0.01476 AFIX 23 H14A 2 0.629143 0.491378 0.236447 11.00000 -1.20000 H14B 2 0.451401 0.517158 0.308586 11.00000 -1.20000 AFIX 0 O15 4 0.313190 1.025373 0.102130 11.00000 0.10655 0.03381 = 0.05955 -0.00743 -0.01605 -0.01445 C16 1 0.317282 0.801309 0.404959 11.00000 0.04421 0.03793 = 0.03857 -0.00936 -0.00122 -0.01534 C17 1 0.168141 0.748991 0.380555 11.00000 0.05027 0.05458 = 0.04041 -0.01680 0.00090 -0.02346 AFIX 43 H17 2 0.159074 0.730032 0.312838 11.00000 -1.20000 AFIX 0 C18 1 0.033764 0.725160 0.456403 11.00000 0.04209 0.04808 = 0.04980 -0.01199 -0.00128 -0.01853 AFIX 43 H18 2 -0.064078 0.687617 0.440906 11.00000 -1.20000 AFIX 0 C19 1 0.047382 0.757939 0.555077 11.00000 0.04430 0.03450 = 0.04157 -0.00507 0.00299 -0.00988 C20 1 0.192309 0.812081 0.581677 11.00000 0.05326 0.03876 = 0.03328 -0.00840 -0.00280 -0.01214 AFIX 43 H20 2 0.197597 0.834745 0.648690 11.00000 -1.20000 AFIX 0 C21 1 0.327824 0.831589 0.507212 11.00000 0.04472 0.04051 = 0.03902 -0.00965 -0.00379 -0.01633 AFIX 43 H21 2 0.427404 0.865103 0.524539 11.00000 -1.20000 AFIX 0 N22 3 -0.099028 0.738098 0.634779 11.00000 0.05117 0.04762 = 0.04810 -0.00462 0.00535 -0.01222 O23 4 -0.089332 0.778125 0.719253 11.00000 0.07905 0.08450 = 0.05080 -0.02125 0.01928 -0.02799 O24 4 -0.222314 0.684675 0.611435 11.00000 0.05517 0.08783 = 0.07421 -0.01926 0.01272 -0.03429 HKLF 4 REM ARM_UK_PMC_2829_a.res in P-1 REM R1 = 0.0510 for 2275 Fo > 4sig(Fo) and 0.0643 for all 2960 data REM 217 parameters refined using 1 restraints END WGHT 0.1222 0.0000 REM Instructions for potential hydrogen bonds HTAB C14 O6 REM Highest difference peak 0.358, deepest hole -0.405, 1-sigma level 0.077 Q1 1 -0.1953 0.7431 0.7850 11.00000 0.05 0.27 Q2 1 0.5393 0.4819 0.3038 11.00000 0.05 0.27 Q3 1 0.1753 0.8352 -0.0231 11.00000 0.05 0.26 Q4 1 0.2472 0.7554 0.0599 11.00000 0.05 0.25 Q5 1 0.6555 0.9081 0.1491 11.00000 0.05 0.23 ; _shelx_res_checksum 43903 _shelx_hkl_file ; 1 0 0 313.37 14.40 -2 0 0 2553.44 112.59 -2 0 0 2407.46 114.49 -2 0 0 2527.95 112.59 -2 0 0 2461.65 113.99 -2 0 0 2498.35 111.79 -2 0 0 2496.85 111.69 2 0 0 2454.75 111.69 2 0 0 2516.65 111.99 2 0 0 2475.95 112.49 2 0 0 2587.14 114.09 2 0 0 2403.96 114.59 2 0 0 2465.55 112.49 -3 0 0 7.70 2.70 -3 0 0 6.00 1.50 -3 0 0 4.50 0.90 -3 0 0 5.30 3.40 -3 0 0 4.20 0.90 -3 0 0 3.90 1.40 3 0 0 3.70 0.80 3 0 0 5.80 1.20 3 0 0 5.20 1.40 3 0 0 2.70 2.50 3 0 0 4.30 1.30 -4 0 0 11.10 1.30 -4 0 0 14.50 2.60 -4 0 0 10.90 3.70 -4 0 0 11.30 1.60 4 0 0 10.20 1.90 4 0 0 11.00 2.30 4 0 0 12.10 3.90 4 0 0 11.70 1.40 -5 0 0 345.17 18.50 -5 0 0 353.16 22.00 -5 0 0 339.87 16.00 -5 0 0 333.77 16.70 5 0 0 354.96 18.40 5 0 0 333.67 22.60 5 0 0 331.47 17.60 -6 0 0 85.29 10.30 -6 0 0 81.89 7.10 6 0 0 79.29 10.50 6 0 0 65.39 6.00 6 0 0 86.19 7.10 -7 0 0 5.70 3.10 -7 0 0 1.10 3.70 7 0 0 0.30 2.20 7 0 0 3.00 4.30 -8 0 0 3.10 3.00 -8 0 0 0.10 4.40 8 0 0 3.80 2.70 8 0 0 -0.50 4.30 -9 0 0 7.50 4.20 9 0 0 7.40 6.80 8 -1 0 47.40 11.20 8 -1 0 44.10 7.10 -8 1 0 47.10 6.50 -8 1 0 41.30 9.60 7 -1 0 215.98 19.00 7 -1 0 193.38 13.50 -7 1 0 198.88 17.80 -7 1 0 195.38 13.10 6 -1 0 92.39 11.30 6 -1 0 88.49 6.30 6 -1 0 86.99 7.60 -6 1 0 90.09 10.80 -6 1 0 85.19 7.20 5 -1 0 5.50 2.30 5 -1 0 5.30 3.40 5 -1 0 6.60 1.90 -5 1 0 3.30 3.20 -5 1 0 3.60 1.30 -5 1 0 4.40 2.00 4 -1 0 192.88 11.10 4 -1 0 183.28 14.00 4 -1 0 184.58 10.30 4 -1 0 184.48 10.30 -4 1 0 199.28 9.70 -4 1 0 187.78 13.50 -4 1 0 186.58 10.60 3 -1 0 212.18 11.10 3 -1 0 217.58 11.00 3 -1 0 190.98 13.70 3 -1 0 215.88 11.60 -3 1 0 215.58 11.20 -3 1 0 219.28 13.60 -3 1 0 227.38 10.80 -3 1 0 218.38 11.60 2 -1 0 6.70 2.30 2 -1 0 6.30 1.00 2 -1 0 5.20 1.20 2 -1 0 6.00 1.40 2 -1 0 4.90 1.80 -2 1 0 4.30 1.20 -2 1 0 5.20 1.90 -2 1 0 4.90 1.00 -2 1 0 4.20 2.00 -2 1 0 4.40 1.20 1 -1 0 619.34 30.30 1 -1 0 659.13 30.00 1 -1 0 620.04 29.10 1 -1 0 652.83 29.60 1 -1 0 626.14 28.80 1 -1 0 587.14 28.80 -1 1 0 645.84 30.50 -1 1 0 632.34 28.90 -1 1 0 668.63 29.50 -1 1 0 651.33 28.80 -1 1 0 664.53 30.00 -1 1 0 619.24 29.20 0 -1 0 32.50 3.90 -1 -1 0 346.17 16.90 -1 -1 0 365.06 17.80 1 1 0 351.56 16.80 1 1 0 354.76 16.60 1 1 0 357.06 17.20 -2 -1 0 670.33 31.50 -2 -1 0 679.23 31.00 -2 -1 0 647.14 33.10 -2 -1 0 685.83 32.70 -2 -1 0 666.63 31.00 -2 -1 0 678.53 31.60 2 1 0 659.13 30.90 2 1 0 637.74 31.40 2 1 0 709.33 32.70 2 1 0 670.33 31.60 2 1 0 660.83 30.90 2 1 0 692.43 33.40 -3 -1 0 1509.95 67.69 -3 -1 0 1481.95 68.59 -3 -1 0 1531.15 67.59 -3 -1 0 1583.94 68.59 -3 -1 0 1461.55 70.39 -3 -1 0 1374.46 70.89 3 1 0 1529.75 68.59 3 1 0 1507.45 67.49 3 1 0 1453.45 67.39 3 1 0 1451.15 71.29 3 1 0 1447.56 68.39 -4 -1 0 70.69 4.50 -4 -1 0 66.69 7.30 -4 -1 0 72.99 4.60 -4 -1 0 73.19 5.70 4 1 0 71.59 5.50 4 1 0 68.59 4.30 4 1 0 66.49 4.30 4 1 0 64.09 7.70 -5 -1 0 738.93 35.90 -5 -1 0 712.13 33.80 -5 -1 0 670.53 38.60 -5 -1 0 723.73 34.00 5 1 0 757.52 33.80 5 1 0 699.53 40.20 5 1 0 726.53 35.50 5 1 0 725.93 33.90 -6 -1 0 302.57 17.20 -6 -1 0 278.47 14.50 -6 -1 0 302.67 20.70 6 1 0 262.27 21.20 6 1 0 289.07 15.20 6 1 0 300.87 16.80 -7 -1 0 646.84 34.50 -7 -1 0 679.63 39.50 7 1 0 694.23 41.50 7 1 0 660.53 34.20 7 1 0 629.74 32.50 -8 -1 0 37.50 9.10 -8 -1 0 47.90 7.10 8 1 0 48.30 6.70 8 1 0 55.99 12.10 -9 -1 0 3.70 3.60 -9 -1 0 -2.20 4.30 9 1 0 -0.60 5.10 9 1 0 1.20 3.20 8 -2 0 75.59 10.00 -8 2 0 89.29 14.30 7 -2 0 11.10 6.00 7 -2 0 8.50 3.50 -7 2 0 13.50 6.20 -7 2 0 11.80 4.30 6 -2 0 9.10 5.00 6 -2 0 10.00 3.20 -6 2 0 7.70 2.50 -6 2 0 8.50 4.60 5 -2 0 167.08 14.30 5 -2 0 164.38 11.20 5 -2 0 163.48 9.30 -5 2 0 168.78 9.10 -5 2 0 176.08 14.00 -5 2 0 168.28 10.10 4 -2 0 9.50 1.80 4 -2 0 9.20 2.50 4 -2 0 5.50 3.20 4 -2 0 5.80 1.50 -4 2 0 7.70 1.90 -4 2 0 8.50 1.80 -4 2 0 9.50 3.60 3 -2 0 84.99 5.10 3 -2 0 86.09 6.30 3 -2 0 82.49 4.90 3 -2 0 83.89 7.80 -3 2 0 89.09 7.60 -3 2 0 85.99 5.10 -3 2 0 73.89 5.70 2 -2 0 9.70 1.50 2 -2 0 11.90 1.20 2 -2 0 10.90 2.30 -2 2 0 6.30 1.70 -2 2 0 9.50 2.80 -2 2 0 10.60 1.30 -2 2 0 7.40 2.20 -2 2 0 10.70 2.40 -2 2 0 12.10 2.10 -2 2 0 11.50 1.10 -2 2 0 5.80 1.50 1 -2 0 5302.97 240.68 1 -2 0 5245.88 240.88 1 -2 0 5063.69 241.58 -1 2 0 5321.37 240.58 -1 2 0 5533.15 242.38 -1 2 0 5319.77 241.38 -1 2 0 5289.47 240.88 -1 2 0 5351.26 241.48 -1 2 0 5575.34 245.48 -1 2 0 5604.54 240.38 0 -2 0 7068.09 322.47 0 -2 0 7059.49 322.57 0 -2 0 7457.25 322.17 0 -2 0 6349.56 324.47 0 2 0 7576.74 322.47 0 2 0 7271.27 322.17 0 2 0 7249.77 322.47 0 2 0 7421.56 324.37 -1 -2 0 1603.54 74.49 -1 -2 0 1703.43 74.79 -1 -2 0 1669.73 74.69 -1 -2 0 1619.34 75.59 -1 -2 0 1558.84 74.69 -1 -2 0 1594.44 74.79 1 2 0 1598.64 74.59 1 2 0 1642.84 76.69 1 2 0 1718.33 75.49 1 2 0 1690.03 74.79 1 2 0 1674.63 74.79 -2 -2 0 389.36 20.60 -2 -2 0 394.06 20.50 -2 -2 0 415.66 20.30 -2 -2 0 425.56 19.90 -2 -2 0 404.16 22.10 -2 -2 0 409.76 20.90 2 2 0 402.26 19.90 2 2 0 421.56 19.80 2 2 0 406.96 19.90 2 2 0 395.46 20.30 2 2 0 426.26 21.90 2 2 0 424.96 20.30 -3 -2 0 297.27 17.00 -3 -2 0 285.47 16.00 -3 -2 0 295.77 17.30 -3 -2 0 325.07 15.50 -3 -2 0 295.17 18.20 -3 -2 0 296.97 15.30 3 2 0 318.87 16.00 3 2 0 330.37 18.70 3 2 0 302.97 15.30 3 2 0 310.07 15.20 -4 -2 0 490.45 24.80 -4 -2 0 474.45 23.50 -4 -2 0 499.85 23.60 -4 -2 0 474.45 26.70 4 2 0 472.75 23.20 4 2 0 452.75 24.20 4 2 0 498.85 28.10 4 2 0 492.85 23.30 -5 -2 0 1.90 2.50 -5 -2 0 0.90 1.40 -5 -2 0 -1.40 1.60 5 2 0 1.10 1.10 5 2 0 -0.40 1.30 5 2 0 1.90 2.90 -6 -2 0 43.20 4.30 -6 -2 0 59.09 6.40 -6 -2 0 56.39 8.80 6 2 0 49.00 4.20 6 2 0 54.89 9.80 6 2 0 58.09 6.60 -7 -2 0 -1.50 1.40 -7 -2 0 -1.20 2.20 -7 -2 0 2.20 4.10 7 2 0 -2.00 2.00 7 2 0 -1.10 3.80 7 2 0 0.60 1.70 -8 -2 0 13.00 4.20 -8 -2 0 13.00 6.30 8 2 0 16.40 4.10 8 2 0 16.70 7.90 -9 -2 0 21.50 5.80 -9 -2 0 23.40 8.50 9 2 0 31.60 10.40 9 2 0 21.90 5.30 7 -3 0 129.39 12.40 -7 3 0 155.58 21.90 -7 3 0 154.68 15.40 6 -3 0 0.40 2.40 -6 3 0 4.80 4.10 -6 3 0 2.90 6.30 5 -3 0 -0.40 1.40 5 -3 0 -0.60 2.10 -5 3 0 0.30 1.30 -5 3 0 0.90 4.40 -5 3 0 1.30 3.00 4 -3 0 32.80 3.40 4 -3 0 24.70 4.20 -4 3 0 28.40 2.90 -4 3 0 25.90 7.90 -4 3 0 22.30 4.90 3 -3 0 69.09 4.90 3 -3 0 68.19 6.10 -3 3 0 82.09 10.50 -3 3 0 73.79 4.30 -3 3 0 53.29 5.00 -3 3 0 65.39 6.70 -3 3 0 66.79 3.70 -3 3 0 56.59 5.50 2 -3 0 2.20 1.00 2 -3 0 0.00 1.40 2 -3 0 2.70 1.30 -2 3 0 1.20 1.20 -2 3 0 2.00 0.90 -2 3 0 1.40 1.40 -2 3 0 2.30 0.80 -2 3 0 1.60 3.10 -2 3 0 0.70 0.60 -2 3 0 2.50 1.70 1 -3 0 1345.17 63.29 1 -3 0 1386.46 63.59 -1 3 0 1377.06 63.49 -1 3 0 1403.96 63.19 -1 3 0 1389.96 62.59 -1 3 0 1390.86 64.39 -1 3 0 1414.66 63.39 -1 3 0 1257.77 67.19 -1 3 0 1371.06 63.49 -1 3 0 1470.25 65.29 0 -3 0 475.25 22.90 0 -3 0 503.95 22.50 0 -3 0 465.65 23.10 0 3 0 467.45 22.80 0 3 0 469.95 25.10 0 3 0 481.45 22.90 0 3 0 469.35 22.40 -1 -3 0 17.40 3.40 -1 -3 0 33.70 3.10 -1 -3 0 31.50 2.30 -1 -3 0 30.40 2.90 -1 -3 0 32.60 2.40 1 3 0 29.50 5.50 1 3 0 28.50 2.90 1 3 0 24.70 3.50 1 3 0 32.90 3.00 1 3 0 30.10 2.90 -2 -3 0 258.77 13.30 -2 -3 0 258.47 13.10 -2 -3 0 205.68 16.10 -2 -3 0 248.08 13.40 -2 -3 0 226.68 13.00 -2 -3 0 246.78 14.00 2 3 0 236.38 13.10 2 3 0 254.17 13.70 2 3 0 266.17 15.10 2 3 0 248.18 13.10 2 3 0 256.87 13.40 2 3 0 241.28 12.90 -3 -3 0 46.40 4.20 -3 -3 0 50.59 5.10 -3 -3 0 49.60 4.70 -3 -3 0 45.50 6.60 -3 -3 0 46.40 5.20 3 3 0 47.00 4.40 3 3 0 48.50 6.10 3 3 0 46.80 4.20 -4 -3 0 114.69 8.30 -4 -3 0 105.89 7.30 -4 -3 0 113.09 9.50 4 3 0 112.69 10.40 4 3 0 109.69 7.20 4 3 0 118.19 8.00 -5 -3 0 133.79 8.30 -5 -3 0 123.39 9.30 -5 -3 0 119.19 11.00 5 3 0 139.59 9.40 5 3 0 114.59 7.80 5 3 0 136.29 12.70 -6 -3 0 2.10 2.70 -6 -3 0 -1.80 1.30 -6 -3 0 0.30 2.60 6 3 0 0.10 1.60 6 3 0 -0.20 1.20 6 3 0 -2.80 3.10 -7 -3 0 317.97 20.10 -7 -3 0 327.77 17.70 -7 -3 0 313.47 23.20 7 3 0 358.76 26.10 7 3 0 319.47 17.30 7 3 0 328.37 19.60 -8 -3 0 -1.60 2.40 -8 -3 0 2.50 2.00 -8 -3 0 1.80 4.20 8 3 0 2.20 4.70 8 3 0 0.60 2.30 8 3 0 1.00 2.60 -9 -3 0 3.50 5.00 -9 -3 0 2.10 3.70 9 3 0 6.20 3.80 9 3 0 -0.20 5.50 7 -4 0 4.30 4.40 -7 4 0 6.30 4.80 -7 4 0 13.40 10.60 6 -4 0 -2.90 3.10 -6 4 0 -1.40 3.20 -6 4 0 0.80 6.50 5 -4 0 92.79 6.60 5 -4 0 91.49 8.80 -5 4 0 69.49 9.20 -5 4 0 82.99 16.70 4 -4 0 6.30 2.10 4 -4 0 7.70 3.20 -4 4 0 7.70 1.50 -4 4 0 3.80 6.10 -4 4 0 7.80 3.60 3 -4 0 124.49 6.70 3 -4 0 128.89 7.90 3 -4 0 118.99 9.10 -3 4 0 116.79 6.20 -3 4 0 130.39 15.60 -3 4 0 113.39 6.40 -3 4 0 115.49 6.20 -3 4 0 122.49 9.30 2 -4 0 131.89 7.90 2 -4 0 147.19 9.70 2 -4 0 155.78 8.90 -2 4 0 137.39 9.00 -2 4 0 137.19 7.00 -2 4 0 140.69 6.90 -2 4 0 152.78 9.10 -2 4 0 139.79 7.80 1 -4 0 676.63 32.50 1 -4 0 658.83 32.00 -1 4 0 645.14 31.00 -1 4 0 680.63 36.90 -1 4 0 662.43 31.50 -1 4 0 637.94 31.70 -1 4 0 720.03 34.20 -1 4 0 699.43 31.70 0 -4 0 1170.18 67.09 0 -4 0 1353.36 62.59 0 -4 0 1362.06 62.39 0 -4 0 1438.56 61.79 0 4 0 1408.26 65.39 0 4 0 1331.17 61.49 -1 -4 0 90.29 6.20 -1 -4 0 83.49 6.00 -1 -4 0 87.59 5.70 1 4 0 88.29 7.30 1 4 0 83.79 5.60 1 4 0 65.09 8.80 -2 -4 0 84.89 6.10 -2 -4 0 76.49 5.50 -2 -4 0 78.09 6.00 -2 -4 0 88.89 5.80 2 4 0 81.19 8.00 2 4 0 78.69 6.70 2 4 0 79.39 6.20 -3 -4 0 0.30 1.60 -3 -4 0 0.40 1.60 -3 -4 0 0.50 1.70 -3 -4 0 -0.30 1.40 3 4 0 0.90 2.00 3 4 0 -1.60 1.20 3 4 0 -0.30 1.30 -4 -4 0 1133.39 55.79 -4 -4 0 1115.19 56.79 -4 -4 0 1200.28 55.09 4 4 0 1127.19 54.89 4 4 0 1174.18 58.99 4 4 0 1212.08 55.99 -5 -4 0 39.80 6.00 -5 -4 0 34.40 6.30 -5 -4 0 48.20 5.40 5 4 0 34.30 4.40 5 4 0 34.70 4.80 5 4 0 33.90 7.20 -6 -4 0 49.50 8.60 -6 -4 0 53.19 7.40 -6 -4 0 55.39 6.10 6 4 0 50.29 5.00 6 4 0 42.20 5.90 6 4 0 57.69 10.30 -7 -4 0 109.39 8.70 -7 -4 0 129.29 11.00 -7 -4 0 123.89 13.10 7 4 0 118.39 8.30 7 4 0 128.79 10.40 7 4 0 119.89 14.50 -8 -4 0 38.10 5.40 -8 -4 0 45.30 9.70 -8 -4 0 44.30 7.70 8 4 0 36.60 4.80 8 4 0 33.00 9.60 8 4 0 30.20 5.80 -9 -4 0 1.20 4.00 -9 -4 0 -1.20 4.20 9 4 0 -2.20 5.10 9 4 0 -1.90 3.10 6 -5 0 3.00 3.80 -6 5 0 2.10 7.50 5 -5 0 10.90 4.60 -5 5 0 2.00 6.70 -5 5 0 11.20 4.90 4 -5 0 12.40 3.00 4 -5 0 9.00 3.60 -4 5 0 5.90 7.00 -4 5 0 7.90 3.70 3 -5 0 2.10 1.40 3 -5 0 1.60 1.70 -3 5 0 0.70 2.20 -3 5 0 1.60 5.20 2 -5 0 447.36 22.50 2 -5 0 464.65 23.40 -2 5 0 459.55 29.60 -2 5 0 443.96 23.10 -2 5 0 452.55 23.00 1 -5 0 23.10 3.20 1 -5 0 22.80 3.80 1 -5 0 19.10 2.90 -1 5 0 24.70 2.30 -1 5 0 36.30 7.20 -1 5 0 7.30 5.40 0 -5 0 717.23 35.20 0 -5 0 692.23 40.30 0 -5 0 699.03 34.80 0 -5 0 761.52 34.10 0 5 0 741.03 38.20 0 5 0 690.33 33.70 -1 -5 0 515.75 25.50 -1 -5 0 496.65 25.60 -1 -5 0 514.05 24.90 1 5 0 524.15 27.60 1 5 0 470.15 24.60 -2 -5 0 7.10 1.70 -2 -5 0 7.10 2.30 -2 -5 0 3.90 4.00 -2 -5 0 6.60 2.10 -2 -5 0 5.00 1.60 2 5 0 4.40 3.40 2 5 0 6.10 2.90 -3 -5 0 29.00 4.10 -3 -5 0 26.00 4.10 -3 -5 0 33.40 4.70 -3 -5 0 29.20 4.30 3 5 0 30.80 4.90 3 5 0 26.50 4.30 3 5 0 32.30 6.20 -4 -5 0 49.40 5.70 -4 -5 0 51.09 6.10 -4 -5 0 53.39 6.00 4 5 0 47.80 7.40 4 5 0 48.00 5.60 4 5 0 53.49 6.50 -5 -5 0 139.59 10.80 -5 -5 0 147.69 11.90 -5 -5 0 151.28 10.20 5 5 0 146.19 10.70 5 5 0 134.29 13.10 5 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8 0 114.29 15.40 1 8 0 148.39 12.00 1 8 0 152.58 13.70 -2 -8 0 4.20 2.50 -2 -8 0 1.80 2.70 2 8 0 2.80 2.90 2 8 0 3.50 3.70 2 8 0 5.20 4.90 -3 -8 0 18.40 4.60 -3 -8 0 17.60 4.30 3 8 0 14.90 4.50 3 8 0 12.90 4.80 3 8 0 16.70 6.00 -4 -8 0 4.50 3.50 -4 -8 0 7.40 3.50 4 8 0 10.70 4.00 4 8 0 9.70 4.80 4 8 0 8.80 4.30 -5 -8 0 67.79 8.80 -5 -8 0 51.49 7.40 5 8 0 53.39 8.30 5 8 0 59.49 10.30 5 8 0 62.19 8.10 -6 -8 0 0.10 2.80 -6 -8 0 3.00 3.40 6 8 0 2.90 3.40 6 8 0 3.20 4.90 6 8 0 1.00 3.50 -7 -8 0 14.10 5.40 -7 -8 0 15.20 5.30 7 8 0 9.90 6.20 7 8 0 15.70 5.50 7 8 0 8.60 4.00 -1 9 0 -1.30 4.90 -1 9 0 2.90 4.10 0 -9 0 4.60 3.30 0 9 0 5.00 4.90 0 9 0 4.00 4.40 -1 -9 0 4.20 3.00 1 9 0 5.60 4.80 1 9 0 -0.70 3.20 -2 -9 0 4.60 3.20 2 9 0 2.00 3.70 2 9 0 4.90 4.30 -3 -9 0 -0.50 2.40 -3 -9 0 2.90 3.70 3 9 0 3.10 3.60 3 9 0 -1.80 3.40 -4 -9 0 3.70 3.20 -4 -9 0 5.30 3.70 4 9 0 3.10 3.80 4 9 0 9.30 5.00 -5 -9 0 4.10 3.50 -5 -9 0 -0.40 3.40 5 9 0 0.70 3.70 5 9 0 1.40 3.70 -6 -9 0 7.00 4.30 6 9 0 10.50 4.50 6 9 0 1.90 4.20 5 9 -1 68.89 10.20 5 9 -1 78.19 10.40 -5 -9 1 69.29 9.60 -5 -9 1 70.49 9.80 4 9 -1 19.80 6.00 4 9 -1 -0.10 3.40 -4 -9 1 7.30 4.20 -4 -9 1 5.60 3.50 3 9 -1 23.60 6.10 3 9 -1 17.50 6.30 -3 -9 1 17.60 5.10 2 9 -1 24.80 6.20 2 9 -1 11.50 5.50 -2 -9 1 20.60 5.30 1 9 -1 -0.30 4.00 1 9 -1 3.50 3.80 -1 -9 1 1.80 3.00 0 9 -1 33.80 9.00 0 -9 1 31.10 5.90 7 8 -1 -0.90 3.00 7 8 -1 -5.20 2.80 7 8 -1 -0.60 4.80 -7 -8 1 -0.30 3.40 -7 -8 1 0.00 3.10 6 8 -1 24.80 6.60 6 8 -1 9.10 4.20 6 8 -1 20.50 7.70 -6 -8 1 20.00 5.80 -6 -8 1 25.20 6.10 5 8 -1 -2.90 2.40 5 8 -1 -1.20 3.00 5 8 -1 3.10 4.40 -5 -8 1 2.20 2.80 -5 -8 1 0.30 2.80 4 8 -1 64.69 10.80 4 8 -1 46.90 7.60 4 8 -1 64.39 9.60 -4 -8 1 48.40 7.30 -4 -8 1 54.09 7.80 3 8 -1 9.70 4.30 3 8 -1 16.20 6.30 3 8 -1 18.30 5.00 -3 -8 1 13.60 4.20 2 8 -1 87.09 11.50 2 8 -1 87.69 12.90 2 8 -1 77.79 9.40 -2 -8 1 79.79 7.30 -2 -8 1 94.59 8.80 1 8 -1 0.80 6.40 1 8 -1 1.80 4.20 -1 -8 1 5.60 3.40 -1 -8 1 2.90 2.70 0 8 -1 8.70 8.40 0 8 -1 8.30 5.50 0 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4 8.10 6.00 -8 -4 4 3.50 2.80 7 4 -4 337.17 20.20 7 4 -4 326.77 17.70 7 4 -4 301.87 26.30 -7 -4 4 291.07 20.20 -7 -4 4 299.77 18.30 -7 -4 4 326.57 23.60 6 4 -4 16.40 3.50 6 4 -4 12.50 3.90 6 4 -4 20.20 7.80 -6 -4 4 18.90 6.10 -6 -4 4 15.60 4.60 -6 -4 4 18.20 4.00 5 4 -4 610.14 32.20 5 4 -4 640.44 33.80 5 4 -4 684.63 40.40 -5 -4 4 651.13 32.50 -5 -4 4 598.14 35.40 -5 -4 4 637.14 33.70 4 4 -4 0.00 2.30 4 4 -4 -0.40 3.40 4 4 -4 -0.90 2.20 -4 -4 4 -0.70 2.00 -4 -4 4 3.70 2.30 -4 -4 4 -0.70 1.70 3 4 -4 25.30 5.20 3 4 -4 22.20 4.50 3 4 -4 30.30 8.80 -3 -4 4 17.90 3.40 -3 -4 4 21.80 3.70 -3 -4 4 22.40 4.00 2 4 -4 668.83 34.80 2 4 -4 637.24 32.30 2 4 -4 584.44 41.50 -2 -4 4 626.14 31.30 -2 -4 4 636.34 31.40 -2 -4 4 626.34 31.40 1 4 -4 488.85 25.00 1 4 -4 433.36 22.20 -1 -4 4 449.16 23.60 -1 -4 4 467.55 23.60 -1 -4 4 454.65 22.90 0 4 -4 209.48 17.40 0 -4 4 213.38 12.30 0 -4 4 207.48 11.10 0 -4 4 222.28 13.50 0 -4 4 200.78 12.50 -1 4 -4 271.67 22.20 1 -4 4 282.07 15.00 1 -4 4 259.97 15.70 1 -4 4 275.97 15.60 -2 4 -4 52.49 8.40 -2 4 -4 27.60 11.20 -3 4 -4 1.20 5.90 -3 4 -4 -0.50 3.40 3 -4 4 3.90 1.70 3 -4 4 2.50 3.10 3 -4 4 7.10 2.80 -4 4 -4 1.80 7.20 -4 4 -4 4.00 4.30 4 -4 4 0.80 2.20 4 -4 4 1.90 3.20 -5 4 -4 12.60 5.90 -5 4 -4 3.50 9.30 5 -4 4 3.60 2.80 5 -4 4 0.40 3.20 -6 4 -4 1.50 5.50 -6 4 -4 2.90 10.00 6 -4 4 2.50 4.70 8 3 -4 5.30 3.30 8 3 -4 7.40 6.80 -8 -3 4 10.10 3.20 -8 -3 4 3.90 3.70 -8 -3 4 1.40 4.60 7 3 -4 7.60 3.40 7 3 -4 6.30 5.50 -7 -3 4 14.30 5.80 -7 -3 4 9.00 3.80 -7 -3 4 11.10 3.30 6 3 -4 129.89 15.00 6 3 -4 118.29 9.60 6 3 -4 130.69 8.30 -6 -3 4 107.79 9.90 -6 -3 4 107.49 11.80 -6 -3 4 125.79 8.80 5 3 -4 43.70 5.90 5 3 -4 55.49 10.10 5 3 -4 41.00 5.00 -5 -3 4 49.70 6.60 -5 -3 4 45.90 5.30 4 3 -4 268.17 20.70 4 3 -4 265.27 17.60 4 3 -4 272.47 16.20 -4 -3 4 252.37 14.50 -4 -3 4 290.57 15.20 -4 -3 4 258.27 15.90 3 3 -4 85.89 8.10 3 3 -4 77.59 7.60 3 3 -4 95.69 11.50 -3 -3 4 91.29 7.10 -3 -3 4 87.19 6.30 -3 -3 4 91.09 6.70 2 3 -4 70.39 7.10 2 3 -4 68.29 6.70 2 3 -4 68.59 12.40 -2 -3 4 74.99 5.60 -2 -3 4 65.49 5.50 -2 -3 4 65.09 5.50 1 3 -4 346.37 17.50 1 3 -4 372.66 21.00 1 3 -4 320.57 21.30 -1 -3 4 381.06 18.60 -1 -3 4 329.77 18.20 -1 -3 4 371.56 18.10 0 3 -4 88.49 11.20 0 -3 4 75.69 8.00 0 -3 4 86.29 6.20 0 -3 4 86.99 6.00 0 -3 4 81.79 5.20 1 -3 4 404.86 21.60 1 -3 4 371.96 18.40 1 -3 4 381.66 18.60 1 -3 4 394.06 20.60 1 -3 4 434.16 20.10 -2 3 -4 45.40 8.10 2 -3 4 66.29 5.80 2 -3 4 55.49 6.70 2 -3 4 62.49 4.70 -3 3 -4 2.50 1.60 -3 3 -4 6.60 6.20 -3 3 -4 2.00 3.20 3 -3 4 0.80 1.20 3 -3 4 4.30 2.30 3 -3 4 0.30 2.00 -4 3 -4 179.68 15.60 4 -3 4 179.08 13.90 4 -3 4 205.98 12.50 4 -3 4 196.38 10.40 -5 3 -4 116.99 22.90 -5 3 -4 142.99 14.40 5 -3 4 169.08 11.10 5 -3 4 152.58 12.70 -6 3 -4 16.80 6.60 -6 3 -4 21.20 12.60 6 -3 4 19.40 5.40 6 -3 4 17.80 4.20 -7 3 -4 -0.70 9.40 -7 3 -4 2.90 5.20 7 -3 4 1.80 4.00 8 2 -4 3.50 5.30 8 2 -4 -1.60 2.70 -8 -2 4 0.60 3.10 -8 -2 4 0.30 4.10 7 2 -4 5.30 2.70 7 2 -4 4.30 4.80 -7 -2 4 4.40 3.20 -7 -2 4 5.00 2.40 -7 -2 4 4.70 4.30 6 2 -4 0.10 1.20 6 2 -4 -0.80 3.70 6 2 -4 -0.60 1.70 -6 -2 4 -0.50 2.90 -6 -2 4 -0.30 2.10 -6 -2 4 -0.90 1.50 5 2 -4 390.76 20.10 5 2 -4 394.46 21.70 5 2 -4 409.76 27.70 -5 -2 4 417.86 22.70 -5 -2 4 403.86 20.80 4 2 -4 1.10 2.50 4 2 -4 2.10 3.00 4 2 -4 0.60 1.50 -4 -2 4 2.20 1.50 -4 -2 4 0.10 1.70 3 2 -4 153.68 11.30 3 2 -4 137.39 9.80 3 2 -4 152.68 13.90 -3 -2 4 153.78 9.20 -3 -2 4 154.18 9.80 -3 -2 4 157.88 8.90 2 2 -4 1252.77 67.79 2 2 -4 1352.76 61.99 2 2 -4 1300.77 61.29 -2 -2 4 1282.27 59.09 -2 -2 4 1251.37 59.39 -2 -2 4 1226.78 59.59 1 2 -4 249.18 16.90 1 2 -4 269.97 13.50 1 2 -4 265.27 16.60 -1 -2 4 278.47 13.90 -1 -2 4 266.47 14.00 0 2 -4 -0.90 4.60 0 2 -4 16.20 5.50 0 -2 4 16.80 2.40 0 -2 4 9.80 3.70 0 -2 4 13.30 1.80 0 -2 4 15.80 2.70 -1 2 -4 711.23 38.80 1 -2 4 793.92 40.10 1 -2 4 880.61 41.40 1 -2 4 833.02 38.10 1 -2 4 815.92 37.60 1 -2 4 873.91 38.70 1 -2 4 837.52 39.50 -2 2 -4 616.14 36.20 -2 2 -4 594.44 32.10 2 -2 4 732.23 31.80 2 -2 4 688.83 30.80 2 -2 4 718.33 33.50 2 -2 4 672.63 34.10 -3 2 -4 16.70 2.20 -3 2 -4 19.30 2.50 -3 2 -4 10.90 6.60 -3 2 -4 16.00 4.70 3 -2 4 15.70 3.50 3 -2 4 19.60 3.60 3 -2 4 13.70 1.70 3 -2 4 20.10 2.30 -4 2 -4 68.59 3.90 -4 2 -4 58.39 8.90 -4 2 -4 66.19 15.30 -4 2 -4 65.19 4.40 4 -2 4 71.19 4.20 4 -2 4 76.99 6.80 4 -2 4 66.69 7.00 -5 2 -4 4.20 1.70 -5 2 -4 6.90 4.30 -5 2 -4 5.20 7.40 5 -2 4 8.70 3.10 5 -2 4 8.10 3.40 -6 2 -4 9.80 9.60 -6 2 -4 10.60 5.60 6 -2 4 9.00 3.20 6 -2 4 5.30 3.50 -7 2 -4 6.20 9.50 -7 2 -4 6.30 5.60 7 -2 4 7.00 4.70 8 1 -4 5.30 2.90 8 1 -4 11.30 7.50 -8 -1 4 3.70 3.00 -8 -1 4 9.00 5.90 7 1 -4 5.40 5.30 7 1 -4 4.80 2.50 -7 -1 4 3.50 3.10 -7 -1 4 4.80 4.10 -7 -1 4 2.50 1.80 6 1 -4 2.70 1.20 6 1 -4 1.80 3.60 6 1 -4 2.70 1.80 -6 -1 4 1.10 3.20 -6 -1 4 4.90 3.40 -6 -1 4 1.30 1.60 5 1 -4 4.60 1.20 5 1 -4 3.50 1.70 5 1 -4 4.00 3.80 5 1 -4 2.90 1.20 -5 -1 4 6.90 1.90 -5 -1 4 4.30 2.50 4 1 -4 51.49 4.40 4 1 -4 34.70 3.10 4 1 -4 35.70 6.10 4 1 -4 33.80 3.00 4 1 -4 38.50 7.40 -4 -1 4 43.60 4.80 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24.00 7.10 -2 -2 -15 10.20 5.90 -2 -2 -15 11.00 11.60 -2 -2 -15 1.80 8.90 2 2 15 22.70 6.50 2 2 15 8.80 5.50 -3 -2 -15 10.40 9.90 -3 -2 -15 12.20 7.20 -3 -2 -15 9.30 12.20 3 2 15 23.40 5.90 3 2 15 28.00 7.50 3 2 15 21.20 6.20 2 -3 -15 2.10 7.50 -2 3 15 -1.10 2.30 -2 3 15 -0.50 4.20 1 -3 -15 -1.80 6.00 1 -3 -15 1.80 9.00 -1 3 15 2.70 4.60 -1 3 15 -0.60 3.50 -1 3 15 1.50 2.90 0 -3 -15 -4.30 6.40 0 -3 -15 -1.00 8.30 0 3 15 2.50 4.00 0 3 15 4.30 4.20 -1 -3 -15 6.70 6.50 -1 -3 -15 -2.50 8.20 -1 -3 -15 17.00 11.10 1 3 15 14.10 5.40 1 3 15 14.60 6.40 -2 -3 -15 6.20 9.30 -2 -3 -15 9.50 10.30 -2 -3 -15 3.90 6.20 2 3 15 7.30 4.60 2 3 15 22.20 7.50 -3 -3 -15 7.20 9.20 -3 -3 -15 10.80 7.40 -3 -3 -15 3.00 8.70 3 3 15 12.50 6.90 3 3 15 18.70 7.10 3 3 15 11.90 5.70 1 -4 -15 63.49 17.20 -1 4 15 60.69 8.90 -1 4 15 58.59 10.00 0 -4 -15 -1.50 5.40 0 -4 -15 3.50 9.70 0 4 15 11.10 5.60 0 4 15 9.40 5.00 -1 -4 -15 5.60 6.80 -1 -4 -15 0.50 8.40 1 4 15 5.20 4.60 1 4 15 10.70 5.80 -2 -4 -15 1.70 5.70 -2 -4 -15 0.00 7.90 2 4 15 1.40 4.80 2 4 15 5.40 4.70 -3 -4 -15 4.70 8.50 -3 -4 -15 0.20 5.80 3 4 15 9.50 6.10 3 4 15 12.10 5.60 0 -5 -15 6.90 6.40 0 -5 -15 -1.10 8.40 0 5 15 1.90 4.50 0 5 15 -0.10 4.30 -1 -5 -15 0.70 8.80 -1 -5 -15 4.70 7.60 1 5 15 18.60 6.00 1 5 15 12.20 5.80 -2 -5 -15 10.40 8.10 -2 -5 -15 6.20 8.90 2 5 15 10.00 5.80 2 5 15 14.10 5.70 -3 -5 -15 3.80 6.50 -3 -5 -15 -1.70 8.00 3 5 15 0.70 3.80 3 5 15 10.30 5.20 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 5232 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_I_CCDC1 _database_code_depnum_ccdc_archive 'CCDC 1875541' _audit_update_record ; 2018-10-26 deposited with the CCDC. 2018-12-12 downloaded from the CCDC. ; _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C20 H19 N O3 S' _chemical_formula_sum 'C20 H19 N O3 S' _chemical_formula_iupac ? _chemical_formula_weight 353.42 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.0131(2) _cell_length_b 11.9246(2) _cell_length_c 14.5681(3) _cell_angle_alpha 90 _cell_angle_beta 107.1060(10) _cell_angle_gamma 90 _cell_volume 1828.55(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9859 _cell_measurement_theta_min 3.1740 _cell_measurement_theta_max 66.8361 _cell_measurement_temperature 296.(2) _exptl_crystal_description block _exptl_crystal_colour 'clear colourless' _exptl_crystal_size_max 0.421 _exptl_crystal_size_mid 0.315 _exptl_crystal_size_min 0.196 _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 1.721 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/4 (Bruker AXS Inc.)' _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.75 _exptl_special_details ; ; _diffrn_ambient_temperature 296.(2) _diffrn_source 'Incoatec Microfocus X-ray Source I\mS' _diffrn_source_type Microfocus _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_monochromator 'Incoatec Montel Multilayer Mirror' _diffrn_measurement_device_type 'Bruker ACS Kappa APEX II DUO diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 22017 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_unetI/netI 0.0144 _diffrn_reflns_theta_min 4.88 _diffrn_reflns_theta_max 67.22 _diffrn_reflns_theta_full 67.22 _diffrn_measured_fraction_theta_max 0.964 _diffrn_measured_fraction_theta_full 0.964 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _refine_special_details ; ; _reflns_number_total 3172 _reflns_number_gt 3041 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_gt 0.1588 _refine_ls_wR_factor_ref 0.1600 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.215 _refine_ls_number_reflns 3172 _refine_ls_number_parameters 255 _refine_ls_number_restraints 72 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+0.8268P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.413 _refine_diff_density_min -0.430 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker Instrument Service v2013.12.0.0' _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.41964(19) 0.78572(18) 0.49732(12) 0.0785(6) Uani d . . . 1.0 . . N N5 0.3296(2) 0.71608(19) 0.52498(14) 0.0690(6) Uani d . . . 1.0 . . C C3 0.3449(2) 0.72514(18) 0.61523(15) 0.0522(5) Uani d . . . 1.0 . . C C4 0.4502(2) 0.79876(18) 0.67220(15) 0.0495(5) Uani d . . . 1.0 . . S S2 0.49018(6) 0.88032(5) 0.57660(5) 0.0661(3) Uani d . . . 1.0 . . C C6 0.2635(2) 0.65840(18) 0.65886(15) 0.0511(5) Uani d . . . 1.0 . . C C7 0.1457(2) 0.6202(2) 0.60385(18) 0.0617(6) Uani d . . . 1.0 . . H H7 0.1159 0.6399 0.5393 0.074 Uiso calc U . R 1.0 . . C C8 0.0722(2) 0.5535(2) 0.6434(2) 0.0671(6) Uani d . . . 1.0 . . H H8 -0.006 0.5284 0.6046 0.08 Uiso calc U . R 1.0 . . C C9 0.1116(2) 0.52245(19) 0.73982(18) 0.0600(6) Uani d . . D 1.0 . . C C10 0.2296(2) 0.5622(2) 0.79431(18) 0.0632(6) Uani d . . . 1.0 . . H H10 0.2591 0.5434 0.859 0.076 Uiso calc U . R 1.0 . . C C11 0.3036(2) 0.6285(2) 0.75510(16) 0.0578(6) Uani d . . . 1.0 . . H H11 0.3819 0.6536 0.7937 0.069 Uiso calc U . R 1.0 . . C C12 0.0296(2) 0.4492(2) 0.78306(19) 0.0760(8) Uani d . . D 1.0 . . C C13A 0.0631(7) 0.4698(8) 0.8922(2) 0.124(3) Uani d U P D 0.531(7) A 1 H H13A 0.0109 0.4231 0.9188 0.186 Uiso calc U P R 0.531(7) A 1 H H13B 0.1509 0.452 0.922 0.186 Uiso calc U P R 0.531(7) A 1 H H13C 0.0484 0.5471 0.9039 0.186 Uiso calc U P R 0.531(7) A 1 C C14A 0.0633(8) 0.3252(2) 0.7740(7) 0.118(3) Uani d U P D 0.531(7) A 1 H H14A 0.0117 0.2786 0.8012 0.177 Uiso calc U P R 0.531(7) A 1 H H14B 0.0479 0.3066 0.7074 0.177 Uiso calc U P R 0.531(7) A 1 H H14C 0.1513 0.3131 0.8076 0.177 Uiso calc U P R 0.531(7) A 1 C C15A -0.1116(2) 0.4740(9) 0.7363(7) 0.139(4) Uani d U P D 0.531(7) A 1 H H15A -0.1617 0.4269 0.7646 0.209 Uiso calc U P R 0.531(7) A 1 H H15B -0.1285 0.5513 0.7465 0.209 Uiso calc U P R 0.531(7) A 1 H H15C -0.1332 0.4593 0.6686 0.209 Uiso calc U P R 0.531(7) A 1 C C13B 0.1107(6) 0.3780(9) 0.8661(7) 0.144(4) Uani d U P D 0.469(7) A 2 H H13D 0.0563 0.3328 0.8918 0.216 Uiso calc U P R 0.469(7) A 2 H H13E 0.1657 0.3303 0.8431 0.216 Uiso calc U P R 0.469(7) A 2 H H13F 0.161 0.4263 0.9155 0.216 Uiso calc U P R 0.469(7) A 2 C C14B -0.0512(8) 0.3679(7) 0.7069(5) 0.123(3) Uani d U P D 0.469(7) A 2 H H14D -0.1023 0.3223 0.7353 0.184 Uiso calc U P R 0.469(7) A 2 H H14E -0.1053 0.4101 0.6546 0.184 Uiso calc U P R 0.469(7) A 2 H H14F 0.0038 0.3207 0.6834 0.184 Uiso calc U P R 0.469(7) A 2 C C15B -0.0723(6) 0.5210(5) 0.8081(7) 0.101(3) Uani d U P D 0.469(7) A 2 H H15D -0.1236 0.4742 0.8354 0.152 Uiso calc U P R 0.469(7) A 2 H H15E -0.0318 0.5777 0.8537 0.152 Uiso calc U P R 0.469(7) A 2 H H15F -0.125 0.5561 0.7509 0.152 Uiso calc U P R 0.469(7) A 2 C C16 0.5712(2) 0.73074(18) 0.72487(17) 0.0531(5) Uani d . . . 1.0 . . C C17 0.6223(2) 0.78206(19) 0.81907(16) 0.0558(5) Uani d . . . 1.0 . . C C18 0.5434(2) 0.86800(18) 0.83148(16) 0.0542(5) Uani d . . . 1.0 . . C C19 0.4263(2) 0.87808(19) 0.74796(17) 0.0569(5) Uani d . . . 1.0 . . H H19A 0.4147 0.9546 0.7243 0.068 Uiso calc U . R 1.0 . . H H19B 0.3517 0.8553 0.7657 0.068 Uiso calc U . R 1.0 . . O O20 0.61174(17) 0.65271(15) 0.68980(14) 0.0733(5) Uani d . . . 1.0 . . C C21 0.7333(3) 0.7555(3) 0.8909(2) 0.0789(8) Uani d . . . 1.0 . . H H21 0.7858 0.6973 0.8833 0.095 Uiso calc U . R 1.0 . . C C22 0.7624(3) 0.8190(3) 0.9739(2) 0.0978(11) Uani d . . . 1.0 . . H H22 0.8358 0.8033 1.0234 0.117 Uiso calc U . R 1.0 . . C C23 0.6843(4) 0.9052(3) 0.9845(2) 0.0928(10) Uani d . . . 1.0 . . H H23 0.7068 0.9472 1.0408 0.111 Uiso calc U . R 1.0 . . C C24 0.5759(3) 0.9303(2) 0.91522(19) 0.0720(7) Uani d . . . 1.0 . . H H24 0.524 0.9885 0.9237 0.086 Uiso calc U . R 1.0 . . O O25 0.4104(2) 0.97988(17) 0.56136(17) 0.0915(7) Uani d . . . 1.0 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0913(13) 0.0936(14) 0.0567(10) -0.0026(10) 0.0311(9) 0.0131(9) N5 0.0775(13) 0.0763(14) 0.0525(11) -0.0069(11) 0.0181(10) 0.0027(10) C3 0.0555(12) 0.0495(11) 0.0494(11) 0.0049(9) 0.0119(9) 0.0040(9) C4 0.0529(11) 0.0444(11) 0.0525(11) 0.0029(8) 0.0174(9) 0.0047(9) S2 0.0706(4) 0.0610(4) 0.0706(4) 0.0026(3) 0.0267(3) 0.0186(3) C6 0.0524(11) 0.0461(11) 0.0539(11) 0.0021(9) 0.0142(9) -0.0002(9) C7 0.0603(13) 0.0652(14) 0.0535(12) -0.0031(10) 0.0074(10) -0.0001(10) C8 0.0525(12) 0.0660(15) 0.0752(16) -0.0077(11) 0.0072(11) -0.0015(12) C9 0.0513(12) 0.0506(12) 0.0784(15) 0.0065(9) 0.0198(11) 0.0090(11) C10 0.0559(12) 0.0690(15) 0.0629(13) 0.0023(11) 0.0146(10) 0.0160(11) C11 0.0492(11) 0.0656(14) 0.0542(12) -0.0037(10) 0.0082(9) 0.0075(10) C12 0.0579(14) 0.0689(16) 0.104(2) -0.0001(12) 0.0280(13) 0.0211(15) C13A 0.137(5) 0.146(6) 0.118(5) -0.051(5) 0.084(4) -0.011(4) C14A 0.161(6) 0.078(4) 0.135(6) -0.020(4) 0.075(5) 0.015(4) C15A 0.083(4) 0.173(7) 0.169(7) -0.010(4) 0.048(4) 0.047(6) C13B 0.129(6) 0.136(6) 0.161(6) -0.019(4) 0.034(4) 0.071(5) C14B 0.134(6) 0.101(5) 0.147(6) -0.054(5) 0.064(5) -0.007(4) C15B 0.093(4) 0.103(5) 0.127(6) -0.001(4) 0.061(4) 0.004(4) C16 0.0516(11) 0.0461(11) 0.0640(13) 0.0038(9) 0.0208(10) 0.0078(10) C17 0.0541(12) 0.0541(12) 0.0575(12) -0.0055(9) 0.0137(10) 0.0093(10) C18 0.0624(13) 0.0488(12) 0.0552(12) -0.0112(9) 0.0230(10) 0.0037(9) C19 0.0593(12) 0.0486(12) 0.0645(13) 0.0035(9) 0.0210(10) -0.0023(10) O20 0.0740(11) 0.0625(10) 0.0844(12) 0.0179(9) 0.0249(9) -0.0030(9) C21 0.0653(15) 0.0764(17) 0.0833(18) -0.0005(13) 0.0036(13) 0.0164(15) C22 0.092(2) 0.105(3) 0.0706(18) -0.024(2) -0.0155(16) 0.0152(18) C23 0.115(3) 0.093(2) 0.0611(16) -0.030(2) 0.0108(16) -0.0046(16) C24 0.0931(18) 0.0666(16) 0.0598(14) -0.0180(14) 0.0279(13) -0.0067(12) O25 0.1101(16) 0.0650(12) 0.1076(15) 0.0220(11) 0.0450(13) 0.0370(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 N5 . 1.439(3) ? O1 S2 . 1.638(2) ? N5 C3 . 1.280(3) ? C3 C6 . 1.475(3) ? C3 C4 . 1.496(3) ? C4 C19 . 1.534(3) ? C4 C16 . 1.556(3) ? C4 S2 . 1.855(2) ? S2 O25 . 1.455(2) ? C6 C7 . 1.386(3) ? C6 C11 . 1.387(3) ? C7 C8 . 1.376(4) ? C7 H7 . 0.93 ? C8 C9 . 1.393(4) ? C8 H8 . 0.93 ? C9 C10 . 1.391(3) ? C9 C12 . 1.520(3) ? C10 C11 . 1.375(3) ? C10 H10 . 0.93 ? C11 H11 . 0.93 ? C12 C13B . 1.532(2) ? C12 C15A . 1.533(2) ? C12 C15B . 1.539(2) ? C12 C14A . 1.539(2) ? C12 C13A . 1.543(2) ? C12 C14B . 1.544(2) ? C13A H13A . 0.96 ? C13A H13B . 0.96 ? C13A H13C . 0.96 ? C14A H14A . 0.96 ? C14A H14B . 0.96 ? C14A H14C . 0.96 ? C15A H15A . 0.96 ? C15A H15B . 0.96 ? C15A H15C . 0.96 ? C13B H13D . 0.96 ? C13B H13E . 0.96 ? C13B H13F . 0.96 ? C14B H14D . 0.96 ? C14B H14E . 0.96 ? C14B H14F . 0.96 ? C15B H15D . 0.96 ? C15B H15E . 0.96 ? C15B H15F . 0.96 ? C16 O20 . 1.208(3) ? C16 C17 . 1.456(3) ? C17 C18 . 1.390(3) ? C17 C21 . 1.392(3) ? C18 C24 . 1.382(3) ? C18 C19 . 1.495(3) ? C19 H19A . 0.97 ? C19 H19B . 0.97 ? C21 C22 . 1.383(5) ? C21 H21 . 0.93 ? C22 C23 . 1.377(5) ? C22 H22 . 0.93 ? C23 C24 . 1.351(5) ? C23 H23 . 0.93 ? C24 H24 . 0.93 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N5 O1 S2 . . 115.03(14) ? C3 N5 O1 . . 110.2(2) ? N5 C3 C6 . . 118.9(2) ? N5 C3 C4 . . 117.8(2) ? C6 C3 C4 . . 123.19(18) ? C3 C4 C19 . . 119.49(18) ? C3 C4 C16 . . 112.30(18) ? C19 C4 C16 . . 105.66(17) ? C3 C4 S2 . . 101.98(14) ? C19 C4 S2 . . 110.23(15) ? C16 C4 S2 . . 106.57(14) ? O25 S2 O1 . . 108.34(13) ? O25 S2 C4 . . 106.04(11) ? O1 S2 C4 . . 90.01(9) ? C7 C6 C11 . . 117.7(2) ? C7 C6 C3 . . 120.8(2) ? C11 C6 C3 . . 121.4(2) ? C8 C7 C6 . . 120.9(2) ? C8 C7 H7 . . 119.5 ? C6 C7 H7 . . 119.5 ? C7 C8 C9 . . 121.9(2) ? C7 C8 H8 . . 119.0 ? C9 C8 H8 . . 119.0 ? C10 C9 C8 . . 116.5(2) ? C10 C9 C12 . . 121.9(2) ? C8 C9 C12 . . 121.6(2) ? C11 C10 C9 . . 121.8(2) ? C11 C10 H10 . . 119.1 ? C9 C10 H10 . . 119.1 ? C10 C11 C6 . . 121.1(2) ? C10 C11 H11 . . 119.4 ? C6 C11 H11 . . 119.4 ? C9 C12 C13B . . 111.5(3) ? C9 C12 C15A . . 110.7(3) ? C9 C12 C15B . . 110.0(2) ? C13B C12 C15B . . 114.7(5) ? C9 C12 C14A . . 109.2(2) ? C15A C12 C14A . . 112.7(5) ? C9 C12 C13A . . 110.2(2) ? C15A C12 C13A . . 109.3(5) ? C14A C12 C13A . . 104.5(5) ? C9 C12 C14B . . 110.5(3) ? C13B C12 C14B . . 107.4(5) ? C15B C12 C14B . . 102.3(5) ? C12 C13A H13A . . 109.5 ? C12 C13A H13B . . 109.5 ? H13A C13A H13B . . 109.5 ? C12 C13A H13C . . 109.5 ? H13A C13A H13C . . 109.5 ? H13B C13A H13C . . 109.5 ? C12 C14A H14A . . 109.5 ? C12 C14A H14B . . 109.5 ? H14A C14A H14B . . 109.5 ? C12 C14A H14C . . 109.5 ? H14A C14A H14C . . 109.5 ? H14B C14A H14C . . 109.5 ? C12 C15A H15A . . 109.5 ? C12 C15A H15B . . 109.5 ? H15A C15A H15B . . 109.5 ? C12 C15A H15C . . 109.5 ? H15A C15A H15C . . 109.5 ? H15B C15A H15C . . 109.5 ? C12 C13B H13D . . 109.5 ? C12 C13B H13E . . 109.5 ? H13D C13B H13E . . 109.5 ? C12 C13B H13F . . 109.5 ? H13D C13B H13F . . 109.5 ? H13E C13B H13F . . 109.5 ? C12 C14B H14D . . 109.5 ? C12 C14B H14E . . 109.5 ? H14D C14B H14E . . 109.5 ? C12 C14B H14F . . 109.5 ? H14D C14B H14F . . 109.5 ? H14E C14B H14F . . 109.5 ? C12 C15B H15D . . 109.5 ? C12 C15B H15E . . 109.5 ? H15D C15B H15E . . 109.5 ? C12 C15B H15F . . 109.5 ? H15D C15B H15F . . 109.5 ? H15E C15B H15F . . 109.5 ? O20 C16 C17 . . 129.3(2) ? O20 C16 C4 . . 124.2(2) ? C17 C16 C4 . . 106.45(18) ? C18 C17 C21 . . 121.0(2) ? C18 C17 C16 . . 110.4(2) ? C21 C17 C16 . . 128.6(2) ? C24 C18 C17 . . 120.1(2) ? C24 C18 C19 . . 127.8(2) ? C17 C18 C19 . . 112.1(2) ? C18 C19 C4 . . 104.29(18) ? C18 C19 H19A . . 110.9 ? C4 C19 H19A . . 110.9 ? C18 C19 H19B . . 110.9 ? C4 C19 H19B . . 110.9 ? H19A C19 H19B . . 108.9 ? C22 C21 C17 . . 117.4(3) ? C22 C21 H21 . . 121.3 ? C17 C21 H21 . . 121.3 ? C23 C22 C21 . . 121.0(3) ? C23 C22 H22 . . 119.5 ? C21 C22 H22 . . 119.5 ? C24 C23 C22 . . 121.7(3) ? C24 C23 H23 . . 119.2 ? C22 C23 H23 . . 119.2 ? C23 C24 C18 . . 118.9(3) ? C23 C24 H24 . . 120.6 ? C18 C24 H24 . . 120.6 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag S2 O1 N5 C3 . . . . -15.2(3) ? O1 N5 C3 C6 . . . . -178.68(18) ? O1 N5 C3 C4 . . . . -2.0(3) ? N5 C3 C4 C19 . . . . 137.0(2) ? C6 C3 C4 C19 . . . . -46.5(3) ? N5 C3 C4 C16 . . . . -98.5(2) ? C6 C3 C4 C16 . . . . 78.0(2) ? N5 C3 C4 S2 . . . . 15.2(2) ? C6 C3 C4 S2 . . . . -168.26(17) ? N5 O1 S2 O25 . . . . -86.37(18) ? N5 O1 S2 C4 . . . . 20.56(17) ? C3 C4 S2 O25 . . . . 90.13(17) ? C19 C4 S2 O25 . . . . -37.79(19) ? C16 C4 S2 O25 . . . . -151.98(17) ? C3 C4 S2 O1 . . . . -18.98(15) ? C19 C4 S2 O1 . . . . -146.90(16) ? C16 C4 S2 O1 . . . . 98.91(15) ? N5 C3 C6 C7 . . . . -23.8(3) ? C4 C3 C6 C7 . . . . 159.7(2) ? N5 C3 C6 C11 . . . . 153.9(2) ? C4 C3 C6 C11 . . . . -22.5(3) ? C11 C6 C7 C8 . . . . -0.9(4) ? C3 C6 C7 C8 . . . . 176.9(2) ? C6 C7 C8 C9 . . . . 0.7(4) ? C7 C8 C9 C10 . . . . -0.2(4) ? C7 C8 C9 C12 . . . . 179.7(2) ? C8 C9 C10 C11 . . . . -0.1(4) ? C12 C9 C10 C11 . . . . 180.0(2) ? C9 C10 C11 C6 . . . . -0.2(4) ? C7 C6 C11 C10 . . . . 0.7(4) ? C3 C6 C11 C10 . . . . -177.2(2) ? C10 C9 C12 C13B . . . . -29.8(6) ? C8 C9 C12 C13B . . . . 150.2(6) ? C10 C9 C12 C15A . . . . 145.8(5) ? C8 C9 C12 C15A . . . . -34.2(6) ? C10 C9 C12 C15B . . . . 98.5(5) ? C8 C9 C12 C15B . . . . -81.4(5) ? C10 C9 C12 C14A . . . . -89.6(5) ? C8 C9 C12 C14A . . . . 90.5(5) ? C10 C9 C12 C13A . . . . 24.7(5) ? C8 C9 C12 C13A . . . . -155.2(5) ? C10 C9 C12 C14B . . . . -149.2(5) ? C8 C9 C12 C14B . . . . 30.9(5) ? C3 C4 C16 O20 . . . . 41.0(3) ? C19 C4 C16 O20 . . . . 172.9(2) ? S2 C4 C16 O20 . . . . -69.9(2) ? C3 C4 C16 C17 . . . . -140.42(19) ? C19 C4 C16 C17 . . . . -8.5(2) ? S2 C4 C16 C17 . . . . 108.72(17) ? O20 C16 C17 C18 . . . . -178.2(2) ? C4 C16 C17 C18 . . . . 3.4(2) ? O20 C16 C17 C21 . . . . 2.2(4) ? C4 C16 C17 C21 . . . . -176.3(2) ? C21 C17 C18 C24 . . . . 1.5(3) ? C16 C17 C18 C24 . . . . -178.2(2) ? C21 C17 C18 C19 . . . . -176.8(2) ? C16 C17 C18 C19 . . . . 3.5(3) ? C24 C18 C19 C4 . . . . 173.1(2) ? C17 C18 C19 C4 . . . . -8.8(2) ? C3 C4 C19 C18 . . . . 137.84(19) ? C16 C4 C19 C18 . . . . 10.2(2) ? S2 C4 C19 C18 . . . . -104.61(17) ? C18 C17 C21 C22 . . . . -1.0(4) ? C16 C17 C21 C22 . . . . 178.6(3) ? C17 C21 C22 C23 . . . . -0.1(5) ? C21 C22 C23 C24 . . . . 0.8(5) ? C22 C23 C24 C18 . . . . -0.4(5) ? C17 C18 C24 C23 . . . . -0.7(4) ? C19 C18 C24 C23 . . . . 177.3(3) ? _shelx_res_file ; TITL PMc_5_456_a.res in P2(1)/c CELL 1.54178 11.0131 11.9246 14.5681 90.000 107.106 90.000 ZERR 4.000 0.0002 0.0002 0.0003 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O S UNIT 80 76 4 12 4 L.S. 5 ACTA BOND $H FMAP 2 PLAN 5 ISOR 0.004 C13A > C15A C14B C15B ISOR 0.003 C13B DFIX 1.54 0.002 C12 C13A C12 C14A C12 C15A DFIX 1.54 0.002 C12 C13B C12 C14B C12 C15B SADI C13A C14A C13A C15A C14A C15A C13B C14B C14B C15B C13B C15B SADI 0.005 C9 C13A C9 C14A C9 C15A C9 C13B C9 C14B C9 C15B CONF SIZE 0.196 0.315 0.421 TEMP 23.000 WGHT 0.088700 0.826800 FVAR 1.17201 0.53116 0.11952 O1 4 0.419639 0.785724 0.497325 11.00000 0.09132 0.09362 = 0.05665 0.01308 0.03105 -0.00263 N5 3 0.329556 0.716078 0.524979 11.00000 0.07753 0.07626 = 0.05249 0.00271 0.01814 -0.00694 C3 1 0.344888 0.725144 0.615226 11.00000 0.05548 0.04955 = 0.04944 0.00403 0.01191 0.00492 C4 1 0.450166 0.798760 0.672204 11.00000 0.05287 0.04436 = 0.05254 0.00468 0.01739 0.00286 S2 5 0.490183 0.880320 0.576599 11.00000 0.07057 0.06098 = 0.07059 0.01857 0.02672 0.00261 C6 1 0.263519 0.658397 0.658865 11.00000 0.05242 0.04611 = 0.05391 -0.00023 0.01422 0.00212 C7 1 0.145722 0.620204 0.603852 11.00000 0.06028 0.06521 = 0.05351 -0.00009 0.00740 -0.00309 AFIX 43 H7 2 0.115942 0.639943 0.539340 11.00000 -1.20000 AFIX 0 C8 1 0.072215 0.553478 0.643364 11.00000 0.05251 0.06600 = 0.07520 -0.00147 0.00718 -0.00765 AFIX 43 H8 2 -0.006003 0.528366 0.604550 11.00000 -1.20000 AFIX 0 C9 1 0.111575 0.522454 0.739823 11.00000 0.05134 0.05063 = 0.07841 0.00899 0.01984 0.00645 C10 1 0.229550 0.562180 0.794313 11.00000 0.05592 0.06897 = 0.06286 0.01604 0.01465 0.00234 AFIX 43 H10 2 0.259126 0.543383 0.859044 11.00000 -1.20000 AFIX 0 C11 1 0.303607 0.628456 0.755099 11.00000 0.04921 0.06559 = 0.05417 0.00755 0.00817 -0.00371 AFIX 43 H11 2 0.381892 0.653634 0.793748 11.00000 -1.20000 AFIX 0 C12 1 0.029636 0.449183 0.783062 11.00000 0.05788 0.06895 = 0.10394 0.02113 0.02800 -0.00006 PART 1 C13A 1 0.063118 0.469804 0.892249 21.00000 0.13749 0.14596 = 0.11797 -0.01106 0.08390 -0.05141 AFIX 33 H13A 2 0.010857 0.423146 0.918812 21.00000 -1.50000 H13B 2 0.150920 0.451951 0.921983 21.00000 -1.50000 H13C 2 0.048404 0.547143 0.903873 21.00000 -1.50000 AFIX 0 C14A 1 0.063310 0.325206 0.773970 21.00000 0.16083 0.07789 = 0.13536 0.01464 0.07511 -0.01974 AFIX 33 H14A 2 0.011724 0.278619 0.801218 21.00000 -1.50000 H14B 2 0.047862 0.306595 0.707402 21.00000 -1.50000 H14C 2 0.151344 0.313085 0.807621 21.00000 -1.50000 AFIX 0 C15A 1 -0.111647 0.473973 0.736324 21.00000 0.08287 0.17306 = 0.16945 0.04688 0.04833 -0.00965 AFIX 33 H15A 2 -0.161746 0.426940 0.764554 21.00000 -1.50000 H15B 2 -0.128465 0.551251 0.746500 21.00000 -1.50000 H15C 2 -0.133228 0.459257 0.668643 21.00000 -1.50000 AFIX 0 PART 2 C13B 1 0.110707 0.377979 0.866147 -21.00000 0.12946 0.13585 = 0.16106 0.07064 0.03425 -0.01926 AFIX 33 H13D 2 0.056275 0.332786 0.891822 -21.00000 -1.50000 H13E 2 0.165656 0.330266 0.843139 -21.00000 -1.50000 H13F 2 0.160988 0.426271 0.915539 -21.00000 -1.50000 AFIX 0 C14B 1 -0.051208 0.367876 0.706897 -21.00000 0.13442 0.10055 = 0.14741 -0.00662 0.06374 -0.05367 AFIX 33 H14D 2 -0.102340 0.322261 0.735320 -21.00000 -1.50000 H14E 2 -0.105314 0.410074 0.654603 -21.00000 -1.50000 H14F 2 0.003754 0.320724 0.683399 -21.00000 -1.50000 AFIX 0 C15B 1 -0.072294 0.521023 0.808119 -21.00000 0.09335 0.10250 = 0.12671 0.00447 0.06147 -0.00141 AFIX 33 H15D 2 -0.123619 0.474152 0.835375 -21.00000 -1.50000 H15E 2 -0.031849 0.577664 0.853705 -21.00000 -1.50000 H15F 2 -0.124998 0.556068 0.750908 -21.00000 -1.50000 AFIX 0 PART 0 C16 1 0.571215 0.730735 0.724871 11.00000 0.05163 0.04611 = 0.06401 0.00777 0.02085 0.00378 C17 1 0.622335 0.782063 0.819066 11.00000 0.05409 0.05411 = 0.05752 0.00926 0.01370 -0.00545 C18 1 0.543396 0.868004 0.831482 11.00000 0.06245 0.04882 = 0.05516 0.00370 0.02303 -0.01119 C19 1 0.426305 0.878078 0.747960 11.00000 0.05933 0.04862 = 0.06448 -0.00228 0.02104 0.00350 AFIX 23 H19A 2 0.414703 0.954556 0.724302 11.00000 -1.20000 H19B 2 0.351659 0.855300 0.765667 11.00000 -1.20000 AFIX 0 O20 4 0.611739 0.652712 0.689802 11.00000 0.07396 0.06249 = 0.08442 -0.00296 0.02491 0.01790 C21 1 0.733304 0.755485 0.890889 11.00000 0.06529 0.07643 = 0.08327 0.01636 0.00363 -0.00051 AFIX 43 H21 2 0.785792 0.697311 0.883335 11.00000 -1.20000 AFIX 0 C22 1 0.762430 0.819019 0.973945 11.00000 0.09249 0.10485 = 0.07055 0.01517 -0.01547 -0.02368 AFIX 43 H22 2 0.835833 0.803327 1.023396 11.00000 -1.20000 AFIX 0 C23 1 0.684332 0.905196 0.984514 11.00000 0.11491 0.09277 = 0.06112 -0.00461 0.01084 -0.03023 AFIX 43 H23 2 0.706814 0.947186 1.040798 11.00000 -1.20000 AFIX 0 C24 1 0.575916 0.930286 0.915218 11.00000 0.09309 0.06662 = 0.05980 -0.00671 0.02791 -0.01805 AFIX 43 H24 2 0.524033 0.988480 0.923707 11.00000 -1.20000 AFIX 0 O25 4 0.410420 0.979881 0.561356 11.00000 0.11011 0.06502 = 0.10758 0.03703 0.04497 0.02196 HKLF 4 REM PMc_5_456_a.res in P2(1)/c REM R1 = 0.0549 for 3041 Fo > 4sig(Fo) and 0.0562 for all 3172 data REM 255 parameters refined using 72 restraints END WGHT 0.0890 0.8264 REM Highest difference peak 0.413, deepest hole -0.430, 1-sigma level 0.042 Q1 1 0.1111 0.3410 0.8132 11.00000 0.05 0.41 Q2 1 0.0988 0.4367 0.9094 11.00000 0.05 0.34 Q3 1 -0.0840 0.3627 0.6756 11.00000 0.05 0.33 Q4 1 0.4077 0.8624 0.5175 11.00000 0.05 0.30 Q5 1 -0.0838 0.5119 0.7745 11.00000 0.05 0.27 ; _shelx_res_checksum 34984 _shelx_hkl_file ; -3 0 0 163.28 5.60 -3 0 0 164.88 5.20 -3 0 0 171.28 5.80 3 0 0 162.78 5.60 4 0 0 266.37 8.70 -4 0 0 281.47 9.00 -4 0 0 263.17 8.20 -4 0 0 256.47 8.60 -5 0 0 431.16 13.40 -5 0 0 389.66 12.80 -5 0 0 396.56 12.20 -5 0 0 389.66 13.20 -6 0 0 2037.70 60.69 -6 0 0 2070.09 60.79 7 0 0 46.50 2.40 -7 0 0 42.90 2.40 -7 0 0 43.80 2.60 7 0 0 41.80 2.20 7 0 0 44.30 2.30 7 0 0 43.30 2.30 8 0 0 52.59 2.80 -8 0 0 54.29 3.00 -8 0 0 55.79 3.30 8 0 0 55.89 2.70 8 0 0 56.29 2.90 8 0 0 53.39 2.50 8 0 0 57.69 2.90 8 0 0 54.89 2.70 9 0 0 1.60 0.70 -9 0 0 1.40 0.90 9 0 0 2.50 0.70 9 0 0 2.40 0.90 -9 0 0 2.80 1.00 9 0 0 1.80 0.80 10 0 0 5.10 1.20 -10 0 0 5.80 1.10 10 0 0 4.90 1.10 10 0 0 6.40 1.10 10 0 0 4.20 0.90 -10 0 0 5.90 1.20 11 0 0 37.80 2.30 11 0 0 40.70 2.60 -11 0 0 45.00 2.70 11 0 0 42.20 2.30 12 0 0 29.80 2.00 -12 0 0 31.10 1.90 12 0 0 31.70 1.70 0 -1 0 -1.50 0.10 0 -1 0 -1.10 0.10 -1 -1 0 580.74 16.90 -1 -1 0 573.34 16.70 -1 -1 0 541.35 16.60 -1 1 0 602.54 16.90 1 1 0 578.34 16.60 1 1 0 522.85 16.60 -1 1 0 568.34 16.80 -1 1 0 594.94 16.60 -2 -1 0 511.65 14.60 2 -1 0 478.45 14.50 -2 -1 0 499.95 14.50 -2 -1 0 491.75 14.50 -2 -1 0 489.85 14.90 2 1 0 502.25 14.60 -2 1 0 487.25 14.50 -2 1 0 507.45 14.50 -2 1 0 483.65 14.20 3 -1 0 131.09 4.60 -3 -1 0 132.89 4.90 -3 -1 0 139.49 4.40 -3 -1 0 129.89 4.60 -3 -1 0 136.49 4.60 -3 1 0 128.49 4.50 3 1 0 137.99 4.70 -3 1 0 129.49 4.50 -3 1 0 132.29 4.10 -4 -1 0 138.99 5.40 -4 -1 0 125.69 4.90 4 -1 0 132.79 4.90 -4 -1 0 135.59 5.00 -4 -1 0 140.89 4.60 -4 1 0 132.79 4.40 -4 1 0 138.79 5.00 4 1 0 130.09 5.00 -4 1 0 142.89 4.90 -4 1 0 132.59 4.30 -5 -1 0 102.29 4.50 -5 -1 0 101.69 4.40 -5 -1 0 98.29 3.80 -5 -1 0 109.99 4.80 -5 1 0 104.29 4.40 -5 1 0 105.79 4.30 -5 1 0 100.89 3.60 5 1 0 102.09 4.40 -6 -1 0 1082.09 33.50 -6 -1 0 1065.19 32.00 -6 1 0 1102.79 32.80 -6 1 0 1088.39 33.50 -7 -1 0 657.33 20.10 7 -1 0 657.93 20.40 -7 -1 0 699.63 20.80 -7 -1 0 709.43 21.20 -7 -1 0 704.63 22.70 7 -1 0 697.03 20.40 7 -1 0 682.33 20.10 7 -1 0 660.03 20.40 7 -1 0 676.53 20.50 -7 1 0 677.03 20.90 -7 1 0 666.63 20.70 7 1 0 694.23 20.50 7 1 0 646.54 20.10 -7 1 0 691.13 22.60 7 1 0 606.34 20.40 7 1 0 702.93 20.40 7 1 0 682.13 20.40 8 -1 0 167.18 6.20 -8 -1 0 166.88 6.40 8 -1 0 164.58 6.00 -8 -1 0 159.38 5.70 -8 -1 0 168.78 6.80 8 -1 0 161.28 6.00 8 -1 0 165.78 5.80 8 1 0 173.98 6.30 8 1 0 165.28 6.00 8 1 0 162.98 6.00 8 1 0 177.78 6.30 8 1 0 155.98 5.80 -8 1 0 171.58 6.60 -8 1 0 166.78 6.40 8 1 0 160.88 6.10 -9 -1 0 -0.10 0.60 9 -1 0 -0.60 0.50 9 -1 0 0.20 0.70 -9 -1 0 -0.10 0.80 -9 -1 0 0.50 0.60 9 -1 0 1.00 0.60 9 -1 0 0.70 0.60 9 1 0 0.30 0.60 -9 1 0 0.20 0.70 9 1 0 0.20 0.60 9 1 0 0.70 0.80 -9 1 0 0.40 0.70 9 1 0 0.10 0.70 -10 -1 0 17.50 1.90 10 -1 0 20.00 1.60 10 -1 0 18.60 1.70 10 -1 0 19.50 2.10 -10 -1 0 18.60 1.60 10 1 0 19.90 1.80 10 1 0 19.90 2.00 10 1 0 19.70 1.90 10 1 0 18.80 1.60 -10 1 0 19.80 2.00 10 1 0 21.40 1.90 -11 -1 0 27.80 2.10 11 -1 0 29.60 2.20 -11 -1 0 27.80 1.90 11 -1 0 26.50 1.80 -11 1 0 27.20 2.20 11 1 0 26.60 2.00 11 1 0 27.20 2.20 11 1 0 28.90 1.90 11 1 0 29.00 1.90 12 -1 0 6.70 0.80 -12 -1 0 5.60 0.80 12 -1 0 7.60 1.10 12 1 0 6.60 1.10 -12 1 0 8.00 1.10 12 1 0 9.30 1.00 0 -2 0 984.00 29.60 0 -2 0 1066.79 30.40 -2 -2 0 4094.99 127.39 -2 -2 0 4522.95 128.79 -2 -2 0 4526.95 126.59 2 2 0 4615.24 128.19 -2 2 0 4371.06 127.19 -3 -2 0 1513.95 40.40 -3 -2 0 1461.05 41.30 -3 -2 0 1311.67 40.50 -3 -2 0 1308.97 40.40 3 2 0 1411.36 40.70 -3 2 0 1387.46 40.50 -3 2 0 1390.06 39.90 3 2 0 1409.56 40.10 -4 -2 0 0.60 0.60 -4 -2 0 0.30 0.40 -4 -2 0 1.10 0.50 4 2 0 2.20 0.40 -4 2 0 0.40 0.50 4 2 0 2.10 0.70 -5 -2 0 439.66 14.80 -5 -2 0 446.66 13.70 -5 2 0 440.96 13.20 -5 2 0 414.56 13.80 5 2 0 449.86 14.20 -6 -2 0 50.89 3.60 -6 -2 0 56.19 2.70 -6 -2 0 54.59 2.80 6 2 0 54.99 3.30 6 2 0 55.39 2.60 6 2 0 56.19 2.40 -6 2 0 56.59 3.10 -6 2 0 56.19 2.40 7 -2 0 61.79 2.80 7 -2 0 59.79 2.70 -7 -2 0 58.49 2.90 -7 -2 0 60.59 2.60 7 -2 0 57.99 2.50 -7 -2 0 59.69 4.20 7 -2 0 57.19 2.60 -7 -2 0 63.49 3.40 7 2 0 58.59 2.70 -7 2 0 62.09 3.20 7 2 0 62.29 2.90 -7 2 0 57.29 3.00 7 2 0 52.49 2.80 -7 2 0 60.89 4.20 7 2 0 63.19 2.90 -7 2 0 62.99 3.60 -8 -2 0 1.70 0.60 -8 -2 0 1.80 0.70 8 -2 0 2.70 0.70 8 -2 0 2.20 0.70 8 -2 0 3.50 0.90 -8 -2 0 2.20 1.00 -8 2 0 2.40 0.90 8 2 0 1.40 0.70 8 2 0 2.60 0.90 -8 2 0 1.30 0.80 -8 2 0 1.90 1.30 8 2 0 2.50 0.80 8 2 0 2.50 0.80 -9 -2 0 0.50 0.70 -9 -2 0 0.10 0.80 9 -2 0 0.60 0.70 -9 -2 0 -0.90 0.50 9 -2 0 0.10 0.70 9 -2 0 -0.60 0.60 9 2 0 1.10 0.80 -9 2 0 -0.40 0.60 9 2 0 -0.40 0.70 9 2 0 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13.20 -4 3 0 396.66 12.10 4 3 0 376.46 12.40 -4 3 0 372.26 11.50 4 3 0 397.76 11.50 -5 -3 0 310.27 10.30 -5 -3 0 320.27 11.60 -5 3 0 320.27 9.70 5 3 0 310.67 9.70 5 3 0 319.17 10.70 -5 3 0 303.87 10.30 -6 -3 0 35.40 2.30 6 -3 0 31.20 1.80 -6 -3 0 38.10 3.20 -6 -3 0 31.40 1.90 -6 -3 0 42.60 3.30 6 -3 0 40.90 2.10 6 3 0 40.30 2.00 6 3 0 34.00 2.00 6 3 0 34.90 1.90 6 3 0 34.10 1.90 -6 3 0 43.70 2.60 6 3 0 32.70 2.60 -6 3 0 33.60 1.80 -7 -3 0 591.64 18.60 -7 -3 0 644.04 19.40 7 -3 0 630.04 18.10 7 -3 0 591.94 18.50 -7 -3 0 605.14 19.20 -7 -3 0 601.54 18.10 -7 -3 0 611.54 21.30 -7 3 0 598.64 18.40 -7 3 0 605.74 19.70 7 3 0 617.64 18.40 7 3 0 615.74 18.60 -7 3 0 620.84 21.20 7 3 0 586.64 18.70 -7 3 0 576.84 18.80 8 -3 0 3.70 1.00 -8 -3 0 4.70 0.90 -8 -3 0 3.70 1.10 8 -3 0 3.20 0.70 -8 -3 0 4.30 1.60 -8 -3 0 2.30 0.80 8 3 0 2.20 0.80 -8 3 0 3.20 1.00 -8 3 0 7.20 2.10 8 3 0 4.80 1.10 8 3 0 5.40 1.10 8 3 0 5.10 1.10 -9 -3 0 12.00 1.50 -9 -3 0 6.90 1.10 9 -3 0 6.20 1.00 9 3 0 7.30 1.30 9 3 0 11.70 1.60 9 3 0 6.70 1.40 -9 3 0 9.30 1.60 9 3 0 5.80 1.20 9 3 0 8.30 1.50 -10 -3 0 61.09 2.90 10 -3 0 61.29 2.80 10 3 0 58.89 3.10 10 3 0 67.89 3.50 -10 3 0 61.09 3.50 10 3 0 56.79 3.30 10 3 0 57.19 3.10 11 -3 0 3.90 0.70 -11 -3 0 4.30 0.80 11 3 0 4.20 1.00 11 3 0 4.50 1.00 11 3 0 4.40 1.00 -11 3 0 3.20 1.00 11 3 0 3.40 1.00 -12 -3 0 38.20 1.80 12 -3 0 35.20 1.50 12 3 0 35.90 2.10 -12 3 0 37.10 2.10 0 -4 0 737.53 21.90 0 -4 0 740.43 21.70 -1 -4 0 1789.32 51.89 1 -4 0 1741.53 50.99 -1 -4 0 1824.82 52.49 1 4 0 1811.12 51.49 1 4 0 1725.03 51.09 -2 -4 0 558.94 16.80 -2 -4 0 520.35 16.10 -2 4 0 530.45 15.60 -2 4 0 535.55 15.50 2 4 0 510.15 15.80 2 4 0 519.25 15.20 2 4 0 541.65 15.80 -3 -4 0 3041.30 85.29 -3 -4 0 2862.91 83.69 3 4 0 2890.71 83.89 -3 4 0 2802.62 82.09 -3 4 0 2853.51 83.59 3 4 0 2825.12 82.29 -4 -4 0 2216.78 64.89 -4 -4 0 2262.67 66.09 4 4 0 2306.07 64.29 -4 4 0 2221.48 63.89 -4 4 0 2165.68 64.49 4 4 0 2247.88 64.99 -5 -4 0 1215.38 38.40 -5 -4 0 1226.98 37.00 -5 4 0 1269.57 36.80 5 4 0 1243.98 36.00 -5 4 0 1254.57 35.90 5 4 0 1234.18 37.20 -6 -4 0 865.11 26.50 -6 -4 0 855.81 28.30 -6 -4 0 835.72 25.20 6 -4 0 900.81 25.70 6 -4 0 876.51 25.20 -6 -4 0 868.01 26.60 -6 4 0 877.01 25.50 -6 4 0 838.82 26.50 6 4 0 837.32 25.80 6 4 0 893.01 25.70 6 4 0 876.71 25.60 6 4 0 871.51 27.10 6 4 0 844.72 25.50 -7 -4 0 43.70 2.10 7 -4 0 46.40 2.10 7 -4 0 53.59 2.60 -7 -4 0 43.50 3.00 -7 -4 0 39.60 3.90 -7 4 0 45.70 2.70 7 4 0 52.19 2.70 7 4 0 44.10 2.40 7 4 0 41.50 2.40 -7 4 0 45.30 3.10 -7 4 0 42.50 4.00 -7 4 0 46.70 2.40 8 -4 0 114.29 4.80 8 -4 0 125.99 4.40 -8 -4 0 120.89 4.50 8 4 0 114.89 4.70 -8 4 0 122.79 5.10 8 4 0 123.39 5.10 8 4 0 117.59 4.90 8 4 0 116.09 4.90 -8 4 0 121.99 5.20 -8 4 0 107.59 7.00 9 -4 0 300.47 9.60 -9 -4 0 322.07 9.80 9 -4 0 295.37 10.30 9 4 0 299.27 10.40 -9 4 0 308.97 10.70 9 4 0 301.27 10.20 9 4 0 302.57 10.30 9 4 0 302.77 10.50 9 4 0 302.27 10.40 -10 -4 0 61.59 2.80 10 -4 0 60.29 2.60 10 4 0 63.09 3.40 10 4 0 60.99 3.30 -10 4 0 64.19 3.50 10 4 0 59.39 3.10 10 4 0 63.29 3.10 11 -4 0 62.29 2.50 -11 -4 0 66.39 2.80 11 4 0 70.69 3.30 11 4 0 67.99 3.30 11 4 0 67.59 3.10 -11 4 0 72.69 3.50 11 4 0 69.79 3.10 -12 -4 0 1.50 0.40 0 -5 0 0.30 0.40 0 -5 0 0.10 0.40 -1 -5 0 33.50 2.10 1 -5 0 33.60 1.70 -1 -5 0 32.00 1.80 1 5 0 36.90 1.40 1 5 0 31.60 1.30 -2 -5 0 2.40 0.70 -3 -5 0 390.16 13.00 -3 -5 0 396.76 13.90 3 5 0 400.56 12.80 3 5 0 416.46 11.90 -3 5 0 424.16 12.40 -4 -5 0 28.10 2.00 -4 -5 0 20.40 2.40 4 5 0 24.00 1.90 4 5 0 23.70 1.20 -4 5 0 23.90 1.60 -4 5 0 24.20 1.20 -5 -5 0 305.37 9.50 -5 -5 0 326.67 11.00 -5 -5 0 327.87 12.40 5 -5 0 298.67 9.70 -5 -5 0 291.27 9.70 -5 5 0 323.17 10.50 -5 5 0 321.27 9.70 5 5 0 313.57 9.70 5 5 0 307.47 10.90 -6 -5 0 330.77 10.00 -6 -5 0 330.67 13.20 6 -5 0 297.27 10.30 -6 -5 0 335.07 11.60 6 -5 0 317.57 9.80 -6 -5 0 333.27 10.40 6 5 0 310.07 10.50 6 5 0 322.87 10.40 6 5 0 324.97 11.80 -6 5 0 328.57 10.20 -6 5 0 335.47 11.30 6 5 0 325.47 10.30 -7 -5 0 196.88 6.80 7 -5 0 190.28 6.20 -7 -5 0 198.58 6.40 7 -5 0 200.48 6.80 -7 -5 0 188.78 7.80 -7 -5 0 179.48 9.40 7 5 0 184.08 8.30 7 5 0 188.88 7.00 -7 5 0 188.08 9.40 -7 5 0 178.18 7.70 7 5 0 184.68 6.80 7 5 0 198.98 6.80 -7 5 0 193.58 6.70 -8 -5 0 311.37 9.90 8 -5 0 309.77 9.70 8 -5 0 314.07 10.50 8 5 0 329.27 10.60 8 5 0 292.67 10.60 8 5 0 326.47 10.60 -8 5 0 295.87 10.30 8 5 0 324.77 10.40 9 -5 0 22.60 2.00 -9 -5 0 20.90 2.00 -9 -5 0 23.20 1.70 9 -5 0 19.80 1.30 9 5 0 19.50 1.90 -9 5 0 23.80 2.10 9 5 0 21.10 1.90 9 5 0 23.70 2.10 9 5 0 19.50 2.00 9 5 0 23.80 2.20 10 -5 0 2.50 0.50 10 -5 0 3.70 1.00 -10 -5 0 2.40 0.70 10 5 0 2.40 0.90 10 5 0 3.20 0.90 10 5 0 3.50 1.00 10 5 0 3.20 0.90 -10 5 0 4.30 1.10 -11 -5 0 0.30 0.40 11 5 0 0.40 0.60 -11 5 0 0.00 0.50 11 5 0 0.50 0.70 11 5 0 -0.10 0.50 11 5 0 0.10 0.60 0 -6 0 2.20 0.80 0 -6 0 0.60 0.50 -1 -6 0 274.37 9.60 -1 -6 0 265.07 9.10 1 -6 0 276.27 8.80 1 6 0 266.37 8.30 -2 -6 0 33.50 2.60 -2 -6 0 33.90 2.20 -2 6 0 31.60 1.40 2 6 0 31.50 1.70 -3 -6 0 24.50 2.00 -3 -6 0 24.10 2.50 -3 6 0 26.80 1.40 3 6 0 20.20 1.60 3 6 0 18.20 1.00 -4 -6 0 55.19 3.20 -4 -6 0 53.59 4.00 4 -6 0 49.20 2.10 4 -6 0 54.29 2.80 -4 -6 0 49.00 2.10 4 6 0 53.79 2.20 4 6 0 55.89 3.10 -4 6 0 54.09 2.00 -4 6 0 56.29 2.60 5 -6 0 28.90 1.60 -5 -6 0 25.10 2.00 -5 -6 0 27.00 1.40 -5 -6 0 26.50 1.60 -5 -6 0 24.60 3.00 -5 -6 0 28.10 2.40 -5 -6 0 22.50 1.80 -5 6 0 26.20 2.00 5 6 0 27.20 2.40 5 6 0 29.90 1.60 -5 6 0 28.50 1.50 -6 -6 0 170.38 6.40 -6 -6 0 172.18 8.80 -6 -6 0 169.08 6.20 -6 -6 0 170.78 7.20 6 -6 0 156.18 5.70 -6 -6 0 158.98 5.40 -6 -6 0 154.98 5.80 6 6 0 167.08 7.30 6 6 0 161.18 5.80 6 6 0 167.48 5.90 -6 6 0 164.38 6.60 -6 6 0 161.38 5.70 -7 -6 0 17.70 1.90 -7 -6 0 10.60 1.40 7 -6 0 12.20 0.90 -7 -6 0 14.50 1.30 7 -6 0 13.00 1.50 -7 -6 0 13.30 2.20 -7 6 0 15.80 3.10 -7 6 0 10.20 1.30 7 6 0 13.60 1.40 7 6 0 16.80 1.70 7 6 0 10.80 1.50 7 6 0 14.20 1.60 -8 -6 0 49.50 2.80 8 -6 0 47.30 2.00 -8 -6 0 50.49 2.40 -8 -6 0 47.80 3.40 8 -6 0 51.59 2.80 8 6 0 55.29 2.90 8 6 0 48.80 2.80 8 6 0 47.10 2.90 8 6 0 49.60 2.90 -8 6 0 50.09 2.70 -9 -6 0 1.70 0.60 9 -6 0 4.20 1.00 9 6 0 3.20 1.00 9 6 0 2.10 0.80 9 6 0 1.80 0.90 9 6 0 2.90 0.90 9 6 0 1.30 0.80 -10 -6 0 2.40 0.60 10 -6 0 1.90 0.80 10 6 0 1.40 0.80 10 6 0 2.60 0.90 10 6 0 1.50 0.80 10 6 0 1.60 0.80 -10 6 0 2.80 0.80 -11 -6 0 18.60 1.10 11 6 0 18.70 1.50 11 6 0 19.30 1.50 11 6 0 18.30 1.40 11 6 0 20.10 1.50 0 -7 0 0.60 0.50 -1 -7 0 66.89 3.40 1 7 0 67.29 2.60 -2 -7 0 57.79 2.20 -2 -7 0 64.19 4.00 -2 -7 0 61.19 3.30 2 -7 0 63.99 3.00 -2 7 0 63.89 2.20 2 7 0 61.49 2.70 3 -7 0 2.30 0.40 3 -7 0 3.20 0.30 -3 -7 0 3.60 0.50 3 -7 0 2.30 0.30 3 -7 0 2.60 0.80 -3 -7 0 3.20 1.30 -3 -7 0 1.90 0.80 -3 -7 0 2.10 0.90 -3 7 0 2.70 0.60 3 7 0 2.80 0.80 3 7 0 2.50 0.40 4 -7 0 5.50 1.10 -4 -7 0 6.90 1.20 -4 -7 0 5.80 1.20 -4 -7 0 6.70 1.50 4 -7 0 4.50 0.60 -4 -7 0 5.30 1.70 -4 -7 0 2.90 0.60 4 -7 0 6.10 0.50 4 7 0 4.00 1.00 4 7 0 4.80 0.70 -4 7 0 4.80 0.60 -4 7 0 6.20 1.00 5 -7 0 60.89 2.40 -5 -7 0 65.59 3.20 -5 -7 0 65.89 5.00 -5 -7 0 59.19 2.70 5 -7 0 60.99 2.60 -5 -7 0 59.19 2.30 -5 -7 0 67.79 4.00 -5 -7 0 65.59 3.30 5 7 0 61.99 2.70 -5 7 0 63.79 2.60 -5 7 0 64.19 3.20 5 7 0 59.29 3.70 -6 -7 0 58.59 3.20 -6 -7 0 59.49 4.00 6 -7 0 61.09 2.80 -6 -7 0 54.69 3.20 -6 -7 0 53.09 2.30 -6 -7 0 56.59 2.80 -6 -7 0 56.29 5.10 6 7 0 53.39 2.70 -6 7 0 59.99 2.70 -6 7 0 59.49 5.10 6 7 0 59.29 2.90 -7 -7 0 189.68 6.80 7 -7 0 187.08 6.70 -7 -7 0 194.88 6.20 -7 7 0 194.48 6.70 7 7 0 194.88 6.90 7 7 0 177.98 6.70 8 -7 0 1.00 0.70 -8 -7 0 0.90 0.70 -8 -7 0 0.30 0.40 8 7 0 0.00 0.70 8 7 0 0.10 0.60 8 7 0 -0.50 0.60 -8 7 0 0.50 0.50 8 7 0 0.80 0.70 8 7 0 0.90 0.80 9 -7 0 22.90 1.80 -9 -7 0 23.70 1.40 9 7 0 24.30 2.00 9 7 0 21.80 1.90 9 7 0 21.00 1.80 9 7 0 21.00 1.80 10 -7 0 0.80 0.60 -10 -7 0 0.80 0.40 10 7 0 0.20 0.60 10 7 0 0.10 0.60 10 7 0 0.00 0.60 10 7 0 1.50 0.70 0 -8 0 1295.67 38.80 0 -8 0 1341.27 39.00 -1 -8 0 1619.24 48.00 -1 -8 0 1625.24 48.80 1 -8 0 1661.13 48.30 -1 -8 0 1683.73 48.30 -1 -8 0 1584.14 46.90 1 8 0 1699.93 47.40 2 -8 0 496.05 14.70 -2 -8 0 518.65 16.10 -2 -8 0 503.25 14.80 2 -8 0 501.45 16.00 -2 -8 0 520.65 14.80 -2 -8 0 499.05 15.80 -2 -8 0 511.65 16.80 -2 -8 0 502.65 14.90 2 8 0 509.25 15.70 2 8 0 515.15 14.70 3 -8 0 550.64 15.40 -3 -8 0 514.85 16.60 -3 -8 0 529.85 15.70 3 -8 0 541.15 15.60 -3 -8 0 546.95 17.90 -3 -8 0 509.75 18.90 3 -8 0 527.05 15.40 -3 -8 0 527.65 15.70 3 -8 0 526.55 16.80 -3 -8 0 511.95 16.70 3 8 0 551.44 15.70 -3 8 0 529.25 15.90 3 8 0 535.05 16.80 -4 -8 0 29.30 2.80 -4 -8 0 35.30 1.70 4 -8 0 31.20 1.30 -4 -8 0 26.30 3.30 -4 -8 0 26.00 1.50 -4 -8 0 23.30 1.90 4 -8 0 32.30 1.30 -4 -8 0 26.10 2.20 4 -8 0 26.20 2.20 4 -8 0 34.60 1.60 -4 8 0 31.90 1.50 4 8 0 30.00 2.40 -4 8 0 35.30 2.00 -5 -8 0 548.05 18.40 -5 -8 0 531.05 17.00 5 -8 0 531.65 15.70 5 -8 0 519.45 16.00 -5 -8 0 513.05 20.10 -5 -8 0 531.95 16.20 -5 8 0 535.95 19.90 -5 8 0 542.75 16.00 5 8 0 528.55 16.20 6 -8 0 171.18 5.90 -6 -8 0 170.28 6.00 -6 -8 0 158.08 6.50 6 8 0 165.38 6.10 -6 8 0 167.08 5.80 6 8 0 166.88 6.00 7 -8 0 24.10 1.70 -7 -8 0 23.40 1.80 7 8 0 21.60 1.80 7 8 0 21.60 1.70 -7 8 0 22.90 1.60 8 -8 0 34.50 2.10 -8 -8 0 33.60 2.10 8 8 0 34.10 2.40 8 8 0 34.80 2.30 8 8 0 31.70 2.40 8 8 0 31.90 2.10 9 -8 0 56.19 2.70 -9 -8 0 54.49 2.70 9 8 0 54.59 2.80 9 8 0 55.09 2.90 9 8 0 52.69 2.60 10 -8 0 57.49 2.50 10 8 0 56.09 2.60 10 8 0 53.39 2.50 0 -9 0 2.80 1.00 -1 -9 0 123.69 5.10 -1 -9 0 116.99 3.80 1 -9 0 125.79 5.20 -1 -9 0 124.29 5.00 1 9 0 124.99 4.20 -2 -9 0 24.00 1.10 -2 -9 0 23.70 1.90 -2 -9 0 21.10 2.00 -2 -9 0 24.00 2.40 2 -9 0 25.20 2.20 -2 -9 0 21.70 1.10 -2 -9 0 21.50 1.10 2 9 0 21.60 1.10 2 9 0 21.80 1.60 3 -9 0 1.00 0.90 3 -9 0 2.00 0.30 -3 -9 0 2.00 0.50 3 -9 0 4.00 0.50 -3 -9 0 1.40 0.50 -3 -9 0 2.20 0.90 3 -9 0 1.80 0.30 -3 -9 0 2.50 1.20 -3 -9 0 1.60 0.80 3 9 0 1.90 0.50 4 -9 0 42.40 1.80 4 -9 0 44.70 1.90 -4 -9 0 41.50 2.10 -4 -9 0 42.10 2.10 4 -9 0 45.10 1.70 -4 -9 0 45.80 2.90 -4 9 0 42.90 1.90 4 9 0 45.20 2.10 -4 9 0 42.90 4.30 -5 -9 0 88.29 3.40 5 -9 0 78.99 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2325.07 66.39 -4 -6 9 2319.77 66.49 -4 -6 9 2255.17 65.49 4 -6 -9 2349.06 66.39 -4 -6 9 2175.68 66.99 4 -6 -9 2344.67 66.59 -4 -6 9 2320.77 66.39 4 6 -9 2257.17 66.19 -4 6 9 2337.47 66.29 -3 -6 9 435.46 14.10 3 -6 -9 429.76 13.00 3 -6 -9 440.26 14.20 -3 -6 9 433.86 13.10 -3 -6 9 410.86 16.10 -3 -6 9 439.56 14.00 3 -6 -9 447.56 14.00 -3 6 9 449.76 13.80 3 6 -9 447.16 13.90 2 -6 -9 1.60 0.70 -2 -6 9 3.10 0.90 -2 -6 9 1.30 0.90 -2 -6 9 2.00 0.50 2 -6 -9 0.90 0.80 2 -6 -9 3.80 0.60 -2 6 9 1.10 0.60 2 6 -9 1.10 0.60 -1 -6 9 11.50 1.50 -1 -6 9 15.70 1.00 1 -6 -9 15.90 1.00 1 -6 -9 16.00 1.50 -1 -6 9 18.50 1.60 1 6 -9 15.90 1.40 1 6 -9 12.90 2.40 -1 6 9 16.00 1.40 0 -6 -9 44.30 2.40 0 -6 9 45.90 2.50 0 -6 -9 42.00 1.90 0 -6 9 42.40 1.80 0 -6 -9 42.80 2.80 0 6 -9 42.40 3.60 0 6 -9 41.50 2.40 0 6 9 42.70 2.30 1 -6 9 102.19 3.40 -1 -6 -9 101.59 3.60 -1 -6 -9 105.09 4.10 -1 -6 -9 93.29 4.60 1 -6 9 107.79 4.20 1 6 9 97.29 4.20 -1 6 -9 100.49 5.50 -1 6 -9 87.49 7.10 -1 6 -9 99.69 4.10 1 6 9 99.39 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169.28 6.40 8 -7 -9 171.08 6.40 8 7 -9 156.18 6.60 7 -7 -9 207.38 7.30 -7 -7 9 190.88 6.20 -7 -7 9 204.98 7.50 7 -7 -9 201.38 7.40 -7 -7 9 187.88 7.20 -7 7 9 189.38 7.20 7 7 -9 185.28 7.50 6 -7 -9 13.40 1.70 -6 -7 9 12.90 1.10 -6 -7 9 15.60 2.00 -6 -7 9 10.80 1.50 6 -7 -9 11.20 1.60 -6 -7 9 10.50 1.50 6 7 -9 12.80 1.90 -6 7 9 11.10 1.50 5 -7 -9 77.59 4.00 -5 -7 9 74.19 2.90 -5 -7 9 83.99 3.90 -5 -7 9 83.49 3.90 -5 -7 9 79.39 4.00 5 -7 -9 79.89 3.80 5 7 -9 80.99 3.80 -5 7 9 75.29 3.60 -4 -7 9 62.79 3.30 -4 -7 9 61.29 2.40 -4 -7 9 67.89 3.60 4 -7 -9 69.49 3.60 4 -7 -9 66.69 3.30 -4 7 9 63.99 3.20 4 7 -9 63.39 3.20 3 -7 -9 25.60 1.90 3 -7 -9 23.70 2.30 -3 -7 9 25.90 2.00 -3 -7 9 25.40 1.20 -3 -7 9 25.30 2.30 3 7 -9 26.30 1.90 -3 7 9 25.40 1.90 -2 -7 9 4.50 1.20 2 -7 -9 5.00 1.00 -2 -7 9 6.50 1.10 2 -7 -9 5.00 0.50 -2 7 9 4.60 0.90 2 7 -9 6.50 1.10 1 -7 -9 155.98 5.70 -1 -7 9 155.48 5.80 1 -7 -9 151.28 6.10 1 -7 -9 147.39 4.80 -1 7 9 147.99 5.60 1 7 -9 158.18 5.80 1 7 -9 163.08 7.60 0 -7 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1 -5 14 2.80 0.40 -1 -5 -14 4.60 0.60 -1 5 -14 4.00 0.90 1 5 14 3.90 0.80 -1 5 -14 3.50 1.00 -2 -5 -14 7.00 0.70 -2 5 -14 7.30 1.00 -2 5 -14 7.20 1.20 2 5 14 7.20 0.90 -7 -6 14 22.40 1.00 7 6 -14 22.40 1.80 -7 6 14 21.10 1.60 -6 -6 14 9.00 0.70 -6 6 14 8.90 1.20 6 6 -14 9.10 1.30 -5 -6 14 0.70 0.30 5 -6 -14 0.20 0.30 5 6 -14 0.80 1.10 5 6 -14 0.20 0.60 -5 6 14 0.20 0.60 4 -6 -14 0.40 0.30 -4 -6 14 0.70 0.30 4 6 -14 1.20 0.70 4 6 -14 0.90 1.10 -4 6 14 0.60 0.50 -3 -6 14 11.70 0.80 3 -6 -14 10.40 0.80 3 6 -14 11.20 1.40 3 6 -14 8.50 1.90 -3 6 14 9.50 1.30 -2 -6 14 20.30 1.00 2 -6 -14 18.00 1.00 -2 6 14 20.40 1.60 2 6 -14 18.50 2.40 2 6 -14 20.40 1.70 1 -6 -14 6.20 0.60 -1 6 14 6.70 1.00 1 6 -14 7.50 1.10 1 6 -14 6.30 1.70 0 -6 -14 2.50 0.40 0 6 -14 2.60 1.00 0 6 14 2.90 0.70 0 6 -14 2.90 0.80 -1 -6 -14 2.00 0.30 -1 6 -14 2.10 0.80 1 6 14 2.30 0.70 -1 6 -14 1.80 0.60 -2 6 -14 6.40 1.00 6 7 -14 24.90 1.80 5 -7 -14 2.40 0.70 -5 -7 14 2.60 0.90 -5 7 14 3.10 0.70 5 7 -14 3.40 0.80 -4 -7 14 9.80 1.20 4 -7 -14 10.10 1.20 -4 7 14 10.70 1.20 4 7 -14 10.70 1.30 3 -7 -14 24.50 1.60 -3 -7 14 22.00 1.60 -3 7 14 23.70 1.60 3 7 -14 24.70 1.70 2 -7 -14 19.50 1.40 -2 -7 14 16.00 1.40 2 7 -14 18.40 1.50 -2 7 14 19.30 1.50 -1 -7 14 0.50 0.50 -1 7 14 0.70 0.50 1 7 -14 0.40 0.50 0 7 -14 8.40 1.30 -9 0 15 0.00 0.50 9 0 -15 -0.20 0.50 -8 0 15 0.20 0.40 -8 0 15 -0.30 0.50 8 0 -15 1.10 0.60 -7 0 15 0.10 0.60 7 0 -15 0.80 0.60 -7 0 15 0.10 0.50 6 0 -15 0.40 0.50 -6 0 15 -1.20 0.50 -6 0 15 0.90 0.60 6 0 -15 -0.10 0.50 -5 0 15 -0.10 0.50 -5 0 15 0.50 0.60 5 0 -15 -0.90 0.50 5 0 -15 0.40 0.60 -4 0 15 -0.10 0.50 4 0 -15 -0.20 0.50 -4 0 15 -0.10 0.50 4 0 -15 -0.20 0.50 3 0 -15 0.40 0.50 -3 0 15 0.60 0.60 3 0 -15 0.20 0.60 -3 0 15 0.20 0.50 -2 0 15 0.30 0.50 2 0 -15 0.80 0.60 2 0 -15 0.20 0.50 -2 0 15 0.40 0.50 -1 0 15 -0.20 0.50 -1 0 15 -0.60 0.50 1 0 -15 0.20 0.50 1 0 -15 -0.10 0.50 0 0 15 0.30 0.50 0 0 -15 -0.20 0.50 0 0 -15 0.40 0.70 0 0 -15 -0.80 0.40 -1 0 -15 0.60 0.50 1 0 15 -0.80 0.40 -1 0 -15 -0.40 0.60 -1 0 -15 0.00 0.40 -2 0 -15 -0.50 0.40 2 0 15 -0.20 0.40 -2 0 -15 0.40 0.60 9 -1 -15 17.40 1.20 -9 -1 15 13.80 1.20 9 1 -15 16.60 1.30 8 -1 -15 1.10 0.60 -8 -1 15 3.30 0.80 8 1 -15 2.00 0.60 8 1 -15 2.70 0.70 -8 1 15 1.90 0.70 7 -1 -15 8.60 1.10 -7 -1 15 8.70 1.10 7 1 -15 7.80 1.10 -7 1 15 7.30 1.10 -7 1 15 6.90 1.50 7 1 -15 7.10 1.00 -6 -1 15 6.50 1.00 6 -1 -15 7.10 1.10 6 1 -15 7.30 1.20 -6 1 15 5.70 1.00 6 1 -15 6.00 1.00 -6 1 15 6.60 1.10 -5 -1 15 41.20 2.20 5 -1 -15 38.10 2.10 5 1 -15 36.70 2.30 5 1 -15 38.60 2.20 -5 1 15 38.90 2.30 -5 1 15 34.90 2.10 4 -1 -15 23.80 1.70 -4 -1 15 23.20 1.70 4 1 -15 25.20 1.80 4 1 -15 26.80 2.00 -4 1 15 22.90 1.70 -4 1 15 26.40 1.90 4 1 -15 22.40 2.60 3 -1 -15 93.59 3.70 -3 -1 15 96.09 3.70 3 -1 -15 91.89 3.70 3 1 -15 86.39 3.70 -3 1 15 97.49 3.90 3 1 -15 85.89 5.10 3 1 -15 97.39 4.10 -3 1 15 92.69 3.70 2 -1 -15 26.80 1.80 2 -1 -15 29.30 1.80 -2 -1 15 29.20 1.70 -2 1 15 25.00 1.70 2 1 -15 28.00 2.00 2 1 -15 28.10 1.80 -2 1 15 28.20 1.80 2 1 -15 27.40 2.40 -1 -1 15 73.69 2.90 1 -1 -15 69.59 3.00 1 -1 -15 67.89 2.90 1 1 -15 69.89 3.60 -1 1 15 68.89 3.00 -1 1 15 71.59 3.10 1 1 -15 69.49 3.60 1 1 -15 74.69 3.30 0 -1 15 71.49 2.80 0 -1 -15 68.99 2.80 0 1 15 67.89 2.80 0 1 -15 71.59 3.20 0 1 -15 64.59 3.50 0 1 15 69.99 2.90 1 -1 15 -0.50 0.40 -1 -1 -15 -0.30 0.40 -1 1 -15 -0.10 0.50 -1 1 -15 0.10 0.60 1 1 15 -0.50 0.40 1 1 15 -0.10 0.40 -2 -1 -15 3.90 0.60 2 -1 15 2.90 0.60 -2 1 -15 3.50 0.70 2 1 15 4.00 0.70 -2 1 -15 4.30 1.00 3 -1 15 12.50 1.30 -9 -2 15 54.89 2.30 9 -2 -15 57.19 2.30 8 -2 -15 12.50 1.20 -8 -2 15 11.20 1.10 8 -2 -15 10.90 1.40 8 2 -15 13.10 1.30 -8 2 15 14.30 1.40 7 -2 -15 1.60 0.80 7 -2 -15 1.90 0.70 -7 -2 15 2.30 0.70 7 2 -15 2.30 0.80 -7 2 15 2.50 0.80 -6 -2 15 71.09 3.10 6 -2 -15 73.59 3.10 6 2 -15 75.09 3.50 -6 2 15 72.29 3.40 5 -2 -15 27.70 1.80 -5 -2 15 30.80 1.90 5 2 -15 25.80 2.90 -5 2 15 27.70 2.00 5 2 -15 30.40 2.20 -4 -2 15 16.20 1.40 4 -2 -15 17.40 1.50 4 2 -15 12.50 2.30 4 2 -15 18.50 1.80 -4 2 15 19.50 1.70 -3 -2 15 3.50 0.80 3 -2 -15 3.20 0.80 3 2 -15 3.50 1.00 3 2 -15 3.70 1.50 -3 2 15 3.10 0.80 -2 -2 15 3.20 0.70 2 -2 -15 3.50 0.70 2 2 -15 2.50 0.90 2 2 -15 2.60 1.30 -2 2 15 3.80 0.90 -1 -2 15 76.19 3.00 1 -2 -15 76.19 3.00 1 2 -15 76.19 3.80 -1 2 15 76.29 3.30 1 2 -15 73.79 3.40 0 -2 -15 44.70 2.10 0 -2 15 45.90 2.00 0 2 -15 47.00 2.80 0 2 15 42.80 2.20 0 2 -15 42.90 2.40 -1 -2 -15 1.20 0.50 1 -2 15 0.60 0.40 -1 2 -15 1.10 0.80 -1 2 -15 0.50 0.50 1 2 15 0.90 0.50 -2 -2 -15 9.10 0.90 2 -2 15 8.00 0.70 2 2 15 9.90 1.10 -2 2 -15 8.30 1.20 -2 2 -15 7.80 1.00 9 -3 -15 4.70 0.60 -9 -3 15 5.30 0.70 -8 -3 15 1.40 0.60 8 -3 -15 0.30 0.70 8 -3 -15 2.50 0.60 8 3 -15 1.30 0.70 -8 3 15 1.30 0.60 7 -3 -15 1.50 0.60 -7 -3 15 1.50 0.60 7 -3 -15 1.00 0.70 -7 3 15 1.80 0.80 7 3 -15 1.70 0.80 6 -3 -15 16.90 1.40 -6 -3 15 13.40 1.20 6 -3 -15 15.60 1.60 -6 3 15 20.90 1.70 6 3 -15 18.30 1.70 6 3 -15 12.40 2.30 5 -3 -15 25.00 1.60 -5 -3 15 27.40 1.60 5 3 -15 19.70 2.70 -5 3 15 27.40 1.90 5 3 -15 27.20 2.10 -4 -3 15 27.60 1.70 4 -3 -15 27.20 1.70 4 3 -15 28.50 2.10 4 3 -15 23.60 2.80 -4 3 15 29.60 2.00 3 -3 -15 4.50 0.80 -3 -3 15 6.60 0.90 3 3 -15 6.90 1.80 -3 3 15 5.90 1.00 3 3 -15 8.60 1.30 -2 -3 15 4.70 0.70 2 -3 -15 4.20 0.70 -2 3 15 5.00 1.00 2 3 -15 5.10 1.70 2 3 -15 4.40 1.00 1 -3 -15 32.10 1.70 -1 -3 15 30.60 1.60 1 3 -15 32.10 2.10 1 3 -15 30.40 2.40 -1 3 15 30.30 1.90 0 -3 -15 45.50 2.10 0 -3 15 44.50 2.00 0 3 15 44.20 2.20 0 3 -15 45.00 2.40 0 3 -15 46.90 2.80 -1 -3 -15 4.90 0.70 1 -3 15 3.60 0.60 -1 3 -15 4.80 1.00 -1 3 -15 4.70 0.90 1 3 15 4.70 0.80 2 -3 15 0.60 0.30 -2 -3 -15 0.40 0.40 -2 3 -15 0.60 0.60 -2 3 -15 0.10 0.60 -8 -4 15 4.90 0.60 8 -4 -15 4.60 0.60 8 -4 -15 4.60 1.00 8 4 -15 5.60 1.00 -8 4 15 4.50 0.90 7 -4 -15 11.70 1.00 7 -4 -15 8.70 1.20 -7 -4 15 11.20 1.00 7 4 -15 12.30 1.40 -7 4 15 11.80 1.40 -6 -4 15 5.70 0.80 6 -4 -15 6.80 0.80 6 4 -15 7.40 1.20 -6 4 15 6.30 1.10 -5 -4 15 14.10 1.20 5 -4 -15 15.00 1.10 5 4 -15 14.60 2.50 5 4 -15 14.90 1.60 -5 4 15 13.70 1.40 -4 -4 15 23.20 1.40 4 -4 -15 23.90 1.40 -4 4 15 21.70 1.70 4 4 -15 22.30 1.80 4 4 -15 20.70 2.60 3 -4 -15 0.00 0.40 -3 -4 15 0.40 0.40 3 4 -15 0.40 0.60 -3 4 15 0.40 0.50 3 4 -15 0.20 1.00 -2 -4 15 4.10 0.60 2 -4 -15 3.40 0.60 -2 4 15 3.20 0.80 2 4 -15 4.30 1.50 2 4 -15 4.00 0.90 1 -4 -15 41.70 1.90 -1 -4 15 42.60 1.80 1 4 -15 43.60 2.40 1 4 -15 42.80 2.80 -1 4 15 43.90 2.30 0 -4 -15 40.00 1.80 0 -4 15 41.40 1.70 0 4 15 41.10 2.10 0 4 -15 42.70 2.30 0 4 -15 41.30 2.60 1 -4 15 18.40 1.00 -1 -4 -15 20.10 1.10 -1 4 -15 19.80 1.70 -1 4 -15 20.10 1.50 1 4 15 18.10 1.30 -2 4 -15 18.20 2.10 7 -5 -15 0.20 0.40 -7 -5 15 0.40 0.30 -7 5 15 0.30 0.50 7 5 -15 0.20 0.50 6 -5 -15 1.20 0.40 -6 -5 15 1.00 0.40 -6 5 15 1.40 0.60 6 5 -15 1.70 0.70 5 -5 -15 2.50 0.50 -5 -5 15 2.90 0.50 5 5 -15 2.00 0.80 -5 5 15 3.10 0.80 -4 -5 15 34.10 1.50 4 -5 -15 33.80 1.50 4 5 -15 33.00 2.10 -4 5 15 35.20 2.10 4 5 -15 32.90 3.30 -3 -5 15 132.49 4.30 3 -5 -15 131.89 4.30 3 5 -15 137.39 5.10 -3 5 15 132.09 5.00 3 5 -15 125.89 6.70 -2 -5 15 38.90 1.60 2 -5 -15 40.60 1.70 2 5 -15 40.90 2.30 -2 5 15 40.40 2.20 -1 -5 15 0.00 0.30 1 -5 -15 0.20 0.30 -1 5 15 0.10 0.50 1 5 -15 0.50 0.70 1 5 -15 0.10 0.50 0 -5 15 3.70 0.40 0 -5 -15 4.00 0.50 0 5 15 4.10 0.80 0 5 -15 3.30 0.80 0 5 -15 4.90 1.10 -1 5 -15 0.40 0.60 -5 6 15 29.00 1.80 5 6 -15 29.30 1.90 -4 6 15 25.50 1.70 4 6 -15 26.50 1.80 3 6 -15 7.80 1.00 -3 6 15 8.00 1.10 2 6 -15 -0.10 0.50 -2 6 15 0.40 0.50 1 6 -15 37.50 2.30 -1 6 15 33.80 1.90 0 6 -15 55.49 2.70 8 0 -16 1.30 0.50 -7 0 16 12.30 1.20 7 0 -16 10.30 1.10 6 0 -16 1.70 0.60 -6 0 16 1.50 0.60 -5 0 16 14.30 1.30 -5 0 16 14.20 1.30 5 0 -16 16.30 1.40 -4 0 16 0.30 0.50 4 0 -16 0.60 0.60 -4 0 16 0.30 0.50 4 0 -16 0.40 0.50 3 0 -16 -0.10 0.50 -3 0 16 0.50 0.50 3 0 -16 0.50 0.50 2 0 -16 8.60 1.00 -2 0 16 10.50 1.10 2 0 -16 11.50 1.10 1 0 -16 63.89 2.90 1 0 -16 63.49 2.60 -1 0 16 65.09 2.60 0 0 16 1.50 0.50 0 0 -16 1.70 0.50 1 0 16 4.40 0.60 -8 -1 16 18.30 1.30 8 -1 -16 18.50 1.20 -7 -1 16 74.69 2.90 7 -1 -16 76.09 2.90 7 1 -16 70.09 2.90 -7 1 16 72.59 3.00 -7 1 16 71.99 2.90 -6 -1 16 97.09 3.60 6 -1 -16 98.39 3.60 -6 1 16 86.79 3.50 6 1 -16 92.89 3.60 -6 1 16 95.89 3.60 6 1 -16 94.49 3.60 5 -1 -16 170.58 5.60 -5 -1 16 172.18 5.60 5 1 -16 166.28 5.60 5 1 -16 164.28 5.80 -5 1 16 147.39 5.50 -5 1 16 168.78 5.70 4 -1 -16 133.99 4.60 -4 -1 16 130.09 4.60 -4 1 16 134.09 4.70 4 1 -16 125.79 4.60 4 1 -16 129.29 4.80 -4 1 16 127.39 4.60 3 -1 -16 57.89 2.50 -3 -1 16 57.49 2.50 -3 1 16 53.99 2.40 3 1 -16 54.99 2.70 3 1 -16 55.19 2.50 -3 1 16 54.69 2.50 -2 -1 16 38.60 1.90 2 -1 -16 37.70 1.90 2 1 -16 34.10 1.90 2 1 -16 36.20 2.00 -2 1 16 33.50 1.80 -2 1 16 39.20 1.90 -1 -1 16 6.10 0.80 1 -1 -16 7.30 0.90 1 1 -16 5.80 1.00 -1 1 16 6.90 0.80 -1 1 16 6.80 0.80 1 1 -16 7.10 1.00 1 1 -16 5.60 1.10 0 -1 -16 -0.30 0.40 0 -1 16 -0.10 0.40 0 1 -16 -0.30 0.40 0 1 16 0.20 0.40 0 1 -16 -0.10 0.60 1 -1 16 2.70 0.50 -1 -1 -16 1.60 0.50 -8 -2 16 4.20 0.60 8 -2 -16 4.30 0.70 -7 -2 16 13.50 1.20 7 -2 -16 15.20 1.10 -7 2 16 13.10 1.20 -6 -2 16 0.20 0.50 6 -2 -16 0.70 0.50 -6 2 16 -0.20 0.50 6 2 -16 0.40 0.50 5 -2 -16 1.00 0.60 -5 -2 16 1.20 0.60 5 2 -16 2.00 0.70 -5 2 16 1.50 0.60 -4 -2 16 0.00 0.50 4 -2 -16 1.10 0.60 -4 2 16 0.50 0.50 4 2 -16 0.30 0.60 -3 -2 16 16.80 1.30 3 -2 -16 15.80 1.30 3 2 -16 16.70 1.80 3 2 -16 15.40 1.50 -3 2 16 17.10 1.40 -2 -2 16 62.19 2.50 2 -2 -16 61.99 2.50 2 2 -16 59.99 3.10 2 2 -16 59.19 2.80 -2 2 16 61.09 2.60 -1 -2 16 15.70 1.10 1 -2 -16 16.70 1.20 1 2 -16 14.40 1.70 -1 2 16 15.50 1.20 1 2 -16 15.40 1.30 0 -2 -16 1.20 0.40 0 -2 16 1.50 0.40 0 2 -16 2.10 0.80 0 2 -16 1.80 0.60 1 -2 16 -0.20 0.30 -1 -2 -16 0.30 0.50 -7 -3 16 37.00 1.70 7 -3 -16 36.10 1.60 -7 3 16 35.40 2.40 6 -3 -16 30.40 1.50 -6 -3 16 28.20 1.50 -6 3 16 28.70 1.70 6 3 -16 28.50 1.80 -5 -3 16 25.60 1.50 5 -3 -16 26.60 1.50 5 3 -16 27.90 1.80 -5 3 16 25.50 1.70 4 -3 -16 7.80 0.90 -4 -3 16 7.90 0.80 4 3 -16 7.90 1.10 -4 3 16 8.50 1.10 3 -3 -16 37.10 1.80 -3 -3 16 38.40 1.70 -3 3 16 35.90 2.00 3 3 -16 37.10 2.10 2 -3 -16 129.19 4.40 -2 -3 16 131.29 4.40 2 3 -16 132.79 5.20 -2 3 16 130.49 4.70 2 3 -16 136.49 4.90 1 -3 -16 43.20 1.90 -1 -3 16 43.60 1.80 1 3 -16 44.00 2.20 1 3 -16 42.20 2.40 -1 3 16 42.10 2.00 0 -3 16 3.50 0.50 0 -3 -16 3.90 0.60 0 3 -16 3.80 0.90 -6 -4 16 0.70 0.40 6 -4 -16 0.70 0.40 -6 4 16 0.70 0.50 6 4 -16 0.50 0.50 -5 -4 16 4.30 0.60 5 -4 -16 3.40 0.50 -5 4 16 2.40 0.60 5 4 -16 3.10 0.70 4 -4 -16 24.00 1.30 -4 -4 16 25.10 1.30 4 4 -16 25.20 1.70 -4 4 16 26.00 1.70 -3 -4 16 -0.10 0.30 3 -4 -16 0.50 0.40 -3 4 16 0.20 0.50 3 4 -16 0.00 0.50 2 -4 -16 3.90 0.60 -2 -4 16 4.50 0.50 -2 4 16 3.80 0.70 2 4 -16 5.60 1.10 2 4 -16 4.50 0.80 -1 -4 16 0.30 0.30 1 -4 -16 0.00 0.30 1 4 -16 0.00 0.60 -1 4 16 0.00 0.70 1 4 -16 0.30 0.50 2 5 -16 18.30 1.70 5 0 -17 0.20 0.40 -5 0 17 0.10 0.40 -4 0 17 0.20 0.40 4 0 -17 0.10 0.40 3 0 -17 0.10 0.40 -3 0 17 0.50 0.40 -2 0 17 0.50 0.40 6 -1 -17 18.20 1.20 -6 -1 17 19.90 1.60 -5 -1 17 25.50 1.40 5 -1 -17 23.60 1.40 4 -1 -17 37.00 1.80 -4 -1 17 36.10 1.70 -3 -1 17 28.20 1.40 3 -1 -17 25.60 1.40 -2 -1 17 0.40 0.40 2 -1 -17 1.00 0.40 -5 -2 17 26.40 1.40 5 -2 -17 26.80 1.40 4 -2 -17 17.40 1.10 -4 -2 17 17.50 1.10 -3 -2 17 72.99 2.60 3 -2 -17 72.49 2.70 2 -2 -17 25.40 1.30 -2 -2 17 26.50 1.30 4 -3 -17 0.50 0.40 -4 -3 17 0.60 0.50 3 -3 -17 2.30 0.60 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 45695 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_I_CCDC2 _database_code_depnum_ccdc_archive 'CCDC 1875542' _audit_update_record ; 2018-10-26 deposited with the CCDC. 2018-12-12 downloaded from the CCDC. ; _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C16 H9 F2 N O2 S' _chemical_formula_sum 'C16 H9 F2 N O2 S' _chemical_formula_iupac ? _chemical_formula_weight 317.30 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.0083(10) _cell_length_b 8.7108(6) _cell_length_c 11.5419(8) _cell_angle_alpha 90 _cell_angle_beta 105.733(2) _cell_angle_gamma 90 _cell_volume 1355.62(16) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2755 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 67.13 _cell_measurement_temperature 296.(2) _exptl_crystal_description block _exptl_crystal_colour 'clear colourless' _exptl_crystal_size_max 0.521 _exptl_crystal_size_mid 0.395 _exptl_crystal_size_min 0.293 _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 2.417 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/4 (Bruker AXS Inc.)' _exptl_absorpt_correction_T_min 0.6190 _exptl_absorpt_correction_T_max 00.7529 _exptl_special_details ; ; _diffrn_ambient_temperature 296.(2) _diffrn_source 'Incoatec Microfocus X-ray Source I\mS' _diffrn_source_type microfocus _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_monochromator 'Incoatec Montel Multilayer Mirror' _diffrn_measurement_device_type 'Bruker AXS Kappa APEX II DUO' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 15370 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_unetI/netI 0.0194 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 67.13 _diffrn_reflns_theta_full 67.13 _diffrn_measured_fraction_theta_max 0.967 _diffrn_measured_fraction_theta_full 0.967 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 6 _refine_special_details ; ; _reflns_number_total 2344 _reflns_number_gt 2299 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_gt 0.0920 _refine_ls_wR_factor_ref 0.0927 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_number_reflns 2344 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.3012P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.245 _refine_diff_density_min -0.205 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ? _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.21938(8) 0.84113(14) 0.27877(12) 0.0608(3) Uani d . . . 1 . . N N2 0.31365(9) 0.82273(16) 0.35939(12) 0.0491(3) Uani d . . . 1 . . C C3 0.36485(10) 0.72042(16) 0.32377(12) 0.0401(3) Uani d . . . 1 . . S S4 0.30739(3) 0.62456(5) 0.18984(3) 0.05135(16) Uani d . . . 1 . . C C5 0.19324(11) 0.72470(18) 0.18534(13) 0.0461(4) Uani d . . . 1 . . C C6 0.46783(10) 0.69062(16) 0.39360(12) 0.0398(3) Uani d . . . 1 . . C C7 0.52710(11) 0.58220(18) 0.36016(14) 0.0468(3) Uani d . . . 1 . . C C8 0.62275(12) 0.5513(2) 0.42701(16) 0.0567(4) Uani d . . . 1 . . H H8 0.6602 0.4773 0.4012 0.068 Uiso calc U . R 1 . . C C9 0.66204(12) 0.6301(2) 0.53146(16) 0.0561(4) Uani d . . . 1 . . H H9 0.7262 0.6106 0.5782 0.067 Uiso calc U . R 1 . . C C10 0.60405(12) 0.7390(2) 0.56525(14) 0.0537(4) Uani d . . . 1 . . C C11 0.50915(12) 0.77203(18) 0.49990(14) 0.0495(4) Uani d . . . 1 . . H H11 0.4727 0.8475 0.5258 0.059 Uiso calc U . R 1 . . F F12 0.49066(7) 0.49952(13) 0.25855(10) 0.0689(3) Uani d . . . 1 . . F F13 0.64282(9) 0.81626(17) 0.66934(10) 0.0849(4) Uani d . . . 1 . . C C14 0.11414(11) 0.62005(18) 0.21701(13) 0.0451(3) Uani d . . . 1 . . C C15 0.02086(11) 0.64572(17) 0.12530(13) 0.0421(3) Uani d . . . 1 . . C C16 0.03522(11) 0.74726(18) 0.03909(13) 0.0455(3) Uani d . . . 1 . . C C17 0.14160(12) 0.7977(2) 0.06469(15) 0.0549(4) Uani d . . . 1 . . H H17A 0.1466 0.9087 0.0695 0.066 Uiso calc U . R 1 . . H H17B 0.1707 0.7621 0.0023 0.066 Uiso calc U . R 1 . . O O18 0.13011(9) 0.53861(16) 0.30499(11) 0.0660(3) Uani d . . . 1 . . C C19 -0.07165(12) 0.5816(2) 0.11833(15) 0.0520(4) Uani d . . . 1 . . H H19 -0.08 0.5131 0.1766 0.062 Uiso calc U . R 1 . . C C20 -0.14971(12) 0.6220(2) 0.02359(17) 0.0614(5) Uani d . . . 1 . . H H20 -0.2125 0.5822 0.0177 0.074 Uiso calc U . R 1 . . C C21 -0.13574(13) 0.7224(2) -0.06390(17) 0.0677(5) Uani d . . . 1 . . H H21 -0.1894 0.7474 -0.1285 0.081 Uiso calc U . R 1 . . C C22 -0.04414(13) 0.7857(2) -0.05734(15) 0.0596(4) Uani d . . . 1 . . H H22 -0.0359 0.8529 -0.1165 0.072 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0382(6) 0.0647(7) 0.0741(8) 0.0105(5) 0.0058(5) -0.0216(6) N2 0.0378(6) 0.0535(7) 0.0540(7) 0.0020(6) 0.0091(5) -0.0093(6) C3 0.0354(7) 0.0441(7) 0.0416(7) -0.0022(6) 0.0120(6) -0.0017(6) S4 0.0355(2) 0.0660(3) 0.0494(2) 0.00683(15) 0.00608(16) -0.01578(17) C5 0.0346(7) 0.0539(8) 0.0484(8) 0.0038(6) 0.0090(6) -0.0033(6) C6 0.0343(7) 0.0435(7) 0.0419(7) -0.0034(6) 0.0109(6) 0.0039(6) C7 0.0392(8) 0.0514(8) 0.0494(8) -0.0007(6) 0.0113(6) -0.0015(7) C8 0.0392(8) 0.0602(10) 0.0699(11) 0.0064(7) 0.0135(7) 0.0051(8) C9 0.0371(8) 0.0626(10) 0.0627(10) -0.0054(7) 0.0035(7) 0.0173(8) C10 0.0467(9) 0.0601(9) 0.0475(9) -0.0146(7) 0.0010(7) 0.0027(7) C11 0.0446(8) 0.0520(9) 0.0505(8) -0.0042(7) 0.0103(7) -0.0032(7) F12 0.0515(6) 0.0825(7) 0.0689(6) 0.0134(5) 0.0097(5) -0.0266(5) F13 0.0697(7) 0.1006(9) 0.0672(7) -0.0092(7) -0.0107(6) -0.0202(6) C14 0.0416(8) 0.0537(8) 0.0404(8) 0.0048(6) 0.0116(6) 0.0003(6) C15 0.0365(7) 0.0490(8) 0.0409(7) 0.0031(6) 0.0107(6) -0.0051(6) C16 0.0389(8) 0.0537(8) 0.0439(8) 0.0091(6) 0.0110(6) 0.0001(6) C17 0.0423(8) 0.0649(10) 0.0575(9) 0.0037(7) 0.0136(7) 0.0139(8) O18 0.0586(7) 0.0857(9) 0.0519(7) 0.0052(6) 0.0117(5) 0.0212(6) C19 0.0440(8) 0.0577(9) 0.0573(9) -0.0041(7) 0.0189(7) -0.0130(7) C20 0.0359(8) 0.0759(12) 0.0703(11) -0.0007(7) 0.0108(8) -0.0264(9) C21 0.0435(9) 0.0877(13) 0.0607(11) 0.0218(9) -0.0051(8) -0.0178(10) C22 0.0508(10) 0.0757(11) 0.0486(9) 0.0211(8) 0.0071(7) 0.0067(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 N2 . 1.4032(17) ? O1 C5 . 1.4530(19) ? N2 C3 . 1.2796(19) ? C3 C6 . 1.472(2) ? C3 S4 . 1.7492(14) ? S4 C5 . 1.8099(15) ? C5 C17 . 1.523(2) ? C5 C14 . 1.553(2) ? C6 C7 . 1.380(2) ? C6 C11 . 1.399(2) ? C7 F12 . 1.3528(19) ? C7 C8 . 1.379(2) ? C8 C9 . 1.367(3) ? C8 H8 . 0.93 ? C9 C10 . 1.372(3) ? C9 H9 . 0.93 ? C10 F13 . 1.3553(19) ? C10 C11 . 1.369(2) ? C11 H11 . 0.93 ? C14 O18 . 1.2088(19) ? C14 C15 . 1.459(2) ? C15 C16 . 1.386(2) ? C15 C19 . 1.393(2) ? C16 C22 . 1.384(2) ? C16 C17 . 1.504(2) ? C17 H17A . 0.97 ? C17 H17B . 0.97 ? C19 C20 . 1.366(3) ? C19 H19 . 0.93 ? C20 C21 . 1.389(3) ? C20 H20 . 0.93 ? C21 C22 . 1.380(3) ? C21 H21 . 0.93 ? C22 H22 . 0.93 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 O1 C5 . . 114.52(11) ? C3 N2 O1 . . 112.03(12) ? N2 C3 C6 . . 119.89(13) ? N2 C3 S4 . . 116.92(11) ? C6 C3 S4 . . 123.18(10) ? C3 S4 C5 . . 89.23(7) ? O1 C5 C17 . . 110.41(13) ? O1 C5 C14 . . 106.70(12) ? C17 C5 C14 . . 105.54(12) ? O1 C5 S4 . . 105.79(9) ? C17 C5 S4 . . 115.10(11) ? C14 C5 S4 . . 113.05(11) ? C7 C6 C11 . . 117.06(14) ? C7 C6 C3 . . 122.83(13) ? C11 C6 C3 . . 120.10(13) ? F12 C7 C8 . . 117.52(14) ? F12 C7 C6 . . 119.51(13) ? C8 C7 C6 . . 122.96(15) ? C9 C8 C7 . . 119.54(16) ? C9 C8 H8 . . 120.2 ? C7 C8 H8 . . 120.2 ? C8 C9 C10 . . 118.05(15) ? C8 C9 H9 . . 121.0 ? C10 C9 H9 . . 121.0 ? F13 C10 C11 . . 118.68(16) ? F13 C10 C9 . . 117.98(15) ? C11 C10 C9 . . 123.34(16) ? C10 C11 C6 . . 119.05(15) ? C10 C11 H11 . . 120.5 ? C6 C11 H11 . . 120.5 ? O18 C14 C15 . . 128.67(15) ? O18 C14 C5 . . 124.12(14) ? C15 C14 C5 . . 107.17(12) ? C16 C15 C19 . . 121.87(15) ? C16 C15 C14 . . 110.06(13) ? C19 C15 C14 . . 128.07(14) ? C22 C16 C15 . . 119.37(15) ? C22 C16 C17 . . 128.63(15) ? C15 C16 C17 . . 111.97(13) ? C16 C17 C5 . . 104.91(12) ? C16 C17 H17A . . 110.8 ? C5 C17 H17A . . 110.8 ? C16 C17 H17B . . 110.8 ? C5 C17 H17B . . 110.8 ? H17A C17 H17B . . 108.8 ? C20 C19 C15 . . 118.21(17) ? C20 C19 H19 . . 120.9 ? C15 C19 H19 . . 120.9 ? C19 C20 C21 . . 120.28(17) ? C19 C20 H20 . . 119.9 ? C21 C20 H20 . . 119.9 ? C22 C21 C20 . . 121.60(16) ? C22 C21 H21 . . 119.2 ? C20 C21 H21 . . 119.2 ? C21 C22 C16 . . 118.65(17) ? C21 C22 H22 . . 120.7 ? C16 C22 H22 . . 120.7 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C5 O1 N2 C3 . . . . 10.33(19) ? O1 N2 C3 C6 . . . . 176.85(12) ? O1 N2 C3 S4 . . . . -1.90(18) ? N2 C3 S4 C5 . . . . -5.05(13) ? C6 C3 S4 C5 . . . . 176.25(12) ? N2 O1 C5 C17 . . . . -138.37(13) ? N2 O1 C5 C14 . . . . 107.42(14) ? N2 O1 C5 S4 . . . . -13.22(16) ? C3 S4 C5 O1 . . . . 9.73(11) ? C3 S4 C5 C17 . . . . 131.93(13) ? C3 S4 C5 C14 . . . . -106.69(11) ? N2 C3 C6 C7 . . . . -179.90(14) ? S4 C3 C6 C7 . . . . -1.2(2) ? N2 C3 C6 C11 . . . . 1.2(2) ? S4 C3 C6 C11 . . . . 179.82(11) ? C11 C6 C7 F12 . . . . 179.59(13) ? C3 C6 C7 F12 . . . . 0.6(2) ? C11 C6 C7 C8 . . . . 0.7(2) ? C3 C6 C7 C8 . . . . -178.29(14) ? F12 C7 C8 C9 . . . . -178.86(15) ? C6 C7 C8 C9 . . . . 0.1(3) ? C7 C8 C9 C10 . . . . -0.5(2) ? C8 C9 C10 F13 . . . . 179.47(15) ? C8 C9 C10 C11 . . . . 0.2(3) ? F13 C10 C11 C6 . . . . -178.70(14) ? C9 C10 C11 C6 . . . . 0.6(2) ? C7 C6 C11 C10 . . . . -1.0(2) ? C3 C6 C11 C10 . . . . 178.02(13) ? O1 C5 C14 O18 . . . . -65.64(19) ? C17 C5 C14 O18 . . . . 176.88(16) ? S4 C5 C14 O18 . . . . 50.23(19) ? O1 C5 C14 C15 . . . . 111.99(13) ? C17 C5 C14 C15 . . . . -5.49(16) ? S4 C5 C14 C15 . . . . -132.14(11) ? O18 C14 C15 C16 . . . . -179.58(16) ? C5 C14 C15 C16 . . . . 2.93(16) ? O18 C14 C15 C19 . . . . 0.0(3) ? C5 C14 C15 C19 . . . . -177.52(14) ? C19 C15 C16 C22 . . . . -0.5(2) ? C14 C15 C16 C22 . . . . 179.13(14) ? C19 C15 C16 C17 . . . . -178.66(14) ? C14 C15 C16 C17 . . . . 0.93(18) ? C22 C16 C17 C5 . . . . 177.60(16) ? C15 C16 C17 C5 . . . . -4.41(18) ? O1 C5 C17 C16 . . . . -109.13(14) ? C14 C5 C17 C16 . . . . 5.82(16) ? S4 C5 C17 C16 . . . . 131.20(12) ? C16 C15 C19 C20 . . . . -0.4(2) ? C14 C15 C19 C20 . . . . -179.93(14) ? C15 C19 C20 C21 . . . . 1.1(2) ? C19 C20 C21 C22 . . . . -1.0(3) ? C20 C21 C22 C16 . . . . 0.1(3) ? C15 C16 C22 C21 . . . . 0.6(2) ? C17 C16 C22 C21 . . . . 178.47(16) ? _shelx_res_file ; TITL cu_ARM_PmC_UK_5_474_0ma_a.res in P2(1)/c CELL 1.54178 14.0083 8.7108 11.5419 90.000 105.733 90.000 ZERR 4.000 0.0010 0.0006 0.0008 0.000 0.002 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H F N O S UNIT 64 36 8 4 8 4 L.S. 10 ACTA BOND $H FMAP 2 PLAN 5 CONF SIZE 0.293 0.395 0.521 TEMP 23.000 WGHT 0.050600 0.301200 FVAR 1.17766 O1 5 0.219382 0.841127 0.278766 11.00000 0.03819 0.06469 = 0.07405 -0.02163 0.00585 0.01050 N2 4 0.313650 0.822734 0.359386 11.00000 0.03782 0.05347 = 0.05402 -0.00930 0.00907 0.00203 C3 1 0.364845 0.720422 0.323772 11.00000 0.03541 0.04411 = 0.04157 -0.00166 0.01204 -0.00218 S4 6 0.307392 0.624556 0.189845 11.00000 0.03547 0.06597 = 0.04943 -0.01578 0.00608 0.00683 C5 1 0.193238 0.724701 0.185341 11.00000 0.03464 0.05394 = 0.04843 -0.00334 0.00898 0.00381 C6 1 0.467834 0.690622 0.393595 11.00000 0.03434 0.04349 = 0.04192 0.00389 0.01089 -0.00345 C7 1 0.527104 0.582196 0.360158 11.00000 0.03919 0.05141 = 0.04945 -0.00152 0.01128 -0.00067 C8 1 0.622750 0.551282 0.427009 11.00000 0.03919 0.06023 = 0.06993 0.00509 0.01345 0.00639 AFIX 43 H8 2 0.660248 0.477292 0.401200 11.00000 -1.20000 AFIX 0 C9 1 0.662042 0.630149 0.531459 11.00000 0.03715 0.06259 = 0.06273 0.01734 0.00354 -0.00541 AFIX 43 H9 2 0.726187 0.610597 0.578248 11.00000 -1.20000 AFIX 0 C10 1 0.604051 0.739039 0.565254 11.00000 0.04674 0.06012 = 0.04751 0.00274 0.00104 -0.01459 C11 1 0.509147 0.772031 0.499900 11.00000 0.04463 0.05198 = 0.05048 -0.00317 0.01025 -0.00417 AFIX 43 H11 2 0.472673 0.847459 0.525794 11.00000 -1.20000 AFIX 0 F12 3 0.490657 0.499518 0.258551 11.00000 0.05150 0.08252 = 0.06888 -0.02659 0.00972 0.01341 F13 3 0.642816 0.816264 0.669336 11.00000 0.06969 0.10056 = 0.06719 -0.02020 -0.01075 -0.00916 C14 1 0.114142 0.620049 0.217006 11.00000 0.04156 0.05368 = 0.04041 0.00034 0.01165 0.00476 C15 1 0.020863 0.645717 0.125303 11.00000 0.03654 0.04898 = 0.04086 -0.00506 0.01072 0.00310 C16 1 0.035215 0.747263 0.039089 11.00000 0.03888 0.05373 = 0.04391 0.00010 0.01103 0.00913 C17 1 0.141604 0.797679 0.064687 11.00000 0.04232 0.06489 = 0.05747 0.01387 0.01364 0.00370 AFIX 23 H17A 2 0.146600 0.908686 0.069512 11.00000 -1.20000 H17B 2 0.170720 0.762082 0.002266 11.00000 -1.20000 AFIX 0 O18 5 0.130107 0.538615 0.304989 11.00000 0.05858 0.08568 = 0.05187 0.02121 0.01165 0.00519 C19 1 -0.071648 0.581585 0.118331 11.00000 0.04403 0.05771 = 0.05725 -0.01303 0.01889 -0.00411 AFIX 43 H19 2 -0.080043 0.513090 0.176593 11.00000 -1.20000 AFIX 0 C20 1 -0.149707 0.622041 0.023586 11.00000 0.03592 0.07585 = 0.07035 -0.02639 0.01084 -0.00066 AFIX 43 H20 2 -0.212451 0.582228 0.017663 11.00000 -1.20000 AFIX 0 C21 1 -0.135738 0.722356 -0.063896 11.00000 0.04346 0.08767 = 0.06072 -0.01777 -0.00510 0.02183 AFIX 43 H21 2 -0.189424 0.747448 -0.128472 11.00000 -1.20000 AFIX 0 C22 1 -0.044142 0.785706 -0.057341 11.00000 0.05079 0.07566 = 0.04858 0.00671 0.00709 0.02107 AFIX 43 H22 2 -0.035897 0.852872 -0.116516 11.00000 -1.20000 AFIX 0 HKLF 4 REM cu_ARM_PmC_UK_5_474_0ma_a.res in P2(1)/c REM R1 = 0.0328 for 2299 Fo > 4sig(Fo) and 0.0335 for all 2344 data REM 199 parameters refined using 0 restraints END WGHT 0.0506 0.3009 REM Highest difference peak 0.245, deepest hole -0.205, 1-sigma level 0.036 Q1 1 0.1587 0.6734 0.2049 11.00000 0.05 0.25 Q2 1 0.0194 0.7159 0.0945 11.00000 0.05 0.19 Q3 1 0.5033 0.6662 0.3581 11.00000 0.05 0.17 Q4 1 -0.0155 0.6029 0.1124 11.00000 0.05 0.16 Q5 1 0.2363 0.6810 0.1864 11.00000 0.05 0.15 ; _shelx_res_checksum 59433 _shelx_hkl_file ; 0 0 -3 3.00 0.30 0 0 -4 53.19 2.00 0 0 -4 44.00 2.40 0 0 -5 0.00 0.20 0 0 -6 712.53 27.00 0 0 -7 1.20 0.20 0 0 -8 1476.65 50.79 0 0 -8 1410.66 52.09 0 0 -8 1354.66 50.69 0 0 -8 1331.67 51.39 0 0 -8 1367.66 50.79 0 0 -9 1.10 0.20 0 0 -9 0.80 0.50 0 0 -9 0.40 0.20 0 0 -10 45.30 2.00 0 0 -10 44.40 2.70 0 0 -10 45.20 2.00 0 0 -10 46.50 2.00 0 0 -10 45.70 1.90 0 0 -10 46.10 2.00 0 0 -10 43.70 1.90 0 0 -11 1.30 0.30 0 0 -11 1.30 0.30 0 0 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1.00 2 8 -8 14.30 0.80 2 8 -7 0.30 0.40 2 8 -7 0.20 0.20 2 8 -7 0.00 0.30 2 8 -6 8.80 0.80 2 8 -6 8.80 1.10 2 8 -6 9.80 0.90 2 8 -5 82.79 3.90 2 8 -5 78.79 3.60 2 8 -5 80.79 3.60 2 8 -5 83.89 3.70 2 8 -4 213.28 8.60 2 8 -4 211.08 8.60 2 8 -3 206.58 8.40 2 8 -3 197.28 8.30 2 8 -2 2.30 0.80 2 8 -1 32.00 2.30 -2 -8 0 11.30 1.30 2 8 0 12.20 1.50 -2 -8 -1 27.30 2.00 2 8 1 28.90 2.20 -2 -8 -2 36.70 2.30 2 8 2 32.90 2.40 -2 -8 -3 0.00 0.50 -2 -8 -4 10.80 1.20 -2 -8 -5 50.69 2.60 -2 -8 -5 50.49 2.70 -2 -8 -6 29.10 1.60 -2 -8 -6 30.20 1.80 -2 -8 -6 28.50 1.60 -2 -8 -7 0.70 0.40 -2 -8 -7 1.40 0.30 2 7 -9 1.30 0.50 2 7 -9 1.70 0.40 2 7 -8 64.79 2.90 2 7 -8 60.69 2.90 2 7 -8 64.29 2.70 2 7 -7 30.20 1.80 2 7 -7 28.20 1.80 2 7 -7 29.40 1.60 2 7 -7 28.60 1.40 2 7 -6 25.00 1.50 2 7 -6 26.00 1.80 2 7 -6 26.80 1.60 2 7 -5 226.48 8.90 2 7 -5 229.78 9.10 2 7 -5 215.98 8.90 2 7 -5 221.38 8.80 2 7 -4 356.56 14.00 2 7 -4 352.76 14.10 2 7 -4 365.26 13.90 2 7 -3 25.70 1.80 2 7 -3 28.50 2.00 2 7 -2 268.77 10.90 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654.23 24.30 2 6 -5 392.96 14.70 2 6 -5 384.56 14.60 2 6 -5 370.66 14.70 2 6 -5 396.26 14.90 2 6 -5 375.16 14.80 2 6 -4 4.50 0.80 2 6 -4 4.40 0.70 2 6 -4 3.90 0.60 2 6 -4 4.50 0.70 2 6 -3 182.48 7.20 2 6 -3 170.68 7.30 2 6 -3 178.98 7.30 2 6 -2 10.90 1.80 2 6 -2 10.00 1.10 2 6 -2 9.20 1.00 2 6 -2 9.30 1.10 2 6 -1 21.30 1.60 2 6 -1 25.90 1.70 2 6 -1 23.20 2.80 2 6 -1 22.50 1.80 -2 -6 0 164.68 7.70 2 6 0 169.28 7.20 2 6 0 175.38 9.80 2 6 0 178.88 7.80 2 6 0 178.48 7.20 -2 -6 -1 179.78 7.60 -2 -6 -1 191.18 8.10 -2 -6 -1 193.78 10.20 2 6 1 169.18 10.80 2 6 1 182.38 7.70 2 6 1 190.98 7.70 2 6 1 185.68 8.30 -2 -6 -2 394.26 15.60 -2 -6 -2 383.36 17.60 2 6 2 406.16 15.40 -2 -6 -3 14.00 1.30 -2 -6 -3 15.30 1.40 2 6 3 14.70 1.50 -2 -6 -4 33.20 2.00 2 6 4 30.80 2.20 -2 -6 -5 304.17 11.50 -2 -6 -5 259.97 12.10 -2 -6 -5 304.77 11.40 2 6 5 300.47 11.90 -2 -6 -6 12.90 1.40 -2 -6 -6 13.20 1.40 -2 -6 -6 12.10 1.10 -2 -6 -6 12.80 1.10 -2 -6 -7 220.88 8.60 -2 -6 -7 201.88 8.70 -2 -6 -7 210.88 8.20 -2 -6 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1.20 2 4 -5 11.60 0.90 2 4 -5 12.80 1.50 2 4 -5 10.50 0.80 2 4 -4 2890.71 108.49 2 4 -4 2924.71 108.59 2 4 -4 2982.30 111.39 2 4 -4 3068.59 109.29 2 4 -3 2522.75 92.19 2 4 -3 2449.16 89.09 2 4 -3 2332.37 89.19 2 4 -2 479.75 18.70 2 4 -2 462.25 18.60 2 4 -2 455.15 17.40 2 4 -2 460.95 17.50 2 4 -1 45.40 2.20 2 4 -1 49.40 3.40 2 4 -1 48.70 2.50 -2 -4 0 4070.39 155.98 -2 -4 0 4021.50 158.48 2 4 0 4406.26 155.98 2 4 0 4181.38 160.98 2 4 0 4415.86 155.28 -2 -4 -1 1328.97 45.50 -2 -4 -1 1259.17 47.10 2 4 1 1244.98 45.10 2 4 1 1163.98 47.40 2 4 1 1128.49 45.60 -2 -4 -2 1678.03 62.79 -2 -4 -2 1610.64 60.79 -2 -4 -3 966.90 36.70 -2 -4 -3 950.40 35.50 -2 -4 -4 1890.81 70.19 -2 -4 -4 1986.20 70.29 -2 -4 -4 1783.02 70.09 -2 -4 -4 1982.20 69.99 -2 -4 -5 895.71 33.20 -2 -4 -5 876.01 33.00 -2 -4 -5 938.81 33.10 -2 -4 -5 872.31 33.20 -2 -4 -5 903.31 33.00 -2 -4 -5 873.71 33.20 -2 -4 -6 277.47 11.10 -2 -4 -6 289.67 11.20 -2 -4 -6 278.57 10.80 -2 -4 -6 289.77 11.10 -2 -4 -6 287.77 10.90 -2 -4 -6 273.57 12.80 -2 -4 -6 287.47 10.90 -2 -4 -6 285.27 10.80 -2 -4 -7 50.79 2.70 -2 -4 -7 49.80 2.60 -2 -4 -7 49.30 2.40 -2 -4 -7 51.59 2.60 -2 -4 -7 48.90 3.90 -2 -4 -7 55.59 2.30 -2 -4 -7 49.30 2.20 -2 -4 -8 189.08 8.50 -2 -4 -8 216.78 8.20 -2 -4 -8 220.48 8.10 -2 -4 -8 217.28 8.70 -2 -4 -8 213.58 8.50 -2 -4 -8 208.58 8.40 -2 -4 -9 0.70 0.40 -2 -4 -9 0.30 0.30 -2 -4 -9 0.30 0.40 -2 -4 -9 -0.10 0.50 -2 -4 -9 0.60 0.40 -2 -4 -10 196.68 8.30 -2 -4 -10 218.88 8.60 -2 -4 -10 219.88 8.30 -2 -4 -10 211.18 7.90 -2 -4 -10 206.78 8.30 -2 -4 -11 104.09 4.30 -2 -4 -11 109.49 4.60 2 3 -12 32.90 1.50 2 3 -12 36.40 1.50 2 3 -11 143.49 5.50 2 3 -11 135.19 5.40 2 3 -11 138.19 5.60 2 3 -11 154.58 5.50 2 3 -11 144.89 5.60 2 3 -10 26.30 1.30 2 3 -10 25.40 1.40 2 3 -10 24.90 1.20 2 3 -10 25.80 1.30 2 3 -10 26.30 1.30 2 3 -9 474.45 18.10 2 3 -9 520.25 18.30 2 3 -9 482.85 18.20 2 3 -9 502.55 18.30 2 3 -9 509.55 18.30 2 3 -9 463.85 18.10 2 3 -9 490.65 18.20 2 3 -9 480.95 18.20 2 3 -8 263.17 9.60 2 3 -8 243.18 9.60 2 3 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13 -1 -6 105.99 5.10 13 -1 -6 116.29 4.70 13 -1 -6 111.29 4.70 13 -1 -6 115.89 4.70 13 -1 -5 659.73 24.40 13 -1 -5 675.83 24.60 13 -1 -5 625.14 24.60 13 -1 -4 94.79 4.30 13 -1 -4 90.49 3.90 13 -1 -3 50.29 2.70 13 -1 -2 61.49 3.20 -13 1 1 151.08 6.50 -13 1 1 154.28 6.60 13 -1 -1 150.08 6.50 -13 1 0 5.60 1.00 -13 1 0 3.30 0.80 13 -1 0 1.80 0.60 -13 1 -1 6.90 1.00 -13 1 -2 3.60 0.70 -13 1 -3 81.39 3.70 -13 1 -4 70.29 2.90 -13 1 -4 62.49 2.90 13 -2 -10 0.10 0.30 13 -2 -10 0.40 0.30 13 -2 -9 10.90 1.10 13 -2 -9 12.90 1.00 13 -2 -9 12.20 1.10 13 -2 -9 12.90 0.70 13 -2 -8 39.90 2.30 13 -2 -8 38.90 1.90 13 -2 -8 41.40 2.00 13 -2 -8 38.30 2.20 13 -2 -7 8.20 0.90 13 -2 -7 8.30 0.80 13 -2 -7 9.50 0.90 13 -2 -7 8.90 1.10 13 -2 -6 53.49 2.60 13 -2 -6 54.19 2.60 13 -2 -6 53.89 2.60 13 -2 -5 32.60 1.90 13 -2 -5 30.10 1.70 13 -2 -5 29.30 1.90 13 -2 -4 150.68 6.30 13 -2 -4 148.79 6.00 13 -2 -3 125.39 5.50 13 -2 -3 130.29 5.20 -13 2 2 163.68 7.10 13 -2 -2 175.58 7.10 13 -2 -2 160.98 6.50 -13 2 1 12.60 1.30 13 -2 -1 13.50 1.30 -13 2 0 30.30 2.00 13 -2 0 31.20 2.00 -13 2 -1 366.76 14.30 -13 2 -1 369.16 14.30 -13 2 -2 4.40 0.70 -13 2 -3 7.20 0.90 -13 2 -4 68.29 2.80 -13 2 -4 61.19 2.80 13 -3 -10 4.20 0.50 13 -3 -9 71.39 3.20 13 -3 -9 70.89 3.10 13 -3 -8 8.30 0.70 13 -3 -8 8.50 1.00 13 -3 -8 8.80 0.80 13 -3 -7 1.10 0.40 13 -3 -7 1.60 0.50 13 -3 -7 0.50 0.50 13 -3 -7 1.30 0.40 13 -3 -6 24.30 1.50 13 -3 -6 25.50 1.50 13 -3 -6 25.00 1.50 13 -3 -5 87.89 3.90 13 -3 -5 86.69 3.70 13 -3 -5 89.89 4.60 13 -3 -4 169.78 6.90 13 -3 -4 183.88 7.30 13 -3 -3 2.90 0.50 13 -3 -3 2.00 0.70 -13 3 2 39.90 2.40 13 -3 -2 42.80 2.10 13 -3 -2 45.40 2.50 -13 3 1 181.68 7.70 13 -3 -1 191.28 7.80 -13 3 0 0.50 0.50 13 -3 0 0.00 0.50 -13 3 -1 0.30 0.40 -13 3 -1 1.00 0.50 -13 3 -2 111.99 4.90 -13 3 -2 114.89 4.90 -13 3 -3 22.00 1.30 -13 3 -3 24.40 1.40 13 -4 -9 47.70 2.20 13 -4 -8 110.99 4.40 13 -4 -8 104.49 4.60 13 -4 -8 105.79 4.20 13 -4 -7 3.00 0.50 13 -4 -7 2.50 0.50 13 -4 -7 2.90 0.40 13 -4 -6 114.39 4.70 13 -4 -6 110.39 4.60 13 -4 -6 110.29 4.60 13 -4 -5 6.10 0.90 13 -4 -5 6.10 0.70 13 -4 -4 147.29 6.00 13 -4 -4 140.19 5.70 13 -4 -3 68.39 3.00 13 -4 -3 69.09 3.30 -13 4 2 21.50 1.60 13 -4 -2 21.70 1.30 13 -4 -2 23.60 1.70 -13 4 1 209.88 8.60 13 -4 -1 212.58 8.60 -13 4 0 620.74 23.10 13 -4 0 604.64 23.20 -13 4 -1 32.70 1.90 -13 4 -2 219.08 8.60 -13 4 -2 219.98 8.60 -13 4 -3 27.30 1.40 13 -5 -8 4.00 0.50 13 -5 -7 1.30 0.40 13 -5 -7 0.60 0.30 13 -5 -6 0.60 0.30 13 -5 -6 1.50 0.40 13 -5 -6 0.70 0.30 13 -5 -5 10.90 0.80 13 -5 -5 10.80 1.00 13 -5 -4 0.30 0.40 13 -5 -4 0.40 0.30 13 -5 -3 6.00 0.70 13 -5 -3 5.30 0.80 -13 5 2 47.90 2.60 13 -5 -2 53.69 2.30 13 -5 -2 52.99 2.70 -13 5 1 29.40 1.80 13 -5 -1 31.00 1.90 -13 5 0 43.90 2.30 -13 5 -1 126.19 5.20 -13 5 -2 0.70 0.30 -13 5 -2 0.70 0.40 13 -6 -6 97.09 3.90 13 -6 -5 4.60 0.70 13 -6 -5 4.70 0.60 13 -6 -4 3.60 0.60 13 -6 -4 3.30 0.50 13 -6 -3 29.40 1.40 13 -6 -3 29.80 1.70 -13 6 2 8.80 1.00 13 -6 -2 9.90 0.80 13 -6 -2 10.10 1.00 -13 6 1 85.39 3.80 13 -6 -1 92.39 3.50 13 -6 -1 86.49 3.80 -13 6 0 5.40 0.70 14 5 -5 44.90 2.10 14 5 -4 108.69 4.50 14 5 -3 53.89 2.60 14 5 -2 64.09 3.00 14 5 -1 92.99 4.00 14 4 -7 22.00 1.10 14 4 -6 2.40 0.40 14 4 -5 16.90 1.10 14 4 -5 16.10 1.10 14 4 -4 85.99 3.80 14 4 -3 15.70 1.30 14 4 -2 494.95 18.80 -14 -4 1 36.10 2.20 14 4 -1 43.80 2.30 -14 -4 0 17.60 1.40 14 4 0 21.00 1.40 -14 -4 -1 8.60 0.90 14 4 1 8.10 1.10 -14 -4 -2 1.10 0.40 14 3 -8 74.29 3.30 14 3 -7 4.80 0.60 14 3 -7 4.40 0.70 14 3 -6 71.19 3.00 14 3 -6 70.99 3.10 14 3 -5 11.50 1.00 14 3 -5 10.00 0.90 14 3 -4 62.09 3.00 14 3 -3 12.60 1.30 14 3 -2 361.16 14.00 -14 -3 1 135.19 6.20 14 3 -1 156.78 6.20 -14 -3 0 17.40 1.50 14 3 0 19.10 1.50 -14 -3 -1 31.00 1.90 14 3 1 30.70 1.90 -14 -3 -2 40.10 2.10 -14 -3 -3 60.89 3.00 14 2 -9 45.20 2.20 14 2 -8 2.40 0.30 14 2 -8 2.50 0.60 14 2 -7 33.70 1.60 14 2 -7 31.10 1.90 14 2 -6 12.40 1.00 14 2 -6 11.30 0.90 14 2 -5 103.79 4.50 14 2 -5 105.79 4.50 14 2 -4 53.89 2.70 14 2 -3 476.65 18.20 14 2 -2 77.09 3.70 -14 -2 1 161.28 7.20 14 2 -1 184.68 7.20 -14 -2 0 21.90 1.70 14 2 0 22.90 1.70 -14 -2 -1 11.70 1.20 -14 -2 -2 37.80 2.10 -14 -2 -3 126.19 5.10 14 1 -9 3.40 0.60 14 1 -8 11.10 1.10 14 1 -8 10.10 0.90 14 1 -8 10.80 0.70 14 1 -7 118.99 5.30 14 1 -7 125.49 5.00 14 1 -6 593.64 21.90 14 1 -6 577.24 21.80 14 1 -5 460.55 17.70 14 1 -5 469.95 17.70 14 1 -4 136.89 5.80 14 1 -3 15.30 1.40 14 1 -2 6.10 0.90 -14 -1 1 42.40 2.50 14 1 -1 43.80 2.50 -14 -1 0 385.36 14.90 14 1 0 383.26 14.90 -14 -1 -1 13.40 1.30 -14 -1 -2 2.20 0.60 -14 -1 -3 24.80 1.50 14 0 -10 4.70 0.50 14 0 -10 4.50 0.90 14 0 -9 0.30 0.30 14 0 -9 0.20 0.30 14 0 -8 7.30 0.60 14 0 -8 6.40 0.80 14 0 -8 7.60 1.00 14 0 -7 0.50 0.30 14 0 -7 0.60 0.50 14 0 -7 0.30 0.40 14 0 -7 -0.10 0.40 14 0 -6 49.30 2.40 14 0 -6 46.50 2.30 14 0 -6 47.00 2.30 14 0 -5 2.70 0.70 14 0 -4 46.90 2.60 14 0 -3 1.70 0.60 14 0 -2 33.00 2.10 -14 0 1 1.20 0.60 14 0 -1 2.20 0.60 -14 0 0 1.10 0.60 14 0 0 1.70 0.60 -14 0 -1 0.30 0.50 -14 0 -2 85.59 3.80 -14 0 -3 0.40 0.40 14 -1 -10 11.40 0.80 14 -1 -9 3.40 0.50 14 -1 -9 3.20 0.60 14 -1 -8 10.70 0.90 14 -1 -8 10.40 0.80 14 -1 -8 10.00 1.10 14 -1 -7 123.39 4.90 14 -1 -7 115.99 5.20 14 -1 -7 123.29 4.90 14 -1 -7 115.59 4.70 14 -1 -6 595.64 22.50 14 -1 -6 616.44 22.50 14 -1 -6 592.94 22.40 14 -1 -5 458.35 17.00 14 -1 -5 444.66 16.70 14 -1 -5 432.76 16.90 14 -1 -4 127.79 5.50 14 -1 -3 15.70 1.50 -14 1 2 8.90 1.10 -14 1 2 10.00 1.40 14 -1 -2 7.90 1.10 -14 1 1 43.90 2.50 14 -1 -1 48.40 2.60 -14 1 0 376.86 14.70 14 -1 0 381.06 14.70 -14 1 -1 13.40 1.20 -14 1 -2 1.80 0.50 -14 1 -3 24.00 1.40 14 -2 -9 48.10 2.20 14 -2 -9 48.30 2.40 14 -2 -8 2.60 0.50 14 -2 -8 1.90 0.50 14 -2 -8 2.30 0.40 14 -2 -7 30.90 1.50 14 -2 -7 32.00 2.10 14 -2 -7 30.50 2.20 14 -2 -7 34.40 1.70 14 -2 -7 33.60 1.70 14 -2 -6 10.40 1.00 14 -2 -6 13.00 1.00 14 -2 -5 101.99 4.50 14 -2 -5 104.89 4.50 14 -2 -5 102.39 4.30 14 -2 -4 51.39 2.30 14 -2 -4 49.10 2.60 14 -2 -3 413.86 16.50 14 -2 -3 467.85 17.00 -14 2 2 70.59 3.60 -14 2 2 71.59 3.60 14 -2 -2 84.19 3.70 -14 2 1 173.18 7.30 -14 2 1 172.88 7.30 14 -2 -1 180.88 7.40 -14 2 0 19.80 1.60 -14 2 0 24.00 1.60 14 -2 0 21.60 1.60 -14 2 -1 15.20 1.30 -14 2 -2 37.10 2.00 -14 2 -3 124.29 5.00 14 -3 -9 1.20 0.30 14 -3 -8 77.89 3.20 14 -3 -8 74.79 3.00 14 -3 -8 72.59 3.50 14 -3 -8 74.89 3.50 14 -3 -7 4.60 0.60 14 -3 -7 4.30 0.60 14 -3 -7 4.40 0.60 14 -3 -6 74.49 3.30 14 -3 -6 73.39 3.20 14 -3 -6 76.39 3.30 14 -3 -5 10.50 0.90 14 -3 -5 10.40 1.10 14 -3 -4 62.79 3.00 14 -3 -4 59.99 2.70 14 -3 -3 11.40 1.20 14 -3 -3 9.90 0.90 -14 3 2 324.77 12.90 14 -3 -2 326.97 12.50 14 -3 -2 344.17 13.00 -14 3 1 139.59 6.00 14 -3 -1 145.89 6.10 -14 3 0 20.40 1.50 -14 3 0 21.60 1.50 14 -3 0 21.70 1.60 -14 3 -1 33.60 1.90 -14 3 -2 42.30 2.10 14 -4 -8 18.60 1.10 14 -4 -7 22.60 1.30 14 -4 -7 22.10 1.20 14 -4 -6 1.60 0.40 14 -4 -6 1.90 0.40 14 -4 -6 2.50 0.50 14 -4 -5 18.60 1.10 14 -4 -5 17.00 1.20 14 -4 -4 85.39 3.50 14 -4 -4 85.79 3.80 14 -4 -3 19.00 1.40 14 -4 -3 13.80 1.00 -14 4 2 467.85 18.30 14 -4 -2 488.05 17.90 14 -4 -2 487.75 18.30 -14 4 1 40.90 2.20 14 -4 -1 41.20 2.20 14 -4 -1 38.70 1.80 -14 4 0 21.80 1.40 -14 4 0 20.70 1.40 14 -4 0 19.70 1.50 -14 4 -1 9.20 0.90 -14 4 -1 8.10 0.90 -14 4 -2 1.40 0.60 14 -5 -6 14.90 0.90 14 -5 -5 52.39 2.30 14 -5 -5 52.59 2.40 14 -5 -4 112.89 4.60 14 -5 -4 108.29 4.40 14 -5 -3 56.49 2.70 14 -5 -3 55.79 2.40 -14 5 2 57.09 2.80 14 -5 -2 59.69 2.50 14 -5 -2 62.09 2.80 -14 5 1 89.19 3.90 14 -5 -1 92.19 3.60 14 -5 -1 90.29 3.90 -14 5 0 77.69 3.30 -14 5 0 78.19 3.40 15 4 -4 78.59 3.30 15 4 -3 46.40 2.30 15 4 -2 48.90 2.40 15 4 -1 5.60 0.70 15 3 -7 18.60 1.00 15 3 -6 32.60 1.60 15 3 -5 57.79 2.50 15 3 -5 56.19 2.60 15 3 -4 376.16 14.30 15 3 -3 221.08 8.70 15 3 -2 104.09 4.50 -15 -3 1 293.47 12.20 15 3 -1 337.97 12.20 -15 -3 0 63.79 3.00 15 3 0 66.39 3.00 -15 -3 -1 4.60 0.70 15 2 -7 311.37 11.70 15 2 -6 248.48 9.30 15 2 -6 234.78 9.10 15 2 -5 14.90 1.10 15 2 -5 15.00 1.10 15 2 -4 66.99 3.10 15 2 -3 7.20 1.00 15 2 -2 -0.30 0.40 -15 -2 1 3.90 0.70 15 2 -1 4.70 0.80 -15 -2 0 0.40 0.40 15 2 0 0.20 0.40 -15 -2 -1 248.28 9.60 15 1 -8 2.00 0.50 15 1 -8 1.80 0.30 15 1 -7 36.80 1.80 15 1 -7 37.60 2.10 15 1 -6 226.28 8.70 15 1 -6 220.78 8.50 15 1 -5 63.99 2.90 15 1 -5 61.79 2.90 15 1 -4 42.40 2.30 15 1 -3 241.58 9.60 15 1 -2 55.89 2.80 -15 -1 1 158.28 6.80 15 1 -1 170.78 6.80 -15 -1 0 104.19 4.60 15 1 0 106.89 4.60 -15 -1 -1 2.70 0.60 -15 -1 -2 1.00 0.40 15 0 -8 115.79 4.70 15 0 -8 118.49 5.00 15 0 -8 120.49 4.50 15 0 -7 0.20 0.30 15 0 -6 940.01 35.00 15 0 -6 962.80 35.20 15 0 -5 0.70 0.40 15 0 -5 -0.10 0.40 15 0 -4 1.70 0.60 15 0 -3 -0.10 0.40 15 0 -2 16.50 1.40 -15 0 1 -0.10 0.40 15 0 -1 -0.50 0.40 -15 0 0 36.40 2.10 15 0 0 36.20 2.10 -15 0 -1 0.50 0.40 -15 0 -2 288.97 11.00 15 -1 -8 1.60 0.30 15 -1 -8 1.80 0.40 15 -1 -7 39.20 1.90 15 -1 -7 40.60 1.90 15 -1 -6 223.58 8.60 15 -1 -6 219.08 8.50 15 -1 -6 225.08 8.70 15 -1 -5 63.79 2.90 15 -1 -5 59.29 2.90 15 -1 -4 42.80 2.30 15 -1 -3 240.18 9.50 -15 1 2 51.19 2.80 15 -1 -2 57.09 2.80 -15 1 1 162.18 6.90 15 -1 -1 170.68 6.90 -15 1 0 107.99 4.60 15 -1 0 104.69 4.60 -15 1 -1 2.10 0.50 -15 1 -2 0.90 0.40 15 -2 -8 21.60 1.00 15 -2 -8 21.80 1.20 15 -2 -7 315.07 12.00 15 -2 -7 318.87 11.90 15 -2 -6 241.18 9.50 15 -2 -6 247.18 9.30 15 -2 -6 247.88 9.40 15 -2 -5 13.10 1.00 15 -2 -5 13.10 1.30 15 -2 -5 14.40 1.10 15 -2 -4 69.49 3.20 15 -2 -3 7.00 1.00 -15 2 2 0.60 0.50 15 -2 -2 2.60 0.70 -15 2 1 4.80 0.80 15 -2 -1 4.20 0.70 -15 2 0 0.30 0.40 15 -2 0 0.80 0.40 -15 2 -1 257.47 9.90 15 -3 -7 18.70 1.20 15 -3 -7 17.70 1.10 15 -3 -6 33.90 1.60 15 -3 -6 33.80 1.60 15 -3 -6 32.50 1.70 15 -3 -5 61.19 2.70 15 -3 -5 56.29 2.50 15 -3 -4 392.96 14.50 15 -3 -4 370.66 14.30 15 -3 -3 242.08 9.50 -15 3 2 99.89 4.50 -15 3 2 102.69 4.50 15 -3 -2 107.59 4.50 -15 3 1 320.67 12.60 15 -3 -1 337.47 12.70 -15 3 0 65.49 3.00 -15 3 -1 6.60 0.80 15 -4 -6 123.39 5.00 15 -4 -5 15.50 1.00 15 -4 -5 15.60 0.90 15 -4 -4 78.69 3.30 15 -4 -4 83.39 3.50 15 -4 -3 44.50 2.00 15 -4 -3 49.10 2.30 15 -4 -2 46.70 2.30 -15 4 1 3.80 0.80 16 3 -3 19.20 1.50 16 2 -5 78.49 3.20 16 2 -4 81.59 3.40 16 2 -3 240.78 9.30 16 2 -2 16.70 1.20 16 1 -5 0.20 0.30 16 1 -4 126.09 5.10 16 1 -3 15.60 1.20 16 1 -2 0.80 0.50 -16 -1 1 5.50 0.80 16 1 -1 6.50 0.90 16 0 -6 9.80 0.80 16 0 -5 0.00 0.30 16 0 -4 0.50 0.40 16 0 -3 0.20 0.40 -16 0 2 329.27 13.40 16 0 -2 369.66 13.40 -16 0 1 0.00 0.40 16 0 -1 -0.50 0.30 -16 0 0 60.59 2.90 16 -1 -5 0.80 0.40 16 -1 -4 130.19 5.30 16 -1 -3 16.00 1.20 -16 1 2 0.40 0.40 16 -1 -2 0.80 0.50 -16 1 1 6.60 0.90 16 -1 -1 6.70 0.90 16 -2 -5 84.49 3.50 16 -2 -4 86.59 3.70 16 -2 -3 243.68 9.40 16 -2 -2 16.80 1.20 16 -3 -4 2.50 0.50 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 30468 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_I_CCDC3 _database_code_depnum_ccdc_archive 'CCDC 1875543' _audit_update_record ; 2018-10-26 deposited with the CCDC. 2018-12-12 downloaded from the CCDC. ; _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C17 H12 F N O3 S' _chemical_formula_sum 'C17 H12 F N O3 S' _chemical_formula_iupac ? _chemical_formula_weight 329.34 _chemical_melting_point ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.237(3) _cell_length_b 11.212(2) _cell_length_c 17.948(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3066.2(10) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9840 _cell_measurement_theta_min 2.9001 _cell_measurement_theta_max 67.1151 _cell_measurement_temperature 296.(2) _exptl_crystal_description block _exptl_crystal_colour 'clear colourless' _exptl_crystal_size_max 0.498 _exptl_crystal_size_mid 0.310 _exptl_crystal_size_min 0.191 _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 2.111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/4 (Bruker AXS Inc.)' _exptl_absorpt_correction_T_min 0.44 _exptl_absorpt_correction_T_max 0.75 _exptl_special_details ; ; _diffrn_ambient_temperature 296.(2) _diffrn_source 'Incoatec Microfocus X-ray Source I\mS' _diffrn_source_type Microfocus _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_monochromator 'Incoatec Montel Multilayer Mirror' _diffrn_measurement_device_type 'Bruker ACS Kappa APEX II DUO diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 16848 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_unetI/netI 0.0276 _diffrn_reflns_theta_min 5.72 _diffrn_reflns_theta_max 67.14 _diffrn_reflns_theta_full 67.14 _diffrn_measured_fraction_theta_max 0.958 _diffrn_measured_fraction_theta_full 0.958 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 11 _refine_special_details ; ; _reflns_number_total 2637 _reflns_number_gt 2617 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_gt 0.1302 _refine_ls_wR_factor_ref 0.1303 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_number_reflns 2637 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+1.4891P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.513 _refine_diff_density_min -0.300 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker Instrument Service v2013.12.0.0' _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.61190(10) 0.19193(16) 0.12733(10) 0.0583(5) Uani d . . . 1 . . N N5 0.55175(11) 0.28150(17) 0.10054(10) 0.0465(4) Uani d . . . 1 . . C C3 0.49574(12) 0.30703(16) 0.15108(10) 0.0330(4) Uani d . . . 1 . . C C4 0.50031(12) 0.24053(16) 0.22371(10) 0.0329(4) Uani d . . . 1 . . S S2 0.61234(3) 0.17485(5) 0.21852(3) 0.0461(2) Uani d . . . 1 . . C C6 0.42913(11) 0.39879(15) 0.13479(9) 0.0314(4) Uani d . . . 1 . . C C7 0.45132(13) 0.49762(17) 0.09121(10) 0.0372(4) Uani d . . . 1 . . H H7 0.5085 0.5059 0.0739 0.045 Uiso calc U . R 1 . . C C8 0.38979(14) 0.58280(19) 0.07353(11) 0.0446(5) Uani d . . . 1 . . H H8 0.4044 0.6484 0.0443 0.054 Uiso calc U . R 1 . . C C9 0.30584(15) 0.56781(18) 0.10043(11) 0.0446(5) Uani d . . . 1 . . C C10 0.28092(13) 0.47222(19) 0.14302(11) 0.0431(5) Uani d . . . 1 . . H H10 0.2233 0.4645 0.1595 0.052 Uiso calc U . R 1 . . C C11 0.34324(12) 0.38754(17) 0.16096(10) 0.0369(4) Uani d . . . 1 . . H H11 0.3279 0.3227 0.1906 0.044 Uiso calc U . R 1 . . F F12 0.24522(10) 0.65212(14) 0.08347(9) 0.0729(5) Uani d . . . 1 . . C C13 0.43539(12) 0.13258(16) 0.22611(10) 0.0346(4) Uani d . . . 1 . . C C14 0.39400(12) 0.13485(18) 0.29978(11) 0.0378(4) Uani d . . . 1 . . C C15 0.33558(14) 0.0520(2) 0.32975(13) 0.0483(5) Uani d . . . 1 . . H H15 0.3172 -0.0141 0.3027 0.058 Uiso calc U . R 1 . . C C16 0.30635(16) 0.0724(2) 0.40123(14) 0.0581(6) Uani d . . . 1 . . H H16 0.2676 0.0189 0.4232 0.07 Uiso calc U . R 1 . . C C17 0.33410(16) 0.1721(2) 0.44110(14) 0.0588(7) Uani d . . . 1 . . H H17 0.3129 0.1831 0.4892 0.071 Uiso calc U . R 1 . . C C18 0.39199(15) 0.2558(2) 0.41221(12) 0.0484(5) Uani d . . . 1 . . C C19 0.42190(13) 0.23428(17) 0.33978(10) 0.0376(4) Uani d . . . 1 . . C C20 0.48534(14) 0.30999(17) 0.29596(11) 0.0392(5) Uani d . . . 1 . . H H20A 0.54 0.3202 0.323 0.047 Uiso calc U . R 1 . . H H20B 0.4605 0.3879 0.2857 0.047 Uiso calc U . R 1 . . O O21 0.42561(10) 0.06335(12) 0.17530(8) 0.0472(4) Uani d . . . 1 . . C C22 0.4231(2) 0.3633(3) 0.45553(14) 0.0666(7) Uani d . . . 1 . . H H22A 0.3887 0.3716 0.5 0.1 Uiso calc U . R 1 . . H H22B 0.4168 0.4335 0.4254 0.1 Uiso calc U . R 1 . . H H22C 0.4837 0.353 0.4687 0.1 Uiso calc U . R 1 . . O O23 0.67174(10) 0.26123(15) 0.25165(11) 0.0616(5) Uani d . . . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0438(9) 0.0665(11) 0.0646(11) 0.0207(7) 0.0078(7) -0.0049(8) N5 0.0404(9) 0.0538(10) 0.0453(9) 0.0097(8) 0.0076(7) 0.0025(8) C3 0.0322(9) 0.0325(9) 0.0342(9) -0.0032(7) 0.0003(7) 0.0000(7) C4 0.0329(9) 0.0300(9) 0.0359(9) -0.0001(7) -0.0029(7) 0.0009(7) S2 0.0368(3) 0.0393(3) 0.0621(4) 0.00463(19) -0.0094(2) 0.0024(2) C6 0.0326(9) 0.0328(9) 0.0289(8) -0.0008(7) 0.0001(7) -0.0001(7) C7 0.0386(10) 0.0410(10) 0.0321(9) -0.0060(8) 0.0007(7) 0.0046(7) C8 0.0573(13) 0.0383(10) 0.0383(10) -0.0019(9) -0.0043(9) 0.0094(8) C9 0.0485(11) 0.0425(11) 0.0429(10) 0.0128(9) -0.0103(9) 0.0013(8) C10 0.0336(10) 0.0503(11) 0.0454(10) 0.0056(8) 0.0019(8) 0.0009(9) C11 0.0358(10) 0.0374(9) 0.0376(9) -0.0008(8) 0.0034(7) 0.0047(7) F12 0.0680(9) 0.0670(9) 0.0839(10) 0.0306(8) -0.0118(8) 0.0172(8) C13 0.0340(9) 0.0282(9) 0.0415(10) 0.0013(7) -0.0062(7) 0.0035(7) C14 0.0336(9) 0.0374(10) 0.0425(10) 0.0035(8) -0.0042(7) 0.0092(8) C15 0.0391(11) 0.0479(11) 0.0581(13) -0.0028(9) -0.0055(9) 0.0168(10) C16 0.0426(12) 0.0678(15) 0.0641(14) 0.0012(11) 0.0086(10) 0.0257(12) C17 0.0551(14) 0.0756(17) 0.0457(12) 0.0170(12) 0.0133(10) 0.0156(11) C18 0.0503(12) 0.0534(12) 0.0413(11) 0.0167(10) 0.0004(9) 0.0046(9) C19 0.0395(10) 0.0372(10) 0.0362(10) 0.0084(8) -0.0024(8) 0.0061(8) C20 0.0477(11) 0.0330(9) 0.0369(10) -0.0013(8) -0.0034(8) -0.0006(7) O21 0.0528(9) 0.0371(7) 0.0518(8) -0.0053(6) -0.0049(6) -0.0079(6) C22 0.0862(18) 0.0692(16) 0.0444(12) 0.0147(15) 0.0034(12) -0.0110(11) O23 0.0424(8) 0.0592(10) 0.0832(12) -0.0047(7) -0.0177(8) -0.0020(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 N5 . 1.442(2) ? O1 S2 . 1.6479(19) ? N5 C3 . 1.278(3) ? C3 C6 . 1.474(2) ? C3 C4 . 1.503(2) ? C4 C20 . 1.530(3) ? C4 C13 . 1.564(2) ? C4 S2 . 1.8614(19) ? S2 O23 . 1.4527(17) ? C6 C11 . 1.396(3) ? C6 C7 . 1.398(2) ? C7 C8 . 1.375(3) ? C7 H7 . 0.93 ? C8 C9 . 1.378(3) ? C8 H8 . 0.93 ? C9 F12 . 1.356(2) ? C9 C10 . 1.370(3) ? C10 C11 . 1.381(3) ? C10 H10 . 0.93 ? C11 H11 . 0.93 ? C13 O21 . 1.207(2) ? C13 C14 . 1.465(3) ? C14 C19 . 1.392(3) ? C14 C15 . 1.394(3) ? C15 C16 . 1.377(4) ? C15 H15 . 0.93 ? C16 C17 . 1.393(4) ? C16 H16 . 0.93 ? C17 C18 . 1.388(4) ? C17 H17 . 0.93 ? C18 C19 . 1.399(3) ? C18 C22 . 1.511(4) ? C19 C20 . 1.508(3) ? C20 H20A . 0.97 ? C20 H20B . 0.97 ? C22 H22A . 0.96 ? C22 H22B . 0.96 ? C22 H22C . 0.96 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N5 O1 S2 . . 114.49(12) ? C3 N5 O1 . . 110.11(16) ? N5 C3 C6 . . 118.38(17) ? N5 C3 C4 . . 118.26(17) ? C6 C3 C4 . . 123.36(15) ? C3 C4 C20 . . 118.40(15) ? C3 C4 C13 . . 112.23(14) ? C20 C4 C13 . . 106.04(15) ? C3 C4 S2 . . 101.27(12) ? C20 C4 S2 . . 112.37(13) ? C13 C4 S2 . . 105.98(12) ? O23 S2 O1 . . 109.36(11) ? O23 S2 C4 . . 106.69(9) ? O1 S2 C4 . . 90.00(8) ? C11 C6 C7 . . 119.12(17) ? C11 C6 C3 . . 121.04(16) ? C7 C6 C3 . . 119.83(16) ? C8 C7 C6 . . 120.97(18) ? C8 C7 H7 . . 119.5 ? C6 C7 H7 . . 119.5 ? C7 C8 C9 . . 117.86(18) ? C7 C8 H8 . . 121.1 ? C9 C8 H8 . . 121.1 ? F12 C9 C10 . . 118.8(2) ? F12 C9 C8 . . 117.95(19) ? C10 C9 C8 . . 123.25(19) ? C9 C10 C11 . . 118.51(18) ? C9 C10 H10 . . 120.7 ? C11 C10 H10 . . 120.7 ? C10 C11 C6 . . 120.27(17) ? C10 C11 H11 . . 119.9 ? C6 C11 H11 . . 119.9 ? O21 C13 C14 . . 129.79(18) ? O21 C13 C4 . . 123.72(17) ? C14 C13 C4 . . 106.48(15) ? C19 C14 C15 . . 122.0(2) ? C19 C14 C13 . . 110.36(17) ? C15 C14 C13 . . 127.7(2) ? C16 C15 C14 . . 117.1(2) ? C16 C15 H15 . . 121.5 ? C14 C15 H15 . . 121.5 ? C15 C16 C17 . . 120.9(2) ? C15 C16 H16 . . 119.5 ? C17 C16 H16 . . 119.5 ? C18 C17 C16 . . 122.9(2) ? C18 C17 H17 . . 118.5 ? C16 C17 H17 . . 118.5 ? C17 C18 C19 . . 116.0(2) ? C17 C18 C22 . . 123.1(2) ? C19 C18 C22 . . 120.9(2) ? C14 C19 C18 . . 121.18(19) ? C14 C19 C20 . . 112.18(17) ? C18 C19 C20 . . 126.64(19) ? C19 C20 C4 . . 104.54(15) ? C19 C20 H20A . . 110.8 ? C4 C20 H20A . . 110.8 ? C19 C20 H20B . . 110.8 ? C4 C20 H20B . . 110.8 ? H20A C20 H20B . . 108.9 ? C18 C22 H22A . . 109.5 ? C18 C22 H22B . . 109.5 ? H22A C22 H22B . . 109.5 ? C18 C22 H22C . . 109.5 ? H22A C22 H22C . . 109.5 ? H22B C22 H22C . . 109.5 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag S2 O1 N5 C3 . . . . -16.6(2) ? O1 N5 C3 C6 . . . . 178.99(15) ? O1 N5 C3 C4 . . . . -1.9(2) ? N5 C3 C4 C20 . . . . 139.61(19) ? C6 C3 C4 C20 . . . . -41.4(2) ? N5 C3 C4 C13 . . . . -96.3(2) ? C6 C3 C4 C13 . . . . 82.7(2) ? N5 C3 C4 S2 . . . . 16.3(2) ? C6 C3 C4 S2 . . . . -164.66(14) ? N5 O1 S2 O23 . . . . -85.38(15) ? N5 O1 S2 C4 . . . . 22.34(15) ? C3 C4 S2 O23 . . . . 89.82(14) ? C20 C4 S2 O23 . . . . -37.51(16) ? C13 C4 S2 O23 . . . . -152.90(13) ? C3 C4 S2 O1 . . . . -20.43(13) ? C20 C4 S2 O1 . . . . -147.76(14) ? C13 C4 S2 O1 . . . . 96.85(13) ? N5 C3 C6 C11 . . . . 142.68(19) ? C4 C3 C6 C11 . . . . -36.3(3) ? N5 C3 C6 C7 . . . . -36.0(3) ? C4 C3 C6 C7 . . . . 145.01(17) ? C11 C6 C7 C8 . . . . -0.5(3) ? C3 C6 C7 C8 . . . . 178.22(17) ? C6 C7 C8 C9 . . . . 0.3(3) ? C7 C8 C9 F12 . . . . 179.57(18) ? C7 C8 C9 C10 . . . . -0.6(3) ? F12 C9 C10 C11 . . . . -179.12(18) ? C8 C9 C10 C11 . . . . 1.1(3) ? C9 C10 C11 C6 . . . . -1.2(3) ? C7 C6 C11 C10 . . . . 0.9(3) ? C3 C6 C11 C10 . . . . -177.75(17) ? C3 C4 C13 O21 . . . . 44.2(2) ? C20 C4 C13 O21 . . . . 174.90(18) ? S2 C4 C13 O21 . . . . -65.5(2) ? C3 C4 C13 C14 . . . . -136.76(16) ? C20 C4 C13 C14 . . . . -6.05(18) ? S2 C4 C13 C14 . . . . 113.57(13) ? O21 C13 C14 C19 . . . . -177.41(19) ? C4 C13 C14 C19 . . . . 3.6(2) ? O21 C13 C14 C15 . . . . 3.4(3) ? C4 C13 C14 C15 . . . . -175.55(18) ? C19 C14 C15 C16 . . . . -0.1(3) ? C13 C14 C15 C16 . . . . 178.96(19) ? C14 C15 C16 C17 . . . . 0.3(3) ? C15 C16 C17 C18 . . . . -0.2(4) ? C16 C17 C18 C19 . . . . -0.2(3) ? C16 C17 C18 C22 . . . . -179.2(2) ? C15 C14 C19 C18 . . . . -0.3(3) ? C13 C14 C19 C18 . . . . -179.50(17) ? C15 C14 C19 C20 . . . . 179.56(18) ? C13 C14 C19 C20 . . . . 0.3(2) ? C17 C18 C19 C14 . . . . 0.4(3) ? C22 C18 C19 C14 . . . . 179.5(2) ? C17 C18 C19 C20 . . . . -179.37(19) ? C22 C18 C19 C20 . . . . -0.3(3) ? C14 C19 C20 C4 . . . . -4.2(2) ? C18 C19 C20 C4 . . . . 175.63(18) ? C3 C4 C20 C19 . . . . 133.15(16) ? C13 C4 C20 C19 . . . . 6.06(19) ? S2 C4 C20 C19 . . . . -109.29(15) ? _shelx_res_file ; TITL PMc_5_478_a.res in Pbca CELL 1.54178 15.2371 11.2116 17.9475 90.000 90.000 90.000 ZERR 8.000 0.0028 0.0021 0.0033 0.000 0.000 0.000 LATT 1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H N O F S UNIT 136 96 8 24 8 8 REM Old TITL PMc_5_478 in Pbca REM SHELXT solution in Pbca REM R1 0.151, Rweak 0.006, Alpha 0.032, Orientation as input REM Formula found by SHELXT: C17 N5 O3 S L.S. 5 ACTA BOND $H FMAP 2 PLAN 5 CONF SIZE 0.191 0.310 0.498 TEMP 23.000 WGHT 0.070900 1.489100 FVAR 0.94628 O1 4 0.611905 0.191934 0.127326 11.00000 0.04378 0.06646 = 0.06464 -0.00495 0.00778 0.02069 N5 3 0.551746 0.281500 0.100539 11.00000 0.04038 0.05385 = 0.04533 0.00255 0.00756 0.00973 C3 1 0.495737 0.307029 0.151078 11.00000 0.03218 0.03254 = 0.03421 0.00004 0.00034 -0.00321 C4 1 0.500314 0.240530 0.223708 11.00000 0.03292 0.03002 = 0.03588 0.00085 -0.00293 -0.00014 S2 6 0.612343 0.174854 0.218519 11.00000 0.03679 0.03931 = 0.06208 0.00240 -0.00945 0.00463 C6 1 0.429125 0.398786 0.134793 11.00000 0.03261 0.03277 = 0.02889 -0.00007 0.00013 -0.00084 C7 1 0.451319 0.497618 0.091209 11.00000 0.03858 0.04097 = 0.03214 0.00458 0.00070 -0.00601 AFIX 43 H7 2 0.508531 0.505895 0.073914 11.00000 -1.20000 AFIX 0 C8 1 0.389793 0.582796 0.073527 11.00000 0.05728 0.03832 = 0.03827 0.00942 -0.00432 -0.00186 AFIX 43 H8 2 0.404397 0.648404 0.044344 11.00000 -1.20000 AFIX 0 C9 1 0.305839 0.567811 0.100434 11.00000 0.04846 0.04247 = 0.04290 0.00128 -0.01027 0.01281 C10 1 0.280921 0.472223 0.143022 11.00000 0.03359 0.05032 = 0.04539 0.00085 0.00195 0.00559 AFIX 43 H10 2 0.223324 0.464543 0.159484 11.00000 -1.20000 AFIX 0 C11 1 0.343235 0.387542 0.160957 11.00000 0.03584 0.03738 = 0.03761 0.00475 0.00342 -0.00083 AFIX 43 H11 2 0.327929 0.322749 0.190587 11.00000 -1.20000 AFIX 0 F12 5 0.245219 0.652116 0.083468 11.00000 0.06798 0.06698 = 0.08389 0.01717 -0.01182 0.03061 C13 1 0.435388 0.132579 0.226105 11.00000 0.03404 0.02818 = 0.04151 0.00348 -0.00623 0.00128 C14 1 0.394004 0.134854 0.299778 11.00000 0.03362 0.03744 = 0.04248 0.00920 -0.00425 0.00354 C15 1 0.335581 0.052017 0.329748 11.00000 0.03907 0.04786 = 0.05811 0.01676 -0.00548 -0.00278 AFIX 43 H15 2 0.317160 -0.014105 0.302650 11.00000 -1.20000 AFIX 0 C16 1 0.306353 0.072403 0.401227 11.00000 0.04258 0.06776 = 0.06409 0.02574 0.00861 0.00125 AFIX 43 H16 2 0.267561 0.018871 0.423184 11.00000 -1.20000 AFIX 0 C17 1 0.334103 0.172126 0.441097 11.00000 0.05506 0.07564 = 0.04571 0.01563 0.01326 0.01704 AFIX 43 H17 2 0.312900 0.183133 0.489199 11.00000 -1.20000 AFIX 0 C18 1 0.391986 0.255766 0.412214 11.00000 0.05032 0.05345 = 0.04132 0.00460 0.00042 0.01670 C19 1 0.421902 0.234278 0.339778 11.00000 0.03951 0.03724 = 0.03615 0.00606 -0.00236 0.00845 C20 1 0.485340 0.309992 0.295961 11.00000 0.04767 0.03297 = 0.03687 -0.00055 -0.00336 -0.00132 AFIX 23 H20A 2 0.539964 0.320200 0.322976 11.00000 -1.20000 H20B 2 0.460476 0.387923 0.285695 11.00000 -1.20000 AFIX 0 O21 4 0.425609 0.063349 0.175300 11.00000 0.05279 0.03714 = 0.05178 -0.00795 -0.00490 -0.00535 C22 1 0.423134 0.363254 0.455534 11.00000 0.08616 0.06922 = 0.04439 -0.01102 0.00343 0.01466 AFIX 137 H22A 2 0.388658 0.371559 0.500003 11.00000 -1.50000 H22B 2 0.416806 0.433508 0.425431 11.00000 -1.50000 H22C 2 0.483733 0.353002 0.468697 11.00000 -1.50000 AFIX 0 O23 4 0.671741 0.261228 0.251648 11.00000 0.04241 0.05919 = 0.08321 -0.00196 -0.01774 -0.00472 HKLF 4 REM PMc_5_478_a.res in Pbca REM R1 = 0.0448 for 2617 Fo > 4sig(Fo) and 0.0449 for all 2637 data REM 209 parameters refined using 0 restraints END WGHT 0.0709 1.4892 REM Highest difference peak 0.513, deepest hole -0.300, 1-sigma level 0.044 Q1 1 0.6518 0.2065 0.1718 11.00000 0.05 0.51 Q2 1 0.5523 0.1919 0.2339 11.00000 0.05 0.34 Q3 1 0.4960 0.2777 0.1909 11.00000 0.05 0.24 Q4 1 0.4712 0.1877 0.2227 11.00000 0.05 0.22 Q5 1 0.7137 0.2830 0.2022 11.00000 0.05 0.21 ; _shelx_res_checksum 79755 _shelx_hkl_file ; 0 4 0 349.67 18.20 0 -4 0 284.97 18.40 0 5 0 0.30 0.60 0 6 0 136.59 8.50 0 -7 0 5.50 1.10 0 -8 0 880.81 50.79 0 8 0 919.11 51.29 0 -9 0 4.70 1.30 0 -10 0 236.98 14.30 0 -11 0 -0.30 1.00 0 -12 0 565.84 32.20 0 -13 0 -0.30 0.50 1 0 0 56.19 3.30 1 1 0 2.70 0.40 1 2 0 0.60 0.50 1 -2 0 0.30 0.50 1 3 0 16.30 1.40 1 -4 0 20.60 1.90 1 -5 0 3.70 1.10 1 -7 0 6.40 1.30 -1 -7 0 3.70 0.90 1 8 0 2.60 1.40 -1 -8 0 3.60 1.10 1 -10 0 1.90 1.20 -1 -10 0 1.10 1.10 -1 -11 0 0.30 1.10 -1 -12 0 0.60 0.90 1 -12 0 4.90 1.20 1 -13 0 -0.10 0.50 1 -13 0 0.40 0.50 -1 -13 0 0.10 0.60 2 1 0 1133.89 67.69 2 -1 0 1154.18 67.89 2 -1 0 1232.08 68.99 2 -4 0 905.31 54.69 2 -4 0 947.01 56.59 2 4 0 941.61 53.29 -2 5 0 442.96 25.50 2 -5 0 468.15 25.90 2 5 0 433.96 25.70 -2 6 0 14.60 1.70 2 6 0 13.70 1.90 -2 7 0 5009.10 266.67 2 -7 0 4444.46 263.27 2 -7 0 4234.98 263.17 2 7 0 4933.11 268.67 -2 -7 0 4867.61 263.47 2 8 0 58.89 5.10 -2 -8 0 65.79 4.40 2 -8 0 62.49 4.50 2 -9 0 3241.48 177.98 -2 -9 0 3037.20 175.78 -2 -10 0 638.84 37.40 2 -10 0 673.33 37.60 2 -11 0 180.28 11.00 -2 -11 0 173.68 10.80 2 -12 0 2.50 1.00 -2 -12 0 1.40 0.90 2 -13 0 597.44 34.80 -2 -13 0 648.84 35.00 3 1 0 3.10 0.90 3 -1 0 3.40 0.90 3 2 0 -1.50 1.30 3 -2 0 0.10 1.20 3 4 0 1.10 0.80 3 -4 0 2.60 1.00 3 -7 0 3.50 1.20 3 8 0 3.60 1.80 -3 8 0 3.70 1.50 3 -8 0 4.50 1.10 -3 -9 0 0.60 1.00 3 -9 0 1.10 1.10 -3 -10 0 3.50 1.20 3 -10 0 0.30 1.10 -3 -11 0 4.60 1.30 3 -11 0 0.00 1.10 3 -12 0 0.20 0.80 -3 -12 0 0.50 0.80 3 -12 0 0.80 0.80 -3 -13 0 0.40 0.50 4 2 0 3152.88 171.98 4 2 0 2823.12 170.88 4 3 0 78.09 5.80 4 -3 0 63.79 5.60 4 3 0 75.99 6.30 4 3 0 77.39 5.70 4 -4 0 4230.28 236.98 4 -4 0 3949.80 237.78 4 4 0 4293.77 238.18 4 -5 0 1678.73 102.09 4 -5 0 1792.92 104.39 4 5 0 1835.42 104.89 4 6 0 211.88 13.20 4 -6 0 203.08 12.80 4 -7 0 3830.22 214.88 4 7 0 3845.52 216.78 -4 -7 0 3919.41 214.28 4 -7 0 3493.25 213.78 -4 7 0 3891.51 216.08 4 -8 0 631.94 35.00 4 -8 0 574.54 35.30 -4 -8 0 604.94 34.80 4 8 0 605.24 36.30 -4 8 0 645.64 35.40 4 -9 0 561.24 32.10 4 -9 0 570.24 32.10 -4 -9 0 543.95 31.90 4 -10 0 6.50 1.50 -4 -10 0 5.40 1.30 -4 -11 0 85.09 5.60 4 -11 0 82.69 5.70 -4 -12 0 205.48 11.90 4 -12 0 197.48 11.80 -4 -13 0 114.59 6.80 5 0 0 -3.70 0.90 5 0 0 -4.60 1.00 5 1 0 32.50 3.10 5 -2 0 3.60 0.60 5 -2 0 2.20 0.90 5 -6 0 11.50 1.60 5 6 0 11.60 2.80 5 -6 0 13.40 2.00 5 -7 0 8.00 1.90 5 -8 0 7.50 1.90 5 -8 0 5.20 1.60 5 -9 0 5.70 1.40 5 -10 0 -0.60 1.00 5 -10 0 0.20 1.00 -5 -10 0 -0.40 0.80 5 -11 0 4.90 1.20 -5 -12 0 2.40 0.80 6 0 0 5433.96 340.37 6 0 0 6636.14 348.47 6 -2 0 492.35 31.80 6 -2 0 550.84 32.00 6 2 0 552.14 32.10 6 2 0 625.74 32.60 6 -2 0 557.64 32.40 6 -3 0 3138.09 179.48 6 -3 0 2820.62 179.08 6 3 0 3526.05 185.58 6 -3 0 2961.60 179.68 6 3 0 3138.19 181.58 6 -4 0 5419.16 342.47 6 4 0 6312.57 346.67 6 -4 0 6129.79 342.97 6 -4 0 6255.57 341.97 6 5 0 2017.00 113.79 6 -5 0 1848.62 111.59 6 -5 0 1891.91 111.39 6 -5 0 1996.10 111.49 6 6 0 1496.15 81.29 6 -6 0 1396.76 82.59 -6 -6 0 1512.65 81.29 6 -6 0 1489.55 81.69 6 -6 0 1457.25 82.79 6 -6 0 1365.26 81.39 6 6 0 1474.05 83.29 6 -6 0 1455.95 81.89 6 -7 0 3577.34 198.18 6 7 0 3808.02 197.68 6 -7 0 3767.32 199.18 6 -7 0 3437.16 198.18 6 -7 0 3054.59 198.38 6 7 0 3156.98 200.28 -6 -7 0 3755.02 198.48 -6 -8 0 119.79 7.40 6 -8 0 101.49 7.90 6 8 0 103.99 9.40 6 -8 0 124.49 7.70 -6 8 0 108.19 8.00 6 -8 0 130.69 7.70 6 -8 0 114.89 8.00 6 8 0 131.49 7.50 6 9 0 680.83 38.70 6 -9 0 630.84 39.20 -6 -9 0 689.33 38.60 6 -9 0 720.23 38.90 -6 -10 0 199.88 12.40 6 -10 0 216.78 12.70 -6 -11 0 3.10 1.00 6 -12 0 37.60 2.60 -6 -12 0 46.00 3.00 7 0 0 1.90 1.10 7 -1 0 6.50 1.30 7 2 0 4.80 1.70 7 2 0 6.30 2.00 7 4 0 3.60 2.10 7 -6 0 15.60 1.90 7 -6 0 17.40 2.40 7 -7 0 10.10 2.00 -7 -8 0 0.50 0.70 7 8 0 1.30 1.00 7 -8 0 0.50 1.00 7 -8 0 1.50 1.30 7 -9 0 0.80 1.30 -7 -9 0 0.30 0.80 7 9 0 1.00 1.00 7 -9 0 1.10 1.10 7 -10 0 1.90 1.00 -7 -10 0 2.10 0.90 -7 -11 0 0.00 0.60 7 11 0 0.40 0.80 7 -11 0 0.30 0.60 -7 -12 0 2.20 0.70 8 0 0 12.20 2.00 8 -1 0 30.00 3.20 8 -1 0 26.80 2.80 8 1 0 27.00 3.00 8 2 0 9999.00 545.95 8 -2 0 9747.72 541.25 8 2 0 9877.81 542.95 8 -2 0 8492.15 537.95 8 -2 0 9700.83 543.45 8 -3 0 580.44 31.80 8 3 0 561.74 33.00 8 -3 0 523.95 31.90 8 -3 0 514.15 31.50 8 -4 0 206.78 13.40 8 -4 0 213.28 13.60 8 -4 0 217.08 12.70 8 4 0 192.48 14.70 8 4 0 240.08 12.70 8 -4 0 227.68 12.90 8 5 0 2652.43 151.18 8 -5 0 2660.23 152.18 8 -5 0 2568.14 151.38 8 -5 0 2588.04 150.58 8 5 0 2750.32 149.88 8 -5 0 2716.53 151.48 8 -5 0 2756.72 150.98 8 -6 0 4942.91 279.57 8 6 0 5543.65 278.47 8 -6 0 4826.32 278.27 -8 -6 0 5380.26 277.67 8 -6 0 4993.20 279.77 8 6 0 4483.15 282.37 8 -6 0 4482.55 278.37 8 -7 0 2982.50 178.58 8 -7 0 3237.38 179.48 -8 -7 0 3028.40 178.88 8 7 0 3188.48 177.88 8 7 0 3482.45 184.68 8 -8 0 920.51 56.09 -8 -8 0 1020.50 55.59 8 8 0 1031.70 55.59 8 -8 0 978.70 55.79 8 9 0 1590.74 87.79 8 -9 0 1494.45 88.29 8 -9 0 1654.63 87.89 -8 -9 0 1534.05 87.69 8 -10 0 63.49 4.20 -8 -10 0 59.79 4.20 8 10 0 61.59 4.40 -8 -11 0 2.10 0.70 8 11 0 1.00 0.80 9 1 0 2.50 1.40 9 1 0 0.00 1.70 9 -2 0 1.50 1.20 9 -2 0 3.20 1.20 9 -2 0 1.10 1.50 9 2 0 0.60 1.90 9 -3 0 1.00 0.80 9 3 0 1.10 4.40 9 -3 0 1.30 0.70 9 -3 0 1.90 1.50 9 3 0 0.60 0.60 9 -3 0 0.60 1.20 9 -3 0 2.70 1.30 9 5 0 7.60 3.20 9 -5 0 7.40 1.60 9 6 0 -0.20 0.70 9 -6 0 1.20 1.20 -9 -6 0 1.20 0.70 9 -6 0 1.40 1.10 9 6 0 5.10 3.00 9 -6 0 0.00 0.90 9 -7 0 4.20 1.20 9 -7 0 2.40 1.40 9 7 0 2.60 1.00 9 -8 0 1.40 1.30 -9 -8 0 0.50 0.80 9 8 0 0.50 0.80 9 -8 0 0.70 1.00 -9 -9 0 0.90 0.80 9 -9 0 3.00 1.10 9 -9 0 -0.50 1.10 9 9 0 0.20 0.80 -9 -10 0 1.30 0.70 9 -10 0 0.60 0.70 9 10 0 0.10 0.80 -9 -11 0 0.40 0.60 9 11 0 0.40 0.70 10 0 0 3202.98 179.08 10 0 0 3067.89 174.68 10 0 0 3068.09 174.98 10 -1 0 3096.19 170.58 10 1 0 2908.21 169.78 10 -1 0 2878.71 170.28 10 -1 0 3079.99 173.88 10 1 0 3160.98 175.78 10 1 0 3071.19 169.98 10 -2 0 1429.56 78.79 10 -2 0 1334.17 79.79 10 2 0 1398.36 81.29 10 -2 0 1440.26 78.59 10 2 0 1380.06 78.59 10 -2 0 1440.36 79.59 10 2 0 1523.95 81.59 10 -2 0 1308.97 80.09 10 -3 0 1807.02 97.39 10 3 0 1745.13 96.39 10 3 0 1947.21 99.79 10 3 0 1579.54 98.49 10 -3 0 1595.84 96.59 10 -3 0 1742.53 96.29 10 -3 0 1554.44 96.59 10 -3 0 1751.52 95.89 10 -4 0 15.20 1.80 10 -4 0 16.70 2.20 10 4 0 14.20 1.70 10 -4 0 18.30 2.50 10 4 0 16.70 4.50 10 -5 0 401.46 24.00 10 -5 0 421.36 23.70 10 -5 0 422.36 23.70 10 -5 0 376.26 23.60 10 5 0 441.86 23.60 10 -6 0 9.30 2.00 10 6 0 8.20 1.60 10 7 0 285.37 16.00 -10 -7 0 279.77 15.90 10 -7 0 243.58 16.40 10 -7 0 278.37 16.00 10 -8 0 1242.28 74.49 10 -8 0 1357.76 73.99 10 8 0 1364.16 73.99 -10 -8 0 1318.17 73.99 -10 -9 0 400.86 23.60 10 -9 0 400.46 24.30 10 -9 0 426.46 23.50 10 9 0 426.06 23.80 -10 -10 0 24.70 2.10 10 10 0 25.50 2.30 -10 -11 0 83.99 5.30 11 0 0 1.30 0.70 11 0 0 0.20 0.70 11 0 0 3.60 1.90 11 -1 0 0.40 0.80 11 1 0 1.20 1.70 11 -1 0 1.00 0.60 11 1 0 2.00 2.40 11 -2 0 2.10 1.40 11 -2 0 1.50 1.50 11 -2 0 2.80 1.60 11 -2 0 3.90 1.10 11 -2 0 2.70 0.80 11 2 0 1.70 0.70 11 2 0 0.10 1.80 11 3 0 3.50 2.80 11 3 0 2.50 3.00 11 -3 0 3.90 1.50 11 -3 0 3.60 1.50 11 -3 0 2.40 1.00 11 -3 0 2.70 1.30 11 -4 0 6.30 1.50 11 4 0 4.40 3.20 11 -5 0 0.70 0.90 11 -5 0 -0.20 1.10 11 5 0 2.50 0.90 11 -6 0 0.50 1.00 11 -7 0 0.10 1.20 11 -7 0 1.40 1.00 11 7 0 2.10 0.90 -11 -7 0 2.00 0.90 -11 -8 0 1.10 0.80 11 -8 0 1.80 1.30 -11 -9 0 0.30 0.60 11 -9 0 1.00 0.60 11 -9 0 0.80 1.10 11 9 0 0.60 0.80 -11 -10 0 0.40 0.60 11 10 0 0.60 0.70 12 0 0 1497.65 82.99 12 0 0 1280.77 81.59 12 0 0 1590.54 83.69 12 -1 0 1848.92 101.49 12 -1 0 1736.13 100.79 12 1 0 1852.61 101.89 12 -1 0 1649.44 99.99 12 1 0 1700.03 102.29 12 1 0 1796.22 100.89 12 -1 0 1962.20 101.39 12 2 0 578.04 32.60 12 2 0 633.34 35.80 12 -2 0 558.04 32.80 12 -2 0 556.74 33.60 12 2 0 556.84 34.70 12 -2 0 574.94 32.50 12 -3 0 1366.46 70.49 12 -3 0 1218.28 70.39 12 3 0 1283.57 73.49 12 -3 0 1158.78 70.29 12 3 0 1154.38 72.49 12 -3 0 1278.97 70.09 12 3 0 1314.57 70.09 12 -4 0 79.79 5.20 12 4 0 72.89 5.10 12 4 0 81.19 8.00 12 -4 0 78.69 5.60 12 -5 0 197.98 11.60 12 -5 0 185.38 12.00 12 5 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394.36 25.30 10 3 -2 419.26 26.10 10 4 2 7.50 3.30 10 -4 -2 8.70 1.80 10 -4 2 9.40 2.50 -10 -4 -2 7.30 1.30 10 4 -2 6.90 3.30 10 4 -2 9.90 1.40 10 -5 -2 119.89 8.20 10 5 2 128.69 7.70 10 5 2 116.39 11.00 10 -5 -2 130.29 7.80 10 -5 2 122.39 9.10 10 5 -2 104.39 11.00 10 5 -2 142.39 7.90 -10 -5 -2 135.99 7.80 10 -5 2 135.39 8.10 10 -6 -2 1497.65 88.09 10 -6 -2 1570.24 88.59 10 6 2 1559.44 88.09 10 6 -2 1736.63 89.09 10 -6 2 1605.34 88.49 -10 -6 -2 1601.44 88.49 10 -6 2 1570.54 89.49 10 6 -2 1489.35 90.99 10 -7 -2 280.27 16.30 10 -7 -2 267.07 17.00 10 7 2 284.87 16.50 -10 -7 -2 291.67 16.50 10 7 -2 290.27 16.60 10 -7 2 282.77 16.80 10 -8 -2 98.29 6.80 10 8 2 96.69 6.10 10 -8 -2 91.99 5.80 10 -8 2 95.99 6.30 -10 -8 -2 88.59 6.00 10 8 -2 95.09 6.20 10 9 2 20.20 2.00 10 -9 -2 19.70 2.70 10 -9 2 19.10 2.10 10 9 -2 19.70 2.10 -10 -9 -2 19.40 1.90 -10 -10 2 1.40 0.70 10 -10 -2 0.80 1.00 10 10 2 0.90 0.70 10 -10 2 0.50 0.70 10 10 -2 1.00 0.80 -10 -10 -2 0.60 0.50 -10 -11 -2 21.90 1.70 10 11 -2 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207.38 12.30 11 -5 -2 202.28 11.70 11 5 2 199.58 11.70 11 5 -2 210.18 11.90 -11 -5 -2 184.58 11.70 11 -5 2 186.98 11.90 11 -5 2 215.88 13.40 11 -5 2 187.78 12.60 11 5 -2 198.18 14.80 11 5 -2 197.68 15.40 11 -6 -2 183.08 11.90 11 -6 -2 194.98 11.30 11 6 2 188.38 11.40 -11 -6 -2 188.88 11.40 11 -6 2 188.48 11.60 11 6 -2 205.98 11.50 11 -7 -2 17.80 1.80 11 -7 -2 22.80 2.90 11 7 2 19.20 2.20 -11 -7 -2 22.80 2.10 11 7 -2 19.50 2.30 11 -7 2 26.50 2.60 11 8 2 2.20 0.90 11 -8 2 0.60 1.00 -11 -8 -2 1.70 0.80 11 8 -2 1.60 0.90 11 -9 -2 141.09 9.00 11 9 2 134.69 8.50 11 -9 2 148.49 8.40 11 9 -2 140.59 8.60 -11 -9 -2 136.29 8.40 -11 -10 2 23.30 2.50 11 10 2 24.10 2.00 11 -10 -2 21.70 2.30 11 -10 2 19.90 1.60 -11 -10 -2 22.30 1.80 11 10 -2 24.20 2.10 12 0 2 305.07 18.10 12 0 -2 322.47 18.10 12 0 -2 321.87 18.30 12 1 2 973.90 55.69 12 -1 -2 1075.69 55.59 12 -1 -2 963.00 55.79 12 1 -2 1044.30 56.79 12 1 -2 1032.10 55.69 12 -1 2 1021.70 55.69 12 1 -2 965.80 55.69 12 1 -2 876.91 56.79 12 2 2 6.50 1.20 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58.19 4.50 1 6 -18 50.59 3.90 1 6 -18 58.19 3.90 1 -7 -18 40.00 2.60 1 7 -18 38.30 3.40 2 0 -18 95.19 5.40 -2 0 -18 95.19 5.60 2 0 -18 82.29 5.90 2 -1 -18 53.59 3.60 -2 1 -18 41.80 3.30 2 1 -18 40.50 3.10 2 1 -18 54.49 4.40 2 1 -18 55.89 3.80 -2 -1 -18 42.80 3.10 2 -2 -18 151.28 8.90 -2 2 -18 144.09 8.80 2 -2 -18 139.89 8.50 -2 -2 -18 148.59 9.50 2 2 -18 147.99 9.60 -2 -2 -18 153.38 8.50 2 2 -18 144.29 8.70 -2 3 -18 54.39 3.80 2 -3 -18 58.59 5.30 2 -3 -18 56.29 3.80 2 -3 -18 48.00 3.30 -2 3 -18 51.19 4.30 -2 -3 -18 52.89 3.40 2 3 -18 54.29 4.60 -2 -3 -18 56.19 4.40 2 3 -18 56.09 3.80 2 -4 -18 37.30 4.40 -2 4 -18 34.10 3.30 -2 4 -18 36.50 2.40 2 -4 -18 31.90 2.20 2 -4 -18 37.00 2.60 -2 4 -18 34.80 2.90 -2 4 -18 33.30 2.40 2 4 -18 36.90 3.80 -2 -4 -18 31.40 2.30 -2 -4 -18 36.70 3.20 2 4 -18 33.10 2.80 -2 5 -18 83.69 5.10 2 -5 -18 80.69 5.00 2 -5 -18 88.19 7.00 -2 5 -18 83.39 5.80 2 -5 -18 87.69 5.20 -2 5 -18 90.49 5.60 -2 -5 -18 80.39 5.00 2 5 -18 83.99 6.30 2 5 -18 85.19 5.40 2 5 -18 89.89 5.50 -2 -5 -18 81.69 5.80 -2 6 -18 14.60 1.50 -2 6 -18 13.70 2.10 -2 6 -18 15.50 1.90 2 -6 -18 13.40 2.70 -2 -6 -18 12.00 1.80 2 6 -18 15.50 1.90 2 6 -18 13.40 2.60 2 6 -18 15.70 1.90 2 7 -18 81.99 5.90 3 0 -18 1167.18 64.59 -3 0 -18 1138.69 64.29 3 -1 -18 1.30 0.80 3 -1 -18 2.40 0.70 -3 1 -18 0.80 0.90 -3 -1 -18 1.70 0.70 3 1 -18 1.80 0.60 3 1 -18 2.10 1.00 3 1 -18 3.50 1.60 3 -2 -18 53.19 3.40 -3 2 -18 58.09 3.90 3 -2 -18 56.99 5.20 3 -2 -18 55.39 3.70 3 2 -18 53.49 4.00 3 2 -18 58.79 4.70 3 2 -18 55.39 3.70 -3 3 -18 19.50 2.10 -3 3 -18 20.40 1.70 -3 3 -18 20.60 1.70 3 -3 -18 19.80 1.40 -3 3 -18 17.90 1.70 3 -3 -18 21.10 3.50 3 3 -18 19.90 2.90 -3 -3 -18 20.10 1.70 3 3 -18 19.80 1.90 3 -4 -18 52.89 5.20 -3 4 -18 52.79 3.70 -3 4 -18 48.00 3.90 -3 4 -18 49.60 3.30 3 4 -18 49.30 3.60 3 4 -18 53.39 4.60 -3 -4 -18 47.90 3.20 -3 5 -18 55.69 5.00 -3 5 -18 53.49 3.60 3 -5 -18 55.59 5.30 -3 5 -18 58.99 4.00 3 5 -18 56.09 3.80 -3 -5 -18 53.99 3.50 3 5 -18 60.79 4.00 3 5 -18 56.69 4.80 3 -6 -18 96.09 6.90 -3 6 -18 86.49 5.40 3 6 -18 94.59 6.40 3 6 -18 86.49 5.60 3 6 -18 85.89 5.70 -4 0 -18 271.07 15.60 4 0 -18 272.47 15.80 4 -1 -18 133.09 8.00 4 -1 -18 151.38 8.30 -4 1 -18 134.59 8.30 -4 -1 -18 135.19 8.20 4 1 -18 141.09 8.50 -4 2 -18 3.90 0.70 -4 2 -18 3.40 1.00 -4 2 -18 5.10 1.00 -4 2 -18 4.30 0.80 4 2 -18 4.10 1.10 -4 -2 -18 4.60 0.90 4 2 -18 6.40 1.90 4 2 -18 4.10 0.80 4 -3 -18 15.70 3.20 -4 3 -18 13.80 1.50 -4 3 -18 13.50 1.60 -4 3 -18 11.20 1.50 -4 3 -18 12.90 1.80 -4 -3 -18 13.20 1.40 4 3 -18 14.60 2.70 4 3 -18 12.50 1.60 4 -4 -18 75.39 6.30 -4 4 -18 70.39 4.60 -4 4 -18 74.69 4.90 4 4 -18 78.49 5.80 -4 -4 -18 74.99 4.60 4 4 -18 74.49 4.80 4 -5 -18 8.70 2.30 -4 5 -18 4.60 0.90 -4 5 -18 4.90 1.10 -4 -5 -18 4.40 1.00 4 5 -18 6.30 1.80 4 5 -18 5.30 1.10 4 5 -18 7.50 1.20 -4 6 -18 511.35 29.10 4 6 -18 542.95 29.40 4 6 -18 497.25 29.10 4 6 -18 526.75 30.00 -5 0 -18 189.88 11.40 5 0 -18 202.28 11.30 5 0 -18 196.18 11.40 -5 1 -18 97.59 6.30 5 -1 -18 117.79 6.30 5 -1 -18 103.69 6.20 -5 1 -18 102.49 6.50 -5 -1 -18 105.79 6.40 5 1 -18 112.29 6.60 -5 2 -18 60.99 4.00 -5 2 -18 61.29 3.80 -5 2 -18 52.29 3.80 -5 2 -18 59.79 4.10 -5 -2 -18 63.59 3.90 5 2 -18 59.39 3.70 5 2 -18 63.29 4.20 5 2 -18 68.89 5.00 -5 3 -18 53.59 3.60 -5 3 -18 56.89 4.00 5 3 -18 63.09 4.80 5 3 -18 58.19 3.70 -5 -3 -18 55.69 3.70 -5 4 -18 53.59 3.50 -5 4 -18 51.59 3.80 5 4 -18 56.79 3.60 -5 -4 -18 52.89 3.50 5 4 -18 54.89 3.60 5 4 -18 56.59 4.60 -5 5 -18 16.10 1.70 5 -5 -18 17.70 3.10 -5 5 -18 19.70 2.40 -5 -5 -18 17.10 1.50 5 5 -18 17.20 1.90 5 5 -18 21.90 1.80 5 5 -18 19.70 2.70 5 6 -18 79.09 5.60 6 0 -18 68.59 4.30 6 0 -18 72.39 4.40 -6 1 -18 123.19 7.60 -6 -1 -18 123.99 7.60 6 1 -18 133.99 7.70 -6 2 -18 58.69 4.00 -6 2 -18 58.69 3.70 6 2 -18 59.79 4.00 -6 -2 -18 61.99 3.90 -6 3 -18 74.39 5.10 -6 3 -18 79.69 4.90 -6 -3 -18 76.59 4.90 6 3 -18 89.59 5.90 6 3 -18 80.19 4.80 -6 4 -18 8.30 1.50 -6 4 -18 7.00 1.30 6 4 -18 8.50 1.20 -6 -4 -18 7.80 1.20 6 4 -18 8.10 1.30 6 4 -18 8.80 1.80 -6 5 -18 69.09 4.40 -6 -5 -18 68.29 4.40 6 5 -18 74.09 4.50 6 5 -18 70.79 4.50 6 5 -18 76.99 5.30 7 0 -18 221.68 12.60 7 0 -18 227.88 12.50 -7 0 -18 211.08 12.70 -7 1 -18 193.88 11.50 -7 -1 -18 193.88 11.40 7 1 -18 204.68 11.50 -7 2 -18 89.09 5.20 -7 2 -18 86.49 5.50 7 2 -18 89.79 5.50 -7 -2 -18 83.19 5.30 -7 3 -18 172.18 9.90 -7 3 -18 164.38 9.70 7 3 -18 161.48 9.90 -7 -3 -18 174.58 9.80 -7 4 -18 34.60 2.60 7 4 -18 38.60 2.50 7 4 -18 39.10 3.40 -7 -4 -18 38.00 2.60 8 0 -18 16.90 1.40 -8 0 -18 16.10 1.70 8 0 -18 17.00 1.40 -8 1 -18 225.88 13.60 8 1 -18 253.27 13.60 -8 -1 -18 231.78 13.60 -8 2 -18 2.60 0.90 8 2 -18 1.70 0.70 -8 -2 -18 1.60 0.70 -8 3 -18 34.40 2.40 -8 -3 -18 34.60 2.50 9 1 -18 10.30 1.20 9 2 -18 25.00 2.40 0 0 -19 3.40 1.20 0 0 -19 2.00 0.60 0 -1 -19 1.60 1.00 0 1 -19 1.30 0.70 0 2 -19 931.81 52.49 0 -2 -19 947.31 52.99 0 -3 -19 0.90 0.90 0 3 -19 0.60 1.30 0 3 -19 0.20 0.80 0 4 -19 320.67 18.70 0 4 -19 331.97 19.20 0 -4 -19 327.37 18.80 0 5 -19 0.70 0.80 0 5 -19 1.20 1.20 0 -5 -19 0.20 0.40 0 -5 -19 0.70 0.70 0 -6 -19 421.06 23.70 1 0 -19 0.20 0.90 1 0 -19 0.60 0.50 -1 0 -19 1.90 0.70 1 -1 -19 5.30 1.30 -1 1 -19 6.60 1.30 -1 -1 -19 5.90 1.50 1 1 -19 8.20 1.10 -1 -1 -19 7.20 1.00 1 1 -19 7.80 1.60 -1 2 -19 105.69 6.40 1 -2 -19 110.09 6.70 -1 -2 -19 100.79 6.10 1 2 -19 103.59 6.30 -1 -2 -19 107.79 7.00 -1 3 -19 1.00 0.90 -1 3 -19 2.60 1.30 1 -3 -19 2.20 0.60 1 -3 -19 3.20 1.00 1 3 -19 1.00 0.80 -1 -3 -19 4.50 1.20 1 3 -19 5.00 1.60 1 -4 -19 22.60 1.80 -1 4 -19 27.40 2.80 1 -4 -19 26.80 2.10 -1 4 -19 26.30 2.30 1 4 -19 27.10 2.30 -1 -4 -19 25.20 2.40 1 4 -19 27.30 3.00 -1 5 -19 65.69 4.70 1 -5 -19 60.99 3.90 1 -5 -19 70.59 4.10 -1 5 -19 62.39 4.30 1 5 -19 62.89 4.30 1 5 -19 67.09 4.90 -1 -5 -19 68.29 4.40 1 6 -19 11.80 2.70 2 0 -19 1.30 0.90 -2 0 -19 0.30 0.60 2 -1 -19 31.40 2.70 -2 1 -19 33.50 2.50 2 1 -19 34.20 2.20 2 1 -19 33.00 2.80 -2 -1 -19 33.40 2.30 2 -2 -19 398.86 21.10 -2 2 -19 365.66 20.90 2 -2 -19 337.67 20.70 -2 -2 -19 342.07 20.70 2 2 -19 366.86 20.80 -2 -2 -19 368.96 21.60 2 2 -19 402.66 21.70 2 -3 -19 230.48 13.90 2 -3 -19 263.77 14.10 -2 3 -19 246.68 14.20 2 3 -19 243.08 14.10 -2 -3 -19 229.58 13.90 -2 -3 -19 250.47 14.70 2 3 -19 261.47 14.90 -2 4 -19 118.19 7.10 2 -4 -19 115.89 8.10 2 4 -19 114.79 7.00 -2 -4 -19 107.99 7.30 2 4 -19 120.49 7.70 -2 5 -19 13.30 2.00 -2 5 -19 15.50 1.80 2 5 -19 15.70 2.40 2 5 -19 13.30 1.70 -2 -5 -19 14.10 1.80 -3 0 -19 6.20 1.20 -3 1 -19 60.39 4.00 3 -1 -19 65.69 4.10 3 -1 -19 60.59 3.80 3 1 -19 61.39 4.20 -3 -1 -19 60.69 3.90 3 -2 -19 1.30 0.60 3 -2 -19 1.70 0.50 -3 2 -19 0.60 0.80 3 2 -19 1.90 0.90 -3 -2 -19 1.30 0.60 3 2 -19 0.70 0.60 -3 3 -19 1.20 0.80 -3 -3 -19 2.10 0.60 3 3 -19 2.00 0.80 3 3 -19 2.80 1.50 -3 4 -19 2.70 0.90 3 -4 -19 2.30 1.70 -3 -4 -19 3.30 1.20 3 4 -19 3.10 0.90 3 4 -19 3.60 1.50 -3 -4 -19 2.90 0.60 3 5 -19 50.39 3.50 3 5 -19 52.29 4.20 4 0 -19 0.10 0.60 4 0 -19 0.80 0.60 -4 0 -19 1.10 0.70 -4 1 -19 36.90 2.80 4 -1 -19 40.30 2.50 -4 -1 -19 36.00 2.70 4 1 -19 42.80 3.00 -4 2 -19 31.80 2.50 -4 -2 -19 31.70 2.30 4 2 -19 31.00 2.60 -4 3 -19 0.00 0.80 4 3 -19 1.10 1.20 4 3 -19 1.70 0.70 -4 -3 -19 0.50 0.50 -4 4 -19 2.20 0.90 4 4 -19 3.40 0.80 4 4 -19 3.40 1.50 -4 -4 -19 1.90 0.60 4 5 -19 30.50 3.10 5 0 -19 0.80 0.60 -5 0 -19 -0.50 0.60 5 0 -19 0.80 0.50 -5 1 -19 105.79 6.50 -5 -1 -19 103.69 6.40 5 1 -19 113.49 6.60 -5 2 -19 198.88 11.30 5 2 -19 195.88 11.40 -5 -2 -19 189.98 11.20 -5 3 -19 11.60 1.60 -5 -3 -19 13.70 1.30 5 3 -19 12.70 1.80 5 4 -19 4.90 1.50 5 4 -19 3.40 0.90 -6 0 -19 0.00 0.70 6 0 -19 0.90 0.60 6 0 -19 0.80 0.50 -6 1 -19 518.65 29.80 -6 -1 -19 512.65 29.70 6 1 -19 558.14 29.80 -6 2 -19 72.19 4.70 -6 -2 -19 72.09 4.50 6 2 -19 77.79 4.70 -6 -3 -19 58.59 3.70 -7 0 -19 1.00 0.70 -7 1 -19 1.90 0.70 -7 -1 -19 1.80 0.70 7 1 -19 2.10 0.70 7 1 -19 1.50 0.60 -7 -2 -19 70.09 4.50 7 2 -19 75.69 4.60 8 1 -19 42.10 2.60 0 0 -20 14.80 1.90 0 -1 -20 0.40 0.80 0 1 -20 0.10 0.50 0 2 -20 11.20 1.20 0 -2 -20 7.70 1.40 0 3 -20 1.70 0.70 0 -3 -20 0.60 0.50 0 -3 -20 0.80 0.70 0 -4 -20 50.79 3.30 0 4 -20 49.80 3.40 0 -4 -20 50.29 3.30 1 0 -20 181.78 10.80 -1 0 -20 178.38 10.20 -1 1 -20 6.00 1.00 1 -1 -20 5.90 1.30 1 1 -20 7.00 1.50 -1 -1 -20 8.40 1.60 1 -2 -20 1.20 0.80 1 -2 -20 0.40 0.50 -1 2 -20 0.90 0.60 -1 -2 -20 0.70 0.90 1 2 -20 1.30 0.60 -1 3 -20 17.40 1.80 1 -3 -20 16.80 1.40 1 -3 -20 22.40 1.70 1 3 -20 18.40 1.70 -1 -3 -20 21.50 2.00 -1 4 -20 3.30 0.90 1 4 -20 3.40 1.00 -1 -4 -20 3.90 0.90 -2 0 -20 22.40 1.70 2 0 -20 23.60 2.10 2 -1 -20 145.29 9.10 2 -1 -20 174.28 9.40 -2 1 -20 158.18 9.10 2 1 -20 166.28 9.50 -2 -1 -20 148.59 9.00 2 -2 -20 73.59 4.30 2 -2 -20 64.79 4.10 -2 2 -20 70.49 4.30 -2 -2 -20 66.39 4.80 2 2 -20 70.89 4.60 -2 3 -20 6.80 1.30 -2 -3 -20 6.90 1.40 2 3 -20 6.00 1.00 3 0 -20 83.89 5.40 3 0 -20 99.09 5.50 -3 0 -20 84.79 5.30 -3 1 -20 60.39 3.90 3 -1 -20 57.69 3.70 3 -1 -20 67.89 3.90 3 1 -20 66.29 4.10 -3 -1 -20 59.59 3.80 -3 2 -20 1.40 0.70 3 2 -20 2.00 0.80 -3 -2 -20 1.40 0.50 -3 3 -20 1.20 0.70 4 0 -20 322.17 18.20 -4 0 -20 305.47 18.30 4 0 -20 344.97 18.30 -4 1 -20 2.90 0.80 -4 -1 -20 3.10 0.70 4 1 -20 3.90 0.80 -4 2 -20 -0.50 0.60 -4 -2 -20 0.60 0.50 4 2 -20 1.00 0.70 -5 0 -20 136.29 7.90 -5 1 -20 60.49 3.90 -5 -1 -20 59.09 3.80 5 1 -20 67.19 3.90 5 2 -20 27.40 2.30 6 1 -20 299.97 16.90 0 -1 -21 -0.10 0.60 0 -2 -21 124.49 7.40 1 0 -21 2.30 0.80 1 -1 -21 77.99 4.80 1 -2 -21 34.80 2.30 2 0 -21 0.10 0.50 2 -1 -21 28.60 1.90 3 0 -21 0.50 0.40 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 82595 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_I_CCDC4 _database_code_depnum_ccdc_archive 'CCDC 1875540' _audit_update_record ; 2018-10-26 deposited with the CCDC. 2018-12-12 downloaded from the CCDC. ; _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C16 H11 N O3 S' _chemical_formula_sum 'C16 H11 N O3 S' _chemical_formula_iupac ? _chemical_formula_weight 297.32 _chemical_melting_point ? _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.342(2) _cell_length_b 8.954(3) _cell_length_c 11.714(3) _cell_angle_alpha 70.226(9) _cell_angle_beta 83.607(9) _cell_angle_gamma 72.230(9) _cell_volume 690.1(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3237 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.05 _cell_measurement_temperature 300.(2) _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.400 _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 308 _exptl_absorpt_coefficient_mu 0.243 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; 'SADABS V2014/4 (Bruker AXS Inc.)' ; _exptl_absorpt_correction_T_min 0.7006 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ; _diffrn_ambient_temperature 300.(2) _diffrn_source 'micro-focus sealed tube' _diffrn_source_type 'Bruker X2S' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'doubly curved silicon crystal' _diffrn_measurement_device_type 'Bruker SMART X2S' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33333 _diffrn_reflns_number 6640 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_unetI/netI 0.0331 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measured_fraction_theta_full 0.982 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _refine_special_details ; ; _reflns_number_total 2407 _reflns_number_gt 1976 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_gt 0.1080 _refine_ls_wR_factor_ref 0.1166 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_number_reflns 2407 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.1657P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.282 _refine_diff_density_min -0.301 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ? _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 1.1012(3) 0.9816(2) 0.23454(16) 0.0785(5) Uani d . . . 1 . . N N5 0.9727(3) 0.9621(2) 0.33808(18) 0.0662(5) Uani d . . . 1 . . C C3 0.8991(3) 0.8456(2) 0.34865(17) 0.0465(5) Uani d . . . 1 . . C C4 0.9499(3) 0.7621(2) 0.25327(16) 0.0447(4) Uani d . . . 1 . . S S2 1.16608(9) 0.82459(8) 0.18166(5) 0.0658(2) Uani d . . . 1 . . O O6 1.3300(2) 0.6997(2) 0.2485(2) 0.0905(6) Uani d . . . 1 . . C C7 0.7619(3) 0.8079(2) 0.44785(17) 0.0464(4) Uani d . . . 1 . . C C8 0.6230(3) 0.7349(3) 0.4392(2) 0.0566(5) Uani d . . . 1 . . H H8 0.6194 0.705 0.3709 0.068 Uiso calc U . R 1 . . C C9 0.4914(3) 0.7071(3) 0.5315(2) 0.0711(6) Uani d . . . 1 . . H H9 0.3999 0.6576 0.5257 0.085 Uiso calc U . R 1 . . C C10 0.4946(4) 0.7527(3) 0.6327(2) 0.0741(7) Uani d . . . 1 . . H H10 0.4059 0.7333 0.695 0.089 Uiso calc U . R 1 . . C C11 0.6294(4) 0.8265(3) 0.6409(2) 0.0665(6) Uani d . . . 1 . . H H11 0.6301 0.8585 0.7085 0.08 Uiso calc U . R 1 . . C C12 0.7625(3) 0.8536(2) 0.55053(18) 0.0544(5) Uani d . . . 1 . . H H12 0.8538 0.9026 0.5576 0.065 Uiso calc U . R 1 . . C C13 0.7975(3) 0.8399(2) 0.15137(17) 0.0507(5) Uani d . . . 1 . . C C14 0.7841(3) 0.7037(2) 0.11370(17) 0.0467(4) Uani d . . . 1 . . C C15 0.6826(3) 0.7138(3) 0.01591(19) 0.0600(6) Uani d . . . 1 . . H H15 0.6106 0.8151 -0.0343 0.072 Uiso calc U . R 1 . . C C16 0.6935(3) 0.5672(4) -0.0032(2) 0.0677(7) Uani d . . . 1 . . H H16 0.6301 0.5697 -0.0685 0.081 Uiso calc U . R 1 . . C C17 0.7975(3) 0.4170(3) 0.0736(2) 0.0651(6) Uani d . . . 1 . . H H17 0.8008 0.3199 0.0598 0.078 Uiso calc U . R 1 . . C C18 0.8966(3) 0.4077(3) 0.17045(19) 0.0531(5) Uani d . . . 1 . . H H18 0.966 0.3058 0.2215 0.064 Uiso calc U . R 1 . . C C19 0.8904(2) 0.5532(2) 0.18994(16) 0.0424(4) Uani d . . . 1 . . C C20 0.9881(3) 0.5747(2) 0.28773(17) 0.0470(5) Uani d . . . 1 . . H H20A 1.1243 0.5196 0.2885 0.056 Uiso calc U . R 1 . . H H20B 0.9343 0.5302 0.367 0.056 Uiso calc U . R 1 . . O O21 0.7146(3) 0.98573(19) 0.11397(15) 0.0781(5) Uani d . . . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0941(12) 0.0652(10) 0.0893(12) -0.0470(9) 0.0231(10) -0.0274(9) N5 0.0829(13) 0.0593(11) 0.0706(12) -0.0380(10) 0.0123(10) -0.0270(9) C3 0.0572(11) 0.0381(10) 0.0460(10) -0.0140(8) -0.0083(9) -0.0130(8) C4 0.0510(11) 0.0383(10) 0.0414(10) -0.0097(8) -0.0070(8) -0.0091(8) S2 0.0678(4) 0.0697(4) 0.0633(4) -0.0279(3) 0.0107(3) -0.0219(3) O6 0.0547(9) 0.0925(13) 0.1220(16) -0.0196(9) -0.0006(10) -0.0329(11) C7 0.0554(11) 0.0339(9) 0.0466(10) -0.0091(8) -0.0071(9) -0.0099(8) C8 0.0593(12) 0.0508(12) 0.0625(13) -0.0186(10) -0.0001(10) -0.0194(10) C9 0.0620(14) 0.0619(14) 0.0875(18) -0.0232(11) 0.0055(13) -0.0187(13) C10 0.0703(15) 0.0632(15) 0.0659(15) -0.0074(12) 0.0158(12) -0.0076(12) C11 0.0827(16) 0.0560(13) 0.0486(12) -0.0063(12) -0.0011(12) -0.0136(10) C12 0.0674(13) 0.0439(11) 0.0487(11) -0.0105(9) -0.0097(10) -0.0128(9) C13 0.0565(11) 0.0425(11) 0.0423(10) -0.0052(9) -0.0095(9) -0.0053(8) C14 0.0411(9) 0.0557(11) 0.0414(10) -0.0120(8) -0.0006(8) -0.0150(9) C15 0.0473(11) 0.0841(16) 0.0457(11) -0.0195(11) -0.0050(9) -0.0154(11) C16 0.0614(13) 0.111(2) 0.0522(12) -0.0472(14) 0.0037(11) -0.0342(14) C17 0.0691(14) 0.0860(17) 0.0677(14) -0.0465(13) 0.0166(12) -0.0430(13) C18 0.0524(11) 0.0546(12) 0.0604(12) -0.0228(9) 0.0087(10) -0.0247(10) C19 0.0389(9) 0.0479(10) 0.0428(10) -0.0141(8) 0.0032(8) -0.0170(8) C20 0.0532(11) 0.0363(10) 0.0484(10) -0.0062(8) -0.0102(9) -0.0127(8) O21 0.0968(12) 0.0464(9) 0.0719(10) 0.0027(8) -0.0292(10) -0.0067(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 N5 . 1.447(3) ? O1 S2 . 1.6441(18) ? N5 C3 . 1.280(2) ? C3 C7 . 1.470(3) ? C3 C4 . 1.500(3) ? C4 C20 . 1.529(2) ? C4 C13 . 1.556(3) ? C4 S2 . 1.861(2) ? S2 O6 . 1.452(2) ? C7 C12 . 1.396(3) ? C7 C8 . 1.398(3) ? C8 C9 . 1.377(3) ? C8 H8 . 0.93 ? C9 C10 . 1.383(4) ? C9 H9 . 0.93 ? C10 C11 . 1.374(4) ? C10 H10 . 0.93 ? C11 C12 . 1.369(3) ? C11 H11 . 0.93 ? C12 H12 . 0.93 ? C13 O21 . 1.206(2) ? C13 C14 . 1.462(3) ? C14 C19 . 1.386(3) ? C14 C15 . 1.398(3) ? C15 C16 . 1.382(3) ? C15 H15 . 0.93 ? C16 C17 . 1.382(3) ? C16 H16 . 0.93 ? C17 C18 . 1.380(3) ? C17 H17 . 0.93 ? C18 C19 . 1.384(3) ? C18 H18 . 0.93 ? C19 C20 . 1.510(3) ? C20 H20A . 0.97 ? C20 H20B . 0.97 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N5 O1 S2 . . 114.49(11) ? C3 N5 O1 . . 110.55(17) ? N5 C3 C7 . . 118.89(17) ? N5 C3 C4 . . 117.31(18) ? C7 C3 C4 . . 123.68(16) ? C3 C4 C20 . . 120.61(16) ? C3 C4 C13 . . 111.60(16) ? C20 C4 C13 . . 105.78(14) ? C3 C4 S2 . . 101.99(12) ? C20 C4 S2 . . 110.55(13) ? C13 C4 S2 . . 105.40(12) ? O6 S2 O1 . . 109.64(11) ? O6 S2 C4 . . 106.86(10) ? O1 S2 C4 . . 89.70(8) ? C12 C7 C8 . . 118.8(2) ? C12 C7 C3 . . 119.73(18) ? C8 C7 C3 . . 121.40(17) ? C9 C8 C7 . . 120.1(2) ? C9 C8 H8 . . 119.9 ? C7 C8 H8 . . 119.9 ? C8 C9 C10 . . 120.3(2) ? C8 C9 H9 . . 119.9 ? C10 C9 H9 . . 119.9 ? C11 C10 C9 . . 119.8(2) ? C11 C10 H10 . . 120.1 ? C9 C10 H10 . . 120.1 ? C12 C11 C10 . . 120.7(2) ? C12 C11 H11 . . 119.6 ? C10 C11 H11 . . 119.6 ? C11 C12 C7 . . 120.3(2) ? C11 C12 H12 . . 119.9 ? C7 C12 H12 . . 119.9 ? O21 C13 C14 . . 129.91(19) ? O21 C13 C4 . . 123.75(18) ? C14 C13 C4 . . 106.33(15) ? C19 C14 C15 . . 121.82(19) ? C19 C14 C13 . . 110.41(16) ? C15 C14 C13 . . 127.77(19) ? C16 C15 C14 . . 117.4(2) ? C16 C15 H15 . . 121.3 ? C14 C15 H15 . . 121.3 ? C17 C16 C15 . . 120.8(2) ? C17 C16 H16 . . 119.6 ? C15 C16 H16 . . 119.6 ? C18 C17 C16 . . 121.5(2) ? C18 C17 H17 . . 119.2 ? C16 C17 H17 . . 119.2 ? C17 C18 C19 . . 118.6(2) ? C17 C18 H18 . . 120.7 ? C19 C18 H18 . . 120.7 ? C18 C19 C14 . . 119.81(18) ? C18 C19 C20 . . 128.25(17) ? C14 C19 C20 . . 111.94(16) ? C19 C20 C4 . . 104.17(14) ? C19 C20 H20A . . 110.9 ? C4 C20 H20A . . 110.9 ? C19 C20 H20B . . 110.9 ? C4 C20 H20B . . 110.9 ? H20A C20 H20B . . 108.9 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag S2 O1 N5 C3 . . . . -16.0(2) ? O1 N5 C3 C7 . . . . -179.16(16) ? O1 N5 C3 C4 . . . . -2.9(3) ? N5 C3 C4 C20 . . . . 140.0(2) ? C7 C3 C4 C20 . . . . -43.9(3) ? N5 C3 C4 C13 . . . . -95.0(2) ? C7 C3 C4 C13 . . . . 81.2(2) ? N5 C3 C4 S2 . . . . 17.1(2) ? C7 C3 C4 S2 . . . . -166.76(15) ? N5 O1 S2 O6 . . . . -85.71(17) ? N5 O1 S2 C4 . . . . 22.11(16) ? C3 C4 S2 O6 . . . . 89.56(14) ? C20 C4 S2 O6 . . . . -39.90(16) ? C13 C4 S2 O6 . . . . -153.76(14) ? C3 C4 S2 O1 . . . . -20.90(13) ? C20 C4 S2 O1 . . . . -150.36(13) ? C13 C4 S2 O1 . . . . 95.77(13) ? N5 C3 C7 C12 . . . . -22.3(3) ? C4 C3 C7 C12 . . . . 161.71(18) ? N5 C3 C7 C8 . . . . 154.2(2) ? C4 C3 C7 C8 . . . . -21.8(3) ? C12 C7 C8 C9 . . . . -0.9(3) ? C3 C7 C8 C9 . . . . -177.35(18) ? C7 C8 C9 C10 . . . . 0.6(3) ? C8 C9 C10 C11 . . . . 0.3(4) ? C9 C10 C11 C12 . . . . -0.9(3) ? C10 C11 C12 C7 . . . . 0.7(3) ? C8 C7 C12 C11 . . . . 0.2(3) ? C3 C7 C12 C11 . . . . 176.77(17) ? C3 C4 C13 O21 . . . . 36.7(3) ? C20 C4 C13 O21 . . . . 169.6(2) ? S2 C4 C13 O21 . . . . -73.3(2) ? C3 C4 C13 C14 . . . . -144.42(17) ? C20 C4 C13 C14 . . . . -11.5(2) ? S2 C4 C13 C14 . . . . 105.65(15) ? O21 C13 C14 C19 . . . . -173.7(2) ? C4 C13 C14 C19 . . . . 7.5(2) ? O21 C13 C14 C15 . . . . 6.6(4) ? C4 C13 C14 C15 . . . . -172.26(18) ? C19 C14 C15 C16 . . . . -0.6(3) ? C13 C14 C15 C16 . . . . 179.0(2) ? C14 C15 C16 C17 . . . . 1.4(3) ? C15 C16 C17 C18 . . . . -1.1(3) ? C16 C17 C18 C19 . . . . 0.0(3) ? C17 C18 C19 C14 . . . . 0.8(3) ? C17 C18 C19 C20 . . . . -179.10(18) ? C15 C14 C19 C18 . . . . -0.5(3) ? C13 C14 C19 C18 . . . . 179.78(17) ? C15 C14 C19 C20 . . . . 179.44(17) ? C13 C14 C19 C20 . . . . -0.3(2) ? C18 C19 C20 C4 . . . . 172.87(19) ? C14 C19 C20 C4 . . . . -7.0(2) ? C3 C4 C20 C19 . . . . 138.71(17) ? C13 C4 C20 C19 . . . . 10.99(19) ? S2 C4 C20 C19 . . . . -102.63(15) ? _shelx_res_file ; TITL scan_0m_P-1 in P-1 CELL 0.71073 7.3422 8.9542 11.7143 70.226 83.607 72.230 ZERR 2.00 0.0022 0.0026 0.0032 0.009 0.009 0.009 LATT 1 SFAC C H N O S UNIT 32 22 2 6 2 OMIT 0 0 1 L.S. 5 ACTA BOND $H FMAP 2 PLAN 5 CONF SIZE 0.400 0.400 0.400 CONF TEMP 27.000 WGHT 0.057600 0.165700 FVAR 0.38217 O1 4 1.101246 0.981639 0.234538 11.00000 0.09407 0.06525 = 0.08933 -0.02740 0.02311 -0.04699 N5 3 0.972723 0.962133 0.338080 11.00000 0.08291 0.05934 = 0.07063 -0.02705 0.01231 -0.03796 C3 1 0.899121 0.845584 0.348650 11.00000 0.05717 0.03809 = 0.04600 -0.01304 -0.00829 -0.01398 C4 1 0.949855 0.762103 0.253266 11.00000 0.05100 0.03831 = 0.04142 -0.00912 -0.00704 -0.00974 S2 5 1.166077 0.824590 0.181661 11.00000 0.06784 0.06973 = 0.06328 -0.02191 0.01068 -0.02791 O6 4 1.329981 0.699718 0.248454 11.00000 0.05467 0.09246 = 0.12204 -0.03294 -0.00060 -0.01964 C7 1 0.761927 0.807857 0.447853 11.00000 0.05541 0.03388 = 0.04659 -0.00993 -0.00713 -0.00907 C8 1 0.622971 0.734896 0.439159 11.00000 0.05935 0.05078 = 0.06251 -0.01940 -0.00012 -0.01858 AFIX 43 H8 2 0.619358 0.705032 0.370920 11.00000 -1.20000 AFIX 0 C9 1 0.491382 0.707147 0.531465 11.00000 0.06199 0.06191 = 0.08751 -0.01873 0.00553 -0.02324 AFIX 43 H9 2 0.399918 0.657579 0.525692 11.00000 -1.20000 AFIX 0 C10 1 0.494644 0.752656 0.632693 11.00000 0.07026 0.06320 = 0.06587 -0.00762 0.01583 -0.00744 AFIX 43 H10 2 0.405942 0.733345 0.695045 11.00000 -1.20000 AFIX 0 C11 1 0.629375 0.826505 0.640858 11.00000 0.08273 0.05603 = 0.04857 -0.01355 -0.00111 -0.00632 AFIX 43 H11 2 0.630133 0.858461 0.708488 11.00000 -1.20000 AFIX 0 C12 1 0.762527 0.853571 0.550531 11.00000 0.06740 0.04395 = 0.04867 -0.01277 -0.00970 -0.01053 AFIX 43 H12 2 0.853760 0.902614 0.557598 11.00000 -1.20000 AFIX 0 C13 1 0.797470 0.839888 0.151367 11.00000 0.05648 0.04246 = 0.04226 -0.00533 -0.00949 -0.00517 C14 1 0.784050 0.703736 0.113700 11.00000 0.04113 0.05569 = 0.04144 -0.01497 -0.00065 -0.01203 C15 1 0.682629 0.713756 0.015912 11.00000 0.04734 0.08412 = 0.04572 -0.01545 -0.00495 -0.01954 AFIX 43 H15 2 0.610623 0.815134 -0.034344 11.00000 -1.20000 AFIX 0 C16 1 0.693526 0.567207 -0.003167 11.00000 0.06136 0.11075 = 0.05224 -0.03420 0.00368 -0.04720 AFIX 43 H16 2 0.630082 0.569701 -0.068511 11.00000 -1.20000 AFIX 0 C17 1 0.797508 0.417004 0.073627 11.00000 0.06911 0.08605 = 0.06774 -0.04301 0.01664 -0.04647 AFIX 43 H17 2 0.800829 0.319888 0.059763 11.00000 -1.20000 AFIX 0 C18 1 0.896590 0.407689 0.170453 11.00000 0.05243 0.05457 = 0.06038 -0.02465 0.00870 -0.02276 AFIX 43 H18 2 0.966047 0.305787 0.221499 11.00000 -1.20000 AFIX 0 C19 1 0.890358 0.553237 0.189943 11.00000 0.03890 0.04791 = 0.04276 -0.01696 0.00317 -0.01411 C20 1 0.988122 0.574651 0.287727 11.00000 0.05324 0.03633 = 0.04844 -0.01267 -0.01015 -0.00623 AFIX 23 H20A 2 1.124313 0.519641 0.288549 11.00000 -1.20000 H20B 2 0.934278 0.530219 0.366984 11.00000 -1.20000 AFIX 0 O21 4 0.714613 0.985734 0.113970 11.00000 0.09679 0.04636 = 0.07189 -0.00666 -0.02916 0.00275 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM scan_0m_P-1 in P-1 REM R1 = 0.0405 for 1976 Fo > 4sig(Fo) and 0.0503 for all 2407 data REM 190 parameters refined using 0 restraints END WGHT 0.0574 0.1658 REM Highest difference peak 0.282, deepest hole -0.301, 1-sigma level 0.043 Q1 1 1.0572 0.7842 0.2258 11.00000 0.05 0.28 Q2 1 0.6189 0.9357 0.1720 11.00000 0.05 0.17 Q3 1 1.2465 0.8959 0.1121 11.00000 0.05 0.17 Q4 1 0.8555 0.8069 0.4073 11.00000 0.05 0.16 Q5 1 1.4440 0.7379 0.1686 11.00000 0.05 0.15 ; _shelx_res_checksum 31720 _shelx_hkl_file ; -1 0 0 201.41 8.42 1 0 0 191.60 10.35 -2 0 0 97.96 5.09 -2 0 0 105.11 4.69 -2 0 0 93.35 4.14 2 0 0 92.95 4.69 2 0 0 91.99 4.14 -3 0 0 1.60 0.16 -3 0 0 1.75 0.16 -3 0 0 2.23 0.20 3 0 0 1.69 0.17 3 0 0 1.73 0.18 3 0 0 1.92 0.17 -4 0 0 0.98 0.15 4 0 0 0.99 0.13 4 0 0 0.75 0.14 -5 0 0 1.46 0.21 5 0 0 1.67 0.22 5 0 0 1.69 0.19 -6 0 0 7.98 0.56 6 0 0 7.95 0.48 6 0 0 7.13 0.53 -7 0 0 2.50 0.33 7 0 0 2.40 0.34 7 0 0 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