# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Marcello Gennari' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; 'Jacques Pecaut' '' '' 'Marie-Noelle Collomb' '' '' 'Carole Duboc' '' '' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email carole.duboc@ujf-grenoble.fr _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_name 'Carole Duboc' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; data_compound2 _database_code_depnum_ccdc_archive 'CCDC 854562' #TrackingRef '- 2.cif' #------------------------------------------------------------------------------ _audit_creation_date 2009-02-24 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'Enraf-Nonius kappa ccd' _computing_cell_refinement 'Enraf-Nonius kappa ccd' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution 'SIR 92' _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 9.109(2) _cell_length_b 12.802(3) _cell_length_c 13.188(2) _cell_angle_alpha 88.37(1) _cell_angle_beta 76.90(2) _cell_angle_gamma 84.81(2) _cell_volume 1491.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 200.0 _cell_measurement_reflns_used 3550 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 25.00 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description needle _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 642.33 _chemical_formula_analytical ? _chemical_formula_sum 'C38 H30 Cu N2 S2 ' _chemical_formula_moiety 'C38 H30 Cu N2 S2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 666.00 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 200.0 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Bruker Enraf Nonius kappa CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? _diffrn_reflns_number 19203 _reflns_number_total 5202 _reflns_number_gt 3550 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.15317 _diffrn_reflns_av_sigmaI/netI 0.070 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 76 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 60 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 4 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 4 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cu 0 2 0.263 1.266 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Cu(1) 0.58841(6) 0.25197(5) 0.99723(5) 0.0191(2) 1.000 . Uani d ? S(1) 0.7204(1) 0.2167(1) 1.11894(9) 0.0226(3) 1.000 . Uani d ? S(2) 0.7896(1) 0.3081(1) 0.88700(9) 0.0236(3) 1.000 . Uani d ? N(1) 0.4216(4) 0.1577(3) 1.0501(3) 0.018(1) 1.000 . Uani d ? N(2) 0.4244(4) 0.3319(3) 0.9392(3) 0.021(1) 1.000 . Uani d ? C(1) 0.2901(5) 0.1895(4) 1.0256(4) 0.022(1) 1.000 . Uani d ? C(2) 0.1605(5) 0.1378(4) 1.0569(4) 0.026(1) 1.000 . Uani d ? C(3) 0.1694(5) 0.0481(4) 1.1163(4) 0.032(2) 1.000 . Uani d ? C(4) 0.3031(6) 0.0157(4) 1.1419(4) 0.028(1) 1.000 . Uani d ? C(5) 0.4283(5) 0.0696(4) 1.1099(4) 0.020(1) 1.000 . Uani d ? C(6) 0.5746(5) 0.0341(4) 1.1382(4) 0.021(1) 1.000 . Uani d ? C(7) 0.6336(5) 0.1094(3) 1.2043(3) 0.017(1) 1.000 . Uani d ? C(8) 0.5019(5) 0.1483(4) 1.2933(3) 0.021(1) 1.000 . Uani d ? C(9) 0.4255(6) 0.2472(4) 1.2976(4) 0.029(1) 1.000 . Uani d ? C(10) 0.3016(6) 0.2746(4) 1.3775(4) 0.033(2) 1.000 . Uani d ? C(11) 0.2525(6) 0.2038(4) 1.4553(4) 0.033(2) 1.000 . Uani d ? C(12) 0.3263(6) 0.1052(4) 1.4527(4) 0.034(2) 1.000 . Uani d ? C(13) 0.4488(6) 0.0774(4) 1.3733(4) 0.026(1) 1.000 . Uani d ? C(14) 0.7606(5) 0.0559(4) 1.2516(3) 0.017(1) 1.000 . Uani d ? C(15) 0.8119(5) -0.0502(4) 1.2390(4) 0.023(1) 1.000 . Uani d ? C(16) 0.9207(5) -0.0934(4) 1.2885(4) 0.030(1) 1.000 . Uani d ? C(17) 0.9824(6) -0.0335(5) 1.3497(4) 0.033(2) 1.000 . Uani d ? C(18) 0.9340(6) 0.0719(4) 1.3618(4) 0.030(1) 1.000 . Uani d ? C(19) 0.8249(5) 0.1148(4) 1.3137(4) 0.025(1) 1.000 . Uani d ? C(20) 0.2924(5) 0.2885(4) 0.9621(4) 0.023(1) 1.000 . Uani d ? C(21) 0.1663(6) 0.3321(4) 0.9306(5) 0.042(2) 1.000 . Uani d ? C(22) 0.1746(7) 0.4261(5) 0.8771(5) 0.056(2) 1.000 . Uani d ? C(23) 0.3099(6) 0.4721(4) 0.8553(5) 0.041(2) 1.000 . Uani d ? C(24) 0.4354(5) 0.4231(4) 0.8850(4) 0.022(1) 1.000 . Uani d ? C(25) 0.5802(5) 0.4713(4) 0.8600(4) 0.023(1) 1.000 . Uani d ? C(26) 0.7170(5) 0.4022(4) 0.7968(4) 0.020(1) 1.000 . Uani d ? C(27) 0.8498(5) 0.4700(4) 0.7512(3) 0.020(1) 1.000 . Uani d ? C(28) 0.8661(6) 0.5646(4) 0.7935(4) 0.031(1) 1.000 . Uani d ? C(29) 0.9846(6) 0.6236(4) 0.7520(4) 0.036(2) 1.000 . Uani d ? C(30) 1.0897(6) 0.5895(4) 0.6662(4) 0.042(2) 1.000 . Uani d ? C(31) 1.0767(7) 0.4952(5) 0.6220(5) 0.055(2) 1.000 . Uani d ? C(32) 0.9574(6) 0.4365(4) 0.6651(4) 0.041(2) 1.000 . Uani d ? C(33) 0.6697(5) 0.3506(4) 0.7082(4) 0.025(1) 1.000 . Uani d ? C(34) 0.5967(7) 0.4106(4) 0.6424(4) 0.038(2) 1.000 . Uani d ? C(35) 0.5531(7) 0.3678(5) 0.5612(4) 0.047(2) 1.000 . Uani d ? C(36) 0.5853(6) 0.2621(5) 0.5420(4) 0.043(2) 1.000 . Uani d ? C(37) 0.6571(6) 0.2033(4) 0.6035(5) 0.040(2) 1.000 . Uani d ? C(38) 0.6988(6) 0.2442(4) 0.6868(4) 0.031(1) 1.000 . Uani d ? H(1) 0.0688 0.1631 1.0383 0.031 1.000 . Uiso c ? H(2) 0.0836 0.0095 1.1391 0.039 1.000 . Uiso c ? H(3) 0.3094 -0.0459 1.1830 0.033 1.000 . Uiso c ? H(4) 0.6490 0.0224 1.0754 0.025 1.000 . Uiso c ? H(5) 0.5617 -0.0301 1.1758 0.025 1.000 . Uiso c ? H(6) 0.4588 0.2973 1.2448 0.034 1.000 . Uiso c ? H(7) 0.2502 0.3427 1.3785 0.040 1.000 . Uiso c ? H(8) 0.1681 0.2229 1.5105 0.039 1.000 . Uiso c ? H(9) 0.2925 0.0559 1.5062 0.041 1.000 . Uiso c ? H(10) 0.4985 0.0088 1.3727 0.031 1.000 . Uiso c ? H(11) 0.7714 -0.0926 1.1959 0.027 1.000 . Uiso c ? H(12) 0.9535 -0.1658 1.2802 0.036 1.000 . Uiso c ? H(13) 1.0577 -0.0641 1.3835 0.040 1.000 . Uiso c ? H(14) 0.9768 0.1143 1.4036 0.036 1.000 . Uiso c ? H(15) 0.7921 0.1872 1.3232 0.030 1.000 . Uiso c ? H(16) 0.0753 0.2981 0.9456 0.050 1.000 . Uiso c ? H(17) 0.0887 0.4587 0.8555 0.067 1.000 . Uiso c ? H(18) 0.3167 0.5377 0.8197 0.049 1.000 . Uiso c ? H(19) 0.6037 0.4889 0.9237 0.028 1.000 . Uiso c ? H(20) 0.5671 0.5335 0.8208 0.028 1.000 . Uiso c ? H(21) 0.7932 0.5896 0.8532 0.037 1.000 . Uiso c ? H(22) 0.9929 0.6882 0.7831 0.043 1.000 . Uiso c ? H(23) 1.1715 0.6301 0.6370 0.050 1.000 . Uiso c ? H(24) 1.1496 0.4707 0.5620 0.066 1.000 . Uiso c ? H(25) 0.9497 0.3716 0.6344 0.049 1.000 . Uiso c ? H(26) 0.5763 0.4839 0.6540 0.046 1.000 . Uiso c ? H(27) 0.5009 0.4106 0.5184 0.056 1.000 . Uiso c ? H(28) 0.5566 0.2315 0.4854 0.051 1.000 . Uiso c ? H(29) 0.6804 0.1306 0.5893 0.048 1.000 . Uiso c ? H(30) 0.7477 0.1994 0.7301 0.037 1.000 . Uiso c ? 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 Cu(1) 0.0207(3) 0.0172(3) 0.0199(3) -0.0021(2) -0.0057(2) 0.0031(2) S(1) 0.0249(7) 0.0234(7) 0.0224(6) -0.0100(6) -0.0095(5) 0.0082(5) S(2) 0.0214(7) 0.0254(7) 0.0236(7) -0.0005(5) -0.0062(5) 0.0102(6) N(1) 0.019(2) 0.018(2) 0.016(2) -0.003(2) -0.002(2) -0.006(2) N(2) 0.020(2) 0.022(2) 0.021(2) 0.003(2) -0.006(2) -0.002(2) C(1) 0.023(3) 0.023(3) 0.021(3) -0.002(2) -0.006(2) -0.009(2) C(2) 0.016(3) 0.036(3) 0.027(3) -0.003(2) -0.007(2) -0.004(2) C(3) 0.023(3) 0.048(3) 0.026(3) -0.023(3) -0.001(2) 0.008(3) C(4) 0.034(3) 0.030(3) 0.021(3) -0.013(2) -0.006(2) 0.007(2) C(5) 0.025(3) 0.017(3) 0.019(3) -0.006(2) -0.001(2) -0.002(2) C(6) 0.027(3) 0.017(3) 0.019(3) -0.005(2) -0.007(2) 0.006(2) C(7) 0.024(2) 0.012(2) 0.018(2) -0.008(2) -0.006(2) 0.002(2) C(8) 0.027(3) 0.025(3) 0.011(2) -0.007(2) -0.005(2) -0.004(2) C(9) 0.038(3) 0.022(3) 0.023(3) 0.006(2) -0.007(2) 0.005(2) C(10) 0.041(3) 0.025(3) 0.030(3) 0.012(3) -0.008(3) 0.000(2) C(11) 0.033(3) 0.033(3) 0.029(3) 0.004(3) -0.001(3) -0.005(3) C(12) 0.036(3) 0.029(3) 0.032(3) -0.007(3) 0.005(3) 0.003(3) C(13) 0.035(3) 0.009(2) 0.032(3) 0.000(2) -0.006(2) 0.000(2) C(14) 0.018(2) 0.020(3) 0.012(2) -0.001(2) -0.001(2) 0.008(2) C(15) 0.028(3) 0.017(3) 0.022(3) -0.003(2) -0.003(2) 0.005(2) C(16) 0.025(3) 0.026(3) 0.034(3) 0.002(2) 0.000(2) 0.017(2) C(17) 0.025(3) 0.052(4) 0.020(3) 0.001(3) -0.007(2) 0.016(3) C(18) 0.029(3) 0.037(3) 0.026(3) -0.002(2) -0.010(2) 0.007(2) C(19) 0.026(3) 0.022(3) 0.029(3) -0.001(2) -0.009(2) 0.001(2) C(20) 0.020(3) 0.022(3) 0.030(3) -0.003(2) -0.010(2) 0.000(2) C(21) 0.028(3) 0.034(3) 0.069(4) -0.013(3) -0.020(3) 0.018(3) C(22) 0.037(3) 0.060(4) 0.078(4) -0.001(3) -0.035(3) 0.025(4) C(23) 0.034(3) 0.030(3) 0.060(4) 0.000(3) -0.017(3) 0.020(3) C(24) 0.028(3) 0.023(3) 0.018(2) 0.000(2) -0.012(2) -0.003(2) C(25) 0.032(3) 0.013(3) 0.027(3) -0.002(2) -0.013(2) -0.003(2) C(26) 0.028(3) 0.015(3) 0.021(3) -0.001(2) -0.012(2) 0.002(2) C(27) 0.030(3) 0.015(2) 0.018(2) -0.003(2) -0.012(2) 0.002(2) C(28) 0.034(3) 0.025(3) 0.036(3) -0.002(2) -0.009(2) -0.002(2) C(29) 0.041(3) 0.018(3) 0.048(3) -0.009(3) -0.007(3) 0.004(3) C(30) 0.047(3) 0.034(3) 0.047(4) -0.027(3) -0.011(3) 0.020(3) C(31) 0.056(4) 0.071(5) 0.031(3) -0.034(3) 0.016(3) -0.007(3) C(32) 0.051(4) 0.035(3) 0.035(3) -0.019(3) -0.002(3) -0.011(3) C(33) 0.028(3) 0.024(3) 0.022(3) -0.006(2) -0.006(2) 0.006(2) C(34) 0.065(4) 0.018(3) 0.038(3) 0.003(3) -0.028(3) -0.001(2) C(35) 0.066(4) 0.045(4) 0.037(3) -0.001(3) -0.030(3) 0.001(3) C(36) 0.043(3) 0.049(4) 0.042(3) -0.009(3) -0.018(3) -0.021(3) C(37) 0.051(3) 0.021(3) 0.053(4) -0.008(3) -0.018(3) -0.014(3) C(38) 0.041(3) 0.013(3) 0.039(3) -0.003(2) -0.009(3) 0.001(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment \`Oconstr\'O _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3550 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_all 0.0711 _refine_ls_wR_factor_ref 0.0672 _refine_ls_goodness_of_fit_all 1.930 _refine_ls_goodness_of_fit_ref 1.930 _refine_ls_shift/su_max 0.0035 _refine_ls_shift/su_mean 0.0002 _refine_diff_density_min -0.69 _refine_diff_density_max 0.92 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag CU1 S1 2.227(1) . . yes CU1 S2 2.227(1) . . yes CU1 N1 2.014(4) . . yes CU1 N2 2.016(4) . . yes S1 C7 1.867(4) . . yes S2 C26 1.853(5) . . yes N1 C1 1.336(6) . . yes N1 C5 1.363(6) . . yes N2 C20 1.339(6) . . yes N2 C24 1.351(6) . . yes C1 C2 1.381(7) . . yes C1 C20 1.498(7) . . yes C2 C3 1.378(7) . . yes C2 H1 0.95 . . no C3 C4 1.362(7) . . yes C3 H2 0.95 . . no C4 C5 1.364(7) . . yes C4 H3 0.95 . . no C5 C6 1.493(7) . . yes C6 C7 1.527(7) . . yes C6 H4 0.95 . . no C6 H5 0.95 . . no C7 C8 1.534(6) . . yes C7 C14 1.534(6) . . yes C8 C9 1.385(7) . . yes C8 C13 1.402(6) . . yes C9 C10 1.385(7) . . yes C9 H6 0.95 . . no C10 C11 1.374(7) . . yes C10 H7 0.95 . . no C11 C12 1.373(7) . . yes C11 H8 0.95 . . no C12 C13 1.374(7) . . yes C12 H9 0.95 . . no C13 H10 0.95 . . no C14 C15 1.398(6) . . yes C14 C19 1.384(7) . . yes C15 C16 1.375(7) . . yes C15 H11 0.95 . . no C16 C17 1.368(7) . . yes C16 H12 0.95 . . no C17 C18 1.383(7) . . yes C17 H13 0.95 . . no C18 C19 1.363(7) . . yes C18 H14 0.95 . . no C19 H15 0.95 . . no C20 C21 1.375(7) . . yes C21 C22 1.376(8) . . yes C21 H16 0.95 . . no C22 C23 1.382(8) . . yes C22 H17 0.95 . . no C23 C24 1.383(7) . . yes C23 H18 0.95 . . no C24 C25 1.472(7) . . yes C25 C26 1.550(6) . . yes C25 H19 0.95 . . no C25 H20 0.95 . . no C26 C27 1.552(7) . . yes C26 C33 1.520(7) . . yes C27 C28 1.381(7) . . yes C27 C32 1.371(7) . . yes C28 C29 1.376(7) . . yes C28 H21 0.95 . . no C29 C30 1.360(7) . . yes C29 H22 0.95 . . no C30 C31 1.381(8) . . yes C30 H23 0.95 . . no C31 C32 1.383(8) . . yes C31 H24 0.95 . . no C32 H25 0.95 . . no C33 C34 1.385(7) . . yes C33 C38 1.388(7) . . yes C34 C35 1.367(8) . . yes C34 H26 0.95 . . no C35 C36 1.377(8) . . yes C35 H27 0.95 . . no C36 C37 1.330(8) . . yes C36 H28 0.95 . . no C37 C38 1.372(8) . . yes C37 H29 0.95 . . no C38 H30 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 CU1 S2 91.49(5) . . . yes S1 CU1 N1 98.5(1) . . . yes S1 CU1 N2 153.3(1) . . . yes S2 CU1 N1 156.4(1) . . . yes S2 CU1 N2 99.0(1) . . . yes N1 CU1 N2 81.5(2) . . . yes CU1 S1 C7 108.3(2) . . . yes CU1 S2 C26 106.8(2) . . . yes CU1 N1 C1 114.6(3) . . . yes CU1 N1 C5 127.1(3) . . . yes C1 N1 C5 118.3(4) . . . yes CU1 N2 C20 113.7(3) . . . yes CU1 N2 C24 126.6(3) . . . yes C20 N2 C24 119.6(4) . . . yes N1 C1 C2 123.7(5) . . . yes N1 C1 C20 114.5(4) . . . yes N1 C1 H1 147.1 . . . no C2 C1 C20 121.8(4) . . . yes C1 C2 C3 117.4(5) . . . yes C1 C2 H1 121.3 . . . no C3 C2 H1 121.3 . . . no C2 C3 C4 119.1(5) . . . yes C2 C3 H2 120.5 . . . no C4 C3 H2 120.5 . . . no C3 C4 C5 121.7(5) . . . yes C3 C4 H3 119.2 . . . no C5 C4 H3 119.2 . . . no N1 C5 C4 119.9(5) . . . yes N1 C5 C6 118.5(4) . . . yes C4 C5 C6 121.6(4) . . . yes C5 C6 C7 116.2(4) . . . yes C5 C6 H4 107.8 . . . no C5 C6 H5 107.8 . . . no C7 C6 H4 107.8 . . . no C7 C6 H5 107.8 . . . no H4 C6 H5 109.5 . . . no S1 C7 C6 108.9(3) . . . yes S1 C7 C8 113.7(3) . . . yes S1 C7 C14 105.6(3) . . . yes C6 C7 C8 108.1(4) . . . yes C6 C7 C14 112.0(4) . . . yes C8 C7 C14 108.5(4) . . . yes C7 C8 C9 124.6(4) . . . yes C7 C8 C13 118.0(4) . . . yes C9 C8 C13 117.2(4) . . . yes C8 C9 C10 121.3(4) . . . yes C8 C9 H6 119.4 . . . no C10 C9 H6 119.4 . . . no C9 C10 C11 120.3(5) . . . yes C9 C10 H7 119.8 . . . no C11 C10 H7 119.8 . . . no C10 C11 C12 119.5(5) . . . yes C10 C11 H8 120.3 . . . no C12 C11 H8 120.3 . . . no C11 C12 C13 120.5(5) . . . yes C11 C12 H9 119.8 . . . no C13 C12 H9 119.8 . . . no C8 C13 C12 121.2(4) . . . yes C8 C13 H10 119.4 . . . no C12 C13 H10 119.4 . . . no C7 C14 C15 123.9(4) . . . yes C7 C14 C19 118.4(4) . . . yes C15 C14 C19 117.6(4) . . . yes C14 C15 C16 120.3(5) . . . yes C14 C15 H11 119.8 . . . no C16 C15 H11 119.8 . . . no C15 C16 C17 120.9(5) . . . yes C15 C16 H12 119.5 . . . no C17 C16 H12 119.5 . . . no C16 C17 C18 119.4(5) . . . yes C16 C17 H13 120.3 . . . no C18 C17 H13 120.3 . . . no C17 C18 C19 119.9(5) . . . yes C17 C18 H14 120.0 . . . no C19 C18 H14 120.0 . . . no C14 C19 C18 121.8(5) . . . yes C14 C19 H15 119.1 . . . no C18 C19 H15 119.1 . . . no N2 C20 C1 115.6(4) . . . yes N2 C20 C21 122.4(5) . . . yes C1 C20 C21 121.9(4) . . . yes C20 C21 C22 118.7(5) . . . yes C20 C21 H16 120.6 . . . no C22 C21 H16 120.6 . . . no C21 C22 C23 118.9(5) . . . yes C21 C22 H17 120.6 . . . no C23 C22 H17 120.6 . . . no C22 C23 C24 120.3(5) . . . yes C22 C23 H18 119.8 . . . no C24 C23 H18 119.8 . . . no N2 C24 C23 119.9(5) . . . yes N2 C24 C25 119.8(4) . . . yes C23 C24 C25 120.2(5) . . . yes C24 C25 C26 115.6(4) . . . yes C24 C25 H19 107.9 . . . no C24 C25 H20 107.9 . . . no C26 C25 H19 107.9 . . . no C26 C25 H20 107.9 . . . no H19 C25 H20 109.5 . . . no S2 C26 C25 108.7(3) . . . yes S2 C26 C27 105.2(3) . . . yes S2 C26 C33 114.0(3) . . . yes C25 C26 C27 110.4(4) . . . yes C25 C26 C33 109.3(4) . . . yes C27 C26 C33 109.2(4) . . . yes C26 C27 C28 122.9(4) . . . yes C26 C27 C32 119.9(4) . . . yes C28 C27 C32 117.2(5) . . . yes C27 C28 C29 122.1(5) . . . yes C27 C28 H21 119.0 . . . no C29 C28 H21 119.0 . . . no C28 C29 C30 119.9(5) . . . yes C28 C29 H22 120.1 . . . no C30 C29 H22 120.1 . . . no C29 C30 C31 119.5(5) . . . yes C29 C30 H23 120.3 . . . no C31 C30 H23 120.3 . . . no C30 C31 C32 119.9(5) . . . yes C30 C31 H24 120.1 . . . no C32 C31 H24 120.1 . . . no C27 C32 C31 121.5(5) . . . yes C27 C32 H25 119.3 . . . no C31 C32 H25 119.3 . . . no C26 C33 C34 120.1(4) . . . yes C26 C33 C38 123.4(5) . . . yes C34 C33 C38 116.5(5) . . . yes C33 C34 C35 122.2(5) . . . yes C33 C34 H26 118.9 . . . no C35 C34 H26 118.9 . . . no C34 C35 C36 119.5(6) . . . yes C34 C35 H27 120.3 . . . no C36 C35 H27 120.3 . . . no C35 C36 C37 119.3(5) . . . yes C35 C36 H28 120.4 . . . no C37 C36 H28 120.4 . . . no C36 C37 C38 122.2(5) . . . yes C36 C37 H29 118.9 . . . no C38 C37 H29 118.9 . . . no C33 C38 C37 120.3(5) . . . yes C33 C38 H30 119.8 . . . no C37 C38 H30 119.8 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N1 C6 3.534(6) . 2_657 no C1 C6 3.590(6) . 2_657 no C3 C17 3.351(7) . 1_455 no C3 C16 3.428(7) . 1_455 no C3 C18 3.459(7) . 1_455 no C5 C5 3.382(9) . 2_657 no C5 C6 3.572(7) . 2_657 no C10 C28 3.519(8) . 2_667 no C10 C29 3.561(8) . 2_667 no C12 C17 3.543(7) . 2_658 no C22 C29 3.519(8) . 1_455 no C22 C28 3.556(8) . 1_455 no #------------------------------------------------------------------------------ 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 ? ? ? ? ? ? ? ? ? ? data_mg190 _database_code_depnum_ccdc_archive 'CCDC 854563' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H80 Cu2 K2 N4 O2.50 S4' _chemical_formula_weight 1543.06 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.7411(4) _cell_length_b 14.8294(4) _cell_length_c 32.7134(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.330(3) _cell_angle_gamma 90.00 _cell_volume 7634.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6206 _cell_measurement_theta_min 3.3923 _cell_measurement_theta_max 28.9223 _exptl_crystal_description bloc _exptl_crystal_colour black _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 0.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7697 _exptl_absorpt_correction_T_max 0.8770 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29519 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.2210 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 26.37 _reflns_number_total 15396 _reflns_number_gt 6479 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -13.00 87.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 17.1550 77.0000 -30.0000 100 #__ type_ start__ end____ width___ exp.time_ 2 omega -13.00 87.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 17.1550 77.0000 90.0000 100 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15396 _refine_ls_number_parameters 928 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.1498 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1607 _refine_ls_wR_factor_gt 0.1499 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.61146(4) 0.20452(5) 0.37497(2) 0.0268(2) Uani 1 1 d . . . Cu2 Cu 0.84378(4) 0.00864(5) 0.30085(2) 0.0250(2) Uani 1 1 d . . . K1 K 0.70353(8) 0.03577(10) 0.43983(4) 0.0340(4) Uani 1 1 d . . . K2 K 0.93026(8) 0.16996(9) 0.36589(5) 0.0353(4) Uani 1 1 d . . . S1 S 0.74899(9) 0.21945(10) 0.39881(5) 0.0279(4) Uani 1 1 d . . . S2 S 0.53273(9) 0.08545(11) 0.39389(5) 0.0268(4) Uani 1 1 d . . . N1 N 0.6013(3) 0.3431(3) 0.37145(17) 0.0290(13) Uani 1 1 d . . . N2 N 0.5724(3) 0.2197(3) 0.31636(14) 0.0241(12) Uani 1 1 d . . . C1 C 0.6368(3) 0.3972(4) 0.4001(2) 0.0303(16) Uani 1 1 d . . . C2 C 0.6569(4) 0.4861(5) 0.3914(2) 0.0401(18) Uani 1 1 d . . . H2 H 0.6822 0.5235 0.4119 0.048 Uiso 1 1 calc R . . C3 C 0.6400(4) 0.5198(5) 0.3529(3) 0.045(2) Uani 1 1 d . . . H3 H 0.6519 0.5812 0.3469 0.055 Uiso 1 1 calc R . . C4 C 0.6051(4) 0.4634(5) 0.3225(2) 0.045(2) Uani 1 1 d . . . H4 H 0.5939 0.4854 0.2957 0.054 Uiso 1 1 calc R . . C5 C 0.5871(3) 0.3740(4) 0.3327(2) 0.0317(17) Uani 1 1 d . . . C6 C 0.5569(3) 0.3053(4) 0.3040(2) 0.0291(16) Uani 1 1 d . . . C7 C 0.5163(4) 0.3241(5) 0.2669(2) 0.0379(19) Uani 1 1 d . . . H7 H 0.5065 0.3847 0.2587 0.046 Uiso 1 1 calc R . . C8 C 0.4901(4) 0.2528(6) 0.2420(2) 0.047(2) Uani 1 1 d . . . H8 H 0.4636 0.2642 0.2161 0.056 Uiso 1 1 calc R . . C9 C 0.5031(3) 0.1646(5) 0.2553(2) 0.0365(18) Uani 1 1 d . . . H9 H 0.4843 0.1153 0.2389 0.044 Uiso 1 1 calc R . . C10 C 0.5441(3) 0.1495(4) 0.29297(19) 0.0258(16) Uani 1 1 d . . . C11 C 0.7413(3) 0.2988(4) 0.4419(2) 0.0306(17) Uani 1 1 d . . . C12 C 0.6562(3) 0.3520(4) 0.44003(19) 0.0304(16) Uani 1 1 d . . . H12A H 0.6093 0.3099 0.4460 0.037 Uiso 1 1 calc R . . H12B H 0.6577 0.3984 0.4618 0.037 Uiso 1 1 calc R . . C13 C 0.8546(4) 0.3917(5) 0.4068(2) 0.049(2) Uani 1 1 d . . . H13 H 0.8409 0.3613 0.3819 0.059 Uiso 1 1 calc R . . C14 C 0.9153(5) 0.4591(6) 0.4071(3) 0.073(3) Uani 1 1 d . . . H14 H 0.9415 0.4756 0.3823 0.087 Uiso 1 1 calc R . . C15 C 0.9385(5) 0.5030(6) 0.4430(3) 0.088(3) Uani 1 1 d . . . H15 H 0.9816 0.5479 0.4431 0.105 Uiso 1 1 calc R . . C16 C 0.8975(5) 0.4802(6) 0.4791(3) 0.085(3) Uani 1 1 d . . . H16 H 0.9123 0.5103 0.5039 0.102 Uiso 1 1 calc R . . C17 C 0.8350(4) 0.4135(5) 0.4788(2) 0.053(2) Uani 1 1 d . . . H17 H 0.8067 0.3985 0.5033 0.064 Uiso 1 1 calc R . . C18 C 0.8138(4) 0.3680(4) 0.4417(2) 0.0351(18) Uani 1 1 d . . . C19 C 0.7464(4) 0.2384(4) 0.4800(2) 0.0279(16) Uani 1 1 d . . . C20 C 0.6776(4) 0.2181(5) 0.5038(2) 0.0386(18) Uani 1 1 d . . . H20 H 0.6253 0.2485 0.4989 0.046 Uiso 1 1 calc R . . C21 C 0.6834(4) 0.1544(5) 0.5346(2) 0.047(2) Uani 1 1 d . . . H21 H 0.6347 0.1406 0.5500 0.056 Uiso 1 1 calc R . . C22 C 0.7585(4) 0.1110(5) 0.5433(2) 0.047(2) Uani 1 1 d . . . H22 H 0.7617 0.0666 0.5643 0.056 Uiso 1 1 calc R . . C23 C 0.8290(4) 0.1322(5) 0.5215(2) 0.043(2) Uani 1 1 d . . . H23 H 0.8818 0.1037 0.5278 0.052 Uiso 1 1 calc R . . C24 C 0.8235(4) 0.1959(5) 0.4898(2) 0.0373(18) Uani 1 1 d . . . H24 H 0.8727 0.2104 0.4748 0.045 Uiso 1 1 calc R . . C31 C 0.5025(3) 0.0276(4) 0.34532(18) 0.0216(15) Uani 1 1 d . . . C32 C 0.5604(3) 0.0569(4) 0.30950(18) 0.0257(15) Uani 1 1 d . . . H32A H 0.6204 0.0535 0.3191 0.031 Uiso 1 1 calc R . . H32B H 0.5529 0.0131 0.2869 0.031 Uiso 1 1 calc R . . C33 C 0.4106(3) 0.0486(4) 0.33166(18) 0.0223(15) Uani 1 1 d . . . C34 C 0.3695(3) -0.0083(4) 0.30348(19) 0.0328(16) Uani 1 1 d . . . H34 H 0.3981 -0.0598 0.2934 0.039 Uiso 1 1 calc R . . C35 C 0.2863(4) 0.0105(5) 0.2900(2) 0.0381(18) Uani 1 1 d . . . H35 H 0.2590 -0.0282 0.2707 0.046 Uiso 1 1 calc R . . C36 C 0.2434(4) 0.0844(5) 0.3046(2) 0.0381(18) Uani 1 1 d . . . H36 H 0.1864 0.0958 0.2959 0.046 Uiso 1 1 calc R . . C37 C 0.2839(4) 0.1417(4) 0.3318(2) 0.0356(17) Uani 1 1 d . . . H37 H 0.2554 0.1936 0.3416 0.043 Uiso 1 1 calc R . . C38 C 0.3671(3) 0.1231(4) 0.34498(18) 0.0279(16) Uani 1 1 d . . . H38 H 0.3945 0.1632 0.3637 0.034 Uiso 1 1 calc R . . C39 C 0.5159(3) -0.0716(4) 0.35455(17) 0.0217(14) Uani 1 1 d . . . C40 C 0.4510(4) -0.1237(4) 0.37032(19) 0.0322(17) Uani 1 1 d . . . H40 H 0.3969 -0.0969 0.3742 0.039 Uiso 1 1 calc R . . C41 C 0.4630(4) -0.2133(4) 0.3805(2) 0.0386(18) Uani 1 1 d . . . H41 H 0.4170 -0.2471 0.3909 0.046 Uiso 1 1 calc R . . C42 C 0.5409(4) -0.2545(5) 0.3758(2) 0.0396(18) Uani 1 1 d . . . H42 H 0.5487 -0.3162 0.3828 0.047 Uiso 1 1 calc R . . C43 C 0.6068(4) -0.2048(5) 0.3608(2) 0.0372(18) Uani 1 1 d . . . H43 H 0.6610 -0.2318 0.3577 0.045 Uiso 1 1 calc R . . C44 C 0.5941(4) -0.1154(4) 0.35013(18) 0.0293(16) Uani 1 1 d . . . H44 H 0.6403 -0.0824 0.3394 0.035 Uiso 1 1 calc R . . S51 S 0.82844(9) -0.01265(10) 0.36984(5) 0.0253(4) Uani 1 1 d . . . S52 S 0.91665(9) 0.12189(11) 0.27177(5) 0.0282(4) Uani 1 1 d . . . N51 N 0.8396(3) -0.1297(3) 0.29307(14) 0.0228(12) Uani 1 1 d . . . N52 N 0.7475(2) -0.0025(3) 0.25894(14) 0.0202(11) Uani 1 1 d . . . C51 C 0.8779(3) -0.1862(4) 0.31977(19) 0.0258(15) Uani 1 1 d . . . C52 C 0.8545(4) -0.2763(4) 0.3224(2) 0.0319(17) Uani 1 1 d . . . H52 H 0.8826 -0.3157 0.3412 0.038 Uiso 1 1 calc R . . C53 C 0.7888(4) -0.3075(4) 0.2969(2) 0.0345(17) Uani 1 1 d . . . H53 H 0.7730 -0.3693 0.2972 0.041 Uiso 1 1 calc R . . C54 C 0.7467(4) -0.2477(4) 0.2710(2) 0.0312(16) Uani 1 1 d . . . H54 H 0.7003 -0.2675 0.2543 0.037 Uiso 1 1 calc R . . C55 C 0.7729(3) -0.1594(4) 0.26996(18) 0.0239(15) Uani 1 1 d . . . C56 C 0.7307(3) -0.0877(4) 0.24546(19) 0.0256(15) Uani 1 1 d . . . C57 C 0.6794(3) -0.1033(4) 0.21102(19) 0.0309(16) Uani 1 1 d . . . H57 H 0.6667 -0.1630 0.2022 0.037 Uiso 1 1 calc R . . C58 C 0.6474(4) -0.0294(5) 0.1899(2) 0.0377(18) Uani 1 1 d . . . H58 H 0.6113 -0.0380 0.1665 0.045 Uiso 1 1 calc R . . C59 C 0.6679(3) 0.0567(4) 0.20260(19) 0.0303(16) Uani 1 1 d . . . H59 H 0.6478 0.1076 0.1876 0.036 Uiso 1 1 calc R . . C60 C 0.7185(3) 0.0679(4) 0.23766(19) 0.0260(15) Uani 1 1 d . . . C61 C 0.9155(3) -0.0920(4) 0.38401(18) 0.0240(15) Uani 1 1 d . . . C62 C 0.9477(3) -0.1429(4) 0.34560(18) 0.0250(15) Uani 1 1 d . . . H62A H 0.9790 -0.0998 0.3284 0.030 Uiso 1 1 calc R . . H62B H 0.9883 -0.1902 0.3547 0.030 Uiso 1 1 calc R . . C63 C 0.9852(4) -0.0315(4) 0.4023(2) 0.0274(16) Uani 1 1 d . . . C64 C 1.0615(4) -0.0105(4) 0.38342(19) 0.0323(16) Uani 1 1 d . . . H64 H 1.0751 -0.0397 0.3586 0.039 Uiso 1 1 calc R . . C65 C 1.1178(4) 0.0519(5) 0.4001(2) 0.0391(18) Uani 1 1 d . . . H65 H 1.1689 0.0656 0.3866 0.047 Uiso 1 1 calc R . . C66 C 1.0996(4) 0.0943(5) 0.4366(2) 0.046(2) Uani 1 1 d . . . H66 H 1.1381 0.1376 0.4477 0.055 Uiso 1 1 calc R . . C67 C 1.0255(4) 0.0742(4) 0.4570(2) 0.0375(18) Uani 1 1 d . . . H67 H 1.0132 0.1028 0.4821 0.045 Uiso 1 1 calc R . . C68 C 0.9694(4) 0.0112(4) 0.4397(2) 0.0322(17) Uani 1 1 d . . . H68 H 0.9190 -0.0033 0.4537 0.039 Uiso 1 1 calc R . . C69 C 0.8871(4) -0.1611(4) 0.41544(19) 0.0310(16) Uani 1 1 d . . . C70 C 0.8029(4) -0.1840(4) 0.4216(2) 0.0413(19) Uani 1 1 d . . . H70 H 0.7602 -0.1544 0.4057 0.050 Uiso 1 1 calc R . . C71 C 0.7785(5) -0.2464(6) 0.4493(3) 0.068(3) Uani 1 1 d . . . H71 H 0.7203 -0.2620 0.4517 0.082 Uiso 1 1 calc R . . C72 C 0.8402(6) -0.2867(6) 0.4739(3) 0.077(3) Uani 1 1 d . . . H72 H 0.8239 -0.3278 0.4946 0.093 Uiso 1 1 calc R . . C73 C 0.9264(5) -0.2675(5) 0.4686(2) 0.057(2) Uani 1 1 d . . . H73 H 0.9688 -0.2966 0.4850 0.068 Uiso 1 1 calc R . . C74 C 0.9484(4) -0.2062(4) 0.4396(2) 0.0383(18) Uani 1 1 d . . . H74 H 1.0069 -0.1937 0.4357 0.046 Uiso 1 1 calc R . . C81 C 0.8348(3) 0.1916(4) 0.24396(19) 0.0222(15) Uani 1 1 d . . . C82 C 0.7432(3) 0.1602(4) 0.25458(19) 0.0262(16) Uani 1 1 d . . . H82A H 0.7384 0.1588 0.2847 0.031 Uiso 1 1 calc R . . H82B H 0.7020 0.2053 0.2438 0.031 Uiso 1 1 calc R . . C83 C 0.8512(3) 0.2874(4) 0.25892(19) 0.0241(15) Uani 1 1 d . . . C84 C 0.8052(3) 0.3304(4) 0.28955(19) 0.0291(16) Uani 1 1 d . . . H84 H 0.7597 0.2993 0.3019 0.035 Uiso 1 1 calc R . . C85 C 0.8248(4) 0.4181(4) 0.3022(2) 0.0345(18) Uani 1 1 d . . . H85 H 0.7930 0.4461 0.3230 0.041 Uiso 1 1 calc R . . C86 C 0.8908(4) 0.4638(4) 0.2844(2) 0.0343(18) Uani 1 1 d . . . H86 H 0.9041 0.5236 0.2927 0.041 Uiso 1 1 calc R . . C87 C 0.9377(4) 0.4227(4) 0.2543(2) 0.0340(17) Uani 1 1 d . . . H87 H 0.9833 0.4540 0.2421 0.041 Uiso 1 1 calc R . . C88 C 0.9178(3) 0.3360(4) 0.24208(19) 0.0290(16) Uani 1 1 d . . . H88 H 0.9505 0.3085 0.2215 0.035 Uiso 1 1 calc R . . C89 C 0.8431(3) 0.1887(4) 0.19772(19) 0.0221(14) Uani 1 1 d . . . C90 C 0.7918(4) 0.2457(4) 0.1737(2) 0.0368(18) Uani 1 1 d . . . H90 H 0.7532 0.2846 0.1869 0.044 Uiso 1 1 calc R . . C91 C 0.7951(4) 0.2475(5) 0.1328(2) 0.049(2) Uani 1 1 d . . . H91 H 0.7581 0.2862 0.1176 0.058 Uiso 1 1 calc R . . C92 C 0.8523(4) 0.1929(5) 0.1123(2) 0.048(2) Uani 1 1 d . . . H92 H 0.8552 0.1943 0.0834 0.057 Uiso 1 1 calc R . . C93 C 0.9053(4) 0.1361(5) 0.1356(2) 0.047(2) Uani 1 1 d . . . H93 H 0.9452 0.0985 0.1224 0.057 Uiso 1 1 calc R . . C94 C 0.8999(4) 0.1347(4) 0.1778(2) 0.0337(17) Uani 1 1 d . . . H94 H 0.9360 0.0957 0.1932 0.040 Uiso 1 1 calc R . . O1 O 0.6308(3) -0.0703(4) 0.49370(16) 0.0614(16) Uani 1 1 d . . . C101 C 0.5552(5) -0.1197(6) 0.4849(3) 0.076(3) Uani 1 1 d . . . H10A H 0.5496 -0.1310 0.4552 0.091 Uiso 1 1 calc R . . H10B H 0.5051 -0.0846 0.4935 0.091 Uiso 1 1 calc R . . C102 C 0.5588(5) -0.2038(7) 0.5066(3) 0.092(3) Uani 1 1 d . . . H10C H 0.5678 -0.2545 0.4875 0.111 Uiso 1 1 calc R . . H10D H 0.5054 -0.2143 0.5213 0.111 Uiso 1 1 calc R . . C103 C 0.6320(6) -0.1956(6) 0.5362(3) 0.074(3) Uani 1 1 d . . . H10E H 0.6147 -0.2107 0.5643 0.089 Uiso 1 1 calc R . . H10F H 0.6792 -0.2358 0.5284 0.089 Uiso 1 1 calc R . . C104 C 0.6569(5) -0.0998(6) 0.5331(2) 0.062(2) Uani 1 1 d . . . H10G H 0.6288 -0.0637 0.5544 0.074 Uiso 1 1 calc R . . H10H H 0.7192 -0.0933 0.5368 0.074 Uiso 1 1 calc R . . O2 O 1.0750(3) 0.2634(4) 0.36151(19) 0.0768(19) Uani 1 1 d . . . C105 C 1.0877(5) 0.3005(5) 0.3209(3) 0.060(2) Uani 1 1 d . . . H10I H 1.0371 0.2908 0.3030 0.072 Uiso 1 1 calc R . . H10J H 1.1378 0.2730 0.3081 0.072 Uiso 1 1 calc R . . C106 C 1.1017(4) 0.3982(5) 0.3289(2) 0.059(2) Uani 1 1 d . . . H10K H 1.0474 0.4305 0.3326 0.071 Uiso 1 1 calc R . . H10L H 1.1334 0.4272 0.3066 0.071 Uiso 1 1 calc R . . C107 C 1.1551(5) 0.3950(5) 0.3691(3) 0.064(2) Uani 1 1 d . . . H10M H 1.2159 0.3851 0.3635 0.077 Uiso 1 1 calc R . . H10N H 1.1491 0.4517 0.3847 0.077 Uiso 1 1 calc R . . C108 C 1.1195(5) 0.3175(6) 0.3918(3) 0.076(3) Uani 1 1 d . . . H10O H 1.1655 0.2823 0.4053 0.092 Uiso 1 1 calc R . . H10P H 1.0800 0.3388 0.4128 0.092 Uiso 1 1 calc R . . O3 O 0.3416(7) 0.5639(7) 0.4253(4) 0.093(3) Uani 0.50 1 d PDU . . C111 C 0.3001(7) 0.5051(11) 0.4509(5) 0.089(4) Uani 0.50 1 d PDU . . H11A H 0.2762 0.5392 0.4739 0.107 Uiso 0.50 1 calc PR . . H11B H 0.2525 0.4759 0.4356 0.107 Uiso 0.50 1 calc PR . . C112 C 0.3553(9) 0.4398(9) 0.4658(5) 0.091(4) Uani 0.50 1 d PDU . . H11C H 0.3297 0.3791 0.4629 0.109 Uiso 0.50 1 calc PR . . H11D H 0.3690 0.4506 0.4951 0.109 Uiso 0.50 1 calc PR . . C113 C 0.4297(8) 0.4470(9) 0.4421(5) 0.091(4) Uani 0.50 1 d PDU . . H11E H 0.4275 0.4046 0.4188 0.109 Uiso 0.50 1 calc PR . . H11F H 0.4814 0.4345 0.4590 0.109 Uiso 0.50 1 calc PR . . C114 C 0.4284(7) 0.5419(9) 0.4278(5) 0.079(3) Uani 0.50 1 d PDU . . H11G H 0.4590 0.5817 0.4475 0.095 Uiso 0.50 1 calc PR . . H11H H 0.4549 0.5474 0.4008 0.095 Uiso 0.50 1 calc PR . . 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 Cu1 0.0276(4) 0.0234(5) 0.0293(5) 0.0019(4) -0.0022(3) -0.0002(3) Cu2 0.0292(4) 0.0197(4) 0.0263(5) 0.0030(4) 0.0013(3) 0.0004(3) K1 0.0359(8) 0.0363(9) 0.0299(10) 0.0012(7) 0.0051(7) 0.0083(6) K2 0.0289(7) 0.0299(9) 0.0472(11) -0.0067(8) 0.0038(7) -0.0031(6) S1 0.0232(8) 0.0267(10) 0.0339(11) -0.0117(8) 0.0013(7) 0.0022(7) S2 0.0301(8) 0.0285(10) 0.0219(10) -0.0019(8) 0.0010(7) -0.0046(7) N1 0.025(3) 0.027(3) 0.035(4) 0.002(3) 0.009(3) 0.008(2) N2 0.021(3) 0.031(3) 0.021(3) 0.006(3) 0.004(2) 0.003(2) C1 0.028(3) 0.022(4) 0.042(5) -0.006(4) 0.013(3) 0.005(3) C2 0.049(4) 0.025(4) 0.047(5) -0.003(4) 0.019(4) 0.007(3) C3 0.041(4) 0.019(4) 0.078(7) 0.004(4) 0.024(4) 0.009(3) C4 0.035(4) 0.037(5) 0.065(6) 0.020(4) 0.024(4) 0.019(3) C5 0.021(3) 0.027(4) 0.047(5) 0.010(4) 0.012(3) 0.010(3) C6 0.018(3) 0.035(4) 0.035(5) 0.017(4) 0.006(3) 0.008(3) C7 0.028(4) 0.044(5) 0.042(5) 0.021(4) 0.006(3) 0.010(3) C8 0.028(4) 0.079(6) 0.035(5) 0.021(5) -0.003(3) -0.001(4) C9 0.027(3) 0.060(5) 0.022(4) 0.008(4) 0.001(3) -0.009(3) C10 0.019(3) 0.039(4) 0.021(4) 0.007(3) 0.007(3) 0.001(3) C11 0.022(3) 0.034(4) 0.035(5) -0.016(3) 0.002(3) 0.001(3) C12 0.037(4) 0.019(4) 0.035(5) -0.007(3) 0.011(3) -0.002(3) C13 0.055(5) 0.039(5) 0.055(6) -0.021(4) 0.025(4) -0.021(4) C14 0.091(6) 0.062(6) 0.066(7) -0.031(5) 0.037(5) -0.043(5) C15 0.093(7) 0.087(8) 0.085(8) -0.039(6) 0.039(6) -0.058(6) C16 0.085(6) 0.077(7) 0.093(9) -0.056(6) 0.009(6) -0.043(5) C17 0.053(5) 0.050(5) 0.057(6) -0.022(4) 0.012(4) -0.020(4) C18 0.033(4) 0.028(4) 0.045(5) -0.021(4) 0.011(3) 0.000(3) C19 0.026(3) 0.033(4) 0.025(4) -0.016(3) -0.001(3) 0.000(3) C20 0.036(4) 0.049(5) 0.032(5) 0.001(4) 0.001(3) 0.008(3) C21 0.043(4) 0.062(6) 0.036(5) 0.005(4) 0.006(4) 0.006(4) C22 0.054(5) 0.048(5) 0.037(5) -0.002(4) -0.012(4) 0.007(4) C23 0.035(4) 0.051(5) 0.043(5) -0.015(4) -0.010(4) 0.008(3) C24 0.032(4) 0.044(5) 0.036(5) -0.010(4) -0.001(3) 0.000(3) C31 0.022(3) 0.026(4) 0.017(4) -0.003(3) 0.001(3) -0.004(2) C32 0.023(3) 0.034(4) 0.020(4) -0.003(3) 0.003(3) 0.001(3) C33 0.023(3) 0.028(4) 0.017(4) 0.004(3) 0.008(3) -0.005(3) C34 0.028(3) 0.038(4) 0.033(4) -0.007(4) 0.005(3) 0.000(3) C35 0.034(4) 0.049(5) 0.031(5) 0.004(4) -0.007(3) -0.013(3) C36 0.029(4) 0.044(5) 0.042(5) 0.015(4) 0.006(3) 0.002(3) C37 0.035(4) 0.033(4) 0.039(5) 0.006(4) 0.009(3) 0.006(3) C38 0.030(3) 0.029(4) 0.025(4) 0.000(3) 0.003(3) -0.006(3) C39 0.024(3) 0.030(4) 0.011(4) -0.003(3) 0.002(3) -0.003(3) C40 0.032(3) 0.030(4) 0.034(5) -0.007(3) 0.008(3) 0.006(3) C41 0.039(4) 0.031(4) 0.046(5) 0.003(4) 0.013(3) -0.003(3) C42 0.055(5) 0.027(4) 0.036(5) 0.000(4) 0.007(4) 0.002(3) C43 0.034(4) 0.040(5) 0.038(5) -0.007(4) -0.003(3) 0.014(3) C44 0.032(3) 0.036(4) 0.021(4) -0.002(3) -0.001(3) -0.006(3) S51 0.0275(8) 0.0243(9) 0.0242(10) 0.0008(8) 0.0052(7) 0.0078(7) S52 0.0221(8) 0.0252(10) 0.0374(12) 0.0083(8) 0.0023(7) 0.0026(7) N51 0.029(3) 0.024(3) 0.015(3) -0.002(2) 0.008(2) 0.005(2) N52 0.022(2) 0.020(3) 0.019(3) 0.004(2) 0.004(2) -0.004(2) C51 0.027(3) 0.023(4) 0.027(4) -0.004(3) 0.014(3) 0.005(3) C52 0.043(4) 0.020(4) 0.033(5) 0.003(3) 0.013(3) 0.010(3) C53 0.039(4) 0.015(4) 0.050(5) -0.008(3) 0.015(3) -0.002(3) C54 0.030(3) 0.029(4) 0.035(5) -0.010(3) 0.007(3) -0.004(3) C55 0.027(3) 0.022(4) 0.023(4) -0.005(3) 0.008(3) 0.001(3) C56 0.025(3) 0.032(4) 0.020(4) -0.002(3) 0.013(3) -0.009(3) C57 0.030(3) 0.032(4) 0.031(5) -0.003(3) 0.008(3) -0.009(3) C58 0.032(4) 0.051(5) 0.030(5) 0.008(4) -0.008(3) -0.008(3) C59 0.023(3) 0.035(4) 0.033(5) -0.001(3) -0.002(3) 0.002(3) C60 0.017(3) 0.034(4) 0.027(4) 0.008(3) 0.009(3) 0.000(3) C61 0.030(3) 0.022(4) 0.020(4) 0.002(3) 0.004(3) 0.004(3) C62 0.026(3) 0.024(4) 0.025(4) 0.001(3) 0.005(3) 0.008(3) C63 0.029(3) 0.026(4) 0.027(4) 0.006(3) -0.001(3) 0.006(3) C64 0.035(4) 0.035(4) 0.027(4) 0.005(3) 0.001(3) 0.003(3) C65 0.031(4) 0.045(5) 0.042(5) 0.006(4) 0.002(3) -0.003(3) C66 0.035(4) 0.043(5) 0.058(6) 0.009(4) -0.014(4) -0.008(3) C67 0.048(4) 0.037(5) 0.027(5) 0.000(3) -0.007(4) 0.004(3) C68 0.031(3) 0.033(4) 0.033(5) 0.006(4) -0.002(3) 0.002(3) C69 0.034(4) 0.028(4) 0.031(5) 0.003(3) 0.005(3) 0.003(3) C70 0.043(4) 0.033(5) 0.048(5) 0.019(4) 0.017(4) 0.006(3) C71 0.054(5) 0.058(6) 0.094(8) 0.028(6) 0.029(5) 0.005(4) C72 0.088(7) 0.076(7) 0.070(7) 0.045(6) 0.039(6) 0.004(5) C73 0.091(6) 0.035(5) 0.045(6) 0.022(4) 0.003(5) 0.006(4) C74 0.047(4) 0.029(4) 0.039(5) 0.009(4) 0.005(3) 0.003(3) C81 0.021(3) 0.018(4) 0.028(4) 0.007(3) 0.007(3) 0.003(2) C82 0.022(3) 0.023(4) 0.033(4) 0.008(3) 0.002(3) 0.003(3) C83 0.024(3) 0.027(4) 0.021(4) 0.007(3) 0.000(3) 0.006(3) C84 0.024(3) 0.032(4) 0.031(5) 0.003(3) 0.003(3) 0.003(3) C85 0.025(3) 0.034(4) 0.044(5) -0.010(4) 0.003(3) 0.005(3) C86 0.036(4) 0.026(4) 0.041(5) -0.006(4) -0.011(3) 0.008(3) C87 0.038(4) 0.030(4) 0.034(5) 0.004(4) 0.005(3) -0.005(3) C88 0.031(3) 0.024(4) 0.033(5) -0.003(3) 0.012(3) -0.001(3) C89 0.023(3) 0.022(4) 0.022(4) 0.001(3) 0.005(3) -0.004(3) C90 0.043(4) 0.038(5) 0.030(5) 0.007(4) 0.010(3) 0.003(3) C91 0.056(5) 0.052(5) 0.038(6) 0.015(4) -0.002(4) -0.003(4) C92 0.062(5) 0.059(6) 0.021(5) -0.001(4) 0.002(4) -0.031(4) C93 0.058(5) 0.046(5) 0.038(6) -0.016(4) 0.012(4) -0.001(4) C94 0.039(4) 0.035(4) 0.028(5) -0.002(3) 0.004(3) 0.000(3) O1 0.049(3) 0.096(5) 0.038(4) 0.020(3) -0.003(3) -0.017(3) C101 0.068(6) 0.071(7) 0.088(8) 0.005(6) -0.024(5) -0.011(5) C102 0.060(6) 0.079(8) 0.139(10) 0.002(7) -0.002(6) -0.021(5) C103 0.097(7) 0.083(8) 0.044(6) 0.006(5) 0.027(5) 0.011(6) C104 0.053(5) 0.089(7) 0.043(6) 0.011(5) 0.000(4) -0.020(4) O2 0.071(4) 0.075(4) 0.083(5) 0.039(4) -0.033(3) -0.038(3) C105 0.062(5) 0.044(5) 0.074(7) 0.014(5) -0.016(5) -0.004(4) C106 0.046(5) 0.064(6) 0.068(7) 0.010(5) 0.002(4) -0.006(4) C107 0.060(5) 0.048(6) 0.083(7) -0.003(5) 0.004(5) -0.014(4) C108 0.075(6) 0.072(7) 0.081(8) 0.022(6) -0.015(5) -0.015(5) O3 0.109(6) 0.076(7) 0.095(7) 0.020(5) 0.027(6) 0.022(5) C111 0.075(6) 0.095(8) 0.099(9) 0.001(7) 0.047(6) 0.003(6) C112 0.108(8) 0.057(8) 0.113(9) 0.023(6) 0.083(7) 0.002(6) C113 0.092(7) 0.065(7) 0.119(9) 0.036(7) 0.073(6) 0.021(6) C114 0.082(5) 0.061(6) 0.097(7) 0.027(6) 0.052(6) -0.008(5) _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 Cu1 N2 2.012(5) . ? Cu1 N1 2.064(5) . ? Cu1 S2 2.2523(17) . ? Cu1 S1 2.2948(15) . ? Cu1 K1 3.5668(15) . ? Cu2 N52 2.026(4) . ? Cu2 N51 2.068(5) . ? Cu2 S52 2.2565(17) . ? Cu2 S51 2.2972(18) . ? Cu2 K2 3.4597(15) . ? K1 O1 2.643(5) . ? K1 S1 3.127(2) . ? K1 S51 3.136(2) . ? K1 S2 3.1371(19) . ? K1 C19 3.342(6) . ? K1 C24 3.425(6) . ? K1 C20 3.449(7) . ? K1 K2 4.790(2) . ? K2 O2 2.673(5) . ? K2 S51 3.151(2) . ? K2 S1 3.160(2) . ? K2 S52 3.163(2) . ? K2 C63 3.323(6) . ? K2 C68 3.419(6) . ? K2 C64 3.421(6) . ? K2 C105 3.497(8) . ? S1 C11 1.843(6) . ? S2 C31 1.858(6) . ? N1 C1 1.344(7) . ? N1 C5 1.360(7) . ? N2 C6 1.353(7) . ? N2 C10 1.360(7) . ? C1 C2 1.388(9) . ? C1 C12 1.494(8) . ? C2 C3 1.375(9) . ? C2 H2 0.9500 . ? C3 C4 1.401(9) . ? C3 H3 0.9500 . ? C4 C5 1.398(9) . ? C4 H4 0.9500 . ? C5 C6 1.460(9) . ? C6 C7 1.384(8) . ? C7 C8 1.393(9) . ? C7 H7 0.9500 . ? C8 C9 1.391(9) . ? C8 H8 0.9500 . ? C9 C10 1.396(8) . ? C9 H9 0.9500 . ? C10 C32 1.496(8) . ? C11 C19 1.534(9) . ? C11 C18 1.536(8) . ? C11 C12 1.553(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C18 1.371(9) . ? C13 C14 1.383(9) . ? C13 H13 0.9500 . ? C14 C15 1.383(10) . ? C14 H14 0.9500 . ? C15 C16 1.402(11) . ? C15 H15 0.9500 . ? C16 C17 1.396(9) . ? C16 H16 0.9500 . ? C17 C18 1.421(9) . ? C17 H17 0.9500 . ? C19 C20 1.382(8) . ? C19 C24 1.397(8) . ? C20 C21 1.382(9) . ? C20 H20 0.9500 . ? C21 C22 1.370(8) . ? C21 H21 0.9500 . ? C22 C23 1.370(9) . ? C22 H22 0.9500 . ? C23 C24 1.405(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C31 C39 1.515(8) . ? C31 C33 1.537(7) . ? C31 C32 1.562(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C38 1.376(8) . ? C33 C34 1.397(7) . ? C34 C35 1.400(7) . ? C34 H34 0.9500 . ? C35 C36 1.378(9) . ? C35 H35 0.9500 . ? C36 C37 1.376(8) . ? C36 H36 0.9500 . ? C37 C38 1.396(7) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.389(8) . ? C39 C44 1.404(8) . ? C40 C41 1.382(8) . ? C40 H40 0.9500 . ? C41 C42 1.382(8) . ? C41 H41 0.9500 . ? C42 C43 1.372(8) . ? C42 H42 0.9500 . ? C43 C44 1.384(8) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? S51 C61 1.857(5) . ? S52 C81 1.871(5) . ? N51 C51 1.343(7) . ? N51 C55 1.352(6) . ? N52 C60 1.330(7) . ? N52 C56 1.363(7) . ? C51 C52 1.390(8) . ? C51 C62 1.514(7) . ? C52 C53 1.393(8) . ? C52 H52 0.9500 . ? C53 C54 1.383(8) . ? C53 H53 0.9500 . ? C54 C55 1.374(8) . ? C54 H54 0.9500 . ? C55 C56 1.479(8) . ? C56 C57 1.390(7) . ? C57 C58 1.385(8) . ? C57 H57 0.9500 . ? C58 C59 1.379(8) . ? C58 H58 0.9500 . ? C59 C60 1.391(7) . ? C59 H59 0.9500 . ? C60 C82 1.523(8) . ? C61 C69 1.525(8) . ? C61 C63 1.529(8) . ? C61 C62 1.561(8) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.399(8) . ? C63 C68 1.405(8) . ? C64 C65 1.385(8) . ? C64 H64 0.9500 . ? C65 C66 1.383(9) . ? C65 H65 0.9500 . ? C66 C67 1.390(9) . ? C66 H66 0.9500 . ? C67 C68 1.395(8) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C70 1.387(8) . ? C69 C74 1.404(8) . ? C70 C71 1.356(9) . ? C70 H70 0.9500 . ? C71 C72 1.382(10) . ? C71 H71 0.9500 . ? C72 C73 1.401(10) . ? C72 H72 0.9500 . ? C73 C74 1.364(9) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C81 C83 1.523(8) . ? C81 C89 1.522(8) . ? C81 C82 1.563(7) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C88 1.395(8) . ? C83 C84 1.403(8) . ? C84 C85 1.397(8) . ? C84 H84 0.9500 . ? C85 C86 1.381(8) . ? C85 H85 0.9500 . ? C86 C87 1.384(8) . ? C86 H86 0.9500 . ? C87 C88 1.380(8) . ? C87 H87 0.9500 . ? C88 H88 0.9500 . ? C89 C94 1.375(8) . ? C89 C90 1.397(8) . ? C90 C91 1.342(9) . ? C90 H90 0.9500 . ? C91 C92 1.393(10) . ? C91 H91 0.9500 . ? C92 C93 1.399(9) . ? C92 H92 0.9500 . ? C93 C94 1.385(8) . ? C93 H93 0.9500 . ? C94 H94 0.9500 . ? O1 C104 1.414(8) . ? O1 C101 1.421(8) . ? C101 C102 1.436(11) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 C103 1.491(10) . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.479(11) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? O2 C108 1.443(9) . ? O2 C105 1.455(8) . ? C105 C106 1.489(10) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 C107 1.543(9) . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.485(10) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? O3 C111 1.383(9) . ? O3 C114 1.405(9) . ? C111 C112 1.383(8) . ? C111 H11A 0.9900 . ? C111 H11B 0.9900 . ? C112 C113 1.424(8) . ? C112 H11C 0.9900 . ? C112 H11D 0.9900 . ? C113 C114 1.484(9) . ? C113 H11E 0.9900 . ? C113 H11F 0.9900 . ? C114 H11G 0.9900 . ? C114 H11H 0.9900 . ? 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 N2 Cu1 N1 79.3(2) . . ? N2 Cu1 S2 101.03(14) . . ? N1 Cu1 S2 138.89(14) . . ? N2 Cu1 S1 125.32(14) . . ? N1 Cu1 S1 89.66(13) . . ? S2 Cu1 S1 120.20(6) . . ? N2 Cu1 K1 139.11(15) . . ? N1 Cu1 K1 139.59(15) . . ? S2 Cu1 K1 60.33(5) . . ? S1 Cu1 K1 59.89(5) . . ? N52 Cu2 N51 79.31(18) . . ? N52 Cu2 S52 98.91(14) . . ? N51 Cu2 S52 134.56(14) . . ? N52 Cu2 S51 124.02(13) . . ? N51 Cu2 S51 88.90(14) . . ? S52 Cu2 S51 125.63(6) . . ? N52 Cu2 K2 138.58(14) . . ? N51 Cu2 K2 140.59(13) . . ? S52 Cu2 K2 63.13(5) . . ? S51 Cu2 K2 62.59(5) . . ? O1 K1 S1 155.74(14) . . ? O1 K1 S51 129.73(14) . . ? S1 K1 S51 74.49(5) . . ? O1 K1 S2 94.56(11) . . ? S1 K1 S2 78.00(5) . . ? S51 K1 S2 104.42(6) . . ? O1 K1 C19 111.09(17) . . ? S1 K1 C19 48.64(12) . . ? S51 K1 C19 111.62(12) . . ? S2 K1 C19 98.06(11) . . ? O1 K1 C24 109.71(17) . . ? S1 K1 C24 58.09(13) . . ? S51 K1 C24 99.15(12) . . ? S2 K1 C24 121.50(12) . . ? C19 K1 C24 23.79(13) . . ? O1 K1 C20 90.16(17) . . ? S1 K1 C20 66.98(13) . . ? S51 K1 C20 135.03(13) . . ? S2 K1 C20 89.70(11) . . ? C19 K1 C20 23.42(14) . . ? C24 K1 C20 40.41(15) . . ? O1 K1 Cu1 129.64(11) . . ? S1 K1 Cu1 39.41(3) . . ? S51 K1 Cu1 88.82(5) . . ? S2 K1 Cu1 38.60(3) . . ? C19 K1 Cu1 71.25(11) . . ? C24 K1 Cu1 90.52(12) . . ? C20 K1 Cu1 76.06(11) . . ? O1 K1 K2 157.40(11) . . ? S1 K1 K2 40.61(4) . . ? S51 K1 K2 40.48(4) . . ? S2 K1 K2 107.51(5) . . ? C19 K1 K2 71.26(12) . . ? C24 K1 K2 62.86(12) . . ? C20 K1 K2 94.63(12) . . ? Cu1 K1 K2 72.87(3) . . ? O2 K2 S51 151.97(14) . . ? O2 K2 S1 132.47(15) . . ? S51 K2 S1 73.82(5) . . ? O2 K2 S52 95.92(15) . . ? S51 K2 S52 79.82(5) . . ? S1 K2 S52 110.05(5) . . ? O2 K2 C63 105.69(16) . . ? S51 K2 C63 48.79(10) . . ? S1 K2 C63 108.43(12) . . ? S52 K2 C63 99.07(12) . . ? O2 K2 C68 104.77(15) . . ? S51 K2 C68 57.51(11) . . ? S1 K2 C68 93.94(12) . . ? S52 K2 C68 122.66(12) . . ? C63 K2 C68 24.01(14) . . ? O2 K2 C64 84.40(16) . . ? S51 K2 C64 68.08(11) . . ? S1 K2 C64 132.16(12) . . ? S52 K2 C64 90.80(12) . . ? C63 K2 C64 23.88(13) . . ? C68 K2 C64 40.94(15) . . ? O2 K2 Cu2 130.48(15) . . ? S51 K2 Cu2 40.33(3) . . ? S1 K2 Cu2 91.42(4) . . ? S52 K2 Cu2 39.52(3) . . ? C63 K2 Cu2 72.20(11) . . ? C68 K2 Cu2 91.16(11) . . ? C64 K2 Cu2 77.86(11) . . ? O2 K2 C105 22.64(15) . . ? S51 K2 C105 149.23(15) . . ? S1 K2 C105 132.03(14) . . ? S52 K2 C105 75.39(14) . . ? C63 K2 C105 117.86(16) . . ? C68 K2 C105 124.09(16) . . ? C64 K2 C105 94.14(16) . . ? Cu2 K2 C105 113.37(14) . . ? O2 K2 K1 152.65(14) . . ? S51 K2 K1 40.24(4) . . ? S1 K2 K1 40.10(4) . . ? S52 K2 K1 111.31(4) . . ? C63 K2 K1 68.67(11) . . ? C68 K2 K1 58.77(10) . . ? C64 K2 K1 92.56(11) . . ? Cu2 K2 K1 74.70(3) . . ? C105 K2 K1 170.47(15) . . ? C11 S1 Cu1 104.07(17) . . ? C11 S1 K1 102.0(2) . . ? Cu1 S1 K1 80.69(5) . . ? C11 S1 K2 119.04(17) . . ? Cu1 S1 K2 135.57(7) . . ? K1 S1 K2 99.29(6) . . ? C31 S2 Cu1 104.97(19) . . ? C31 S2 K1 120.04(18) . . ? Cu1 S2 K1 81.07(5) . . ? C1 N1 C5 120.2(6) . . ? C1 N1 Cu1 121.6(4) . . ? C5 N1 Cu1 113.5(4) . . ? C6 N2 C10 119.6(5) . . ? C6 N2 Cu1 116.1(4) . . ? C10 N2 Cu1 122.6(4) . . ? N1 C1 C2 121.2(6) . . ? N1 C1 C12 114.5(6) . . ? C2 C1 C12 124.2(6) . . ? C3 C2 C1 119.5(7) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.8(7) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 118.4(7) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? N1 C5 C4 120.8(7) . . ? N1 C5 C6 114.2(6) . . ? C4 C5 C6 124.9(7) . . ? N2 C6 C7 121.9(6) . . ? N2 C6 C5 114.0(5) . . ? C7 C6 C5 124.1(6) . . ? C6 C7 C8 118.9(6) . . ? C6 C7 H7 120.6 . . ? C8 C7 H7 120.6 . . ? C9 C8 C7 119.4(6) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 119.3(6) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N2 C10 C9 120.8(6) . . ? N2 C10 C32 116.6(5) . . ? C9 C10 C32 122.6(6) . . ? C19 C11 C18 111.6(5) . . ? C19 C11 C12 111.0(5) . . ? C18 C11 C12 107.5(5) . . ? C19 C11 S1 104.2(4) . . ? C18 C11 S1 111.2(4) . . ? C12 C11 S1 111.4(4) . . ? C1 C12 C11 114.9(5) . . ? C1 C12 H12A 108.5 . . ? C11 C12 H12A 108.5 . . ? C1 C12 H12B 108.5 . . ? C11 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C18 C13 C14 121.0(7) . . ? C18 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C15 121.1(8) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 118.9(8) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C17 C16 C15 120.3(8) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 119.5(8) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C13 C18 C17 119.1(6) . . ? C13 C18 C11 122.5(6) . . ? C17 C18 C11 118.2(6) . . ? C20 C19 C24 117.4(6) . . ? C20 C19 C11 123.9(5) . . ? C24 C19 C11 118.6(6) . . ? C20 C19 K1 82.7(4) . . ? C24 C19 K1 81.5(4) . . ? C11 C19 K1 101.5(3) . . ? C21 C20 C19 121.4(6) . . ? C21 C20 K1 84.3(4) . . ? C19 C20 K1 73.9(4) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? K1 C20 H20 112.6 . . ? C22 C21 C20 121.0(7) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C23 C22 C21 119.3(7) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 C24 120.2(6) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C19 C24 C23 120.7(6) . . ? C19 C24 K1 74.7(3) . . ? C23 C24 K1 84.8(4) . . ? C19 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? K1 C24 H24 111.0 . . ? C39 C31 C33 112.3(4) . . ? C39 C31 C32 109.8(5) . . ? C33 C31 C32 106.7(4) . . ? C39 C31 S2 104.3(4) . . ? C33 C31 S2 112.1(4) . . ? C32 C31 S2 111.8(4) . . ? C10 C32 C31 115.4(5) . . ? C10 C32 H32A 108.4 . . ? C31 C32 H32A 108.4 . . ? C10 C32 H32B 108.4 . . ? C31 C32 H32B 108.4 . . ? H32A C32 H32B 107.5 . . ? C38 C33 C34 117.9(5) . . ? C38 C33 C31 122.9(5) . . ? C34 C33 C31 119.2(5) . . ? C33 C34 C35 120.2(6) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 120.7(6) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C37 119.4(6) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C36 C37 C38 119.7(6) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C33 C38 C37 122.0(6) . . ? C33 C38 H38 119.0 . . ? C37 C38 H38 119.0 . . ? C40 C39 C44 115.8(6) . . ? C40 C39 C31 121.0(5) . . ? C44 C39 C31 123.1(5) . . ? C41 C40 C39 121.8(6) . . ? C41 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? C42 C41 C40 121.1(6) . . ? C42 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? C43 C42 C41 118.8(6) . . ? C43 C42 H42 120.6 . . ? C41 C42 H42 120.6 . . ? C42 C43 C44 120.0(6) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C43 C44 C39 122.6(6) . . ? C43 C44 H44 118.7 . . ? C39 C44 H44 118.7 . . ? C61 S51 Cu2 103.8(2) . . ? C61 S51 K1 115.7(2) . . ? Cu2 S51 K1 140.16(6) . . ? C61 S51 K2 100.48(19) . . ? Cu2 S51 K2 77.08(5) . . ? K1 S51 K2 99.28(6) . . ? C81 S52 Cu2 105.38(18) . . ? C81 S52 K2 112.3(2) . . ? Cu2 S52 K2 77.35(6) . . ? C51 N51 C55 119.4(5) . . ? C51 N51 Cu2 121.7(4) . . ? C55 N51 Cu2 114.5(4) . . ? C60 N52 C56 119.8(5) . . ? C60 N52 Cu2 122.2(4) . . ? C56 N52 Cu2 115.5(4) . . ? N51 C51 C52 121.6(5) . . ? N51 C51 C62 114.1(5) . . ? C52 C51 C62 124.3(6) . . ? C51 C52 C53 118.4(6) . . ? C51 C52 H52 120.8 . . ? C53 C52 H52 120.8 . . ? C54 C53 C52 119.5(6) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C55 C54 C53 119.1(6) . . ? C55 C54 H54 120.5 . . ? C53 C54 H54 120.5 . . ? N51 C55 C54 121.7(6) . . ? N51 C55 C56 113.7(5) . . ? C54 C55 C56 124.6(5) . . ? N52 C56 C57 121.4(6) . . ? N52 C56 C55 114.2(5) . . ? C57 C56 C55 124.4(6) . . ? C58 C57 C56 118.1(6) . . ? C58 C57 H57 120.9 . . ? C56 C57 H57 120.9 . . ? C59 C58 C57 120.1(6) . . ? C59 C58 H58 119.9 . . ? C57 C58 H58 119.9 . . ? C58 C59 C60 119.0(6) . . ? C58 C59 H59 120.5 . . ? C60 C59 H59 120.5 . . ? N52 C60 C59 121.5(6) . . ? N52 C60 C82 115.7(5) . . ? C59 C60 C82 122.9(5) . . ? C69 C61 C63 110.4(5) . . ? C69 C61 C62 108.9(5) . . ? C63 C61 C62 110.8(5) . . ? C69 C61 S51 111.6(4) . . ? C63 C61 S51 104.1(4) . . ? C62 C61 S51 110.9(4) . . ? C51 C62 C61 114.1(4) . . ? C51 C62 H62A 108.7 . . ? C61 C62 H62A 108.7 . . ? C51 C62 H62B 108.7 . . ? C61 C62 H62B 108.7 . . ? H62A C62 H62B 107.6 . . ? C64 C63 C68 117.1(6) . . ? C64 C63 C61 125.0(6) . . ? C68 C63 C61 117.8(5) . . ? C64 C63 K2 82.0(3) . . ? C68 C63 K2 81.8(4) . . ? C61 C63 K2 102.1(3) . . ? C65 C64 C63 121.5(6) . . ? C65 C64 K2 85.5(4) . . ? C63 C64 K2 74.1(3) . . ? C65 C64 H64 119.3 . . ? C63 C64 H64 119.3 . . ? K2 C64 H64 111.1 . . ? C66 C65 C64 120.1(6) . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C65 C66 C67 120.6(7) . . ? C65 C66 H66 119.7 . . ? C67 C66 H66 119.7 . . ? C66 C67 C68 118.7(7) . . ? C66 C67 H67 120.7 . . ? C68 C67 H67 120.7 . . ? C67 C68 C63 122.1(6) . . ? C67 C68 K2 85.8(4) . . ? C63 C68 K2 74.2(3) . . ? C67 C68 H68 119.0 . . ? C63 C68 H68 119.0 . . ? K2 C68 H68 111.0 . . ? C70 C69 C74 116.6(6) . . ? C70 C69 C61 124.0(5) . . ? C74 C69 C61 119.5(5) . . ? C71 C70 C69 123.4(7) . . ? C71 C70 H70 118.3 . . ? C69 C70 H70 118.3 . . ? C70 C71 C72 118.5(7) . . ? C70 C71 H71 120.7 . . ? C72 C71 H71 120.7 . . ? C71 C72 C73 120.6(8) . . ? C71 C72 H72 119.7 . . ? C73 C72 H72 119.7 . . ? C74 C73 C72 119.0(7) . . ? C74 C73 H73 120.5 . . ? C72 C73 H73 120.5 . . ? C73 C74 C69 121.8(7) . . ? C73 C74 H74 119.1 . . ? C69 C74 H74 119.1 . . ? C83 C81 C89 109.2(5) . . ? C83 C81 C82 110.9(5) . . ? C89 C81 C82 108.3(4) . . ? C83 C81 S52 104.4(4) . . ? C89 C81 S52 113.2(4) . . ? C82 C81 S52 110.8(4) . . ? C60 C82 C81 114.6(5) . . ? C60 C82 H82A 108.6 . . ? C81 C82 H82A 108.6 . . ? C60 C82 H82B 108.6 . . ? C81 C82 H82B 108.6 . . ? H82A C82 H82B 107.6 . . ? C88 C83 C84 116.8(6) . . ? C88 C83 C81 118.6(6) . . ? C84 C83 C81 124.6(5) . . ? C85 C84 C83 121.4(6) . . ? C85 C84 H84 119.3 . . ? C83 C84 H84 119.3 . . ? C86 C85 C84 119.6(6) . . ? C86 C85 H85 120.2 . . ? C84 C85 H85 120.2 . . ? C85 C86 C87 120.2(6) . . ? C85 C86 H86 119.9 . . ? C87 C86 H86 119.9 . . ? C88 C87 C86 119.6(6) . . ? C88 C87 H87 120.2 . . ? C86 C87 H87 120.2 . . ? C87 C88 C83 122.3(6) . . ? C87 C88 H88 118.8 . . ? C83 C88 H88 118.8 . . ? C94 C89 C90 117.3(6) . . ? C94 C89 C81 124.1(5) . . ? C90 C89 C81 118.6(5) . . ? C91 C90 C89 122.5(7) . . ? C91 C90 H90 118.7 . . ? C89 C90 H90 118.7 . . ? C90 C91 C92 120.5(7) . . ? C90 C91 H91 119.7 . . ? C92 C91 H91 119.7 . . ? C91 C92 C93 118.2(7) . . ? C91 C92 H92 120.9 . . ? C93 C92 H92 120.9 . . ? C94 C93 C92 120.0(7) . . ? C94 C93 H93 120.0 . . ? C92 C93 H93 120.0 . . ? C89 C94 C93 121.4(6) . . ? C89 C94 H94 119.3 . . ? C93 C94 H94 119.3 . . ? C104 O1 C101 104.5(6) . . ? C104 O1 K1 132.1(4) . . ? C101 O1 K1 123.1(5) . . ? O1 C101 C102 108.9(6) . . ? O1 C101 H10A 109.9 . . ? C102 C101 H10A 109.9 . . ? O1 C101 H10B 109.9 . . ? C102 C101 H10B 109.9 . . ? H10A C101 H10B 108.3 . . ? C101 C102 C103 105.8(7) . . ? C101 C102 H10C 110.6 . . ? C103 C102 H10C 110.6 . . ? C101 C102 H10D 110.6 . . ? C103 C102 H10D 110.6 . . ? H10C C102 H10D 108.7 . . ? C104 C103 C102 103.7(7) . . ? C104 C103 H10E 111.0 . . ? C102 C103 H10E 111.0 . . ? C104 C103 H10F 111.0 . . ? C102 C103 H10F 111.0 . . ? H10E C103 H10F 109.0 . . ? O1 C104 C103 106.6(6) . . ? O1 C104 H10G 110.4 . . ? C103 C104 H10G 110.4 . . ? O1 C104 H10H 110.4 . . ? C103 C104 H10H 110.4 . . ? H10G C104 H10H 108.6 . . ? C108 O2 C105 109.9(6) . . ? C108 O2 K2 130.7(5) . . ? C105 O2 K2 112.4(4) . . ? O2 C105 C106 103.3(7) . . ? O2 C105 K2 45.0(3) . . ? C106 C105 K2 124.6(5) . . ? O2 C105 H10I 111.1 . . ? C106 C105 H10I 111.1 . . ? K2 C105 H10I 66.4 . . ? O2 C105 H10J 111.1 . . ? C106 C105 H10J 111.1 . . ? K2 C105 H10J 122.0 . . ? H10I C105 H10J 109.1 . . ? C105 C106 C107 101.2(6) . . ? C105 C106 H10K 111.5 . . ? C107 C106 H10K 111.5 . . ? C105 C106 H10L 111.5 . . ? C107 C106 H10L 111.5 . . ? H10K C106 H10L 109.3 . . ? C108 C107 C106 104.2(6) . . ? C108 C107 H10M 110.9 . . ? C106 C107 H10M 110.9 . . ? C108 C107 H10N 110.9 . . ? C106 C107 H10N 110.9 . . ? H10M C107 H10N 108.9 . . ? O2 C108 C107 105.7(7) . . ? O2 C108 H10O 110.6 . . ? C107 C108 H10O 110.6 . . ? O2 C108 H10P 110.6 . . ? C107 C108 H10P 110.6 . . ? H10O C108 H10P 108.7 . . ? C111 O3 C114 106.9(7) . . ? C112 C111 O3 110.7(7) . . ? C112 C111 H11A 109.5 . . ? O3 C111 H11A 109.5 . . ? C112 C111 H11B 109.5 . . ? O3 C111 H11B 109.5 . . ? H11A C111 H11B 108.1 . . ? C111 C112 C113 105.8(6) . . ? C111 C112 H11C 110.5 . . ? C113 C112 H11C 110.6 . . ? C111 C112 H11D 110.6 . . ? C113 C112 H11D 110.6 . . ? H11C C112 H11D 108.7 . . ? C112 C113 C114 103.7(6) . . ? C112 C113 H11E 111.0 . . ? C114 C113 H11E 111.0 . . ? C112 C113 H11F 111.0 . . ? C114 C113 H11F 111.0 . . ? H11E C113 H11F 109.0 . . ? O3 C114 C113 104.2(7) . . ? O3 C114 H11G 110.9 . . ? C113 C114 H11G 110.9 . . ? O3 C114 H11H 110.9 . . ? C113 C114 H11H 110.9 . . ? H11G C114 H11H 108.9 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.022 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.083