# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Biao Wu' _publ_contact_author_name 'Biao Wu' _publ_contact_author_address ; Gansu China 730000 ; _publ_contact_author_email wubiao@lzb.ac.cn # Attachment '- LCuSO4.cif' data_CuSO4 _database_code_depnum_ccdc_archive 'CCDC 787488' #TrackingRef '- LCuSO4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C228 H240 Cu4 N48 O40 S4' _chemical_formula_weight 4675.08 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 38.231(6) _cell_length_b 38.231(6) _cell_length_c 13.424(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 16992(5) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7332 _exptl_absorpt_coefficient_mu 0.492 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8746 _exptl_absorpt_correction_T_max 0.8995 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39100 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.34 _reflns_number_total 6911 _reflns_number_gt 4417 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0500P)^2^+1.9900P] 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 6911 _refine_ls_number_parameters 519 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.05598(8) 0.01363(8) 0.8219(2) 0.0460(7) Uani 1 1 d . . . H1 H 0.0376 0.0185 0.7877 0.055 Uiso 1 1 calc R . . C2 C 0.08625(8) 0.01648(8) 0.7706(2) 0.0435(6) Uani 1 1 d . . . C3 C 0.11508(8) 0.01152(8) 0.8210(2) 0.0441(6) Uani 1 1 d . . . H3 H 0.1371 0.0133 0.7869 0.053 Uiso 1 1 calc R . . C4 C 0.11083(8) 0.00379(7) 0.92268(19) 0.0402(6) Uani 1 1 d . . . H4 H 0.1304 0.0009 0.9569 0.048 Uiso 1 1 calc R . . C5 C 0.07761(8) 0.00031(8) 0.9738(2) 0.0508(7) Uani 1 1 d . . . H5 H 0.0753 -0.0045 1.0420 0.061 Uiso 1 1 calc R . . C6 C 0.12275(8) 0.05138(8) 0.6214(2) 0.0416(6) Uani 1 1 d . . . C7 C 0.14562(8) 0.08521(8) 0.4538(2) 0.0428(6) Uani 1 1 d . . . C8 C 0.17381(8) 0.12324(8) 0.4846(2) 0.0493(7) Uani 1 1 d . . . H8 H 0.1717 0.1321 0.5477 0.059 Uiso 1 1 calc R . . C9 C 0.20537(9) 0.14863(9) 0.4229(2) 0.0518(7) Uani 1 1 d . . . H9 H 0.2242 0.1744 0.4445 0.062 Uiso 1 1 calc R . . C10 C 0.20909(8) 0.13571(9) 0.3286(2) 0.0579(9) Uani 1 1 d . . . H10 H 0.2312 0.1523 0.2890 0.069 Uiso 1 1 calc R . . C11 C 0.17947(8) 0.09748(8) 0.2928(2) 0.0441(7) Uani 1 1 d . . . C12 C 0.14857(9) 0.07166(8) 0.3573(2) 0.0492(7) Uani 1 1 d . . . C13 C 0.12135(8) 0.03305(8) 0.3280(2) 0.0436(6) Uani 1 1 d . . . H13 H 0.1013 0.0156 0.3717 0.052 Uiso 1 1 calc R . . C14 C 0.12373(8) 0.02007(8) 0.2335(2) 0.0474(7) Uani 1 1 d . . . H14 H 0.1049 -0.0059 0.2130 0.057 Uiso 1 1 calc R . . C15 C 0.15456(9) 0.04599(9) 0.1687(2) 0.0570(8) Uani 1 1 d . . . H15 H 0.1564 0.0373 0.1052 0.068 Uiso 1 1 calc R . . C16 C 0.18166(9) 0.08387(8) 0.1989(2) 0.0473(7) Uani 1 1 d . . . H16 H 0.2021 0.1010 0.1558 0.057 Uiso 1 1 calc R . . C17 C 0.11354(8) 0.31988(8) 0.5114(2) 0.0427(6) Uani 1 1 d . . . H17 H 0.1329 0.3171 0.5465 0.051 Uiso 1 1 calc R . . C18 C 0.07959(7) 0.31562(8) 0.5599(2) 0.0391(6) Uani 1 1 d . . . C19 C 0.05109(8) 0.32079(8) 0.5076(2) 0.0438(7) Uani 1 1 d . . . H19 H 0.0285 0.3184 0.5401 0.053 Uiso 1 1 calc R . . C20 C 0.05653(8) 0.32937(9) 0.4079(2) 0.0506(7) Uani 1 1 d . . . H20 H 0.0375 0.3328 0.3729 0.061 Uiso 1 1 calc R . . C21 C 0.08982(8) 0.33297(8) 0.3583(2) 0.0453(7) Uani 1 1 d . . . H21 H 0.0928 0.3385 0.2904 0.054 Uiso 1 1 calc R . . C22 C 0.04254(8) 0.28133(8) 0.7088(2) 0.0417(6) Uani 1 1 d . . . C23 C 0.01514(8) 0.25096(8) 0.8621(2) 0.0452(7) Uani 1 1 d . . . C24 C -0.01237(9) 0.21253(8) 0.8306(2) 0.0511(8) Uani 1 1 d . . . H24 H -0.0094 0.2038 0.7682 0.061 Uiso 1 1 calc R . . C25 C -0.04423(8) 0.18688(9) 0.8909(2) 0.0490(7) Uani 1 1 d . . . H25 H -0.0629 0.1612 0.8684 0.059 Uiso 1 1 calc R . . C26 C -0.04846(9) 0.19925(8) 0.9840(2) 0.0501(7) Uani 1 1 d . . . H26 H -0.0697 0.1816 1.0246 0.060 Uiso 1 1 calc R . . C27 C -0.02024(8) 0.23951(8) 1.0195(2) 0.0453(7) Uani 1 1 d . . . C28 C 0.01237(8) 0.26532(8) 0.9591(2) 0.0429(6) Uani 1 1 d . . . C29 C 0.04048(9) 0.30307(9) 0.9923(2) 0.0496(7) Uani 1 1 d . . . H29 H 0.0624 0.3198 0.9523 0.060 Uiso 1 1 calc R . . C30 C 0.03630(8) 0.31633(9) 1.0857(2) 0.0483(7) Uani 1 1 d . . . H30 H 0.0549 0.3422 1.1073 0.058 Uiso 1 1 calc R . . C31 C 0.00379(9) 0.29045(9) 1.1473(2) 0.0567(8) Uani 1 1 d . . . H31 H 0.0012 0.2988 1.2105 0.068 Uiso 1 1 calc R . . C32 C -0.02462(8) 0.25194(8) 1.1126(2) 0.0425(7) Uani 1 1 d . . . H32 H -0.0464 0.2348 1.1524 0.051 Uiso 1 1 calc R . . C33 C 0.15683(8) 0.38985(8) 0.1323(2) 0.0465(7) Uani 1 1 d . . . H33 H 0.1514 0.3746 0.0744 0.056 Uiso 1 1 calc R . . C34 C 0.16521(8) 0.45404(8) 0.2127(2) 0.0496(7) Uani 1 1 d . . . H34A H 0.1410 0.4453 0.2508 0.074 Uiso 1 1 calc R . . H34B H 0.1752 0.4813 0.1907 0.074 Uiso 1 1 calc R . . H34C H 0.1852 0.4528 0.2534 0.074 Uiso 1 1 calc R . . C35 C 0.14635(9) 0.43815(9) 0.0242(2) 0.0534(8) Uani 1 1 d . . . H35A H 0.1620 0.4348 -0.0269 0.080 Uiso 1 1 calc R . . H35B H 0.1528 0.4658 0.0261 0.080 Uiso 1 1 calc R . . H35C H 0.1181 0.4211 0.0103 0.080 Uiso 1 1 calc R . . C36 C 0.22576(8) 0.40622(8) 0.5455(2) 0.0472(7) Uani 1 1 d . . . H36 H 0.2173 0.3958 0.6091 0.057 Uiso 1 1 calc R . . C37 C 0.27906(9) 0.46400(9) 0.4382(2) 0.0551(8) Uani 1 1 d . . . H37B H 0.3072 0.4735 0.4494 0.083 Uiso 1 1 calc R . . H37C H 0.2757 0.4859 0.4152 0.083 Uiso 1 1 calc R . . H37A H 0.2689 0.4430 0.3890 0.083 Uiso 1 1 calc R . . C38 C 0.26630(9) 0.47642(9) 0.6208(2) 0.0505(7) Uani 1 1 d . . . H38C H 0.2877 0.5027 0.6017 0.076 Uiso 1 1 calc R . . H38A H 0.2749 0.4668 0.6765 0.076 Uiso 1 1 calc R . . H38B H 0.2429 0.4781 0.6390 0.076 Uiso 1 1 calc R . . Cu1 Cu 0.0000 0.0000 1.0000 0.03472(18) Uani 1 6 d S . . Cu2 Cu 0.1667 0.3333 0.3333 0.05241(16) Uani 1 2 d S . . N1 N 0.04814(6) 0.00398(6) 0.92394(17) 0.0433(5) Uani 1 1 d . . . N2 N 0.08811(6) 0.02526(6) 0.67247(16) 0.0382(5) Uani 1 1 d . . . H2A H 0.0659 0.0136 0.6393 0.046 Uiso 1 1 calc R . . N3 N 0.11740(6) 0.05674(6) 0.52596(16) 0.0434(5) Uani 1 1 d . . . H3A H 0.0935 0.0409 0.5034 0.052 Uiso 1 1 calc R . . N4 N 0.11849(7) 0.32851(7) 0.40837(17) 0.0445(6) Uani 1 1 d . . . N5 N 0.07789(6) 0.30683(6) 0.66366(16) 0.0383(5) Uani 1 1 d . . . H5A H 0.0998 0.3180 0.6981 0.046 Uiso 1 1 calc R . . N6 N 0.04885(7) 0.27588(7) 0.80619(17) 0.0463(6) Uani 1 1 d . . . H6A H 0.0728 0.2873 0.8310 0.056 Uiso 1 1 d R . . N7 N 0.15608(7) 0.42675(7) 0.12323(16) 0.0435(5) Uani 1 1 d . . . N8 N 0.25605(7) 0.44762(7) 0.53449(17) 0.0448(6) Uani 1 1 d . . . O1 O 0.15681(5) 0.06742(5) 0.66479(14) 0.0472(5) Uani 1 1 d . . . O2 O 0.01134(5) 0.26671(5) 0.66867(14) 0.0451(5) Uani 1 1 d . . . O3 O 0.16412(6) 0.37514(6) 0.21042(14) 0.0501(5) Uani 1 1 d . . . O4 O 0.21053(6) 0.38395(6) 0.47275(14) 0.0474(5) Uani 1 1 d . . . S1 S 0.0000 0.0000 0.5000 0.0362(4) Uani 1 6 d S . . O5 O 0.0000 0.0000 0.6021(5) 0.0504(17) Uani 0.50 3 d SP . . O6 O 0.02651(12) 0.03601(11) 0.5423(3) 0.0527(10) Uani 0.50 1 d P . . S2 S 0.1667 0.3333 0.8333 0.0490(3) Uani 1 2 d S . . O7 O 0.17658(11) 0.34037(12) 0.9315(3) 0.0525(10) Uani 0.50 1 d P . . O8 O 0.19778(11) 0.37195(12) 0.8448(3) 0.0502(10) Uani 0.50 1 d P . . O9 O 0.15247(11) 0.35584(11) 0.7912(3) 0.0570(11) Uani 0.50 1 d P . . O10 O 0.13111(11) 0.32481(12) 0.8761(3) 0.0489(9) Uani 0.50 1 d P . . 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 C1 0.0415(15) 0.0550(16) 0.0296(15) -0.0088(12) -0.0115(12) 0.0153(13) C2 0.0473(16) 0.0420(15) 0.0282(15) -0.0102(11) -0.0039(12) 0.0125(12) C3 0.0398(14) 0.0410(15) 0.0443(17) 0.0126(12) 0.0158(12) 0.0147(12) C4 0.0381(14) 0.0413(14) 0.0355(15) -0.0150(12) -0.0153(12) 0.0157(12) C5 0.0450(16) 0.0546(17) 0.0464(17) 0.0229(14) 0.0153(13) 0.0202(14) C6 0.0419(15) 0.0428(14) 0.0330(15) -0.0029(12) 0.0009(12) 0.0157(12) C7 0.0366(14) 0.0452(15) 0.0393(16) 0.0032(12) 0.0128(12) 0.0150(12) C8 0.0463(16) 0.0430(15) 0.0461(17) -0.0076(13) 0.0178(13) 0.0131(13) C9 0.0482(17) 0.0416(15) 0.054(2) -0.0033(14) 0.0110(14) 0.0140(13) C10 0.0416(15) 0.0461(16) 0.0397(17) -0.0010(13) 0.0145(13) -0.0127(13) C11 0.0425(15) 0.0415(15) 0.0376(16) -0.0008(12) 0.0113(12) 0.0129(12) C12 0.0508(16) 0.0422(15) 0.0338(16) 0.0072(12) 0.0076(13) 0.0076(13) C13 0.0381(14) 0.0461(15) 0.0361(15) 0.0169(12) 0.0141(12) 0.0132(12) C14 0.0408(15) 0.0434(16) 0.0463(18) -0.0068(13) 0.0013(13) 0.0122(12) C15 0.0563(18) 0.0532(18) 0.0489(19) -0.0104(14) 0.0216(15) 0.0178(15) C16 0.0533(17) 0.0436(15) 0.0368(16) 0.0067(12) 0.0084(13) 0.0180(13) C17 0.0388(14) 0.0516(16) 0.0313(15) 0.0120(12) 0.0195(11) 0.0178(12) C18 0.0276(12) 0.0460(15) 0.0434(16) 0.0125(12) 0.0086(11) 0.0182(12) C19 0.0460(15) 0.0412(14) 0.0404(17) 0.0195(12) -0.0035(12) 0.0189(12) C20 0.0420(15) 0.0594(18) 0.0372(17) 0.0156(13) 0.0123(13) 0.0155(14) C21 0.0439(15) 0.0473(15) 0.0399(16) 0.0188(13) 0.0075(12) 0.0192(13) C22 0.0364(15) 0.0442(15) 0.0351(15) -0.0038(12) 0.0069(12) 0.0131(12) C23 0.0448(15) 0.0425(15) 0.0415(17) 0.0093(12) 0.0071(12) 0.0166(13) C24 0.0484(16) 0.0495(17) 0.0489(19) -0.0077(13) 0.0159(14) 0.0196(14) C25 0.0414(15) 0.0459(15) 0.0440(18) 0.0112(13) -0.0127(13) 0.0100(12) C26 0.0553(17) 0.0438(16) 0.0394(18) 0.0167(13) -0.0016(13) 0.0159(14) C27 0.0447(16) 0.0470(16) 0.0407(17) 0.0135(13) 0.0145(13) 0.0204(13) C28 0.0389(14) 0.0397(14) 0.0447(17) 0.0131(12) 0.0121(12) 0.0156(12) C29 0.0491(16) 0.0524(17) 0.0413(17) 0.0075(13) 0.0132(13) 0.0208(14) C30 0.0402(15) 0.0463(16) 0.056(2) -0.0020(13) 0.0107(14) 0.0198(13) C31 0.0542(18) 0.0561(18) 0.055(2) -0.0079(15) 0.0216(15) 0.0236(15) C32 0.0369(14) 0.0444(15) 0.0436(17) 0.0190(12) 0.0089(12) 0.0182(12) C33 0.0472(16) 0.0467(16) 0.0485(18) 0.0043(13) 0.0047(13) 0.0257(13) C34 0.0490(16) 0.0376(15) 0.0468(18) -0.0035(13) 0.0099(13) 0.0102(13) C35 0.0449(16) 0.0533(17) 0.0522(19) 0.0090(14) -0.0134(14) 0.0171(14) C36 0.0450(16) 0.0445(16) 0.0410(17) -0.0094(13) -0.0060(13) 0.0140(13) C37 0.0494(17) 0.0491(17) 0.062(2) -0.0038(15) 0.0063(15) 0.0211(14) C38 0.0564(17) 0.0498(16) 0.0433(18) -0.0179(13) -0.0205(14) 0.0250(14) Cu1 0.0375(3) 0.0375(3) 0.0292(4) 0.000 0.000 0.01875(13) Cu2 0.0437(3) 0.0525(3) 0.0428(3) 0.0085(2) 0.0146(2) 0.0103(2) N1 0.0395(12) 0.0423(12) 0.0383(13) 0.0073(10) 0.0084(10) 0.0132(10) N2 0.0345(11) 0.0374(12) 0.0349(13) -0.0082(9) 0.0043(9) 0.0121(9) N3 0.0353(11) 0.0441(13) 0.0361(13) 0.0013(10) 0.0046(10) 0.0088(10) N4 0.0373(12) 0.0535(13) 0.0301(13) 0.0105(10) 0.0022(9) 0.0132(10) N5 0.0324(11) 0.0452(12) 0.0320(12) 0.0014(10) 0.0053(9) 0.0154(10) N6 0.0408(12) 0.0496(13) 0.0421(15) 0.0176(11) 0.0048(10) 0.0177(11) N7 0.0528(13) 0.0463(13) 0.0297(13) 0.0062(10) 0.0081(10) 0.0236(11) N8 0.0417(12) 0.0494(13) 0.0405(14) -0.0087(11) -0.0149(10) 0.0207(11) O1 0.0345(10) 0.0448(11) 0.0468(12) 0.0103(9) 0.0017(8) 0.0082(8) O2 0.0376(10) 0.0423(10) 0.0433(12) 0.0228(8) -0.0009(8) 0.0110(8) O3 0.0447(11) 0.0504(11) 0.0369(12) 0.0079(9) 0.0113(9) 0.0100(9) O4 0.0494(11) 0.0498(11) 0.0334(11) -0.0127(9) 0.0033(8) 0.0177(9) S1 0.0343(5) 0.0343(5) 0.0402(10) 0.000 0.000 0.0171(3) O5 0.055(3) 0.055(3) 0.040(4) 0.000 0.000 0.0277(13) O6 0.051(2) 0.039(2) 0.039(2) -0.0085(17) -0.0065(18) 0.0002(17) S2 0.0428(6) 0.0443(6) 0.0503(7) 0.0133(5) 0.0073(5) 0.0146(5) O7 0.037(2) 0.056(2) 0.053(3) 0.004(2) -0.0084(18) 0.0144(18) O8 0.040(2) 0.051(2) 0.050(3) -0.0017(19) -0.0079(18) 0.0156(19) O9 0.040(2) 0.046(2) 0.069(3) 0.004(2) -0.016(2) 0.0103(18) O10 0.040(2) 0.061(2) 0.040(2) -0.0100(19) -0.0106(17) 0.0207(19) _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 C1 C2 1.304(4) . ? C1 N1 1.411(4) . ? C1 H1 0.9300 . ? C2 N2 1.352(3) . ? C2 C3 1.384(4) . ? C3 C4 1.389(4) . ? C3 H3 0.9300 . ? C4 C5 1.390(4) . ? C4 H4 0.9300 . ? C5 N1 1.376(4) . ? C5 H5 0.9300 . ? C6 O1 1.270(3) . ? C6 N3 1.329(3) . ? C6 N2 1.378(3) . ? C7 C8 1.371(4) . ? C7 C12 1.420(4) . ? C7 N3 1.454(3) . ? C8 C9 1.383(4) . ? C8 H8 0.9300 . ? C9 C10 1.391(4) . ? C9 H9 0.9300 . ? C10 C11 1.412(4) . ? C10 H10 0.9300 . ? C11 C16 1.382(4) . ? C11 C12 1.398(4) . ? C12 C13 1.371(4) . ? C13 C14 1.381(4) . ? C13 H13 0.9300 . ? C14 C15 1.400(4) . ? C14 H14 0.9300 . ? C15 C16 1.355(4) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.387(3) . ? C17 N4 1.412(3) . ? C17 H17 0.9300 . ? C18 C19 1.391(4) . ? C18 N5 1.427(3) . ? C19 C20 1.369(4) . ? C19 H19 0.9300 . ? C20 C21 1.381(4) . ? C20 H20 0.9300 . ? C21 N4 1.367(3) . ? C21 H21 0.9300 . ? C22 O2 1.166(3) . ? C22 N5 1.352(3) . ? C22 N6 1.364(3) . ? C23 C24 1.378(4) . ? C23 N6 1.380(3) . ? C23 C28 1.437(4) . ? C24 C25 1.380(4) . ? C24 H24 0.9300 . ? C25 C26 1.374(4) . ? C25 H25 0.9300 . ? C26 C27 1.449(4) . ? C26 H26 0.9300 . ? C27 C32 1.376(4) . ? C27 C28 1.398(4) . ? C28 C29 1.373(4) . ? C29 C30 1.391(4) . ? C29 H29 0.9300 . ? C30 C31 1.406(4) . ? C30 H30 0.9300 . ? C31 C32 1.402(4) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O3 1.285(3) . ? C33 N7 1.430(3) . ? C33 H33 0.9300 . ? C34 N7 1.513(3) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 N7 1.502(3) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 O4 1.234(3) . ? C36 N8 1.426(4) . ? C36 H36 0.9300 . ? C37 N8 1.511(4) . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C37 H37A 0.9600 . ? C38 N8 1.509(3) . ? C38 H38C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? Cu1 N1 2.043(2) 10_557 ? Cu1 N1 2.043(2) 3 ? Cu1 N1 2.043(2) 12_557 ? Cu1 N1 2.043(2) . ? Cu1 N1 2.043(2) 2 ? Cu1 N1 2.043(2) 11_557 ? Cu2 N4 2.025(2) . ? Cu2 N4 2.025(2) 16 ? Cu2 O3 2.333(2) . ? Cu2 O3 2.333(2) 16 ? N2 H2A 0.8600 . ? N3 H3A 0.8600 . ? N5 H5A 0.8600 . ? N6 H6A 0.8596 . ? S1 O6 1.360(3) 2 ? S1 O6 1.360(3) . ? S1 O6 1.360(3) 12_556 ? S1 O6 1.360(3) 10_556 ? S1 O6 1.360(3) 11_556 ? S1 O6 1.360(3) 3 ? S1 O5 1.370(7) . ? S1 O5 1.370(7) 10_556 ? O5 O6 1.473(5) 2 ? O5 O6 1.473(5) 3 ? O5 O6 1.473(5) . ? O6 O6 1.678(6) 12_556 ? O6 O6 1.678(6) 11_556 ? S2 O9 1.350(4) . ? S2 O9 1.350(4) 16_556 ? S2 O10 1.357(4) . ? S2 O10 1.357(4) 16_556 ? S2 O7 1.360(4) 16_556 ? S2 O7 1.360(4) . ? S2 O8 1.365(4) 16_556 ? S2 O8 1.365(4) . ? O7 O9 1.433(6) 16_556 ? O7 O8 1.578(6) . ? O7 O10 1.701(5) . ? O8 O10 1.441(5) 16_556 ? O8 O9 1.682(5) . ? O9 O7 1.433(6) 16_556 ? O9 O10 1.550(6) . ? O10 O8 1.441(5) 16_556 ? 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 C2 C1 N1 126.7(3) . . ? C2 C1 H1 116.6 . . ? N1 C1 H1 116.6 . . ? C1 C2 N2 118.0(3) . . ? C1 C2 C3 117.7(3) . . ? N2 C2 C3 124.3(3) . . ? C2 C3 C4 119.5(2) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 120.6(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? N1 C5 C4 120.4(3) . . ? N1 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? O1 C6 N3 124.6(2) . . ? O1 C6 N2 120.2(2) . . ? N3 C6 N2 115.2(2) . . ? C8 C7 C12 119.9(2) . . ? C8 C7 N3 119.3(2) . . ? C12 C7 N3 120.0(2) . . ? C7 C8 C9 120.7(3) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C8 C9 C10 120.2(3) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C11 120.4(2) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C16 C11 C12 119.2(3) . . ? C16 C11 C10 122.1(2) . . ? C12 C11 C10 118.5(3) . . ? C13 C12 C11 120.0(3) . . ? C13 C12 C7 119.9(2) . . ? C11 C12 C7 120.0(2) . . ? C12 C13 C14 120.0(2) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C15 120.0(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 119.6(3) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C11 121.2(3) . . ? C15 C16 H16 119.4 . . ? C11 C16 H16 119.4 . . ? C18 C17 N4 119.7(3) . . ? C18 C17 H17 120.2 . . ? N4 C17 H17 120.2 . . ? C17 C18 C19 120.0(3) . . ? C17 C18 N5 114.6(2) . . ? C19 C18 N5 125.4(2) . . ? C20 C19 C18 119.4(3) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 121.1(3) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? N4 C21 C20 120.5(3) . . ? N4 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? O2 C22 N5 123.5(3) . . ? O2 C22 N6 125.9(2) . . ? N5 C22 N6 110.5(2) . . ? C24 C23 N6 121.3(3) . . ? C24 C23 C28 121.5(2) . . ? N6 C23 C28 116.8(2) . . ? C23 C24 C25 120.6(3) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 120.2(3) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 120.8(3) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C32 C27 C28 120.1(3) . . ? C32 C27 C26 120.7(2) . . ? C28 C27 C26 119.1(3) . . ? C29 C28 C27 120.5(3) . . ? C29 C28 C23 121.8(2) . . ? C27 C28 C23 117.7(3) . . ? C28 C29 C30 120.2(3) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C30 C31 119.7(3) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C32 C31 C30 119.4(3) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? C27 C32 C31 120.0(2) . . ? C27 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? O3 C33 N7 128.1(3) . . ? O3 C33 H33 116.0 . . ? N7 C33 H33 116.0 . . ? N7 C34 H34A 109.5 . . ? N7 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N7 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N7 C35 H35A 109.5 . . ? N7 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N7 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O4 C36 N8 121.7(3) . . ? O4 C36 H36 119.2 . . ? N8 C36 H36 119.2 . . ? N8 C37 H37B 109.5 . . ? N8 C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N8 C37 H37A 109.5 . . ? H37B C37 H37A 109.5 . . ? H37C C37 H37A 109.5 . . ? N8 C38 H38C 109.5 . . ? N8 C38 H38A 109.5 . . ? H38C C38 H38A 109.5 . . ? N8 C38 H38B 109.5 . . ? H38C C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N1 Cu1 N1 82.80(9) 10_557 3 ? N1 Cu1 N1 97.20(9) 10_557 12_557 ? N1 Cu1 N1 180.00(12) 3 12_557 ? N1 Cu1 N1 180.00(7) 10_557 . ? N1 Cu1 N1 97.20(9) 3 . ? N1 Cu1 N1 82.80(9) 12_557 . ? N1 Cu1 N1 82.80(9) 10_557 2 ? N1 Cu1 N1 97.20(9) 3 2 ? N1 Cu1 N1 82.80(9) 12_557 2 ? N1 Cu1 N1 97.20(9) . 2 ? N1 Cu1 N1 97.20(9) 10_557 11_557 ? N1 Cu1 N1 82.80(9) 3 11_557 ? N1 Cu1 N1 97.20(9) 12_557 11_557 ? N1 Cu1 N1 82.80(9) . 11_557 ? N1 Cu1 N1 180.00(8) 2 11_557 ? N4 Cu2 N4 180.0 . 16 ? N4 Cu2 O3 93.82(8) . . ? N4 Cu2 O3 86.18(8) 16 . ? N4 Cu2 O3 86.18(8) . 16 ? N4 Cu2 O3 93.81(8) 16 16 ? O3 Cu2 O3 180.0 . 16 ? C5 N1 C1 114.9(2) . . ? C5 N1 Cu1 120.16(19) . . ? C1 N1 Cu1 124.77(19) . . ? C2 N2 C6 125.2(2) . . ? C2 N2 H2A 117.4 . . ? C6 N2 H2A 117.4 . . ? C6 N3 C7 130.1(2) . . ? C6 N3 H3A 115.0 . . ? C7 N3 H3A 115.0 . . ? C21 N4 C17 119.2(2) . . ? C21 N4 Cu2 119.58(18) . . ? C17 N4 Cu2 121.19(18) . . ? C22 N5 C18 121.3(2) . . ? C22 N5 H5A 119.4 . . ? C18 N5 H5A 119.4 . . ? C22 N6 C23 116.8(2) . . ? C22 N6 H6A 121.2 . . ? C23 N6 H6A 122.0 . . ? C33 N7 C35 119.4(2) . . ? C33 N7 C34 120.1(2) . . ? C35 N7 C34 120.5(2) . . ? C36 N8 C38 120.1(2) . . ? C36 N8 C37 122.0(2) . . ? C38 N8 C37 118.0(2) . . ? C33 O3 Cu2 165.88(19) . . ? O6 S1 O6 103.79(19) 2 . ? O6 S1 O6 76.2(2) 2 12_556 ? O6 S1 O6 76.2(2) . 12_556 ? O6 S1 O6 76.2(2) 2 10_556 ? O6 S1 O6 180.0(5) . 10_556 ? O6 S1 O6 103.8(2) 12_556 10_556 ? O6 S1 O6 180.0(4) 2 11_556 ? O6 S1 O6 76.2(2) . 11_556 ? O6 S1 O6 103.8(2) 12_556 11_556 ? O6 S1 O6 103.79(19) 10_556 11_556 ? O6 S1 O6 103.8(2) 2 3 ? O6 S1 O6 103.8(2) . 3 ? O6 S1 O6 180.0(4) 12_556 3 ? O6 S1 O6 76.2(2) 10_556 3 ? O6 S1 O6 76.2(2) 11_556 3 ? O6 S1 O5 65.32(17) 2 . ? O6 S1 O5 65.32(17) . . ? O6 S1 O5 114.68(17) 12_556 . ? O6 S1 O5 114.68(17) 10_556 . ? O6 S1 O5 114.68(17) 11_556 . ? O6 S1 O5 65.32(17) 3 . ? O6 S1 O5 114.68(17) 2 10_556 ? O6 S1 O5 114.68(17) . 10_556 ? O6 S1 O5 65.32(17) 12_556 10_556 ? O6 S1 O5 65.32(17) 10_556 10_556 ? O6 S1 O5 65.32(17) 11_556 10_556 ? O6 S1 O5 114.68(17) 3 10_556 ? O5 S1 O5 180.000(1) . 10_556 ? S1 O5 O6 57.0(3) . 2 ? S1 O5 O6 57.0(3) . 3 ? O6 O5 O6 93.2(4) 2 3 ? S1 O5 O6 57.0(3) . . ? O6 O5 O6 93.2(4) 2 . ? O6 O5 O6 93.2(4) 3 . ? S1 O6 O5 57.7(3) . . ? S1 O6 O6 51.90(10) . 12_556 ? O5 O6 O6 93.4(2) . 12_556 ? S1 O6 O6 51.90(10) . 11_556 ? O5 O6 O6 93.4(2) . 11_556 ? O6 O6 O6 79.2(3) 12_556 11_556 ? O9 S2 O9 180.0(2) . 16_556 ? O9 S2 O10 69.9(2) . . ? O9 S2 O10 110.1(2) 16_556 . ? O9 S2 O10 110.1(2) . 16_556 ? O9 S2 O10 69.9(2) 16_556 16_556 ? O10 S2 O10 179.995(2) . 16_556 ? O9 S2 O7 63.9(2) . 16_556 ? O9 S2 O7 116.1(2) 16_556 16_556 ? O10 S2 O7 102.5(2) . 16_556 ? O10 S2 O7 77.5(2) 16_556 16_556 ? O9 S2 O7 116.1(2) . . ? O9 S2 O7 63.9(2) 16_556 . ? O10 S2 O7 77.5(2) . . ? O10 S2 O7 102.5(2) 16_556 . ? O7 S2 O7 180.000(2) 16_556 . ? O9 S2 O8 103.4(2) . 16_556 ? O9 S2 O8 76.6(2) 16_556 16_556 ? O10 S2 O8 64.0(2) . 16_556 ? O10 S2 O8 116.0(2) 16_556 16_556 ? O7 S2 O8 70.8(2) 16_556 16_556 ? O7 S2 O8 109.2(2) . 16_556 ? O9 S2 O8 76.6(2) . . ? O9 S2 O8 103.4(2) 16_556 . ? O10 S2 O8 116.0(2) . . ? O10 S2 O8 64.0(2) 16_556 . ? O7 S2 O8 109.2(2) 16_556 . ? O7 S2 O8 70.8(2) . . ? O8 S2 O8 180.0(3) 16_556 . ? S2 O7 O9 57.7(2) . 16_556 ? S2 O7 O8 54.7(2) . . ? O9 O7 O8 89.9(3) 16_556 . ? S2 O7 O10 51.13(18) . . ? O9 O7 O10 89.7(3) 16_556 . ? O8 O7 O10 89.4(3) . . ? S2 O8 O10 57.8(2) . 16_556 ? S2 O8 O7 54.5(2) . . ? O10 O8 O7 89.0(3) 16_556 . ? S2 O8 O9 51.30(18) . . ? O10 O8 O9 90.2(3) 16_556 . ? O7 O8 O9 89.7(3) . . ? S2 O9 O7 58.4(2) . 16_556 ? S2 O9 O10 55.3(2) . . ? O7 O9 O10 90.4(3) 16_556 . ? S2 O9 O8 52.10(19) . . ? O7 O9 O8 90.6(3) 16_556 . ? O10 O9 O8 91.0(3) . . ? S2 O10 O8 58.3(2) . 16_556 ? S2 O10 O9 54.8(2) . . ? O8 O10 O9 90.7(3) 16_556 . ? S2 O10 O7 51.32(19) . . ? O8 O10 O7 89.6(3) 16_556 . ? O9 O10 O7 89.9(3) . . ? 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 N1 C1 C2 N2 178.6(2) . . . . ? N1 C1 C2 C3 -3.3(4) . . . . ? C1 C2 C3 C4 0.0(4) . . . . ? N2 C2 C3 C4 177.9(2) . . . . ? C2 C3 C4 C5 1.1(4) . . . . ? C3 C4 C5 N1 0.8(4) . . . . ? C12 C7 C8 C9 -0.4(5) . . . . ? N3 C7 C8 C9 168.7(3) . . . . ? C7 C8 C9 C10 -0.5(5) . . . . ? C8 C9 C10 C11 3.7(5) . . . . ? C9 C10 C11 C16 178.7(3) . . . . ? C9 C10 C11 C12 -5.8(5) . . . . ? C16 C11 C12 C13 1.3(5) . . . . ? C10 C11 C12 C13 -174.3(3) . . . . ? C16 C11 C12 C7 -179.5(3) . . . . ? C10 C11 C12 C7 4.9(5) . . . . ? C8 C7 C12 C13 177.3(3) . . . . ? N3 C7 C12 C13 8.3(4) . . . . ? C8 C7 C12 C11 -1.9(5) . . . . ? N3 C7 C12 C11 -170.9(3) . . . . ? C11 C12 C13 C14 -2.0(5) . . . . ? C7 C12 C13 C14 178.8(3) . . . . ? C12 C13 C14 C15 1.7(5) . . . . ? C13 C14 C15 C16 -0.6(5) . . . . ? C14 C15 C16 C11 0.0(5) . . . . ? C12 C11 C16 C15 -0.3(5) . . . . ? C10 C11 C16 C15 175.1(3) . . . . ? N4 C17 C18 C19 -1.5(4) . . . . ? N4 C17 C18 N5 179.8(2) . . . . ? C17 C18 C19 C20 1.1(4) . . . . ? N5 C18 C19 C20 179.7(3) . . . . ? C18 C19 C20 C21 0.0(4) . . . . ? C19 C20 C21 N4 -0.8(4) . . . . ? N6 C23 C24 C25 175.0(3) . . . . ? C28 C23 C24 C25 1.7(5) . . . . ? C23 C24 C25 C26 -1.1(5) . . . . ? C24 C25 C26 C27 1.4(4) . . . . ? C25 C26 C27 C32 179.7(3) . . . . ? C25 C26 C27 C28 -2.3(4) . . . . ? C32 C27 C28 C29 0.6(4) . . . . ? C26 C27 C28 C29 -177.4(3) . . . . ? C32 C27 C28 C23 -179.2(3) . . . . ? C26 C27 C28 C23 2.7(4) . . . . ? C24 C23 C28 C29 177.7(3) . . . . ? N6 C23 C28 C29 4.1(4) . . . . ? C24 C23 C28 C27 -2.5(4) . . . . ? N6 C23 C28 C27 -176.1(3) . . . . ? C27 C28 C29 C30 -1.4(5) . . . . ? C23 C28 C29 C30 178.4(3) . . . . ? C28 C29 C30 C31 1.9(5) . . . . ? C29 C30 C31 C32 -1.7(4) . . . . ? C28 C27 C32 C31 -0.4(4) . . . . ? C26 C27 C32 C31 177.6(3) . . . . ? C30 C31 C32 C27 0.9(4) . . . . ? C4 C5 N1 C1 -3.5(4) . . . . ? C4 C5 N1 Cu1 -178.72(19) . . . . ? C2 C1 N1 C5 5.1(4) . . . . ? C2 C1 N1 Cu1 -180.0(2) . . . . ? N1 Cu1 N1 C5 -11.9(4) 10_557 . . . ? N1 Cu1 N1 C5 -120.7(2) 3 . . . ? N1 Cu1 N1 C5 59.3(2) 12_557 . . . ? N1 Cu1 N1 C5 141.1(2) 2 . . . ? N1 Cu1 N1 C5 -38.9(2) 11_557 . . . ? N1 Cu1 N1 C1 173.4(3) 10_557 . . . ? N1 Cu1 N1 C1 64.62(17) 3 . . . ? N1 Cu1 N1 C1 -115.38(17) 12_557 . . . ? N1 Cu1 N1 C1 -33.6(2) 2 . . . ? N1 Cu1 N1 C1 146.4(2) 11_557 . . . ? C1 C2 N2 C6 139.0(3) . . . . ? C3 C2 N2 C6 -38.9(4) . . . . ? O1 C6 N2 C2 4.6(4) . . . . ? N3 C6 N2 C2 -177.5(2) . . . . ? O1 C6 N3 C7 -10.6(5) . . . . ? N2 C6 N3 C7 171.6(2) . . . . ? C8 C7 N3 C6 -35.8(4) . . . . ? C12 C7 N3 C6 133.3(3) . . . . ? C20 C21 N4 C17 0.5(4) . . . . ? C20 C21 N4 Cu2 179.3(2) . . . . ? C18 C17 N4 C21 0.7(4) . . . . ? C18 C17 N4 Cu2 -178.13(19) . . . . ? N4 Cu2 N4 C21 -123.7(17) 16 . . . ? O3 Cu2 N4 C21 26.5(2) . . . . ? O3 Cu2 N4 C21 -153.5(2) 16 . . . ? N4 Cu2 N4 C17 55.1(17) 16 . . . ? O3 Cu2 N4 C17 -154.7(2) . . . . ? O3 Cu2 N4 C17 25.3(2) 16 . . . ? O2 C22 N5 C18 -4.2(4) . . . . ? N6 C22 N5 C18 176.4(2) . . . . ? C17 C18 N5 C22 -142.8(3) . . . . ? C19 C18 N5 C22 38.6(4) . . . . ? O2 C22 N6 C23 -0.4(4) . . . . ? N5 C22 N6 C23 178.9(2) . . . . ? C24 C23 N6 C22 52.4(4) . . . . ? C28 C23 N6 C22 -134.0(3) . . . . ? O3 C33 N7 C35 -179.3(3) . . . . ? O3 C33 N7 C34 0.9(4) . . . . ? O4 C36 N8 C38 164.3(3) . . . . ? O4 C36 N8 C37 -16.3(4) . . . . ? N7 C33 O3 Cu2 149.8(6) . . . . ? N4 Cu2 O3 C33 -88.8(7) . . . . ? N4 Cu2 O3 C33 91.2(7) 16 . . . ? O3 Cu2 O3 C33 71.9(10) 16 . . . ? O6 S1 O5 O6 120.000(1) . . . 2 ? O6 S1 O5 O6 60.000(1) 12_556 . . 2 ? O6 S1 O5 O6 -60.000(1) 10_556 . . 2 ? O6 S1 O5 O6 180.0 11_556 . . 2 ? O6 S1 O5 O6 -120.000(1) 3 . . 2 ? O5 S1 O5 O6 -165(100) 10_556 . . 2 ? O6 S1 O5 O6 120.000(1) 2 . . 3 ? O6 S1 O5 O6 -120.000(1) . . . 3 ? O6 S1 O5 O6 180.000(1) 12_556 . . 3 ? O6 S1 O5 O6 60.000(1) 10_556 . . 3 ? O6 S1 O5 O6 -60.000(1) 11_556 . . 3 ? O5 S1 O5 O6 -45(97) 10_556 . . 3 ? O6 S1 O5 O6 -120.000(1) 2 . . . ? O6 S1 O5 O6 -60.0 12_556 . . . ? O6 S1 O5 O6 180.0 10_556 . . . ? O6 S1 O5 O6 60.000(1) 11_556 . . . ? O6 S1 O5 O6 120.0 3 . . . ? O5 S1 O5 O6 75(97) 10_556 . . . ? O6 S1 O6 O5 54.12(17) 2 . . . ? O6 S1 O6 O5 125.88(17) 12_556 . . . ? O6 S1 O6 O5 180.00(14) 10_556 . . . ? O6 S1 O6 O5 -125.88(17) 11_556 . . . ? O6 S1 O6 O5 -54.12(17) 3 . . . ? O5 S1 O6 O5 180.0 10_556 . . . ? O6 S1 O6 O6 -71.8(3) 2 . . 12_556 ? O6 S1 O6 O6 54.1(3) 10_556 . . 12_556 ? O6 S1 O6 O6 108.2(3) 11_556 . . 12_556 ? O6 S1 O6 O6 180.0 3 . . 12_556 ? O5 S1 O6 O6 -125.88(17) . . . 12_556 ? O5 S1 O6 O6 54.12(17) 10_556 . . 12_556 ? O6 S1 O6 O6 180.0 2 . . 11_556 ? O6 S1 O6 O6 -108.2(3) 12_556 . . 11_556 ? O6 S1 O6 O6 -54.12(13) 10_556 . . 11_556 ? O6 S1 O6 O6 71.8(3) 3 . . 11_556 ? O5 S1 O6 O6 125.88(17) . . . 11_556 ? O5 S1 O6 O6 -54.12(17) 10_556 . . 11_556 ? O6 O5 O6 S1 -46.7(2) 2 . . . ? O6 O5 O6 S1 46.7(2) 3 . . . ? S1 O5 O6 O6 39.70(16) . . . 12_556 ? O6 O5 O6 O6 -7.0(3) 2 . . 12_556 ? O6 O5 O6 O6 86.4(2) 3 . . 12_556 ? S1 O5 O6 O6 -39.70(16) . . . 11_556 ? O6 O5 O6 O6 -86.4(2) 2 . . 11_556 ? O6 O5 O6 O6 7.0(3) 3 . . 11_556 ? O9 S2 O7 O9 180.002(3) . . . 16_556 ? O10 S2 O7 O9 120.0(3) . . . 16_556 ? O10 S2 O7 O9 -60.0(3) 16_556 . . 16_556 ? O7 S2 O7 O9 -128(100) 16_556 . . 16_556 ? O8 S2 O7 O9 63.6(3) 16_556 . . 16_556 ? O8 S2 O7 O9 -116.4(3) . . . 16_556 ? O9 S2 O7 O8 -63.6(3) . . . . ? O9 S2 O7 O8 116.4(3) 16_556 . . . ? O10 S2 O7 O8 -123.6(2) . . . . ? O10 S2 O7 O8 56.4(2) 16_556 . . . ? O7 S2 O7 O8 -11(100) 16_556 . . . ? O8 S2 O7 O8 180.000(1) 16_556 . . . ? O9 S2 O7 O10 60.0(3) . . . . ? O9 S2 O7 O10 -120.0(3) 16_556 . . . ? O10 S2 O7 O10 -179.995(2) 16_556 . . . ? O7 S2 O7 O10 112(100) 16_556 . . . ? O8 S2 O7 O10 -56.4(2) 16_556 . . . ? O8 S2 O7 O10 123.6(2) . . . . ? O9 S2 O8 O10 -120.7(3) . . . 16_556 ? O9 S2 O8 O10 59.3(3) 16_556 . . 16_556 ? O10 S2 O8 O10 180.0 . . . 16_556 ? O7 S2 O8 O10 -64.9(3) 16_556 . . 16_556 ? O7 S2 O8 O10 115.1(3) . . . 16_556 ? O8 S2 O8 O10 0(100) 16_556 . . 16_556 ? O9 S2 O8 O7 124.2(3) . . . . ? O9 S2 O8 O7 -55.8(3) 16_556 . . . ? O10 S2 O8 O7 64.9(3) . . . . ? O10 S2 O8 O7 -115.1(3) 16_556 . . . ? O7 S2 O8 O7 180.000(1) 16_556 . . . ? O8 S2 O8 O7 0(100) 16_556 . . . ? O9 S2 O8 O9 180.0 16_556 . . . ? O10 S2 O8 O9 -59.4(3) . . . . ? O10 S2 O8 O9 120.7(3) 16_556 . . . ? O7 S2 O8 O9 55.8(3) 16_556 . . . ? O7 S2 O8 O9 -124.2(3) . . . . ? O8 S2 O8 O9 0(100) 16_556 . . . ? O9 O7 O8 S2 49.2(2) 16_556 . . . ? O10 O7 O8 S2 -40.45(18) . . . . ? S2 O7 O8 O10 -50.0(2) . . . 16_556 ? O9 O7 O8 O10 -0.8(3) 16_556 . . 16_556 ? O10 O7 O8 O10 -90.4(3) . . . 16_556 ? S2 O7 O8 O9 40.18(19) . . . . ? O9 O7 O8 O9 89.4(3) 16_556 . . . ? O10 O7 O8 O9 -0.3(3) . . . . ? O9 S2 O9 O7 29(13) 16_556 . . 16_556 ? O10 S2 O9 O7 -115.8(3) . . . 16_556 ? O10 S2 O9 O7 64.2(3) 16_556 . . 16_556 ? O7 S2 O9 O7 180.000(3) . . . 16_556 ? O8 S2 O9 O7 -60.4(3) 16_556 . . 16_556 ? O8 S2 O9 O7 119.6(3) . . . 16_556 ? O9 S2 O9 O10 145(13) 16_556 . . . ? O10 S2 O9 O10 179.997(2) 16_556 . . . ? O7 S2 O9 O10 115.8(3) 16_556 . . . ? O7 S2 O9 O10 -64.2(3) . . . . ? O8 S2 O9 O10 55.4(3) 16_556 . . . ? O8 S2 O9 O10 -124.6(3) . . . . ? O9 S2 O9 O8 -91(13) 16_556 . . . ? O10 S2 O9 O8 124.6(3) . . . . ? O10 S2 O9 O8 -55.4(3) 16_556 . . . ? O7 S2 O9 O8 -119.6(3) 16_556 . . . ? O7 S2 O9 O8 60.4(3) . . . . ? O8 S2 O9 O8 180.0 16_556 . . . ? O10 O8 O9 S2 46.7(2) 16_556 . . . ? O7 O8 O9 S2 -42.3(2) . . . . ? S2 O8 O9 O7 -47.8(2) . . . 16_556 ? O10 O8 O9 O7 -1.1(3) 16_556 . . 16_556 ? O7 O8 O9 O7 -90.1(3) . . . 16_556 ? S2 O8 O9 O10 42.6(2) . . . . ? O10 O8 O9 O10 89.3(3) 16_556 . . . ? O7 O8 O9 O10 0.3(3) . . . . ? O9 S2 O10 O8 117.0(3) . . . 16_556 ? O9 S2 O10 O8 -63.0(3) 16_556 . . 16_556 ? O10 S2 O10 O8 -31(5) 16_556 . . 16_556 ? O7 S2 O10 O8 61.1(3) 16_556 . . 16_556 ? O7 S2 O10 O8 -118.9(3) . . . 16_556 ? O8 S2 O10 O8 180.0 . . . 16_556 ? O9 S2 O10 O9 180.003(2) 16_556 . . . ? O10 S2 O10 O9 -148(5) 16_556 . . . ? O7 S2 O10 O9 -55.8(2) 16_556 . . . ? O7 S2 O10 O9 124.2(2) . . . . ? O8 S2 O10 O9 -117.0(3) 16_556 . . . ? O8 S2 O10 O9 63.0(3) . . . . ? O9 S2 O10 O7 -124.2(2) . . . . ? O9 S2 O10 O7 55.9(2) 16_556 . . . ? O10 S2 O10 O7 88(5) 16_556 . . . ? O7 S2 O10 O7 180.000(2) 16_556 . . . ? O8 S2 O10 O7 118.9(3) 16_556 . . . ? O8 S2 O10 O7 -61.1(3) . . . . ? O7 O9 O10 S2 50.1(2) 16_556 . . . ? O8 O9 O10 S2 -40.52(19) . . . . ? S2 O9 O10 O8 -49.3(2) . . . 16_556 ? O7 O9 O10 O8 0.8(3) 16_556 . . 16_556 ? O8 O9 O10 O8 -89.8(3) . . . 16_556 ? S2 O9 O10 O7 40.25(19) . . . . ? O7 O9 O10 O7 90.3(3) 16_556 . . . ? O8 O9 O10 O7 -0.3(3) . . . . ? O9 O7 O10 S2 -47.0(2) 16_556 . . . ? O8 O7 O10 S2 42.9(2) . . . . ? S2 O7 O10 O8 48.2(2) . . . 16_556 ? O9 O7 O10 O8 1.1(3) 16_556 . . 16_556 ? O8 O7 O10 O8 91.0(3) . . . 16_556 ? S2 O7 O10 O9 -42.6(2) . . . . ? O9 O7 O10 O9 -89.6(3) 16_556 . . . ? O8 O7 O10 O9 0.3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O5 0.86 2.36 3.149(3) 153.4 . N2 H2A O6 0.86 2.45 3.120(5) 135.7 . N2 H2A O6 0.86 2.32 3.171(5) 169.3 3 N3 H3A O6 0.86 2.53 3.162(5) 131.3 . N3 H3A O6 0.86 2.00 2.857(4) 172.3 11_556 N5 H5A O7 0.86 2.10 2.885(4) 151.9 16_556 N5 H5A O8 0.86 2.58 3.257(4) 136.8 16_556 N5 H5A O9 0.86 2.19 3.038(4) 168.5 . N6 H6A O8 0.86 2.28 3.027(4) 146.2 16_556 N6 H6A O10 0.86 2.05 2.896(4) 168.4 . C34 H34C O1 0.96 2.45 3.120(3) 126.7 9_554 C37 H37C O1 0.96 2.17 3.047(4) 152.1 9_554 C3 H3 O1 0.93 2.44 2.846(3) 106.1 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.249 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.043 #######################END data_CuSO4 _database_code_depnum_ccdc_archive 'CCDC 805456' #TrackingRef '- 150K CuSO4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C228 H240 Cu4 N48 O40 S4' _chemical_formula_weight 4675.08 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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 37.5437(15) _cell_length_b 37.5437(15) _cell_length_c 13.5170(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 16500.0(16) _cell_formula_units_Z 3 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7332 _exptl_absorpt_coefficient_mu 0.507 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8629 _exptl_absorpt_correction_T_max 0.8967 _exptl_absorpt_process_details SADABS _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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39685 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7196 _reflns_number_gt 5076 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0237P)^2^+5.2674P] 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 7196 _refine_ls_number_parameters 525 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.0692 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O6 O 0.02456(11) 0.03921(11) 0.5254(3) 0.0400(9) Uani 0.33 1 d P . . O5 O 0.01747(13) 0.02355(11) 0.4174(3) 0.0511(11) Uani 0.33 1 d P . . S1 S 0.0000 0.0000 0.5000 0.0331(2) Uani 1 6 d S . . C1 C 0.03963(5) 0.05425(5) 0.17731(14) 0.0393(4) Uani 1 1 d . . . H1A H 0.0150 0.0352 0.2103 0.047 Uiso 1 1 calc R . . C2 C 0.07050(5) 0.08758(5) 0.22839(13) 0.0318(4) Uani 1 1 d . . . C3 C 0.10632(5) 0.11592(5) 0.18014(14) 0.0343(4) Uani 1 1 d . . . H3A H 0.1273 0.1387 0.2151 0.041 Uiso 1 1 calc R . . C4 C 0.11113(6) 0.11054(5) 0.08043(15) 0.0411(4) Uani 1 1 d . . . H4A H 0.1355 0.1299 0.0470 0.049 Uiso 1 1 calc R . . C5 C 0.08070(5) 0.07715(5) 0.02911(14) 0.0355(4) Uani 1 1 d . . . H5A H 0.0843 0.0736 -0.0391 0.043 Uiso 1 1 calc R . . C6 C 0.07800(6) 0.12166(5) 0.40659(15) 0.0421(4) Uani 1 1 d . . . C7 C 0.05822(5) 0.14662(5) 0.54706(13) 0.0328(4) Uani 1 1 d . . . C8 C 0.05029(5) 0.17682(5) 0.51249(14) 0.0390(4) Uani 1 1 d . . . H8A H 0.0396 0.1748 0.4477 0.047 Uiso 1 1 calc R . . C9 C 0.05794(5) 0.20980(5) 0.57238(14) 0.0374(4) Uani 1 1 d . . . H9A H 0.0526 0.2305 0.5483 0.045 Uiso 1 1 calc R . . C10 C 0.07336(5) 0.21286(5) 0.66772(14) 0.0373(4) Uani 1 1 d . . . H10A H 0.0785 0.2355 0.7088 0.045 Uiso 1 1 calc R . . C11 C 0.08116(5) 0.18256(5) 0.70220(14) 0.0343(4) Uani 1 1 d . . . C12 C 0.07385(5) 0.14962(5) 0.64221(14) 0.0336(4) Uani 1 1 d . . . C13 C 0.08165(5) 0.11952(5) 0.67765(14) 0.0360(4) Uani 1 1 d . . . H13A H 0.0762 0.0967 0.6369 0.043 Uiso 1 1 calc R . . C14 C 0.09739(5) 0.12244(6) 0.77243(14) 0.0366(4) Uani 1 1 d . . . H14A H 0.1030 0.1019 0.7960 0.044 Uiso 1 1 calc R . . C15 C 0.10493(5) 0.15548(5) 0.83248(14) 0.0386(4) Uani 1 1 d . . . H15A H 0.1154 0.1574 0.8975 0.046 Uiso 1 1 calc R . . C16 C 0.09719(5) 0.18587(5) 0.79732(14) 0.0366(4) Uani 1 1 d . . . H16A H 0.1028 0.2088 0.8379 0.044 Uiso 1 1 calc R . . C17 C 0.11228(5) 0.32067(5) 0.50341(14) 0.0352(4) Uani 1 1 d . . . H17A H 0.1332 0.3186 0.5377 0.042 Uiso 1 1 calc R . . C18 C 0.07874(5) 0.31682(5) 0.55410(14) 0.0328(4) Uani 1 1 d . . . C19 C 0.04826(5) 0.31982(5) 0.50558(13) 0.0333(4) Uani 1 1 d . . . H19A H 0.0253 0.3172 0.5416 0.040 Uiso 1 1 calc R . . C20 C 0.05069(5) 0.32667(5) 0.40339(14) 0.0368(4) Uani 1 1 d . . . H20A H 0.0296 0.3288 0.3698 0.044 Uiso 1 1 calc R . . C21 C 0.08464(5) 0.33036(5) 0.35118(15) 0.0392(4) Uani 1 1 d . . . H21A H 0.0866 0.3347 0.2817 0.047 Uiso 1 1 calc R . . C22 C 0.04160(5) 0.27684(5) 0.70425(14) 0.0362(4) Uani 1 1 d . . . C23 C 0.01376(5) 0.25096(5) 0.86232(13) 0.0314(4) Uani 1 1 d . . . C24 C -0.01411(5) 0.21165(5) 0.82977(14) 0.0372(4) Uani 1 1 d . . . H24A H -0.0121 0.2034 0.7645 0.045 Uiso 1 1 calc R . . C25 C -0.04518(5) 0.18416(6) 0.89296(15) 0.0384(4) Uani 1 1 d . . . H25A H -0.0645 0.1573 0.8705 0.046 Uiso 1 1 calc R . . C26 C -0.04778(5) 0.19598(5) 0.98766(14) 0.0367(4) Uani 1 1 d . . . H26A H -0.0688 0.1771 1.0306 0.044 Uiso 1 1 calc R . . C27 C -0.01949(5) 0.23582(5) 1.02149(14) 0.0364(4) Uani 1 1 d . . . C28 C 0.01115(5) 0.26348(6) 0.95769(14) 0.0409(4) Uani 1 1 d . . . C29 C 0.03880(5) 0.30235(5) 0.99057(13) 0.0323(4) Uani 1 1 d . . . H29A H 0.0600 0.3211 0.9477 0.039 Uiso 1 1 calc R . . C30 C 0.03597(5) 0.31444(6) 1.08652(15) 0.0419(5) Uani 1 1 d . . . H30A H 0.0550 0.3414 1.1089 0.050 Uiso 1 1 calc R . . C31 C 0.00508(5) 0.28672(5) 1.14923(15) 0.0375(4) Uani 1 1 d . . . H31A H 0.0032 0.2948 1.2148 0.045 Uiso 1 1 calc R . . C32 C -0.02294(6) 0.24741(6) 1.11653(14) 0.0409(4) Uani 1 1 d . . . H32A H -0.0443 0.2287 1.1590 0.049 Uiso 1 1 calc R . . C33 C 0.22129(6) 0.39055(6) 0.47662(15) 0.0442(5) Uani 1 1 d . . . H33 H 0.2181 0.3663 0.5069 0.053 Uiso 1 1 calc R . . C34 C 0.25306(5) 0.43129(6) 0.62990(13) 0.0365(4) Uani 1 1 d . . . H34A H 0.2332 0.4052 0.6608 0.055 Uiso 1 1 calc R . . H34B H 0.2493 0.4535 0.6564 0.055 Uiso 1 1 calc R . . H34C H 0.2811 0.4371 0.6442 0.055 Uiso 1 1 calc R . . C35 C 0.26931(5) 0.46769(5) 0.46323(14) 0.0364(4) Uani 1 1 d . . . H35A H 0.2858 0.4645 0.4116 0.055 Uiso 1 1 calc R . . H35B H 0.2874 0.4900 0.5080 0.055 Uiso 1 1 calc R . . H35C H 0.2497 0.4743 0.4327 0.055 Uiso 1 1 calc R . . C36 C 0.16888(5) 0.25278(6) 0.48437(16) 0.0423(5) Uani 1 1 d . . . H36 H 0.1499 0.2301 0.4456 0.051 Uiso 1 1 calc R . . C37 C 0.17239(6) 0.20260(5) 0.59459(15) 0.0423(4) Uani 1 1 d . . . H37A H 0.1508 0.1921 0.6452 0.063 Uiso 1 1 calc R . . H37C H 0.1962 0.2012 0.6193 0.063 Uiso 1 1 calc R . . H37B H 0.1619 0.1859 0.5345 0.063 Uiso 1 1 calc R . . C38 C 0.20891(6) 0.27487(6) 0.65293(18) 0.0541(6) Uani 1 1 d . . . H38A H 0.1912 0.2686 0.7111 0.081 Uiso 1 1 calc R . . H38B H 0.2189 0.3034 0.6323 0.081 Uiso 1 1 calc R . . H38C H 0.2323 0.2713 0.6695 0.081 Uiso 1 1 calc R . . Cu1 Cu 0.0000 0.0000 0.0000 0.03443(13) Uani 1 6 d S . . Cu2 Cu 0.1667 0.3333 0.3333 0.03961(9) Uani 1 2 d S . . N1 N 0.04500(4) 0.04890(4) 0.07767(12) 0.0360(3) Uani 1 1 d . . . N2 N 0.06467(4) 0.09357(5) 0.33281(11) 0.0368(3) Uani 1 1 d . . . H2A H 0.0451 0.0700 0.3566 0.044 Uiso 1 1 calc R . . N3 N 0.05101(4) 0.11176(5) 0.48240(12) 0.0398(4) Uani 1 1 d . . . H3B H 0.0307 0.0865 0.4924 0.048 Uiso 1 1 calc R . . N4 N 0.11547(4) 0.32763(4) 0.40181(11) 0.0361(3) Uani 1 1 d . . . N5 N 0.07698(4) 0.30896(4) 0.65871(11) 0.0384(4) Uani 1 1 d . . . H5B H 0.0986 0.3247 0.6954 0.046 Uiso 1 1 calc R . . N6 N 0.04715(4) 0.27670(4) 0.80523(11) 0.0358(3) Uani 1 1 d . . . H6A H 0.0714 0.2926 0.8322 0.043 Uiso 1 1 calc R . . N7 N 0.24641(4) 0.42840(5) 0.52046(12) 0.0382(4) Uani 1 1 d . . . N8 N 0.18517(5) 0.24666(4) 0.57114(11) 0.0379(4) Uani 1 1 d . . . O1 O 0.11236(4) 0.15386(4) 0.40854(10) 0.0400(3) Uani 1 1 d . . . O2 O 0.01122(4) 0.25474(3) 0.65936(9) 0.0361(3) Uani 1 1 d . . . O3 O 0.20286(3) 0.38805(3) 0.39781(10) 0.0373(3) Uani 1 1 d . . . O4 O 0.17985(3) 0.28905(3) 0.45847(9) 0.0321(3) Uani 1 1 d . . . O7 O 0.18408(7) 0.31548(7) 0.8881(2) 0.0388(6) Uani 0.50 1 d P . . O8 O 0.12984(7) 0.32551(7) 0.8723(2) 0.0381(6) Uani 0.50 1 d P . . O9 O 0.19176(7) 0.37525(7) 0.83584(19) 0.0369(6) Uani 0.50 1 d P . . O10 O 0.16011(7) 0.32010(7) 0.73756(18) 0.0370(6) Uani 0.50 1 d P . . S2 S 0.1667 0.3333 0.8333 0.03404(13) Uani 1 2 d S . . 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 O6 0.033(2) 0.037(2) 0.034(2) 0.0037(17) 0.0104(17) 0.0063(17) O5 0.051(3) 0.036(2) 0.055(3) 0.0045(19) 0.015(2) 0.0133(19) S1 0.0314(3) 0.0314(3) 0.0364(7) 0.000 0.000 0.01570(16) C1 0.0347(9) 0.0352(9) 0.0323(11) 0.0044(8) 0.0052(8) 0.0058(8) C2 0.0306(8) 0.0317(8) 0.0301(10) -0.0016(7) 0.0026(7) 0.0133(7) C3 0.0296(9) 0.0304(9) 0.0356(11) -0.0043(8) -0.0012(7) 0.0094(7) C4 0.0381(10) 0.0318(9) 0.0355(11) 0.0010(8) 0.0020(8) 0.0040(8) C5 0.0330(9) 0.0365(9) 0.0324(11) -0.0072(8) 0.0017(8) 0.0139(7) C6 0.0378(10) 0.0359(10) 0.0359(11) -0.0004(8) 0.0028(8) 0.0060(8) C7 0.0354(9) 0.0319(9) 0.0299(10) -0.0071(7) -0.0010(7) 0.0159(7) C8 0.0349(9) 0.0413(10) 0.0352(11) -0.0096(8) -0.0157(8) 0.0147(8) C9 0.0359(9) 0.0317(9) 0.0410(12) 0.0027(8) 0.0055(8) 0.0142(8) C10 0.0441(10) 0.0354(9) 0.0298(11) -0.0058(8) 0.0073(8) 0.0178(8) C11 0.0350(9) 0.0345(9) 0.0311(10) -0.0053(8) 0.0053(8) 0.0157(8) C12 0.0309(9) 0.0329(9) 0.0345(11) -0.0042(8) 0.0030(7) 0.0140(7) C13 0.0362(9) 0.0365(9) 0.0330(10) -0.0039(8) 0.0077(8) 0.0162(8) C14 0.0349(9) 0.0419(10) 0.0339(11) 0.0058(8) 0.0071(8) 0.0199(8) C15 0.0320(9) 0.0417(10) 0.0360(11) -0.0072(8) -0.0121(8) 0.0139(8) C16 0.0406(10) 0.0309(9) 0.0317(11) 0.0019(8) 0.0101(8) 0.0130(8) C17 0.0369(9) 0.0373(9) 0.0293(11) 0.0028(8) -0.0047(8) 0.0171(8) C18 0.0368(9) 0.0233(8) 0.0275(10) 0.0076(7) 0.0025(7) 0.0069(7) C19 0.0333(9) 0.0317(9) 0.0319(10) -0.0009(7) 0.0083(8) 0.0139(7) C20 0.0353(9) 0.0381(9) 0.0336(11) 0.0053(8) -0.0063(8) 0.0159(8) C21 0.0322(9) 0.0349(9) 0.0311(11) 0.0056(8) 0.0027(8) 0.0021(7) C22 0.0371(10) 0.0295(9) 0.0333(11) 0.0034(8) 0.0026(8) 0.0100(8) C23 0.0340(9) 0.0323(9) 0.0312(10) -0.0036(7) 0.0017(7) 0.0189(7) C24 0.0330(9) 0.0411(10) 0.0313(11) -0.0006(8) -0.0001(8) 0.0138(8) C25 0.0358(9) 0.0379(9) 0.0366(12) 0.0019(8) -0.0002(8) 0.0147(8) C26 0.0351(9) 0.0366(9) 0.0299(11) 0.0022(8) 0.0056(8) 0.0115(8) C27 0.0327(9) 0.0401(10) 0.0298(11) 0.0009(8) 0.0074(8) 0.0132(8) C28 0.0341(9) 0.0470(11) 0.0310(11) -0.0007(8) 0.0066(8) 0.0124(8) C29 0.0346(9) 0.0339(9) 0.0290(10) 0.0057(7) 0.0063(7) 0.0175(7) C30 0.0347(9) 0.0373(10) 0.0351(11) -0.0039(8) 0.0006(8) 0.0042(8) C31 0.0343(9) 0.0368(9) 0.0367(11) -0.0021(8) 0.0111(8) 0.0143(8) C32 0.0418(10) 0.0389(10) 0.0359(11) -0.0060(8) 0.0124(8) 0.0156(8) C33 0.0423(10) 0.0414(10) 0.0327(11) 0.0012(9) 0.0000(9) 0.0089(8) C34 0.0352(9) 0.0401(10) 0.0322(11) -0.0081(8) -0.0053(8) 0.0174(8) C35 0.0367(9) 0.0354(9) 0.0357(11) 0.0072(8) 0.0095(8) 0.0169(8) C36 0.0365(10) 0.0342(10) 0.0491(13) 0.0032(9) 0.0005(9) 0.0125(8) C37 0.0411(10) 0.0306(9) 0.0444(12) 0.0071(8) 0.0061(9) 0.0099(8) C38 0.0599(13) 0.0500(12) 0.0726(17) -0.0199(11) -0.0231(12) 0.0427(11) Cu1 0.03446(17) 0.03446(17) 0.0344(3) 0.000 0.000 0.01723(9) Cu2 0.03701(17) 0.03892(17) 0.03121(18) 0.01174(14) 0.00458(14) 0.01022(14) N1 0.0355(8) 0.0319(7) 0.0355(9) 0.0087(7) 0.0034(7) 0.0130(6) N2 0.0357(8) 0.0383(8) 0.0310(9) -0.0013(7) 0.0004(6) 0.0144(7) N3 0.0324(8) 0.0409(8) 0.0390(10) -0.0158(7) -0.0060(7) 0.0131(7) N4 0.0336(8) 0.0355(8) 0.0288(9) 0.0030(6) 0.0015(6) 0.0093(6) N5 0.0376(8) 0.0374(8) 0.0335(9) 0.0090(7) 0.0022(7) 0.0138(7) N6 0.0310(7) 0.0392(8) 0.0316(9) -0.0040(7) 0.0070(6) 0.0133(6) N7 0.0370(8) 0.0378(8) 0.0310(9) 0.0064(7) 0.0011(7) 0.0122(7) N8 0.0566(9) 0.0333(8) 0.0289(9) -0.0035(6) 0.0090(7) 0.0262(7) O1 0.0379(7) 0.0374(7) 0.0401(8) -0.0046(6) 0.0069(6) 0.0154(6) O2 0.0376(6) 0.0312(6) 0.0314(7) 0.0001(5) -0.0019(6) 0.0110(5) O3 0.0309(6) 0.0355(6) 0.0366(8) 0.0107(5) 0.0044(6) 0.0099(5) O4 0.0367(6) 0.0378(6) 0.0331(7) -0.0054(5) 0.0068(5) 0.0270(5) O7 0.0347(13) 0.0316(12) 0.0429(17) -0.0074(11) -0.0055(11) 0.0112(11) O8 0.0354(13) 0.0337(12) 0.0452(17) 0.0105(11) 0.0099(11) 0.0172(10) O9 0.0323(12) 0.0393(13) 0.0377(16) -0.0070(11) -0.0048(11) 0.0168(11) O10 0.0367(13) 0.0347(13) 0.0315(14) 0.0092(10) 0.0099(11) 0.0119(11) S2 0.0329(3) 0.0330(3) 0.0332(3) -0.0047(3) 0.0027(3) 0.0142(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 O6 O5 1.284(6) 12_556 ? O6 S1 1.333(4) . ? O6 O5 1.449(6) 11_556 ? O6 O6 1.460(5) 12_556 ? O6 O6 1.460(5) 11_556 ? O6 O5 1.546(6) . ? O5 O6 1.284(6) 11_556 ? O5 S1 1.370(4) . ? O5 O5 1.377(6) 2 ? O5 O5 1.377(6) 3 ? O5 O6 1.449(6) 12_556 ? S1 O6 1.333(4) 10_556 ? S1 O6 1.333(4) 11_556 ? S1 O6 1.333(3) 2 ? S1 O6 1.333(4) 12_556 ? S1 O6 1.333(4) 3 ? S1 O5 1.371(4) 11_556 ? S1 O5 1.371(4) 2 ? S1 O5 1.371(4) 12_556 ? S1 O5 1.371(4) 3 ? S1 O5 1.371(4) 10_556 ? C1 C2 1.391(2) . ? C1 N1 1.391(2) . ? C1 H1A 0.9500 . ? C2 C3 1.391(2) . ? C2 N2 1.463(2) . ? C3 C4 1.388(3) . ? C3 H3A 0.9500 . ? C4 C5 1.388(2) . ? C4 H4A 0.9500 . ? C5 N1 1.389(2) . ? C5 H5A 0.9500 . ? C6 O1 1.252(2) . ? C6 N2 1.353(2) . ? C6 N3 1.356(2) . ? C7 C8 1.389(2) . ? C7 C12 1.395(3) . ? C7 N3 1.482(2) . ? C8 C9 1.384(2) . ? C8 H8A 0.9500 . ? C9 C10 1.394(3) . ? C9 H9A 0.9500 . ? C10 C11 1.389(3) . ? C10 H10A 0.9500 . ? C11 C12 1.387(2) . ? C11 C16 1.399(3) . ? C12 C13 1.387(2) . ? C13 C14 1.392(3) . ? C13 H13A 0.9500 . ? C14 C15 1.388(3) . ? C14 H14A 0.9500 . ? C15 C16 1.394(3) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.376(2) . ? C17 N4 1.392(2) . ? C17 H17A 0.9500 . ? C18 C19 1.372(2) . ? C18 N5 1.439(2) . ? C19 C20 1.400(2) . ? C19 H19A 0.9500 . ? C20 C21 1.402(3) . ? C20 H20A 0.9500 . ? C21 N4 1.392(2) . ? C21 H21A 0.9500 . ? C22 O2 1.188(2) . ? C22 N6 1.381(2) . ? C22 N5 1.413(2) . ? C23 N6 1.375(2) . ? C23 C24 1.387(2) . ? C23 C28 1.392(2) . ? C24 C25 1.397(2) . ? C24 H24A 0.9500 . ? C25 C26 1.374(3) . ? C25 H25A 0.9500 . ? C26 C27 1.409(2) . ? C26 H26A 0.9500 . ? C27 C32 1.383(3) . ? C27 C28 1.397(2) . ? C28 C29 1.375(2) . ? C29 C30 1.396(3) . ? C29 H29A 0.9500 . ? C30 C31 1.393(2) . ? C30 H30A 0.9500 . ? C31 C32 1.388(2) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 O3 1.248(2) . ? C33 N7 1.385(2) . ? C33 H33 0.9500 . ? C34 N7 1.495(2) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 N7 1.498(2) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 O4 1.259(2) . ? C36 N8 1.394(2) . ? C36 H36 0.9500 . ? C37 N8 1.508(2) . ? C37 H37A 0.9800 . ? C37 H37C 0.9800 . ? C37 H37B 0.9800 . ? C38 N8 1.481(2) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? Cu1 N1 2.0555(15) . ? Cu1 N1 2.0556(15) 10 ? Cu1 N1 2.0556(15) 12 ? Cu1 N1 2.0556(15) 3 ? Cu1 N1 2.0556(15) 2 ? Cu1 N1 2.0556(15) 11 ? Cu2 O3 2.0087(12) . ? Cu2 O3 2.0088(12) 16 ? Cu2 N4 2.0457(15) . ? Cu2 N4 2.0459(15) 16 ? N2 H2A 0.8800 . ? N3 H3B 0.8800 . ? N5 H5B 0.8800 . ? N6 H6A 0.8800 . ? O7 S2 1.365(3) . ? O7 O10 1.520(3) 16_556 ? O7 O8 1.538(3) 16_556 ? O7 O9 1.588(3) 16_556 ? O8 S2 1.367(2) . ? O8 O7 1.538(3) 16_556 ? O8 O10 1.606(3) 16_556 ? O8 O9 1.647(3) 16_556 ? O9 S2 1.372(2) . ? O9 O10 1.576(3) 16_556 ? O9 O7 1.588(3) 16_556 ? O9 O8 1.647(3) 16_556 ? O10 S2 1.364(3) . ? O10 O7 1.520(3) 16_556 ? O10 O9 1.576(3) 16_556 ? O10 O8 1.606(3) 16_556 ? S2 O10 1.364(3) 16_556 ? S2 O7 1.365(3) 16_556 ? S2 O8 1.367(2) 16_556 ? S2 O9 1.372(2) 16_556 ? 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 O6 S1 63.1(2) 12_556 . ? O5 O6 O5 60.2(4) 12_556 11_556 ? S1 O6 O5 58.9(2) . 11_556 ? O5 O6 O6 68.3(2) 12_556 12_556 ? S1 O6 O6 56.81(7) . 12_556 ? O5 O6 O6 109.8(2) 11_556 12_556 ? O5 O6 O6 112.5(2) 12_556 11_556 ? S1 O6 O6 56.81(7) . 11_556 ? O5 O6 O6 64.2(2) 11_556 11_556 ? O6 O6 O6 99.7(4) 12_556 11_556 ? O5 O6 O5 113.4(4) 12_556 . ? S1 O6 O5 56.3(2) . . ? O5 O6 O5 104.6(4) 11_556 . ? O6 O6 O5 57.5(3) 12_556 . ? O6 O6 O5 50.5(3) 11_556 . ? O6 O5 S1 60.2(3) 11_556 . ? O6 O5 O5 112.9(3) 11_556 2 ? S1 O5 O5 59.84(14) . 2 ? O6 O5 O5 65.9(4) 11_556 3 ? S1 O5 O5 59.84(14) . 3 ? O5 O5 O5 60.003(1) 2 3 ? O6 O5 O6 109.3(5) 11_556 12_556 ? S1 O5 O6 56.4(2) . 12_556 ? O5 O5 O6 54.0(3) 2 12_556 ? O5 O5 O6 103.4(3) 3 12_556 ? O6 O5 O6 61.3(2) 11_556 . ? S1 O5 O6 54.0(2) . . ? O5 O5 O6 102.6(2) 2 . ? O5 O5 O6 108.9(2) 3 . ? O6 O5 O6 58.2(2) 12_556 . ? O6 S1 O6 180.0(5) . 10_556 ? O6 S1 O6 66.38(14) . 11_556 ? O6 S1 O6 113.62(14) 10_556 11_556 ? O6 S1 O6 113.62(14) . 2 ? O6 S1 O6 66.38(14) 10_556 2 ? O6 S1 O6 180.00(15) 11_556 2 ? O6 S1 O6 66.38(14) . 12_556 ? O6 S1 O6 113.62(14) 10_556 12_556 ? O6 S1 O6 113.62(14) 11_556 12_556 ? O6 S1 O6 66.38(14) 2 12_556 ? O6 S1 O6 113.62(14) . 3 ? O6 S1 O6 66.38(14) 10_556 3 ? O6 S1 O6 66.38(14) 11_556 3 ? O6 S1 O6 113.62(14) 2 3 ? O6 S1 O6 180.0(4) 12_556 3 ? O6 S1 O5 69.7(2) . . ? O6 S1 O5 110.3(2) 10_556 . ? O6 S1 O5 56.7(2) 11_556 . ? O6 S1 O5 123.3(2) 2 . ? O6 S1 O5 64.8(3) 12_556 . ? O6 S1 O5 115.2(3) 3 . ? O6 S1 O5 64.8(3) . 11_556 ? O6 S1 O5 115.2(3) 10_556 11_556 ? O6 S1 O5 69.7(2) 11_556 11_556 ? O6 S1 O5 110.3(2) 2 11_556 ? O6 S1 O5 123.3(2) 12_556 11_556 ? O6 S1 O5 56.7(2) 3 11_556 ? O5 S1 O5 119.7(3) . 11_556 ? O6 S1 O5 115.2(3) . 2 ? O6 S1 O5 64.8(3) 10_556 2 ? O6 S1 O5 110.3(2) 11_556 2 ? O6 S1 O5 69.7(2) 2 2 ? O6 S1 O5 56.7(2) 12_556 2 ? O6 S1 O5 123.3(2) 3 2 ? O5 S1 O5 60.3(3) . 2 ? O5 S1 O5 180.0(3) 11_556 2 ? O6 S1 O5 56.7(2) . 12_556 ? O6 S1 O5 123.3(2) 10_556 12_556 ? O6 S1 O5 115.2(3) 11_556 12_556 ? O6 S1 O5 64.8(3) 2 12_556 ? O6 S1 O5 69.7(2) 12_556 12_556 ? O6 S1 O5 110.3(2) 3 12_556 ? O5 S1 O5 119.7(3) . 12_556 ? O5 S1 O5 60.3(3) 11_556 12_556 ? O5 S1 O5 119.7(3) 2 12_556 ? O6 S1 O5 123.3(2) . 3 ? O6 S1 O5 56.7(2) 10_556 3 ? O6 S1 O5 64.8(3) 11_556 3 ? O6 S1 O5 115.2(3) 2 3 ? O6 S1 O5 110.3(2) 12_556 3 ? O6 S1 O5 69.7(2) 3 3 ? O5 S1 O5 60.3(3) . 3 ? O5 S1 O5 119.7(3) 11_556 3 ? O5 S1 O5 60.3(3) 2 3 ? O5 S1 O5 180.0(3) 12_556 3 ? O6 S1 O5 110.3(2) . 10_556 ? O6 S1 O5 69.7(2) 10_556 10_556 ? O6 S1 O5 123.3(2) 11_556 10_556 ? O6 S1 O5 56.7(2) 2 10_556 ? O6 S1 O5 115.2(3) 12_556 10_556 ? O6 S1 O5 64.8(3) 3 10_556 ? O5 S1 O5 180.0(6) . 10_556 ? O5 S1 O5 60.3(3) 11_556 10_556 ? O5 S1 O5 119.7(3) 2 10_556 ? O5 S1 O5 60.3(3) 12_556 10_556 ? O5 S1 O5 119.7(3) 3 10_556 ? C2 C1 N1 119.65(16) . . ? C2 C1 H1A 120.2 . . ? N1 C1 H1A 120.2 . . ? C3 C2 C1 120.49(17) . . ? C3 C2 N2 119.76(15) . . ? C1 C2 N2 119.73(15) . . ? C4 C3 C2 119.36(16) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C5 C4 C3 120.57(17) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C4 C5 N1 119.85(17) . . ? C4 C5 H5A 120.1 . . ? N1 C5 H5A 120.1 . . ? O1 C6 N2 124.71(17) . . ? O1 C6 N3 121.12(17) . . ? N2 C6 N3 114.14(15) . . ? C8 C7 C12 119.83(16) . . ? C8 C7 N3 120.22(16) . . ? C12 C7 N3 119.94(16) . . ? C9 C8 C7 120.01(17) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 120.42(17) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C11 C10 C9 119.44(16) . . ? C11 C10 H10A 120.3 . . ? C9 C10 H10A 120.3 . . ? C12 C11 C10 120.36(17) . . ? C12 C11 C16 120.07(17) . . ? C10 C11 C16 119.56(16) . . ? C11 C12 C13 119.78(17) . . ? C11 C12 C7 119.94(16) . . ? C13 C12 C7 120.28(16) . . ? C12 C13 C14 120.51(17) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C15 C14 C13 119.85(17) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C14 C15 C16 119.94(17) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C15 C16 C11 119.83(17) . . ? C15 C16 H16A 120.1 . . ? C11 C16 H16A 120.1 . . ? C18 C17 N4 119.96(16) . . ? C18 C17 H17A 120.0 . . ? N4 C17 H17A 120.0 . . ? C19 C18 C17 120.70(17) . . ? C19 C18 N5 122.13(16) . . ? C17 C18 N5 117.17(16) . . ? C18 C19 C20 120.43(16) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C19 C20 C21 119.18(16) . . ? C19 C20 H20A 120.4 . . ? C21 C20 H20A 120.4 . . ? N4 C21 C20 119.58(17) . . ? N4 C21 H21A 120.2 . . ? C20 C21 H21A 120.2 . . ? O2 C22 N6 126.59(16) . . ? O2 C22 N5 122.57(17) . . ? N6 C22 N5 110.77(15) . . ? N6 C23 C24 120.51(16) . . ? N6 C23 C28 118.43(16) . . ? C24 C23 C28 120.67(16) . . ? C23 C24 C25 119.95(18) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C26 C25 C24 119.94(17) . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C25 C26 C27 120.50(16) . . ? C25 C26 H26A 119.8 . . ? C27 C26 H26A 119.8 . . ? C32 C27 C28 120.76(17) . . ? C32 C27 C26 119.74(16) . . ? C28 C27 C26 119.49(17) . . ? C29 C28 C23 120.96(17) . . ? C29 C28 C27 119.58(18) . . ? C23 C28 C27 119.45(17) . . ? C28 C29 C30 120.39(16) . . ? C28 C29 H29A 119.8 . . ? C30 C29 H29A 119.8 . . ? C31 C30 C29 119.53(17) . . ? C31 C30 H30A 120.2 . . ? C29 C30 H30A 120.2 . . ? C32 C31 C30 120.39(18) . . ? C32 C31 H31A 119.8 . . ? C30 C31 H31A 119.8 . . ? C27 C32 C31 119.33(18) . . ? C27 C32 H32A 120.3 . . ? C31 C32 H32A 120.3 . . ? O3 C33 N7 120.64(18) . . ? O3 C33 H33 119.7 . . ? N7 C33 H33 119.7 . . ? N7 C34 H34A 109.5 . . ? N7 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N7 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N7 C35 H35A 109.5 . . ? N7 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N7 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O4 C36 N8 118.61(17) . . ? O4 C36 H36 120.7 . . ? N8 C36 H36 120.7 . . ? N8 C37 H37A 109.5 . . ? N8 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? N8 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? H37C C37 H37B 109.5 . . ? N8 C38 H38A 109.5 . . ? N8 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N8 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N1 Cu1 N1 180.0 . 10 ? N1 Cu1 N1 83.76(5) . 12 ? N1 Cu1 N1 96.24(5) 10 12 ? N1 Cu1 N1 96.24(5) . 3 ? N1 Cu1 N1 83.76(5) 10 3 ? N1 Cu1 N1 180.00(11) 12 3 ? N1 Cu1 N1 96.24(5) . 2 ? N1 Cu1 N1 83.76(5) 10 2 ? N1 Cu1 N1 83.76(5) 12 2 ? N1 Cu1 N1 96.24(5) 3 2 ? N1 Cu1 N1 83.76(5) . 11 ? N1 Cu1 N1 96.24(5) 10 11 ? N1 Cu1 N1 96.24(5) 12 11 ? N1 Cu1 N1 83.76(5) 3 11 ? N1 Cu1 N1 180.00(11) 2 11 ? O3 Cu2 O3 180.0 . 16 ? O3 Cu2 N4 91.75(5) . . ? O3 Cu2 N4 88.26(5) 16 . ? O3 Cu2 N4 88.26(5) . 16 ? O3 Cu2 N4 91.74(5) 16 16 ? N4 Cu2 N4 180.0 . 16 ? C5 N1 C1 120.08(15) . . ? C5 N1 Cu1 119.27(12) . . ? C1 N1 Cu1 120.64(11) . . ? C6 N2 C2 143.69(16) . . ? C6 N2 H2A 108.2 . . ? C2 N2 H2A 108.2 . . ? C6 N3 C7 114.97(15) . . ? C6 N3 H3B 122.5 . . ? C7 N3 H3B 122.5 . . ? C17 N4 C21 120.14(16) . . ? C17 N4 Cu2 117.02(12) . . ? C21 N4 Cu2 122.83(12) . . ? C22 N5 C18 122.04(15) . . ? C22 N5 H5B 119.0 . . ? C18 N5 H5B 119.0 . . ? C23 N6 C22 118.11(15) . . ? C23 N6 H6A 120.9 . . ? C22 N6 H6A 120.9 . . ? C33 N7 C34 120.06(15) . . ? C33 N7 C35 123.38(16) . . ? C34 N7 C35 116.53(15) . . ? C36 N8 C38 131.82(15) . . ? C36 N8 C37 115.63(15) . . ? C38 N8 C37 112.04(15) . . ? C33 O3 Cu2 120.89(12) . . ? S2 O7 O10 56.12(13) . 16_556 ? S2 O7 O8 55.80(13) . 16_556 ? O10 O7 O8 92.51(18) 16_556 16_556 ? S2 O7 O9 54.75(12) . 16_556 ? O10 O7 O9 92.04(18) 16_556 16_556 ? O8 O7 O9 88.89(19) 16_556 16_556 ? S2 O8 O7 55.68(13) . 16_556 ? S2 O8 O10 53.89(12) . 16_556 ? O7 O8 O10 92.25(17) 16_556 16_556 ? S2 O8 O9 53.19(12) . 16_556 ? O7 O8 O9 88.81(18) 16_556 16_556 ? O10 O8 O9 86.89(16) 16_556 16_556 ? S2 O9 O10 54.59(13) . 16_556 ? S2 O9 O7 54.34(12) . 16_556 ? O10 O9 O7 91.53(18) 16_556 16_556 ? S2 O9 O8 52.92(11) . 16_556 ? O10 O9 O8 86.54(17) 16_556 16_556 ? O7 O9 O8 88.56(17) 16_556 16_556 ? S2 O10 O7 56.19(14) . 16_556 ? S2 O10 O9 55.07(12) . 16_556 ? O7 O10 O9 92.13(19) 16_556 16_556 ? S2 O10 O8 54.08(13) . 16_556 ? O7 O10 O8 92.48(18) 16_556 16_556 ? O9 O10 O8 86.95(17) 16_556 16_556 ? O10 S2 O10 179.998(1) 16_556 . ? O10 S2 O7 112.32(14) 16_556 16_556 ? O10 S2 O7 67.68(14) . 16_556 ? O10 S2 O7 67.68(14) 16_556 . ? O10 S2 O7 112.31(14) . . ? O7 S2 O7 180.00(15) 16_556 . ? O10 S2 O8 107.98(15) 16_556 16_556 ? O10 S2 O8 72.02(15) . 16_556 ? O7 S2 O8 111.48(14) 16_556 16_556 ? O7 S2 O8 68.51(14) . 16_556 ? O10 S2 O8 72.02(15) 16_556 . ? O10 S2 O8 107.98(15) . . ? O7 S2 O8 68.52(14) 16_556 . ? O7 S2 O8 111.49(14) . . ? O8 S2 O8 179.996(1) 16_556 . ? O10 S2 O9 70.34(14) 16_556 . ? O10 S2 O9 109.66(14) . . ? O7 S2 O9 70.91(13) 16_556 . ? O7 S2 O9 109.09(13) . . ? O8 S2 O9 73.89(14) 16_556 . ? O8 S2 O9 106.11(14) . . ? O10 S2 O9 109.67(14) 16_556 16_556 ? O10 S2 O9 70.33(14) . 16_556 ? O7 S2 O9 109.10(13) 16_556 16_556 ? O7 S2 O9 70.90(13) . 16_556 ? O8 S2 O9 106.10(14) 16_556 16_556 ? O8 S2 O9 73.90(14) . 16_556 ? O9 S2 O9 179.992(1) . 16_556 ? 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 O6 O5 O6 -100.5(2) 12_556 . . 11_556 ? S1 O6 O5 O6 -72.40(18) . . . 11_556 ? O5 O6 O5 O6 -37.1(3) 11_556 . . 11_556 ? O6 O6 O5 O6 -141.6(3) 12_556 . . 11_556 ? O5 O6 O5 S1 -28.1(3) 12_556 . . . ? O5 O6 O5 S1 35.3(2) 11_556 . . . ? O6 O6 O5 S1 -69.18(15) 12_556 . . . ? O6 O6 O5 S1 72.40(18) 11_556 . . . ? O5 O6 O5 O5 8.9(6) 12_556 . . 2 ? S1 O6 O5 O5 37.0(3) . . . 2 ? O5 O6 O5 O5 72.3(4) 11_556 . . 2 ? O6 O6 O5 O5 -32.1(4) 12_556 . . 2 ? O6 O6 O5 O5 109.4(4) 11_556 . . 2 ? O5 O6 O5 O5 -53.4(6) 12_556 . . 3 ? S1 O6 O5 O5 -25.2(3) . . . 3 ? O5 O6 O5 O5 10.0(5) 11_556 . . 3 ? O6 O6 O5 O5 -94.4(4) 12_556 . . 3 ? O6 O6 O5 O5 47.2(4) 11_556 . . 3 ? O5 O6 O5 O6 41.0(3) 12_556 . . 12_556 ? S1 O6 O5 O6 69.18(15) . . . 12_556 ? O5 O6 O5 O6 104.46(17) 11_556 . . 12_556 ? O6 O6 O5 O6 141.6(3) 11_556 . . 12_556 ? O5 O6 S1 O6 -26.8(6) 12_556 . . 10_556 ? O5 O6 S1 O6 42.9(6) 11_556 . . 10_556 ? O6 O6 S1 O6 -107.4(6) 12_556 . . 10_556 ? O6 O6 S1 O6 120.7(6) 11_556 . . 10_556 ? O5 O6 S1 O6 -177.8(6) . . . 10_556 ? O5 O6 S1 O6 -147.6(4) 12_556 . . 11_556 ? O5 O6 S1 O6 -77.8(3) 11_556 . . 11_556 ? O6 O6 S1 O6 131.9(5) 12_556 . . 11_556 ? O5 O6 S1 O6 61.5(3) . . . 11_556 ? O5 O6 S1 O6 32.4(4) 12_556 . . 2 ? O5 O6 S1 O6 102.2(3) 11_556 . . 2 ? O6 O6 S1 O6 -48.1(5) 12_556 . . 2 ? O6 O6 S1 O6 180.0 11_556 . . 2 ? O5 O6 S1 O6 -118.5(3) . . . 2 ? O5 O6 S1 O6 80.5(3) 12_556 . . 12_556 ? O5 O6 S1 O6 150.3(3) 11_556 . . 12_556 ? O6 O6 S1 O6 -131.9(5) 11_556 . . 12_556 ? O5 O6 S1 O6 -70.5(3) . . . 12_556 ? O5 O6 S1 O6 -99.5(3) 12_556 . . 3 ? O5 O6 S1 O6 -29.7(3) 11_556 . . 3 ? O6 O6 S1 O6 180.0 12_556 . . 3 ? O6 O6 S1 O6 48.1(5) 11_556 . . 3 ? O5 O6 S1 O6 109.5(3) . . . 3 ? O5 O6 S1 O5 151.0(4) 12_556 . . . ? O5 O6 S1 O5 -139.2(3) 11_556 . . . ? O6 O6 S1 O5 70.5(3) 12_556 . . . ? O6 O6 S1 O5 -61.5(3) 11_556 . . . ? O5 O6 S1 O5 -69.8(4) 12_556 . . 11_556 ? O6 O6 S1 O5 -150.3(3) 12_556 . . 11_556 ? O6 O6 S1 O5 77.8(3) 11_556 . . 11_556 ? O5 O6 S1 O5 139.2(3) . . . 11_556 ? O5 O6 S1 O5 110.2(4) 12_556 . . 2 ? O5 O6 S1 O5 180.0 11_556 . . 2 ? O6 O6 S1 O5 29.7(3) 12_556 . . 2 ? O6 O6 S1 O5 -102.2(3) 11_556 . . 2 ? O5 O6 S1 O5 -40.8(3) . . . 2 ? O5 O6 S1 O5 69.8(4) 11_556 . . 12_556 ? O6 O6 S1 O5 -80.5(3) 12_556 . . 12_556 ? O6 O6 S1 O5 147.6(4) 11_556 . . 12_556 ? O5 O6 S1 O5 -151.0(4) . . . 12_556 ? O5 O6 S1 O5 180.0 12_556 . . 3 ? O5 O6 S1 O5 -110.2(4) 11_556 . . 3 ? O6 O6 S1 O5 99.5(3) 12_556 . . 3 ? O6 O6 S1 O5 -32.4(4) 11_556 . . 3 ? O5 O6 S1 O5 29.0(4) . . . 3 ? O5 O6 S1 O5 -29.0(4) 12_556 . . 10_556 ? O5 O6 S1 O5 40.8(3) 11_556 . . 10_556 ? O6 O6 S1 O5 -109.5(3) 12_556 . . 10_556 ? O6 O6 S1 O5 118.5(3) 11_556 . . 10_556 ? O5 O6 S1 O5 180.0 . . . 10_556 ? O6 O5 S1 O6 74.43(15) 11_556 . . . ? O5 O5 S1 O6 -137.2(4) 2 . . . ? O5 O5 S1 O6 152.2(4) 3 . . . ? O6 O5 S1 O6 -72.65(16) 12_556 . . . ? O6 O5 S1 O6 -105.57(15) 11_556 . . 10_556 ? O5 O5 S1 O6 42.8(4) 2 . . 10_556 ? O5 O5 S1 O6 -27.8(4) 3 . . 10_556 ? O6 O5 S1 O6 107.35(16) 12_556 . . 10_556 ? O6 O5 S1 O6 180.0 . . . 10_556 ? O5 O5 S1 O6 148.4(4) 2 . . 11_556 ? O5 O5 S1 O6 77.8(4) 3 . . 11_556 ? O6 O5 S1 O6 -147.1(3) 12_556 . . 11_556 ? O6 O5 S1 O6 -74.43(15) . . . 11_556 ? O6 O5 S1 O6 180.0 11_556 . . 2 ? O5 O5 S1 O6 -31.6(4) 2 . . 2 ? O5 O5 S1 O6 -102.2(4) 3 . . 2 ? O6 O5 S1 O6 32.9(3) 12_556 . . 2 ? O6 O5 S1 O6 105.57(15) . . . 2 ? O6 O5 S1 O6 147.1(3) 11_556 . . 12_556 ? O5 O5 S1 O6 -64.5(4) 2 . . 12_556 ? O5 O5 S1 O6 -135.2(3) 3 . . 12_556 ? O6 O5 S1 O6 72.65(16) . . . 12_556 ? O6 O5 S1 O6 -32.9(3) 11_556 . . 3 ? O5 O5 S1 O6 115.5(4) 2 . . 3 ? O5 O5 S1 O6 44.8(3) 3 . . 3 ? O6 O5 S1 O6 180.0 12_556 . . 3 ? O6 O5 S1 O6 -107.35(16) . . . 3 ? O6 O5 S1 O5 31.6(4) 11_556 . . 11_556 ? O5 O5 S1 O5 180.0 2 . . 11_556 ? O5 O5 S1 O5 109.34(11) 3 . . 11_556 ? O6 O5 S1 O5 -115.5(4) 12_556 . . 11_556 ? O6 O5 S1 O5 -42.8(4) . . . 11_556 ? O6 O5 S1 O5 -148.4(4) 11_556 . . 2 ? O5 O5 S1 O5 -70.66(11) 3 . . 2 ? O6 O5 S1 O5 64.5(4) 12_556 . . 2 ? O6 O5 S1 O5 137.2(4) . . . 2 ? O6 O5 S1 O5 102.2(4) 11_556 . . 12_556 ? O5 O5 S1 O5 -109.34(11) 2 . . 12_556 ? O5 O5 S1 O5 180.0 3 . . 12_556 ? O6 O5 S1 O5 -44.8(3) 12_556 . . 12_556 ? O6 O5 S1 O5 27.8(4) . . . 12_556 ? O6 O5 S1 O5 -77.8(4) 11_556 . . 3 ? O5 O5 S1 O5 70.66(11) 2 . . 3 ? O6 O5 S1 O5 135.2(3) 12_556 . . 3 ? O6 O5 S1 O5 -152.2(4) . . . 3 ? O6 O5 S1 O5 -113.9(4) 11_556 . . 10_556 ? O5 O5 S1 O5 34.5(4) 2 . . 10_556 ? O5 O5 S1 O5 -36.2(3) 3 . . 10_556 ? O6 O5 S1 O5 99.0(3) 12_556 . . 10_556 ? O6 O5 S1 O5 171.6(3) . . . 10_556 ? N1 C1 C2 C3 1.1(3) . . . . ? N1 C1 C2 N2 179.16(16) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? N2 C2 C3 C4 -178.41(16) . . . . ? C2 C3 C4 C5 -0.3(3) . . . . ? C3 C4 C5 N1 0.3(3) . . . . ? C12 C7 C8 C9 0.1(3) . . . . ? N3 C7 C8 C9 -178.57(16) . . . . ? C7 C8 C9 C10 -0.4(3) . . . . ? C8 C9 C10 C11 0.2(3) . . . . ? C9 C10 C11 C12 0.3(3) . . . . ? C9 C10 C11 C16 179.07(16) . . . . ? C10 C11 C12 C13 -179.80(16) . . . . ? C16 C11 C12 C13 1.4(3) . . . . ? C10 C11 C12 C7 -0.6(3) . . . . ? C16 C11 C12 C7 -179.39(16) . . . . ? C8 C7 C12 C11 0.4(3) . . . . ? N3 C7 C12 C11 179.07(16) . . . . ? C8 C7 C12 C13 179.63(16) . . . . ? N3 C7 C12 C13 -1.7(3) . . . . ? C11 C12 C13 C14 -1.0(3) . . . . ? C7 C12 C13 C14 179.75(16) . . . . ? C12 C13 C14 C15 0.7(3) . . . . ? C13 C14 C15 C16 -0.8(3) . . . . ? C14 C15 C16 C11 1.1(3) . . . . ? C12 C11 C16 C15 -1.5(3) . . . . ? C10 C11 C16 C15 179.74(17) . . . . ? N4 C17 C18 C19 -0.1(3) . . . . ? N4 C17 C18 N5 178.97(15) . . . . ? C17 C18 C19 C20 0.3(3) . . . . ? N5 C18 C19 C20 -178.71(15) . . . . ? C18 C19 C20 C21 0.1(3) . . . . ? C19 C20 C21 N4 -0.7(3) . . . . ? N6 C23 C24 C25 172.62(16) . . . . ? C28 C23 C24 C25 0.0(3) . . . . ? C23 C24 C25 C26 -0.8(3) . . . . ? C24 C25 C26 C27 0.5(3) . . . . ? C25 C26 C27 C32 179.00(18) . . . . ? C25 C26 C27 C28 0.5(3) . . . . ? N6 C23 C28 C29 6.9(3) . . . . ? C24 C23 C28 C29 179.70(17) . . . . ? N6 C23 C28 C27 -171.74(17) . . . . ? C24 C23 C28 C27 1.1(3) . . . . ? C32 C27 C28 C29 1.6(3) . . . . ? C26 C27 C28 C29 -179.95(17) . . . . ? C32 C27 C28 C23 -179.76(18) . . . . ? C26 C27 C28 C23 -1.3(3) . . . . ? C23 C28 C29 C30 -179.67(18) . . . . ? C27 C28 C29 C30 -1.0(3) . . . . ? C28 C29 C30 C31 0.5(3) . . . . ? C29 C30 C31 C32 -0.5(3) . . . . ? C28 C27 C32 C31 -1.6(3) . . . . ? C26 C27 C32 C31 179.98(18) . . . . ? C30 C31 C32 C27 1.0(3) . . . . ? C4 C5 N1 C1 0.5(3) . . . . ? C4 C5 N1 Cu1 179.30(13) . . . . ? C2 C1 N1 C5 -1.2(3) . . . . ? C2 C1 N1 Cu1 -179.97(13) . . . . ? N1 Cu1 N1 C5 -119.6(4) 10 . . . ? N1 Cu1 N1 C5 -64.19(15) 12 . . . ? N1 Cu1 N1 C5 115.81(15) 3 . . . ? N1 Cu1 N1 C5 -147.18(14) 2 . . . ? N1 Cu1 N1 C5 32.82(14) 11 . . . ? N1 Cu1 N1 C1 59.2(4) 10 . . . ? N1 Cu1 N1 C1 114.61(11) 12 . . . ? N1 Cu1 N1 C1 -65.39(11) 3 . . . ? N1 Cu1 N1 C1 31.62(13) 2 . . . ? N1 Cu1 N1 C1 -148.38(13) 11 . . . ? O1 C6 N2 C2 -22.1(4) . . . . ? N3 C6 N2 C2 159.5(2) . . . . ? C3 C2 N2 C6 17.6(3) . . . . ? C1 C2 N2 C6 -160.5(2) . . . . ? O1 C6 N3 C7 20.1(3) . . . . ? N2 C6 N3 C7 -161.38(15) . . . . ? C8 C7 N3 C6 71.0(2) . . . . ? C12 C7 N3 C6 -107.6(2) . . . . ? C18 C17 N4 C21 -0.5(2) . . . . ? C18 C17 N4 Cu2 179.54(12) . . . . ? C20 C21 N4 C17 0.9(2) . . . . ? C20 C21 N4 Cu2 -179.16(12) . . . . ? O3 Cu2 N4 C17 -70.36(12) . . . . ? O3 Cu2 N4 C17 109.63(12) 16 . . . ? N4 Cu2 N4 C17 53.1(4) 16 . . . ? O3 Cu2 N4 C21 109.73(14) . . . . ? O3 Cu2 N4 C21 -70.28(14) 16 . . . ? N4 Cu2 N4 C21 -126.8(4) 16 . . . ? O2 C22 N5 C18 -0.7(3) . . . . ? N6 C22 N5 C18 -177.79(15) . . . . ? C19 C18 N5 C22 49.0(2) . . . . ? C17 C18 N5 C22 -129.98(17) . . . . ? C24 C23 N6 C22 39.8(2) . . . . ? C28 C23 N6 C22 -147.38(17) . . . . ? O2 C22 N6 C23 -5.6(3) . . . . ? N5 C22 N6 C23 171.36(14) . . . . ? O3 C33 N7 C34 152.56(17) . . . . ? O3 C33 N7 C35 -29.8(3) . . . . ? O4 C36 N8 C38 12.1(3) . . . . ? O4 C36 N8 C37 -176.89(15) . . . . ? N7 C33 O3 Cu2 179.61(12) . . . . ? O3 Cu2 O3 C33 -54(3) 16 . . . ? N4 Cu2 O3 C33 94.18(15) . . . . ? N4 Cu2 O3 C33 -85.81(15) 16 . . . ? O7 O10 S2 O10 -152(15) 16_556 . . 16_556 ? O9 O10 S2 O10 86(15) 16_556 . . 16_556 ? O8 O10 S2 O10 -29(15) 16_556 . . 16_556 ? O9 O10 S2 O7 -121.48(16) 16_556 . . 16_556 ? O8 O10 S2 O7 123.33(15) 16_556 . . 16_556 ? O7 O10 S2 O7 180.001(2) 16_556 . . . ? O9 O10 S2 O7 58.52(16) 16_556 . . . ? O8 O10 S2 O7 -56.67(15) 16_556 . . . ? O7 O10 S2 O8 -123.33(15) 16_556 . . 16_556 ? O9 O10 S2 O8 115.19(15) 16_556 . . 16_556 ? O7 O10 S2 O8 56.67(15) 16_556 . . . ? O9 O10 S2 O8 -64.81(15) 16_556 . . . ? O8 O10 S2 O8 180.001(1) 16_556 . . . ? O7 O10 S2 O9 -58.52(16) 16_556 . . . ? O9 O10 S2 O9 179.992(1) 16_556 . . . ? O8 O10 S2 O9 64.80(15) 16_556 . . . ? O7 O10 S2 O9 121.48(16) 16_556 . . 16_556 ? O8 O10 S2 O9 -115.19(15) 16_556 . . 16_556 ? O8 O7 S2 O10 -121.34(16) 16_556 . . 16_556 ? O9 O7 S2 O10 121.81(16) 16_556 . . 16_556 ? O10 O7 S2 O10 179.999(2) 16_556 . . . ? O8 O7 S2 O10 58.66(16) 16_556 . . . ? O9 O7 S2 O10 -58.19(16) 16_556 . . . ? O10 O7 S2 O7 170(12) 16_556 . . 16_556 ? O8 O7 S2 O7 49(12) 16_556 . . 16_556 ? O9 O7 S2 O7 -68(12) 16_556 . . 16_556 ? O10 O7 S2 O8 121.34(16) 16_556 . . 16_556 ? O9 O7 S2 O8 -116.85(17) 16_556 . . 16_556 ? O10 O7 S2 O8 -58.66(16) 16_556 . . . ? O8 O7 S2 O8 179.996(1) 16_556 . . . ? O9 O7 S2 O8 63.15(17) 16_556 . . . ? O10 O7 S2 O9 58.20(16) 16_556 . . . ? O8 O7 S2 O9 -63.14(17) 16_556 . . . ? O9 O7 S2 O9 -180.0 16_556 . . . ? O10 O7 S2 O9 -121.81(16) 16_556 . . 16_556 ? O8 O7 S2 O9 116.85(17) 16_556 . . 16_556 ? O7 O8 S2 O10 123.83(15) 16_556 . . 16_556 ? O9 O8 S2 O10 -117.51(16) 16_556 . . 16_556 ? O7 O8 S2 O10 -56.17(15) 16_556 . . . ? O10 O8 S2 O10 179.999(1) 16_556 . . . ? O9 O8 S2 O10 62.49(16) 16_556 . . . ? O10 O8 S2 O7 -123.83(15) 16_556 . . 16_556 ? O9 O8 S2 O7 118.66(16) 16_556 . . 16_556 ? O7 O8 S2 O7 180.003(1) 16_556 . . . ? O10 O8 S2 O7 56.17(16) 16_556 . . . ? O9 O8 S2 O7 -61.34(16) 16_556 . . . ? O7 O8 S2 O8 -71(9) 16_556 . . 16_556 ? O10 O8 S2 O8 165(9) 16_556 . . 16_556 ? O9 O8 S2 O8 48(9) 16_556 . . 16_556 ? O7 O8 S2 O9 61.34(16) 16_556 . . . ? O10 O8 S2 O9 -62.49(16) 16_556 . . . ? O9 O8 S2 O9 180.0 16_556 . . . ? O7 O8 S2 O9 -118.66(16) 16_556 . . 16_556 ? O10 O8 S2 O9 117.51(16) 16_556 . . 16_556 ? O7 O9 S2 O10 -123.40(17) 16_556 . . 16_556 ? O8 O9 S2 O10 116.38(17) 16_556 . . 16_556 ? O10 O9 S2 O10 180.0 16_556 . . . ? O7 O9 S2 O10 56.61(17) 16_556 . . . ? O8 O9 S2 O10 -63.61(17) 16_556 . . . ? O10 O9 S2 O7 123.40(17) 16_556 . . 16_556 ? O8 O9 S2 O7 -120.22(17) 16_556 . . 16_556 ? O10 O9 S2 O7 -56.61(17) 16_556 . . . ? O7 O9 S2 O7 180.0 16_556 . . . ? O8 O9 S2 O7 59.78(17) 16_556 . . . ? O10 O9 S2 O8 -116.38(17) 16_556 . . 16_556 ? O7 O9 S2 O8 120.22(17) 16_556 . . 16_556 ? O10 O9 S2 O8 63.62(17) 16_556 . . . ? O7 O9 S2 O8 -59.78(17) 16_556 . . . ? O8 O9 S2 O8 180.0 16_556 . . . ? O10 O9 S2 O9 -104(5) 16_556 . . 16_556 ? O7 O9 S2 O9 132(5) 16_556 . . 16_556 ? O8 O9 S2 O9 12(5) 16_556 . . 16_556 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.237 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.034