#=============================================================================== data_SRX-PTSA #=============================================================================== _audit_creation_method 'SHELXL-2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H7 O3 S, C23 H24 Cl N6 O2' _chemical_formula_sum 'C30 H31 Cl N6 O5 S' _chemical_formula_weight 623.12 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 21' _space_group_name_Hall 'P 2yb' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.247(6) _cell_length_b 7.6192(16) _cell_length_c 15.469(10) _cell_angle_alpha 90 _cell_angle_beta 92.42(6) _cell_angle_gamma 90 _cell_volume 1559.9(13) _cell_formula_units_Z 2 _cell_measurement_temperature 394(2) _cell_measurement_reflns_used 1100 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 29.1 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_F_000 652 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_absorpt_coefficient_mu 0.238 _shelx_estimated_absorpt_T_min 0.932 _shelx_estimated_absorpt_T_max 0.977 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.923 _exptl_absorpt_correction_T_max 0.954 _exptl_absorpt_process_details SADABS _exptl_absorpt_special_details ? _diffrn_ambient_temperature 394(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6458 _diffrn_reflns_av_unetI/netI 0.3514 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.636 _diffrn_reflns_theta_max 29.146 _diffrn_reflns_theta_full 26.000 _diffrn_measured_fraction_theta_max 0.823 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.823 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.822 _diffrn_reflns_point_group_measured_fraction_full 0.989 _reflns_number_total 5302 _reflns_number_gt 1092 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.863 _reflns_Friedel_fraction_max 0.821 _reflns_Friedel_fraction_full 0.993 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.2(3) _chemical_absolute_configuration rm _refine_ls_number_reflns 5302 _refine_ls_number_parameters 392 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.4052 _refine_ls_R_factor_gt 0.0956 _refine_ls_wR_factor_ref 0.2293 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.7402(5) 0.4980(7) 0.1502(5) 0.099(2) Uani 1 1 d . . . . . Cl Cl 0.8270(7) 1.0503(12) 0.4747(5) 0.227(5) Uani 1 1 d . . . . . O1 O 0.9331(10) 0.8480(17) 0.1273(11) 0.080(4) Uani 1 1 d . . . . . N2 N 0.8882(13) 0.984(2) 0.0010(14) 0.080(5) Uani 1 1 d . . . . . N3 N 0.8319(10) 0.7939(18) -0.1563(9) 0.063(5) Uani 1 1 d . . . . . C24 C 0.6548(18) 0.500(3) 0.2341(16) 0.086(7) Uani 1 1 d . . . . . O5 O 0.8419(10) 0.4723(17) 0.1857(10) 0.109(5) Uani 1 1 d . . . . . O3 O 0.7080(11) 0.3510(18) 0.0926(10) 0.122(6) Uani 1 1 d . . . . . C15 C 0.7030(15) 0.556(2) -0.174(2) 0.074(8) Uani 1 1 d . . . . . C16 C 0.6445(18) 0.543(2) -0.1071(15) 0.083(7) Uani 1 1 d . . . . . H16 H 0.6710 0.5767 -0.0529 0.100 Uiso 1 1 calc R U . . . C7 C 0.8830(16) 0.976(3) 0.0831(19) 0.071(7) Uani 1 1 d . . . . . C12 C 0.8295(15) 1.118(2) -0.0498(13) 0.081(7) Uani 1 1 d . . . . . H12A H 0.8708 1.1668 -0.0941 0.097 Uiso 1 1 calc R U . . . H12B H 0.8096 1.2120 -0.0120 0.097 Uiso 1 1 calc R U . . . C6 C 0.9156(16) 0.873(3) 0.2153(19) 0.070(7) Uani 1 1 d . . . . . C20 C 0.669(2) 0.499(3) -0.2566(17) 0.079(7) Uani 1 1 d . . . . . C9 C 0.9354(12) 0.849(2) -0.1402(13) 0.069(6) Uani 1 1 d . . . . . H9A H 0.9464 0.9620 -0.1675 0.082 Uiso 1 1 calc R U . . . H9B H 0.9811 0.7646 -0.1641 0.082 Uiso 1 1 calc R U . . . C1 C 0.8479(19) 1.016(3) 0.2206(17) 0.095(8) Uani 1 1 d . . . . . O4 O 0.7254(11) 0.6650(17) 0.1060(8) 0.108(6) Uani 1 1 d . . . . . N1 N 0.8281(13) 1.066(2) 0.1378(13) 0.088(6) Uani 1 1 d . . . . . H1 H 0.7854 1.1468 0.1226 0.106 Uiso 1 1 calc R U . . . C4 C 0.921(2) 0.852(3) 0.3632(18) 0.116(9) Uani 1 1 d . . . . . H4 H 0.9432 0.7933 0.4132 0.139 Uiso 1 1 calc R U . . . C2 C 0.8213(19) 1.071(3) 0.3020(18) 0.121(10) Uani 1 1 d . . . . . H2 H 0.7752 1.1617 0.3069 0.146 Uiso 1 1 calc R U . . . C11 C 0.7342(12) 1.029(3) -0.0923(14) 0.093(7) Uani 1 1 d . . . . . H11A H 0.7061 0.9482 -0.0511 0.112 Uiso 1 1 calc R U . . . H11B H 0.6838 1.1181 -0.1058 0.112 Uiso 1 1 calc R U . . . N4 N 0.728(3) 0.515(3) -0.3254(14) 0.117(9) Uani 1 1 d . . . . . C8 C 0.9554(13) 0.864(2) -0.0423(12) 0.070(6) Uani 1 1 d . . . . . H8A H 0.9493 0.7487 -0.0169 0.084 Uiso 1 1 calc R U . . . H8B H 1.0244 0.9035 -0.0314 0.084 Uiso 1 1 calc R U . . . C14 C 0.810(2) 0.609(3) -0.1576(16) 0.093(9) Uani 1 1 d . . . . . C17 C 0.545(3) 0.482(4) -0.113(2) 0.124(12) Uani 1 1 d . . . . . O2 O 0.8800(11) 0.5149(18) -0.1380(10) 0.111(6) Uani 1 1 d . . . . . C13 C 0.7772(14) 1.041(3) -0.2551(12) 0.115(8) Uani 1 1 d . . . . . H13A H 0.8397 1.1032 -0.2455 0.173 Uiso 1 1 calc R U . . . H13B H 0.7232 1.1238 -0.2646 0.173 Uiso 1 1 calc R U . . . H13C H 0.7815 0.9669 -0.3049 0.173 Uiso 1 1 calc R U . . . C28 C 0.5130(18) 0.404(3) 0.308(2) 0.114(9) Uani 1 1 d . . . . . H28 H 0.4574 0.3297 0.3111 0.137 Uiso 1 1 calc R U . . . C30 C 0.4594(15) 0.525(3) 0.4500(13) 0.145(11) Uani 1 1 d . . . . . H30A H 0.3993 0.4621 0.4322 0.217 Uiso 1 1 calc R U . . . H30B H 0.4423 0.6444 0.4629 0.217 Uiso 1 1 calc R U . . . H30C H 0.4900 0.4708 0.5006 0.217 Uiso 1 1 calc R U . . . C18 C 0.517(3) 0.418(4) -0.190(3) 0.15(2) Uani 1 1 d . . . . . H18 H 0.4556 0.3585 -0.1948 0.185 Uiso 1 1 calc R U . . . C25 C 0.6752(19) 0.616(3) 0.3001(18) 0.106(9) Uani 1 1 d . . . . . H25 H 0.7307 0.6909 0.2984 0.127 Uiso 1 1 calc R U . . . C27 C 0.534(3) 0.522(4) 0.3766(19) 0.123(11) Uani 1 1 d . . . . . C10 C 0.7566(15) 0.928(3) -0.1753(13) 0.076(6) Uani 1 1 d . . . . . H10 H 0.6943 0.8640 -0.1907 0.091 Uiso 1 1 calc R U . . . C26 C 0.611(2) 0.623(3) 0.371(2) 0.121(12) Uani 1 1 d . . . . . H26 H 0.6252 0.7026 0.4154 0.146 Uiso 1 1 calc R U . . . C23 C 0.4798(19) 0.460(3) -0.0368(16) 0.178(15) Uani 1 1 d . . . . . H23A H 0.5117 0.3796 0.0037 0.266 Uiso 1 1 calc R U . . . H23B H 0.4152 0.4139 -0.0560 0.266 Uiso 1 1 calc R U . . . H23C H 0.4708 0.5713 -0.0093 0.266 Uiso 1 1 calc R U . . . C19 C 0.570(2) 0.433(3) -0.263(2) 0.118(12) Uani 1 1 d . . . . . H19 H 0.5420 0.3988 -0.3163 0.142 Uiso 1 1 calc R U . . . C29 C 0.5744(18) 0.394(3) 0.2359(19) 0.119(10) Uani 1 1 d . . . . . H29 H 0.5593 0.3166 0.1908 0.143 Uiso 1 1 calc R U . . . C5 C 0.9537(18) 0.787(3) 0.286(2) 0.110(9) Uani 1 1 d . . . . . H5 H 0.9977 0.6922 0.2828 0.132 Uiso 1 1 calc R U . . . C3 C 0.861(3) 0.994(4) 0.3740(19) 0.160(13) Uani 1 1 d . . . . . C22 C 0.783(5) 0.506(7) -0.4541(19) 0.20(2) Uani 1 1 d . . . . . H22 H 0.7889 0.4882 -0.5132 0.246 Uiso 1 1 calc R U . . . C21 C 0.839(4) 0.584(6) -0.406(3) 0.22(3) Uani 1 1 d . . . . . H21 H 0.9027 0.6241 -0.4208 0.264 Uiso 1 1 calc R U . . . N6 N 0.705(2) 0.445(4) -0.400(2) 0.205(15) Uani 1 1 d . . . . . N5 N 0.805(3) 0.607(4) -0.336(2) 0.26(2) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.101(5) 0.062(4) 0.135(6) -0.008(5) 0.021(5) 0.010(4) Cl 0.398(13) 0.183(9) 0.106(6) -0.021(6) 0.092(8) 0.038(9) O1 0.092(11) 0.053(9) 0.094(14) 0.008(10) 0.011(10) -0.014(8) N2 0.090(14) 0.061(12) 0.090(15) 0.006(14) 0.014(13) -0.002(11) N3 0.034(10) 0.067(11) 0.089(14) 0.003(9) 0.011(9) 0.025(8) C24 0.13(2) 0.017(9) 0.12(2) 0.003(14) 0.055(16) 0.003(12) O5 0.080(11) 0.065(9) 0.183(16) 0.012(10) 0.001(11) -0.001(8) O3 0.133(14) 0.074(9) 0.157(16) -0.023(11) -0.014(12) -0.004(10) C15 0.041(14) 0.052(13) 0.13(3) 0.010(15) 0.046(16) -0.003(11) C16 0.077(17) 0.055(14) 0.12(2) 0.009(14) 0.006(17) -0.005(13) C7 0.073(15) 0.030(12) 0.11(2) 0.003(17) 0.045(17) -0.030(12) C12 0.102(18) 0.042(12) 0.099(19) 0.001(12) 0.028(16) 0.012(12) C6 0.084(17) 0.037(13) 0.09(2) 0.018(15) 0.039(17) -0.012(11) C20 0.14(3) 0.038(11) 0.056(18) -0.010(15) 0.007(18) 0.011(15) C9 0.026(11) 0.071(12) 0.11(2) 0.001(14) 0.003(12) 0.005(10) C1 0.18(2) 0.049(14) 0.061(18) -0.027(16) 0.022(18) 0.001(16) O4 0.165(16) 0.063(8) 0.098(13) 0.000(9) 0.024(11) 0.019(9) N1 0.129(16) 0.055(11) 0.083(15) -0.013(12) 0.038(14) 0.019(11) C4 0.19(3) 0.066(16) 0.10(2) -0.018(17) 0.03(2) -0.008(19) C2 0.21(3) 0.073(16) 0.09(2) -0.038(18) 0.03(2) 0.027(18) C11 0.045(13) 0.082(16) 0.15(2) -0.030(16) 0.009(14) 0.006(12) N4 0.24(3) 0.063(13) 0.048(16) 0.004(15) 0.01(2) 0.028(18) C8 0.056(13) 0.067(13) 0.088(19) -0.015(14) 0.010(13) -0.004(11) C14 0.13(3) 0.050(15) 0.10(2) -0.011(13) 0.048(19) 0.031(15) C17 0.13(3) 0.060(19) 0.19(4) -0.01(2) 0.01(3) 0.01(2) O2 0.113(13) 0.057(9) 0.163(16) -0.011(11) 0.014(11) 0.005(10) C13 0.14(2) 0.089(16) 0.112(19) 0.057(17) 0.009(17) 0.011(16) C28 0.10(2) 0.11(2) 0.13(3) 0.02(2) 0.03(2) -0.033(16) C30 0.16(2) 0.13(2) 0.16(3) 0.03(2) 0.06(2) 0.03(2) C18 0.13(3) 0.035(15) 0.30(7) 0.01(3) 0.04(4) -0.008(17) C25 0.12(2) 0.09(2) 0.11(3) 0.004(19) 0.04(2) 0.011(17) C27 0.20(4) 0.066(19) 0.10(2) -0.02(2) 0.00(2) 0.04(2) C10 0.075(16) 0.070(14) 0.083(18) -0.003(14) 0.003(14) -0.006(11) C26 0.16(3) 0.07(2) 0.13(3) -0.02(2) -0.02(3) -0.008(19) C23 0.21(3) 0.10(2) 0.23(4) 0.00(2) 0.13(3) 0.00(2) C19 0.11(3) 0.071(18) 0.17(4) -0.01(2) -0.06(2) -0.018(18) C29 0.10(2) 0.090(18) 0.17(3) 0.011(18) 0.05(2) -0.031(16) C5 0.14(2) 0.071(16) 0.12(3) 0.00(2) 0.02(2) 0.011(15) C3 0.28(4) 0.10(2) 0.11(3) 0.05(2) 0.05(3) 0.02(3) C22 0.35(6) 0.22(4) 0.05(2) -0.02(3) 0.08(4) 0.06(4) C21 0.35(7) 0.24(5) 0.08(3) -0.07(3) 0.08(4) 0.00(4) N6 0.31(4) 0.23(3) 0.07(2) -0.01(2) 0.02(3) -0.07(3) N5 0.38(5) 0.23(3) 0.20(4) -0.11(3) 0.22(3) -0.13(3) _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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O5 1.447(13) . ? S1 O4 1.454(13) . ? S1 O3 1.482(14) . ? S1 C24 1.76(2) . ? Cl C3 1.69(3) . ? O1 C7 1.35(2) . ? O1 C6 1.40(2) . ? N2 C7 1.28(2) . ? N2 C8 1.45(2) . ? N2 C12 1.49(2) . ? N3 C14 1.44(2) . ? N3 C9 1.446(17) . ? N3 C10 1.45(2) . ? C24 C29 1.34(2) . ? C24 C25 1.37(3) . ? C15 C16 1.32(2) . ? C15 C20 1.41(3) . ? C15 C14 1.49(3) . ? C16 C17 1.39(3) . ? C16 H16 0.9300 . ? C7 N1 1.33(2) . ? C12 C11 1.55(2) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C6 C5 1.35(3) . ? C6 C1 1.42(3) . ? C20 N4 1.35(3) . ? C20 C19 1.40(3) . ? C9 C8 1.53(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C1 N1 1.35(2) . ? C1 C2 1.39(2) . ? N1 H1 0.8600 . ? C4 C3 1.36(3) . ? C4 C5 1.38(3) . ? C4 H4 0.9300 . ? C2 C3 1.34(3) . ? C2 H2 0.9300 . ? C11 C10 1.54(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? N4 N5 1.26(3) . ? N4 N6 1.29(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C14 O2 1.20(2) . ? C17 C18 1.33(4) . ? C17 C23 1.51(4) . ? C13 C10 1.54(2) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C28 C27 1.41(3) . ? C28 C29 1.42(3) . ? C28 H28 0.9300 . ? C30 C27 1.54(3) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C18 C19 1.36(4) . ? C18 H18 0.9300 . ? C25 C26 1.42(3) . ? C25 H25 0.9300 . ? C27 C26 1.28(3) . ? C10 H10 0.9800 . ? C26 H26 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C19 H19 0.9300 . ? C29 H29 0.9300 . ? C5 H5 0.9300 . ? C22 C21 1.19(7) . ? C22 N6 1.44(5) . ? C22 H22 0.9300 . ? C21 N5 1.20(4) . ? C21 H21 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 S1 O4 113.7(9) . . ? O5 S1 O3 111.4(9) . . ? O4 S1 O3 110.4(9) . . ? O5 S1 C24 109.9(11) . . ? O4 S1 C24 105.1(9) . . ? O3 S1 C24 105.9(12) . . ? C7 O1 C6 107.2(18) . . ? C7 N2 C8 119(2) . . ? C7 N2 C12 120(2) . . ? C8 N2 C12 120.1(17) . . ? C14 N3 C9 118.4(16) . . ? C14 N3 C10 123.6(17) . . ? C9 N3 C10 117.9(14) . . ? C29 C24 C25 120(2) . . ? C29 C24 S1 123(2) . . ? C25 C24 S1 116(2) . . ? C16 C15 C20 121(2) . . ? C16 C15 C14 118(3) . . ? C20 C15 C14 120(2) . . ? C15 C16 C17 124(3) . . ? C15 C16 H16 118.2 . . ? C17 C16 H16 118.2 . . ? N2 C7 N1 132(3) . . ? N2 C7 O1 119(2) . . ? N1 C7 O1 109(2) . . ? N2 C12 C11 108.8(14) . . ? N2 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? N2 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? C5 C6 O1 130(2) . . ? C5 C6 C1 123(3) . . ? O1 C6 C1 107(2) . . ? N4 C20 C19 123(3) . . ? N4 C20 C15 121(3) . . ? C19 C20 C15 116(2) . . ? N3 C9 C8 108.5(15) . . ? N3 C9 H9A 110.0 . . ? C8 C9 H9A 110.0 . . ? N3 C9 H9B 110.0 . . ? C8 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? N1 C1 C2 137(3) . . ? N1 C1 C6 105(2) . . ? C2 C1 C6 118(3) . . ? C7 N1 C1 111(2) . . ? C7 N1 H1 124.3 . . ? C1 N1 H1 124.3 . . ? C3 C4 C5 127(3) . . ? C3 C4 H4 116.6 . . ? C5 C4 H4 116.6 . . ? C3 C2 C1 121(3) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.5 . . ? C10 C11 C12 112.9(14) . . ? C10 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? C10 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N5 N4 N6 106(3) . . ? N5 N4 C20 131(3) . . ? N6 N4 C20 123(4) . . ? N2 C8 C9 114.8(16) . . ? N2 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? N2 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? O2 C14 N3 116(2) . . ? O2 C14 C15 126.8(19) . . ? N3 C14 C15 117.2(18) . . ? C18 C17 C16 115(4) . . ? C18 C17 C23 121(4) . . ? C16 C17 C23 124(3) . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C27 C28 C29 122(3) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C17 C18 C19 125(5) . . ? C17 C18 H18 117.5 . . ? C19 C18 H18 117.5 . . ? C24 C25 C26 120(3) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C26 C27 C28 118(3) . . ? C26 C27 C30 125(3) . . ? C28 C27 C30 117(3) . . ? N3 C10 C11 109.8(16) . . ? N3 C10 C13 114.4(16) . . ? C11 C10 C13 116.0(16) . . ? N3 C10 H10 105.2 . . ? C11 C10 H10 105.2 . . ? C13 C10 H10 105.2 . . ? C27 C26 C25 122(3) . . ? C27 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? C17 C23 H23A 109.5 . . ? C17 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C17 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C18 C19 C20 119(4) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C24 C29 C28 118(2) . . ? C24 C29 H29 121.0 . . ? C28 C29 H29 121.0 . . ? C6 C5 C4 114(2) . . ? C6 C5 H5 123.0 . . ? C4 C5 H5 123.0 . . ? C2 C3 C4 117(3) . . ? C2 C3 Cl 123(3) . . ? C4 C3 Cl 120(3) . . ? C21 C22 N6 104(4) . . ? C21 C22 H22 128.0 . . ? N6 C22 H22 128.0 . . ? C22 C21 N5 113(7) . . ? C22 C21 H21 123.7 . . ? N5 C21 H21 123.7 . . ? N4 N6 C22 104(3) . . ? C21 N5 N4 113(4) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 S1 C24 C29 -125(2) . . . . ? O4 S1 C24 C29 112(2) . . . . ? O3 S1 C24 C29 -5(2) . . . . ? O5 S1 C24 C25 53.8(19) . . . . ? O4 S1 C24 C25 -69(2) . . . . ? O3 S1 C24 C25 174.2(18) . . . . ? C20 C15 C16 C17 -3(3) . . . . ? C14 C15 C16 C17 -175(2) . . . . ? C8 N2 C7 N1 -179.0(17) . . . . ? C12 N2 C7 N1 4(3) . . . . ? C8 N2 C7 O1 -6(3) . . . . ? C12 N2 C7 O1 176.7(14) . . . . ? C6 O1 C7 N2 179.2(17) . . . . ? C6 O1 C7 N1 -6(2) . . . . ? C7 N2 C12 C11 -102(2) . . . . ? C8 N2 C12 C11 81(2) . . . . ? C7 O1 C6 C5 -175(2) . . . . ? C7 O1 C6 C1 3(2) . . . . ? C16 C15 C20 N4 179(2) . . . . ? C14 C15 C20 N4 -9(3) . . . . ? C16 C15 C20 C19 1(3) . . . . ? C14 C15 C20 C19 172.7(19) . . . . ? C14 N3 C9 C8 -87.4(19) . . . . ? C10 N3 C9 C8 96.0(19) . . . . ? C5 C6 C1 N1 179(2) . . . . ? O1 C6 C1 N1 1(2) . . . . ? C5 C6 C1 C2 1(3) . . . . ? O1 C6 C1 C2 -177.7(19) . . . . ? N2 C7 N1 C1 -179(2) . . . . ? O1 C7 N1 C1 7(2) . . . . ? C2 C1 N1 C7 173(3) . . . . ? C6 C1 N1 C7 -5(2) . . . . ? N1 C1 C2 C3 -175(3) . . . . ? C6 C1 C2 C3 2(4) . . . . ? N2 C12 C11 C10 -81(2) . . . . ? C19 C20 N4 N5 161(4) . . . . ? C15 C20 N4 N5 -17(5) . . . . ? C19 C20 N4 N6 -11(4) . . . . ? C15 C20 N4 N6 171(2) . . . . ? C7 N2 C8 C9 164.3(17) . . . . ? C12 N2 C8 C9 -18(2) . . . . ? N3 C9 C8 N2 -57(2) . . . . ? C9 N3 C14 O2 6(3) . . . . ? C10 N3 C14 O2 -178(2) . . . . ? C9 N3 C14 C15 180(2) . . . . ? C10 N3 C14 C15 -4(3) . . . . ? C16 C15 C14 O2 85(3) . . . . ? C20 C15 C14 O2 -87(3) . . . . ? C16 C15 C14 N3 -88(3) . . . . ? C20 C15 C14 N3 100(2) . . . . ? C15 C16 C17 C18 7(4) . . . . ? C15 C16 C17 C23 177(2) . . . . ? C16 C17 C18 C19 -10(5) . . . . ? C23 C17 C18 C19 180(3) . . . . ? C29 C24 C25 C26 1(4) . . . . ? S1 C24 C25 C26 -178.4(19) . . . . ? C29 C28 C27 C26 0(4) . . . . ? C29 C28 C27 C30 178(2) . . . . ? C14 N3 C10 C11 109.9(19) . . . . ? C9 N3 C10 C11 -74(2) . . . . ? C14 N3 C10 C13 -118(2) . . . . ? C9 N3 C10 C13 59(2) . . . . ? C12 C11 C10 N3 59(2) . . . . ? C12 C11 C10 C13 -73(2) . . . . ? C28 C27 C26 C25 -1(5) . . . . ? C30 C27 C26 C25 -178(2) . . . . ? C24 C25 C26 C27 0(4) . . . . ? C17 C18 C19 C20 9(5) . . . . ? N4 C20 C19 C18 179(3) . . . . ? C15 C20 C19 C18 -3(4) . . . . ? C25 C24 C29 C28 -1(4) . . . . ? S1 C24 C29 C28 177.7(17) . . . . ? C27 C28 C29 C24 1(4) . . . . ? O1 C6 C5 C4 178(2) . . . . ? C1 C6 C5 C4 -1(3) . . . . ? C3 C4 C5 C6 -3(4) . . . . ? C1 C2 C3 C4 -5(5) . . . . ? C1 C2 C3 Cl -177.0(19) . . . . ? C5 C4 C3 C2 6(5) . . . . ? C5 C4 C3 Cl 178(2) . . . . ? N6 C22 C21 N5 -10(7) . . . . ? N5 N4 N6 C22 2(4) . . . . ? C20 N4 N6 C22 176(3) . . . . ? C21 C22 N6 N4 5(6) . . . . ? C22 C21 N5 N4 12(7) . . . . ? N6 N4 N5 C21 -8(5) . . . . ? C20 N4 N5 C21 179(4) . . . . ? _refine_diff_density_max 0.207 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.046 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL red in P21 #4 REM Best SHELXD solution FINAL CC 73.14 REM Fragments: 27 11 2 REM reset to P21 #4 CELL 0.71073 13.247061 7.619237 15.469059 90 92.4171 90 ZERR 2 0.005823 0.001642 0.010269 0 0.0591 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H Cl N O S UNIT 60 62 2 12 10 2 L.S. 10 PLAN 30 MORE -1 BOND $H TEMP 121 SIZE 0.3 0.1 0.1 CONF fmap 2 53 acta 52 TWIN -1 0 0 0 -1 0 0 0 -1 2 WGHT 0.024400 BASF 0.23745 FVAR 3.11964 S1 6 0.740167 0.498013 0.150246 11.00000 0.10078 0.06163 = 0.13490 -0.00802 0.02129 0.01014 CL 3 0.827011 1.050269 0.474653 11.00000 0.39786 0.18336 = 0.10554 -0.02116 0.09151 0.03756 O1 5 0.933123 0.848003 0.127298 11.00000 0.09210 0.05349 = 0.09437 0.00788 0.01115 -0.01413 N2 4 0.888215 0.983571 0.000996 11.00000 0.08995 0.06098 = 0.08971 0.00632 0.01430 -0.00188 N3 4 0.831931 0.793894 -0.156349 11.00000 0.03447 0.06675 = 0.08937 0.00277 0.01119 0.02482 C24 1 0.654783 0.500381 0.234103 11.00000 0.12650 0.01706 = 0.11786 0.00341 0.05498 0.00304 O5 5 0.841891 0.472342 0.185719 11.00000 0.07970 0.06546 = 0.18258 0.01221 0.00071 -0.00132 O3 5 0.708015 0.351037 0.092637 11.00000 0.13296 0.07433 = 0.15705 -0.02262 -0.01364 -0.00433 C15 1 0.702974 0.555847 -0.173724 11.00000 0.04111 0.05246 = 0.13125 0.00977 0.04647 -0.00314 C16 1 0.644538 0.543146 -0.107095 11.00000 0.07651 0.05530 = 0.11721 0.00909 0.00573 -0.00451 AFIX 43 H16 2 0.670992 0.576664 -0.052946 11.00000 -1.20000 AFIX 0 C7 1 0.883023 0.976403 0.083123 11.00000 0.07281 0.03014 = 0.11361 0.00255 0.04480 -0.02982 C12 1 0.829512 1.117569 -0.049754 11.00000 0.10214 0.04231 = 0.09938 0.00058 0.02847 0.01186 AFIX 23 H12A 2 0.870759 1.166766 -0.094083 11.00000 -1.20000 H12B 2 0.809602 1.211991 -0.012016 11.00000 -1.20000 AFIX 0 C6 1 0.915635 0.872693 0.215255 11.00000 0.08444 0.03710 = 0.09214 0.01847 0.03864 -0.01161 C20 1 0.668626 0.499404 -0.256603 11.00000 0.14382 0.03763 = 0.05642 -0.01007 0.00677 0.01056 C9 1 0.935362 0.849405 -0.140170 11.00000 0.02639 0.07120 = 0.10809 0.00085 0.00265 0.00549 AFIX 23 H9A 2 0.946373 0.961975 -0.167503 11.00000 -1.20000 H9B 2 0.981125 0.764574 -0.164073 11.00000 -1.20000 AFIX 0 C1 1 0.847861 1.015515 0.220578 11.00000 0.17645 0.04863 = 0.06140 -0.02715 0.02238 0.00140 O4 5 0.725384 0.664984 0.106033 11.00000 0.16531 0.06336 = 0.09824 -0.00048 0.02438 0.01941 N1 4 0.828080 1.066424 0.137841 11.00000 0.12899 0.05549 = 0.08286 -0.01348 0.03782 0.01877 AFIX 43 H1 2 0.785390 1.146810 0.122552 11.00000 -1.20000 AFIX 0 C4 1 0.921408 0.852500 0.363240 11.00000 0.18802 0.06587 = 0.09610 -0.01817 0.02524 -0.00779 AFIX 43 H4 2 0.943205 0.793335 0.413194 11.00000 -1.20000 AFIX 0 C2 1 0.821298 1.070574 0.302031 11.00000 0.20781 0.07349 = 0.08506 -0.03805 0.03258 0.02684 AFIX 43 H2 2 0.775171 1.161696 0.306880 11.00000 -1.20000 AFIX 0 C11 1 0.734200 1.028807 -0.092273 11.00000 0.04504 0.08249 = 0.15256 -0.02989 0.00892 0.00595 AFIX 23 H11A 2 0.706091 0.948162 -0.051147 11.00000 -1.20000 H11B 2 0.683777 1.118109 -0.105760 11.00000 -1.20000 AFIX 0 N4 4 0.727870 0.515242 -0.325423 11.00000 0.24067 0.06335 = 0.04766 0.00447 0.01318 0.02847 C8 1 0.955367 0.864443 -0.042323 11.00000 0.05565 0.06719 = 0.08783 -0.01515 0.00957 -0.00375 AFIX 23 H8A 2 0.949334 0.748698 -0.016944 11.00000 -1.20000 H8B 2 1.024413 0.903524 -0.031368 11.00000 -1.20000 AFIX 0 C14 1 0.810304 0.609110 -0.157552 11.00000 0.12991 0.05004 = 0.10331 -0.01120 0.04830 0.03106 C17 1 0.545297 0.482244 -0.113362 11.00000 0.12767 0.06024 = 0.18507 -0.00714 0.00726 0.00510 O2 5 0.879988 0.514913 -0.137989 11.00000 0.11301 0.05673 = 0.16312 -0.01144 0.01423 0.00482 C13 1 0.777188 1.041129 -0.255082 11.00000 0.14477 0.08872 = 0.11193 0.05677 0.00912 0.01060 AFIX 137 H13A 2 0.839731 1.103202 -0.245533 11.00000 -1.50000 H13B 2 0.723160 1.123791 -0.264573 11.00000 -1.50000 H13C 2 0.781531 0.966878 -0.304925 11.00000 -1.50000 AFIX 0 C28 1 0.513022 0.403622 0.308447 11.00000 0.10442 0.11002 = 0.12980 0.01742 0.03353 -0.03318 AFIX 43 H28 2 0.457382 0.329689 0.311136 11.00000 -1.20000 AFIX 0 C30 1 0.459421 0.525135 0.449954 11.00000 0.15693 0.12707 = 0.15514 0.03002 0.06131 0.03455 AFIX 137 H30A 2 0.399321 0.462078 0.432208 11.00000 -1.50000 H30B 2 0.442317 0.644447 0.462887 11.00000 -1.50000 H30C 2 0.489958 0.470807 0.500581 11.00000 -1.50000 AFIX 0 C18 1 0.516865 0.418088 -0.190263 11.00000 0.12853 0.03547 = 0.30158 0.00731 0.03993 -0.00759 AFIX 43 H18 2 0.455600 0.358508 -0.194839 11.00000 -1.20000 AFIX 0 C25 1 0.675158 0.616488 0.300101 11.00000 0.11868 0.09155 = 0.11136 0.00389 0.04071 0.01114 AFIX 43 H25 2 0.730703 0.690859 0.298362 11.00000 -1.20000 AFIX 0 C27 1 0.534107 0.522049 0.376632 11.00000 0.20333 0.06598 = 0.09985 -0.02319 0.00357 0.03595 C10 1 0.756590 0.928226 -0.175332 11.00000 0.07477 0.07034 = 0.08283 -0.00313 0.00291 -0.00567 AFIX 13 H10 2 0.694301 0.863957 -0.190663 11.00000 -1.20000 AFIX 0 C26 1 0.610953 0.622563 0.371158 11.00000 0.15895 0.07401 = 0.12895 -0.02087 -0.01958 -0.00778 AFIX 43 H26 2 0.625247 0.702567 0.415402 11.00000 -1.20000 AFIX 0 C23 1 0.479777 0.459713 -0.036780 11.00000 0.21136 0.10226 = 0.22950 0.00176 0.13409 0.00361 AFIX 137 H23A 2 0.511671 0.379604 0.003739 11.00000 -1.50000 H23B 2 0.415154 0.413915 -0.056008 11.00000 -1.50000 H23C 2 0.470785 0.571275 -0.009307 11.00000 -1.50000 AFIX 0 C19 1 0.570462 0.432807 -0.262881 11.00000 0.10537 0.07138 = 0.17284 -0.01056 -0.05597 -0.01840 AFIX 43 H19 2 0.542000 0.398821 -0.316265 11.00000 -1.20000 AFIX 0 C29 1 0.574368 0.394213 0.235883 11.00000 0.09925 0.08968 = 0.17186 0.01109 0.05256 -0.03057 AFIX 43 H29 2 0.559274 0.316591 0.190775 11.00000 -1.20000 AFIX 0 C5 1 0.953708 0.786910 0.285983 11.00000 0.14368 0.07104 = 0.11565 0.00341 0.01962 0.01085 AFIX 43 H5 2 0.997703 0.692230 0.282797 11.00000 -1.20000 AFIX 0 C3 1 0.861099 0.994448 0.374019 11.00000 0.27671 0.09900 = 0.10660 0.05044 0.05004 0.02195 C22 1 0.783423 0.505911 -0.454113 11.00000 0.35285 0.22082 = 0.04708 -0.01675 0.07802 0.05951 AFIX 43 H22 2 0.788873 0.488170 -0.513215 11.00000 -1.20000 AFIX 0 C21 1 0.839340 0.584380 -0.406010 11.00000 0.34874 0.24161 = 0.07699 -0.07148 0.08316 -0.00395 AFIX 43 H21 2 0.902704 0.624094 -0.420827 11.00000 -1.20000 AFIX 0 N6 4 0.705491 0.444877 -0.399728 11.00000 0.31444 0.23278 = 0.06749 -0.01216 0.02221 -0.07364 N5 4 0.805182 0.606734 -0.336365 11.00000 0.38431 0.23076 = 0.19584 -0.10784 0.22025 -0.13114 HKLF 4 REM red in P21 #4 REM R1 = 0.0956 for 1092 Fo > 4sig(Fo) and 0.4052 for all 5302 data REM 392 parameters refined using 1 restraints END WGHT 0.0241 0.0000 REM Highest difference peak 0.207, deepest hole -0.205, 1-sigma level 0.046 Q1 1 0.7420 0.5138 -0.0143 11.00000 0.05 0.21 Q2 1 0.4966 0.5083 0.1037 11.00000 0.05 0.20 Q3 1 0.6339 0.5043 0.1409 11.00000 0.05 0.18 Q4 1 0.9286 0.4894 0.1767 11.00000 0.05 0.18 Q5 1 0.4742 0.5357 -0.3565 11.00000 0.05 0.16 Q6 1 0.7661 0.4999 -0.2188 11.00000 0.05 0.16 Q7 1 0.8445 0.4985 -0.3363 11.00000 0.05 0.16 Q8 1 0.6315 0.4980 0.4326 11.00000 0.05 0.16 Q9 1 0.9357 1.0287 -0.2448 11.00000 0.05 0.16 Q10 1 0.6186 0.9850 -0.0376 11.00000 0.05 0.16 Q11 1 0.6836 0.3630 0.2791 11.00000 0.05 0.15 Q12 1 0.6117 0.6630 0.0069 11.00000 0.05 0.15 Q13 1 0.6391 0.4936 -0.1023 11.00000 0.05 0.15 Q14 1 0.7652 1.0642 -0.3673 11.00000 0.05 0.15 Q15 1 0.8696 1.0055 -0.0162 11.00000 0.05 0.15 Q16 1 0.6254 1.1964 0.3610 11.00000 0.05 0.15 Q17 1 0.4843 0.1873 0.2812 11.00000 0.05 0.14 Q18 1 1.0069 0.9776 -0.0934 11.00000 0.05 0.14 Q19 1 0.4068 0.4360 -0.2834 11.00000 0.05 0.14 Q20 1 0.6879 1.0640 0.2995 11.00000 0.05 0.13 Q21 1 0.5567 0.1344 -0.2336 11.00000 0.05 0.13 Q22 1 0.9789 1.0429 0.4923 11.00000 0.05 0.13 Q23 1 0.8552 0.5060 0.0668 11.00000 0.05 0.13 Q24 1 0.8955 0.4511 -0.5779 11.00000 0.05 0.13 Q25 1 0.6508 0.5166 0.3638 11.00000 0.05 0.13 Q26 1 0.6920 0.6226 -0.2210 11.00000 0.05 0.13 Q27 1 0.8476 0.6575 0.0051 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