_publ_requested_journal 'Inorganic Chemistry' _publ_contact_author_name 'Shim Sung Lee' _publ_contact_author_address ; Department of Chemistry (BK21) and Research Institute of Natural Science, Gyeongsang National University, Jinju 660-701, South Korea ; _publ_contact_author_email sslee@gnu.ac.kr _publ_contact_author_phone +82-55-751-6021 _publ_contact_author_fax +82-55-753-7614 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Lee, Jai Young' ; Department of Chemistry (BK21) and Research Institute of Natural Science, Gyeongsang National University, Jinju 660-701, South Korea, Department of Chemistry, Konyang University, Nonsan 320-711, S. Korea ; . 'Lee, So Young' ; Department of Chemistry (BK21) and Research Institute of Natural Science, Gyeongsang National University, Jinju 660-701, South Korea ; . 'Park, Sunhong' ; Department of Chemistry (BK21) and Research Institute of Natural Science, Gyeongsang National University, Jinju 660-701, South Korea ; . 'Kwon, Jongchul' ; Department of Chemistry, Konyang University, Nonsan 320-711, S. Korea ; . 'Sim, Wonbo' ; Department of Chemistry, Konyang University, Nonsan 320-711, S. Korea ; . 'Lee, Shim Sung ' ; Department of Chemistry (BK21) and Research Institute of Natural Science, Gyeongsang National University, Jinju 660-701, South Korea ; 'The author to whom correspondence should be addressed' data_L1 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H52 O9 S' _chemical_formula_weight 756.92 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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.9237(7) _cell_length_b 11.0439(6) _cell_length_c 29.8966(17) _cell_angle_alpha 90.00 _cell_angle_beta 100.3600(10) _cell_angle_gamma 90.00 _cell_volume 3872.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2621 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 24.26 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 0.141 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9458 _exptl_absorpt_correction_T_max 0.9861 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21659 _diffrn_reflns_av_R_equivalents 0.1120 _diffrn_reflns_av_sigmaI/netI 0.1695 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7586 _reflns_number_gt 3455 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.1209P)^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 7586 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1902 _refine_ls_R_factor_gt 0.0811 _refine_ls_wR_factor_ref 0.2511 _refine_ls_wR_factor_gt 0.1861 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 S1 S -0.02997(14) 0.36177(14) 0.04865(5) 0.0375(4) Uani 1 1 d . . . O1 O 0.4015(3) 0.6116(3) 0.06532(11) 0.0248(9) Uani 1 1 d . . . O2 O 0.2325(3) 0.4208(3) 0.04438(13) 0.0318(10) Uani 1 1 d . . . O3 O 0.0304(3) 0.6500(3) 0.13300(13) 0.0310(10) Uani 1 1 d . . . O4 O 0.3021(3) 0.7909(3) 0.16882(11) 0.0201(8) Uani 1 1 d . . . O5 O 0.4452(3) 0.9640(3) 0.10671(11) 0.0192(8) Uani 1 1 d . . . O6 O 0.6629(3) 1.1814(3) 0.10384(12) 0.0315(10) Uani 1 1 d . . . O7 O 0.8487(3) 1.0382(3) 0.16867(12) 0.0306(10) Uani 1 1 d . . . O8 O 0.8220(4) 0.7896(4) 0.20215(13) 0.0415(11) Uani 1 1 d . . . O9 O 0.5877(4) 0.6870(3) 0.19495(13) 0.0334(10) Uani 1 1 d . . . C1 C 0.3516(5) 0.5699(5) 0.02046(17) 0.0296(14) Uani 1 1 d . . . H1A H 0.4059 0.5842 -0.0005 0.036 Uiso 1 1 calc R . . H1B H 0.2816 0.6169 0.0092 0.036 Uiso 1 1 calc R . . C2 C 0.3229(5) 0.4383(5) 0.02035(19) 0.0340(15) Uani 1 1 d . . . H2A H 0.3001 0.4094 -0.0113 0.041 Uiso 1 1 calc R . . H2B H 0.3904 0.3915 0.0349 0.041 Uiso 1 1 calc R . . C3 C 0.1945(5) 0.2990(5) 0.0419(2) 0.0338(15) Uani 1 1 d . . . H3A H 0.2589 0.2443 0.0535 0.041 Uiso 1 1 calc R . . H3B H 0.1641 0.2770 0.0100 0.041 Uiso 1 1 calc R . . C4 C 0.1018(5) 0.2858(5) 0.0705(2) 0.0378(16) Uani 1 1 d . . . H4A H 0.1314 0.3173 0.1013 0.045 Uiso 1 1 calc R . . H4B H 0.0857 0.1985 0.0734 0.045 Uiso 1 1 calc R . . C5 C -0.0007(5) 0.5155(5) 0.06698(18) 0.0302(14) Uani 1 1 d . . . H5A H 0.0744 0.5399 0.0602 0.036 Uiso 1 1 calc R . . H5B H -0.0591 0.5694 0.0495 0.036 Uiso 1 1 calc R . . C6 C -0.0002(5) 0.5318(5) 0.11668(18) 0.0312(14) Uani 1 1 d . . . H6A H -0.0771 0.5127 0.1229 0.037 Uiso 1 1 calc R . . H6B H 0.0539 0.4731 0.1338 0.037 Uiso 1 1 calc R . . C7 C 0.1481(4) 0.6748(5) 0.13341(19) 0.0265(13) Uani 1 1 d . . . H7A H 0.1581 0.7116 0.1042 0.032 Uiso 1 1 calc R . . H7B H 0.1929 0.5989 0.1378 0.032 Uiso 1 1 calc R . . C8 C 0.1882(5) 0.7612(5) 0.17214(18) 0.0259(13) Uani 1 1 d . . . H8A H 0.1400 0.8348 0.1692 0.031 Uiso 1 1 calc R . . H8B H 0.1852 0.7222 0.2017 0.031 Uiso 1 1 calc R . . C9 C 0.3557(4) 0.8733(4) 0.20003(17) 0.0207(12) Uani 1 1 d . . . C10 C 0.3471(4) 0.9966(4) 0.18910(16) 0.0181(12) Uani 1 1 d . . . C11 C 0.4120(5) 1.0781(5) 0.21864(18) 0.0270(13) Uani 1 1 d . . . H11A H 0.4083 1.1621 0.2117 0.032 Uiso 1 1 calc R . . C12 C 0.4818(5) 1.0381(5) 0.25795(18) 0.0287(14) Uani 1 1 d . . . H12A H 0.5260 1.0944 0.2777 0.034 Uiso 1 1 calc R . . C13 C 0.4872(5) 0.9162(5) 0.26835(17) 0.0280(13) Uani 1 1 d . . . H13A H 0.5351 0.8895 0.2955 0.034 Uiso 1 1 calc R . . C14 C 0.4239(5) 0.8317(5) 0.23995(16) 0.0213(12) Uani 1 1 d . . . C15 C 0.4271(5) 0.6997(5) 0.25482(17) 0.0299(14) Uani 1 1 d . . . H15A H 0.4974 0.6879 0.2777 0.036 Uiso 1 1 calc R . . H15B H 0.3619 0.6864 0.2706 0.036 Uiso 1 1 calc R . . C16 C 0.4236(5) 0.6013(5) 0.21955(17) 0.0227(13) Uani 1 1 d . . . C17 C 0.3423(5) 0.5096(4) 0.21638(17) 0.0238(13) Uani 1 1 d . . . H17A H 0.2883 0.5099 0.2362 0.029 Uiso 1 1 calc R . . C18 C 0.3395(5) 0.4183(5) 0.18455(19) 0.0313(14) Uani 1 1 d . . . H18A H 0.2848 0.3552 0.1830 0.038 Uiso 1 1 calc R . . C19 C 0.4156(5) 0.4187(5) 0.15527(18) 0.0294(14) Uani 1 1 d . . . H19A H 0.4113 0.3568 0.1330 0.035 Uiso 1 1 calc R . . C20 C 0.4989(5) 0.5073(5) 0.15740(17) 0.0271(14) Uani 1 1 d . . . C21 C 0.5029(5) 0.5981(4) 0.19018(17) 0.0246(13) Uani 1 1 d . . . C22 C 0.5833(5) 0.5040(5) 0.12451(19) 0.0345(15) Uani 1 1 d . . . H22A H 0.6590 0.4812 0.1419 0.041 Uiso 1 1 calc R . . H22B H 0.5594 0.4390 0.1020 0.041 Uiso 1 1 calc R . . C23 C 0.5969(5) 0.6195(5) 0.09887(17) 0.0270(14) Uani 1 1 d . . . C24 C 0.7034(5) 0.6771(5) 0.10336(19) 0.0321(15) Uani 1 1 d . . . H24A H 0.7670 0.6452 0.1237 0.038 Uiso 1 1 calc R . . C25 C 0.7162(5) 0.7790(5) 0.07862(18) 0.0295(14) Uani 1 1 d . . . H25A H 0.7892 0.8155 0.0808 0.035 Uiso 1 1 calc R . . C26 C 0.6236(5) 0.8282(5) 0.05068(17) 0.0271(14) Uani 1 1 d . . . H26A H 0.6337 0.8986 0.0335 0.033 Uiso 1 1 calc R . . C27 C 0.5153(5) 0.7779(5) 0.04675(16) 0.0221(12) Uani 1 1 d . . . C28 C 0.5058(4) 0.6703(4) 0.06930(16) 0.0197(12) Uani 1 1 d . . . C29 C 0.4147(5) 0.8446(5) 0.01851(16) 0.0249(13) Uani 1 1 d . . . H29A H 0.4446 0.9183 0.0059 0.030 Uiso 1 1 calc R . . H29B H 0.3826 0.7922 -0.0075 0.030 Uiso 1 1 calc R . . C30 C 0.3183(4) 0.8822(4) 0.04188(16) 0.0190(12) Uani 1 1 d . . . C31 C 0.2049(5) 0.8642(5) 0.01988(18) 0.0286(14) Uani 1 1 d . . . H31A H 0.1906 0.8259 -0.0090 0.034 Uiso 1 1 calc R . . C32 C 0.1155(5) 0.9004(5) 0.03910(19) 0.0315(14) Uani 1 1 d . . . H32A H 0.0397 0.8856 0.0240 0.038 Uiso 1 1 calc R . . C33 C 0.1350(5) 0.9589(5) 0.08077(18) 0.0265(13) Uani 1 1 d . . . H33A H 0.0722 0.9853 0.0938 0.032 Uiso 1 1 calc R . . C34 C 0.2458(5) 0.9792(4) 0.10372(17) 0.0209(12) Uani 1 1 d . . . C35 C 0.3345(4) 0.9425(4) 0.08313(16) 0.0176(12) Uani 1 1 d . . . C36 C 0.2647(5) 1.0466(5) 0.14844(16) 0.0236(13) Uani 1 1 d . . . H36A H 0.1895 1.0553 0.1577 0.028 Uiso 1 1 calc R . . H36B H 0.2909 1.1292 0.1425 0.028 Uiso 1 1 calc R . . C37 C 0.4917(4) 1.0756(5) 0.09572(17) 0.0234(13) Uani 1 1 d . . . H37A H 0.4415 1.1432 0.1015 0.028 Uiso 1 1 calc R . . H37B H 0.4980 1.0769 0.0632 0.028 Uiso 1 1 calc R . . C38 C 0.6061(4) 1.0897(5) 0.12442(17) 0.0229(12) Uani 1 1 d . . . H38A H 0.5991 1.1134 0.1557 0.027 Uiso 1 1 calc R . . H38B H 0.6490 1.0126 0.1258 0.027 Uiso 1 1 calc R . . C39 C 0.7714(5) 1.2138(5) 0.1281(2) 0.0340(15) Uani 1 1 d . . . H39A H 0.7631 1.2388 0.1591 0.041 Uiso 1 1 calc R . . H39B H 0.7988 1.2850 0.1130 0.041 Uiso 1 1 calc R . . C40 C 0.8600(5) 1.1176(5) 0.13196(18) 0.0320(14) Uani 1 1 d . . . H40A H 0.8511 1.0711 0.1032 0.038 Uiso 1 1 calc R . . H40B H 0.9367 1.1548 0.1375 0.038 Uiso 1 1 calc R . . C41 C 0.9309(5) 0.9450(5) 0.17524(19) 0.0298(14) Uani 1 1 d . . . H41A H 1.0083 0.9806 0.1806 0.036 Uiso 1 1 calc R . . H41B H 0.9225 0.8938 0.1477 0.036 Uiso 1 1 calc R . . C42 C 0.9158(5) 0.8701(5) 0.21479(19) 0.0305(14) Uani 1 1 d . . . H42A H 0.9862 0.8231 0.2256 0.037 Uiso 1 1 calc R . . H42B H 0.9017 0.9231 0.2399 0.037 Uiso 1 1 calc R . . C43 C 0.7692(7) 0.7609(7) 0.2375(2) 0.060(2) Uani 1 1 d . . . H43A H 0.7251 0.8316 0.2451 0.072 Uiso 1 1 calc R . . H43B H 0.8272 0.7409 0.2646 0.072 Uiso 1 1 calc R . . C44 C 0.6902(5) 0.6545(6) 0.2257(2) 0.0483(18) Uani 1 1 d . . . H44A H 0.7304 0.5904 0.2116 0.058 Uiso 1 1 calc R . . H44B H 0.6700 0.6210 0.2539 0.058 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0309(9) 0.0401(9) 0.0409(9) -0.0092(8) 0.0051(7) -0.0138(8) O1 0.028(2) 0.031(2) 0.0178(18) -0.0043(16) 0.0101(16) -0.0096(18) O2 0.029(2) 0.027(2) 0.044(2) -0.0074(19) 0.018(2) -0.0069(18) O3 0.023(2) 0.023(2) 0.048(2) -0.0081(19) 0.0074(19) 0.0015(18) O4 0.024(2) 0.0161(18) 0.0198(18) -0.0022(15) 0.0021(16) -0.0024(16) O5 0.019(2) 0.0192(19) 0.0193(18) 0.0016(15) 0.0042(16) 0.0024(16) O6 0.023(2) 0.034(2) 0.035(2) 0.0116(18) -0.0017(18) -0.0100(18) O7 0.019(2) 0.036(2) 0.037(2) 0.0021(19) 0.0078(18) 0.0015(18) O8 0.045(3) 0.044(3) 0.040(2) -0.014(2) 0.018(2) -0.026(2) O9 0.053(3) 0.017(2) 0.038(2) -0.0032(17) 0.029(2) -0.0088(19) C1 0.033(4) 0.035(3) 0.022(3) -0.005(3) 0.009(3) -0.011(3) C2 0.030(4) 0.040(4) 0.035(3) -0.012(3) 0.014(3) -0.013(3) C3 0.037(4) 0.018(3) 0.047(4) -0.002(3) 0.010(3) -0.001(3) C4 0.047(4) 0.027(3) 0.043(4) 0.005(3) 0.017(3) 0.002(3) C5 0.028(3) 0.030(3) 0.031(3) 0.001(3) 0.001(3) -0.003(3) C6 0.029(3) 0.031(3) 0.035(3) -0.001(3) 0.008(3) -0.003(3) C7 0.020(3) 0.021(3) 0.038(3) -0.005(3) 0.003(3) -0.002(2) C8 0.024(3) 0.020(3) 0.035(3) -0.002(2) 0.009(3) 0.000(2) C9 0.024(3) 0.019(3) 0.023(3) -0.003(2) 0.014(2) -0.002(2) C10 0.019(3) 0.015(3) 0.024(3) -0.001(2) 0.015(2) 0.002(2) C11 0.037(4) 0.016(3) 0.030(3) -0.005(2) 0.011(3) -0.003(3) C12 0.036(4) 0.021(3) 0.029(3) -0.006(2) 0.004(3) -0.002(3) C13 0.034(4) 0.032(3) 0.018(3) -0.004(2) 0.004(3) 0.004(3) C14 0.031(3) 0.020(3) 0.015(3) 0.000(2) 0.010(2) 0.003(2) C15 0.047(4) 0.021(3) 0.025(3) -0.002(2) 0.016(3) 0.003(3) C16 0.030(3) 0.017(3) 0.021(3) 0.003(2) 0.004(3) 0.005(2) C17 0.029(3) 0.018(3) 0.025(3) 0.010(2) 0.005(3) 0.007(2) C18 0.032(4) 0.018(3) 0.040(3) 0.007(3) -0.006(3) 0.001(3) C19 0.042(4) 0.018(3) 0.026(3) -0.005(2) 0.000(3) 0.003(3) C20 0.047(4) 0.015(3) 0.018(3) 0.001(2) 0.004(3) 0.012(3) C21 0.036(4) 0.013(3) 0.027(3) 0.002(2) 0.011(3) -0.001(2) C22 0.048(4) 0.029(3) 0.028(3) 0.003(3) 0.012(3) 0.017(3) C23 0.039(4) 0.024(3) 0.020(3) -0.009(2) 0.011(3) 0.007(3) C24 0.027(3) 0.039(4) 0.030(3) -0.012(3) 0.004(3) 0.009(3) C25 0.025(3) 0.037(4) 0.029(3) -0.014(3) 0.012(3) -0.006(3) C26 0.042(4) 0.023(3) 0.020(3) -0.010(2) 0.015(3) -0.002(3) C27 0.026(3) 0.024(3) 0.019(3) -0.010(2) 0.008(2) 0.000(2) C28 0.024(3) 0.018(3) 0.019(3) -0.005(2) 0.011(2) -0.005(2) C29 0.038(4) 0.023(3) 0.014(3) 0.004(2) 0.005(2) -0.008(3) C30 0.025(3) 0.016(3) 0.015(2) 0.005(2) 0.000(2) 0.000(2) C31 0.031(4) 0.026(3) 0.025(3) -0.002(3) -0.002(3) -0.007(3) C32 0.020(3) 0.031(3) 0.039(3) 0.005(3) -0.008(3) -0.006(3) C33 0.018(3) 0.025(3) 0.036(3) 0.007(3) 0.003(3) 0.005(2) C34 0.027(3) 0.013(3) 0.024(3) 0.008(2) 0.007(3) 0.000(2) C35 0.018(3) 0.015(3) 0.019(3) 0.003(2) -0.002(2) -0.003(2) C36 0.028(3) 0.019(3) 0.026(3) -0.004(2) 0.009(3) 0.000(2) C37 0.021(3) 0.019(3) 0.030(3) 0.000(2) 0.005(3) -0.003(2) C38 0.023(3) 0.026(3) 0.019(3) 0.000(2) 0.000(2) -0.004(2) C39 0.025(3) 0.035(4) 0.042(4) 0.006(3) 0.006(3) -0.007(3) C40 0.031(4) 0.039(4) 0.029(3) 0.002(3) 0.012(3) -0.009(3) C41 0.020(3) 0.028(3) 0.040(3) -0.006(3) 0.001(3) 0.000(3) C42 0.022(3) 0.024(3) 0.044(4) -0.002(3) 0.001(3) -0.009(3) C43 0.069(6) 0.065(5) 0.052(4) -0.013(4) 0.027(4) -0.025(4) C44 0.034(4) 0.060(5) 0.052(4) -0.003(4) 0.011(3) -0.023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C4 1.797(6) . ? S1 C5 1.799(6) . ? O1 C28 1.389(6) . ? O1 C1 1.441(6) . ? O2 C2 1.412(6) . ? O2 C3 1.417(6) . ? O3 C6 1.418(6) . ? O3 C7 1.428(6) . ? O4 C9 1.375(6) . ? O4 C8 1.418(6) . ? O5 C35 1.400(6) . ? O5 C37 1.414(6) . ? O6 C39 1.410(6) . ? O6 C38 1.419(6) . ? O7 C41 1.411(6) . ? O7 C40 1.430(6) . ? O8 C43 1.362(7) . ? O8 C42 1.426(6) . ? O9 C21 1.397(6) . ? O9 C44 1.437(7) . ? C1 C2 1.492(8) . ? C3 C4 1.520(8) . ? C5 C6 1.496(8) . ? C7 C8 1.510(7) . ? C9 C14 1.395(7) . ? C9 C10 1.400(7) . ? C10 C11 1.394(7) . ? C10 C36 1.523(7) . ? C11 C12 1.385(7) . ? C12 C13 1.381(7) . ? C13 C14 1.389(7) . ? C14 C15 1.523(7) . ? C15 C16 1.509(7) . ? C16 C17 1.394(7) . ? C16 C21 1.402(7) . ? C17 C18 1.383(7) . ? C18 C19 1.370(8) . ? C19 C20 1.387(8) . ? C20 C21 1.397(7) . ? C20 C22 1.529(8) . ? C22 C23 1.511(7) . ? C23 C28 1.389(7) . ? C23 C24 1.405(8) . ? C24 C25 1.370(8) . ? C25 C26 1.371(8) . ? C26 C27 1.392(7) . ? C27 C28 1.381(7) . ? C27 C29 1.526(7) . ? C29 C30 1.507(7) . ? C30 C35 1.384(7) . ? C30 C31 1.407(7) . ? C31 C32 1.359(8) . ? C32 C33 1.385(7) . ? C33 C34 1.393(7) . ? C34 C35 1.378(7) . ? C34 C36 1.511(7) . ? C37 C38 1.484(7) . ? C39 C40 1.488(8) . ? C41 C42 1.480(7) . ? C43 C44 1.508(9) . ? 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 C4 S1 C5 102.8(3) . . ? C28 O1 C1 116.2(4) . . ? C2 O2 C3 111.7(4) . . ? C6 O3 C7 111.8(4) . . ? C9 O4 C8 116.1(4) . . ? C35 O5 C37 113.8(4) . . ? C39 O6 C38 115.0(4) . . ? C41 O7 C40 113.3(4) . . ? C43 O8 C42 112.9(5) . . ? C21 O9 C44 114.0(4) . . ? O1 C1 C2 111.7(4) . . ? O2 C2 C1 109.2(5) . . ? O2 C3 C4 108.7(5) . . ? C3 C4 S1 115.4(4) . . ? C6 C5 S1 112.5(4) . . ? O3 C6 C5 114.0(5) . . ? O3 C7 C8 107.6(4) . . ? O4 C8 C7 105.5(4) . . ? O4 C9 C14 119.4(4) . . ? O4 C9 C10 118.6(4) . . ? C14 C9 C10 121.8(5) . . ? C11 C10 C9 118.1(5) . . ? C11 C10 C36 118.5(4) . . ? C9 C10 C36 123.3(5) . . ? C12 C11 C10 120.8(5) . . ? C13 C12 C11 119.9(5) . . ? C12 C13 C14 121.3(5) . . ? C13 C14 C9 118.1(5) . . ? C13 C14 C15 118.8(5) . . ? C9 C14 C15 123.0(5) . . ? C16 C15 C14 119.3(4) . . ? C17 C16 C21 118.6(5) . . ? C17 C16 C15 120.1(5) . . ? C21 C16 C15 121.3(5) . . ? C18 C17 C16 120.4(5) . . ? C19 C18 C17 120.1(5) . . ? C18 C19 C20 121.6(5) . . ? C19 C20 C21 118.2(5) . . ? C19 C20 C22 120.1(5) . . ? C21 C20 C22 121.7(5) . . ? C20 C21 O9 120.6(5) . . ? C20 C21 C16 121.0(5) . . ? O9 C21 C16 118.4(4) . . ? C23 C22 C20 116.7(4) . . ? C28 C23 C24 117.9(5) . . ? C28 C23 C22 121.4(5) . . ? C24 C23 C22 120.7(5) . . ? C25 C24 C23 120.5(5) . . ? C24 C25 C26 119.9(6) . . ? C25 C26 C27 121.8(5) . . ? C28 C27 C26 117.3(5) . . ? C28 C27 C29 124.1(5) . . ? C26 C27 C29 118.6(5) . . ? C27 C28 O1 120.7(5) . . ? C27 C28 C23 122.4(5) . . ? O1 C28 C23 116.8(5) . . ? C30 C29 C27 117.7(4) . . ? C35 C30 C31 116.9(5) . . ? C35 C30 C29 123.3(5) . . ? C31 C30 C29 119.6(5) . . ? C32 C31 C30 121.4(5) . . ? C31 C32 C33 120.0(5) . . ? C32 C33 C34 120.6(5) . . ? C35 C34 C33 118.0(5) . . ? C35 C34 C36 122.4(5) . . ? C33 C34 C36 119.5(5) . . ? C34 C35 C30 123.0(5) . . ? C34 C35 O5 117.1(4) . . ? C30 C35 O5 119.9(5) . . ? C34 C36 C10 120.0(4) . . ? O5 C37 C38 108.3(4) . . ? O6 C38 C37 106.5(4) . . ? O6 C39 C40 115.6(5) . . ? O7 C40 C39 109.5(5) . . ? O7 C41 C42 109.7(5) . . ? O8 C42 C41 109.8(5) . . ? O8 C43 C44 110.8(5) . . ? O9 C44 C43 112.3(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.756 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.085 #=====================================================END data_1 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H104 Cu11 I15 K4 N3 O18 S2' _chemical_formula_weight 4386.76 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' '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' 'I' 'I' -0.4742 1.8119 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.6363(13) _cell_length_b 19.3555(12) _cell_length_c 29.7445(18) _cell_angle_alpha 90.00 _cell_angle_beta 97.8050(10) _cell_angle_gamma 90.00 _cell_volume 12911.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6812 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.33 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8220 _exptl_absorpt_coefficient_mu 5.576 _exptl_absorpt_correction_type 'empirical (SADABS)' _exptl_absorpt_correction_T_min 0.2855 _exptl_absorpt_correction_T_max 0.6055 _exptl_absorpt_process_details 'SADABS, sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37348 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.1004 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 27.00 _reflns_number_total 14058 _reflns_number_gt 8021 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.1517P)^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 14058 _refine_ls_number_parameters 668 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1316 _refine_ls_R_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.2618 _refine_ls_wR_factor_gt 0.2161 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.018 _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 Cu1 Cu 0.08033(7) 0.86216(9) 0.53024(6) 0.0417(4) Uani 1 1 d . . . Cu2 Cu 0.03073(8) 0.77852(10) 0.45795(6) 0.0485(5) Uani 1 1 d . . . Cu3 Cu 0.08631(9) 0.65830(10) 0.48816(7) 0.0557(5) Uani 1 1 d . . . Cu4 Cu 0.07015(18) 0.5925(2) 0.55949(15) 0.0623(11) Uani 0.50 1 d P . . Cu5 Cu 0.10400(19) 0.5387(2) 0.45961(16) 0.0646(12) Uani 0.50 1 d P . . Cu6 Cu 0.03254(16) 0.44903(19) 0.41689(13) 0.0475(9) Uani 0.50 1 d P . . Cu7 Cu -0.00206(8) 1.07302(9) 0.52866(6) 0.0455(4) Uani 1 1 d . . . K1 K 0.21916(13) 0.86754(13) 0.68282(9) 0.0352(6) Uani 1 1 d . . . K2 K 0.22856(13) 0.84154(14) 0.85871(10) 0.0370(6) Uani 1 1 d . . . I1 I 0.11005(4) 0.88038(5) 0.44857(3) 0.0415(2) Uani 1 1 d . . . I2 I -0.07534(4) 0.83466(5) 0.43889(3) 0.0422(2) Uani 1 1 d . . . I3 I 0.03863(4) 0.73345(4) 0.54513(3) 0.0407(2) Uani 1 1 d . . . I4 I 0.05085(5) 0.67115(6) 0.40438(4) 0.0596(3) Uani 1 1 d . . . I5 I 0.17568(5) 0.58875(5) 0.52552(4) 0.0529(3) Uani 1 1 d . . . I6 I 0.00797(15) 0.48737(16) 0.49532(12) 0.0520(7) Uani 0.50 1 d P . . I7 I 0.14177(8) 0.44833(9) 0.40642(6) 0.0417(4) Uani 0.50 1 d P . . I8 I -0.05078(10) 0.41357(11) 0.35643(7) 0.0550(5) Uani 0.50 1 d P . . I9 I 0.00369(4) 0.94623(4) 0.56198(3) 0.0374(2) Uani 1 1 d . . . S1 S 0.17113(15) 0.86189(17) 0.57685(11) 0.0366(7) Uani 1 1 d . . . O1 O 0.2493(4) 0.7419(4) 0.7139(3) 0.038(2) Uani 1 1 d . . . O2 O 0.2714(5) 0.7711(5) 0.6271(3) 0.057(3) Uani 1 1 d . . . O3 O 0.1934(4) 0.9911(5) 0.6375(3) 0.042(2) Uani 1 1 d . . . O4 O 0.1858(4) 0.9763(4) 0.7307(3) 0.0312(18) Uani 1 1 d . . . O5 O 0.3311(4) 0.8815(4) 0.8216(3) 0.0341(19) Uani 1 1 d . . . O6 O 0.3327(5) 0.8803(7) 0.9141(4) 0.067(3) Uani 1 1 d . . . O7 O 0.2327(5) 0.8343(6) 0.9512(4) 0.061(3) Uani 1 1 d . . . O8 O 0.1276(5) 0.8074(7) 0.8969(4) 0.069(3) Uani 1 1 d . . . O9 O 0.1219(4) 0.8079(4) 0.8023(3) 0.0320(19) Uani 1 1 d . . . C1 C 0.2701(8) 0.6868(7) 0.6857(5) 0.053(4) Uani 1 1 d . . . H1A H 0.2518 0.6422 0.6923 0.064 Uiso 1 1 calc R . . H1B H 0.3140 0.6820 0.6923 0.064 Uiso 1 1 calc R . . C2 C 0.2525(9) 0.7059(8) 0.6372(5) 0.064(5) Uani 1 1 d . . . H2A H 0.2694 0.6718 0.6178 0.077 Uiso 1 1 calc R . . H2B H 0.2085 0.7038 0.6301 0.077 Uiso 1 1 calc R . . C3 C 0.2746(6) 0.7843(8) 0.5797(4) 0.044(3) Uani 1 1 d . . . H3A H 0.2941 0.7445 0.5668 0.053 Uiso 1 1 calc R . . H3B H 0.2998 0.8255 0.5771 0.053 Uiso 1 1 calc R . . C4 C 0.2153(8) 0.7958(11) 0.5527(5) 0.069(4) Uani 1 1 d . . . H4A H 0.1929 0.7518 0.5505 0.082 Uiso 1 1 calc R . . H4B H 0.2210 0.8098 0.5215 0.082 Uiso 1 1 calc R . . C5 C 0.2102(8) 0.9391(9) 0.5669(6) 0.069(3) Uani 1 1 d . . . H5A H 0.2527 0.9342 0.5797 0.083 Uiso 1 1 calc R . . H5B H 0.2080 0.9471 0.5339 0.083 Uiso 1 1 calc R . . C6 C 0.1832(6) 1.0009(7) 0.5889(4) 0.042(3) Uani 1 1 d . . . H6A H 0.2023 1.0443 0.5807 0.050 Uiso 1 1 calc R . . H6B H 0.1399 1.0038 0.5783 0.050 Uiso 1 1 calc R . . C7 C 0.1526(6) 1.0313(7) 0.6596(4) 0.037(3) Uani 1 1 d . . . H7A H 0.1139 1.0070 0.6577 0.044 Uiso 1 1 calc R . . H7B H 0.1457 1.0764 0.6441 0.044 Uiso 1 1 calc R . . C8 C 0.1774(6) 1.0428(6) 0.7085(4) 0.038(3) Uani 1 1 d . . . H8A H 0.2159 1.0676 0.7106 0.045 Uiso 1 1 calc R . . H8B H 0.1494 1.0713 0.7236 0.045 Uiso 1 1 calc R . . C9 C 0.1888(6) 0.9802(6) 0.7769(4) 0.034(3) Uani 1 1 d . . . C10 C 0.2427(5) 1.0012(6) 0.8037(4) 0.029(3) Uani 1 1 d . . . C11 C 0.2429(6) 1.0100(6) 0.8507(4) 0.037(3) Uani 1 1 d . . . H11A H 0.2776 1.0334 0.8688 0.044 Uiso 1 1 calc R . . C12 C 0.1925(6) 0.9976(6) 0.8703(4) 0.041(3) Uani 1 1 d . . . H12A H 0.1903 1.0158 0.9015 0.049 Uiso 1 1 calc R . . C13 C 0.1409(6) 0.9734(6) 0.8447(4) 0.035(3) Uani 1 1 d . . . H13A H 0.1028 0.9729 0.8583 0.042 Uiso 1 1 calc R . . C14 C 0.1389(6) 0.9650(6) 0.7970(4) 0.032(3) Uani 1 1 d . . . C15 C 0.0814(5) 0.9417(6) 0.7686(4) 0.033(3) Uani 1 1 d . . . H15A H 0.0520 0.9305 0.7893 0.039 Uiso 1 1 calc R . . H15B H 0.0653 0.9809 0.7493 0.039 Uiso 1 1 calc R . . C16 C 0.0870(5) 0.8801(6) 0.7384(4) 0.031(3) Uani 1 1 d . . . C17 C 0.0702(5) 0.8844(6) 0.6919(4) 0.033(3) Uani 1 1 d . . . H17A H 0.0482 0.9262 0.6789 0.040 Uiso 1 1 calc R . . C18 C 0.0760(5) 0.8283(7) 0.6642(5) 0.036(3) Uani 1 1 d . . . H18A H 0.0551 0.8291 0.6323 0.043 Uiso 1 1 calc R . . C19 C 0.1024(6) 0.7683(7) 0.6809(5) 0.039(3) Uani 1 1 d . . . H19A H 0.0992 0.7263 0.6611 0.047 Uiso 1 1 calc R . . C20 C 0.1183(6) 0.7604(7) 0.7270(4) 0.037(3) Uani 1 1 d . . . C21 C 0.1087(6) 0.8150(7) 0.7551(4) 0.034(3) Uani 1 1 d . . . C22 C 0.1451(7) 0.6920(7) 0.7463(5) 0.046(3) Uani 1 1 d . . . H22A H 0.1161 0.6696 0.7638 0.055 Uiso 1 1 calc R . . H22B H 0.1506 0.6612 0.7207 0.055 Uiso 1 1 calc R . . C23 C 0.2040(6) 0.6986(6) 0.7766(4) 0.033(3) Uani 1 1 d . . . C24 C 0.2105(7) 0.6766(6) 0.8211(4) 0.039(3) Uani 1 1 d . . . H24A H 0.1781 0.6482 0.8314 0.047 Uiso 1 1 calc R . . C25 C 0.2637(7) 0.6824(7) 0.8492(5) 0.046(4) Uani 1 1 d . . . H25A H 0.2708 0.6531 0.8771 0.056 Uiso 1 1 calc R . . C26 C 0.3115(6) 0.7139(6) 0.8338(4) 0.039(3) Uani 1 1 d . . . H26A H 0.3517 0.7083 0.8520 0.046 Uiso 1 1 calc R . . C27 C 0.3088(6) 0.7337(6) 0.7874(4) 0.033(3) Uani 1 1 d . . . C28 C 0.2547(6) 0.7222(6) 0.7606(4) 0.033(3) Uani 1 1 d . . . C29 C 0.3641(6) 0.7651(6) 0.7707(5) 0.039(3) Uani 1 1 d . . . H29A H 0.3965 0.7684 0.7966 0.047 Uiso 1 1 calc R . . H29B H 0.3779 0.7337 0.7480 0.047 Uiso 1 1 calc R . . C30 C 0.3532(6) 0.8366(7) 0.7496(4) 0.037(3) Uani 1 1 d . . . C31 C 0.3631(7) 0.8500(8) 0.7055(5) 0.049(4) Uani 1 1 d . . . H31A H 0.3830 0.8138 0.6889 0.058 Uiso 1 1 calc R . . C32 C 0.3529(6) 0.9140(7) 0.6855(5) 0.043(3) Uani 1 1 d . . . H32A H 0.3692 0.9254 0.6568 0.051 Uiso 1 1 calc R . . C33 C 0.3308(6) 0.9661(8) 0.7111(5) 0.046(4) Uani 1 1 d . . . H33A H 0.3291 1.0141 0.6986 0.055 Uiso 1 1 calc R . . C34 C 0.3215(6) 0.9572(6) 0.7552(4) 0.034(3) Uani 1 1 d . . . C35 C 0.3346(6) 0.8914(6) 0.7756(4) 0.034(3) Uani 1 1 d . . . C36 C 0.2984(5) 1.0173(6) 0.7832(5) 0.037(3) Uani 1 1 d . . . H36A H 0.3304 1.0301 0.8079 0.044 Uiso 1 1 calc R . . H36B H 0.2906 1.0580 0.7631 0.044 Uiso 1 1 calc R . . C37 C 0.3823(6) 0.9003(9) 0.8519(5) 0.053(4) Uani 1 1 d . . . H37A H 0.4177 0.8800 0.8406 0.064 Uiso 1 1 calc R . . H37B H 0.3866 0.9511 0.8510 0.064 Uiso 1 1 calc R . . C38 C 0.3828(7) 0.8802(11) 0.8969(5) 0.069(5) Uani 1 1 d . . . H38A H 0.3994 0.8329 0.9001 0.082 Uiso 1 1 calc R . . H38B H 0.4110 0.9108 0.9159 0.082 Uiso 1 1 calc R . . C39 C 0.3345(8) 0.8657(12) 0.9597(5) 0.073(5) Uani 1 1 d . . . H39A H 0.3655 0.8947 0.9773 0.088 Uiso 1 1 calc R . . H39B H 0.3460 0.8168 0.9651 0.088 Uiso 1 1 calc R . . C40 C 0.2758(8) 0.8785(10) 0.9765(5) 0.069(4) Uani 1 1 d . . . H40A H 0.2789 0.8679 1.0093 0.082 Uiso 1 1 calc R . . H40B H 0.2639 0.9274 0.9718 0.082 Uiso 1 1 calc R . . C41 C 0.1767(8) 0.8402(10) 0.9692(6) 0.069(3) Uani 1 1 d . . . H41A H 0.1613 0.8881 0.9657 0.083 Uiso 1 1 calc R . . H41B H 0.1819 0.8280 1.0018 0.083 Uiso 1 1 calc R . . C42 C 0.1344(8) 0.7908(13) 0.9425(5) 0.080(7) Uani 1 1 d . . . H42A H 0.1500 0.7431 0.9468 0.096 Uiso 1 1 calc R . . H42B H 0.0952 0.7927 0.9536 0.096 Uiso 1 1 calc R . . C43 C 0.0839(7) 0.7681(11) 0.8687(6) 0.070(5) Uani 1 1 d . . . H43A H 0.0973 0.7194 0.8694 0.084 Uiso 1 1 calc R . . H43B H 0.0463 0.7697 0.8822 0.084 Uiso 1 1 calc R . . C44 C 0.0712(6) 0.7885(9) 0.8228(5) 0.052(4) Uani 1 1 d . . . H44A H 0.0432 0.8280 0.8208 0.062 Uiso 1 1 calc R . . H44B H 0.0508 0.7499 0.8052 0.062 Uiso 1 1 calc R . . N1 N 0.0032(12) 1.129(2) 0.6664(11) 0.225(14) Uani 1 1 d D . . C45 C -0.0371(11) 1.1265(9) 0.6938(8) 0.148(11) Uani 1 1 d D . . C46 C -0.0822(11) 1.1212(13) 0.7231(9) 0.101(6) Uani 1 1 d D . . N2 N 0.5000 0.9131(19) 0.7500 0.225(14) Uani 1 2 d SDU . . C47 C 0.5000 0.9804(11) 0.7500 0.148(11) Uani 1 2 d SDU . . C48 C 0.5000 1.0551(11) 0.7500 0.101(6) Uani 1 2 d SDU . . 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 0.0436(9) 0.0402(10) 0.0386(9) -0.0020(8) -0.0041(7) 0.0052(8) Cu2 0.0532(11) 0.0427(10) 0.0477(10) -0.0041(8) 0.0003(8) 0.0041(8) Cu3 0.0644(12) 0.0416(11) 0.0615(12) -0.0044(9) 0.0105(10) 0.0113(9) Cu4 0.061(2) 0.060(3) 0.067(3) 0.013(2) 0.009(2) -0.003(2) Cu5 0.064(2) 0.054(3) 0.076(3) -0.038(2) 0.011(2) -0.012(2) Cu6 0.052(2) 0.039(2) 0.048(2) -0.0015(16) -0.0061(16) -0.0001(17) Cu7 0.0530(10) 0.0350(9) 0.0449(10) 0.0049(8) -0.0063(8) 0.0022(8) K1 0.0497(16) 0.0189(13) 0.0341(14) -0.0020(11) -0.0042(12) 0.0043(12) K2 0.0449(15) 0.0272(14) 0.0384(15) -0.0006(12) 0.0037(13) 0.0037(12) I1 0.0458(5) 0.0388(5) 0.0392(5) 0.0028(4) 0.0033(4) 0.0031(4) I2 0.0464(5) 0.0387(5) 0.0384(5) -0.0006(4) -0.0052(4) -0.0001(4) I3 0.0529(5) 0.0275(4) 0.0416(5) -0.0039(4) 0.0060(4) 0.0030(4) I4 0.0534(6) 0.0750(8) 0.0505(6) -0.0275(6) 0.0073(5) -0.0049(5) I5 0.0635(6) 0.0354(5) 0.0572(6) -0.0016(5) -0.0018(5) 0.0056(5) I6 0.0578(19) 0.056(2) 0.0435(16) -0.0095(14) 0.0117(11) -0.0111(14) I7 0.0571(11) 0.0281(9) 0.0398(9) -0.0070(7) 0.0064(8) 0.0014(8) I8 0.0654(13) 0.0446(11) 0.0487(11) 0.0046(9) -0.0151(10) -0.0102(10) I9 0.0494(5) 0.0255(4) 0.0359(5) -0.0001(3) 0.0003(4) 0.0066(4) S1 0.0410(17) 0.0326(17) 0.0339(16) -0.0034(14) -0.0032(14) 0.0014(14) O1 0.061(6) 0.021(4) 0.031(5) 0.000(4) 0.004(4) 0.007(4) O2 0.097(8) 0.027(5) 0.051(6) 0.018(5) 0.022(6) 0.033(5) O3 0.068(6) 0.031(5) 0.025(4) -0.001(4) -0.002(4) 0.008(5) O4 0.048(5) 0.017(4) 0.029(4) -0.006(3) 0.007(4) 0.002(4) O5 0.045(5) 0.024(4) 0.030(4) -0.003(4) -0.005(4) -0.002(4) O6 0.057(7) 0.102(10) 0.039(6) 0.004(6) -0.003(5) -0.017(7) O7 0.058(6) 0.080(9) 0.048(6) -0.007(6) 0.016(5) -0.025(6) O8 0.064(7) 0.100(10) 0.042(6) -0.004(6) 0.009(5) -0.016(7) O9 0.042(5) 0.024(4) 0.029(4) -0.003(4) 0.000(4) -0.001(4) C1 0.095(12) 0.031(8) 0.033(7) -0.013(6) 0.008(8) 0.017(8) C2 0.107(14) 0.046(9) 0.043(9) -0.010(8) 0.023(9) -0.012(10) C3 0.056(9) 0.039(8) 0.036(7) 0.010(6) 0.002(6) 0.004(7) C4 0.073(8) 0.090(10) 0.041(6) -0.016(6) 0.001(6) -0.017(7) C5 0.074(8) 0.068(9) 0.066(8) -0.007(7) 0.009(7) -0.002(7) C6 0.059(9) 0.032(7) 0.030(7) -0.005(6) -0.009(6) 0.005(6) C7 0.044(7) 0.027(6) 0.038(7) -0.001(6) -0.004(6) 0.006(6) C8 0.057(8) 0.013(6) 0.044(8) -0.001(5) 0.009(6) 0.007(6) C9 0.055(8) 0.010(5) 0.035(7) -0.002(5) 0.000(6) 0.004(5) C10 0.046(7) 0.014(5) 0.024(6) -0.010(5) -0.001(5) 0.003(5) C11 0.051(8) 0.017(6) 0.040(7) -0.010(5) -0.005(6) 0.001(5) C12 0.064(9) 0.025(7) 0.034(7) -0.016(6) 0.010(6) 0.011(6) C13 0.045(7) 0.022(6) 0.039(7) -0.005(5) 0.009(6) 0.009(5) C14 0.045(7) 0.023(6) 0.029(6) 0.000(5) 0.000(5) 0.007(5) C15 0.037(6) 0.029(7) 0.031(6) 0.002(5) 0.001(5) 0.004(5) C16 0.029(6) 0.027(6) 0.035(7) 0.014(5) -0.002(5) 0.002(5) C17 0.024(6) 0.025(6) 0.048(8) 0.000(6) -0.004(5) -0.011(5) C18 0.025(6) 0.039(8) 0.045(8) -0.003(6) 0.007(5) -0.003(5) C19 0.048(8) 0.031(7) 0.041(7) -0.005(6) 0.010(6) -0.008(6) C20 0.043(7) 0.032(7) 0.032(7) -0.007(6) -0.011(6) -0.001(6) C21 0.045(7) 0.035(7) 0.022(6) 0.015(5) 0.007(5) 0.009(6) C22 0.069(10) 0.031(7) 0.038(8) 0.003(6) 0.010(7) 0.009(7) C23 0.046(7) 0.010(5) 0.042(7) 0.001(5) -0.001(6) 0.003(5) C24 0.065(9) 0.015(6) 0.038(7) 0.012(5) 0.005(7) 0.008(6) C25 0.073(10) 0.032(7) 0.034(7) 0.011(6) 0.011(7) 0.008(7) C26 0.053(8) 0.023(6) 0.039(7) 0.002(6) 0.003(6) 0.013(6) C27 0.045(7) 0.015(5) 0.037(7) 0.000(5) 0.004(6) 0.017(5) C28 0.052(8) 0.015(6) 0.033(7) 0.005(5) 0.009(6) 0.011(5) C29 0.063(9) 0.014(6) 0.041(7) 0.000(5) 0.011(7) 0.009(6) C30 0.040(7) 0.030(7) 0.039(7) -0.005(6) 0.001(6) 0.005(6) C31 0.059(9) 0.046(9) 0.041(8) -0.016(7) 0.006(7) -0.004(7) C32 0.046(8) 0.033(7) 0.049(8) 0.002(6) 0.006(6) -0.004(6) C33 0.049(8) 0.037(8) 0.047(8) 0.007(7) -0.017(7) -0.006(7) C34 0.046(7) 0.018(6) 0.035(7) -0.003(5) -0.007(6) -0.013(5) C35 0.043(7) 0.021(6) 0.037(7) 0.005(5) 0.001(6) -0.005(5) C36 0.038(7) 0.017(6) 0.049(8) -0.004(6) -0.012(6) -0.013(5) C37 0.038(7) 0.064(10) 0.055(9) 0.007(8) -0.004(7) -0.015(7) C38 0.055(10) 0.118(17) 0.031(8) -0.012(9) 0.002(7) 0.005(10) C39 0.064(11) 0.111(17) 0.041(9) -0.002(10) -0.003(8) -0.007(11) C40 0.073(8) 0.090(10) 0.041(6) -0.016(6) 0.001(6) -0.017(7) C41 0.074(8) 0.068(9) 0.066(8) -0.007(7) 0.009(7) -0.002(7) C42 0.057(10) 0.15(2) 0.034(9) -0.004(11) 0.014(8) -0.016(12) C43 0.057(10) 0.100(15) 0.060(11) 0.006(10) 0.035(9) -0.019(10) C44 0.044(8) 0.067(11) 0.044(8) 0.027(8) 0.003(7) -0.010(8) N1 0.131(18) 0.39(4) 0.18(2) -0.05(3) 0.083(17) 0.02(3) C45 0.20(2) 0.016(7) 0.19(2) -0.013(13) -0.123(18) -0.008(14) C46 0.104(14) 0.085(14) 0.117(16) -0.006(15) 0.028(12) -0.002(14) N2 0.131(18) 0.39(4) 0.18(2) -0.05(3) 0.083(17) 0.02(3) C47 0.20(2) 0.016(7) 0.19(2) -0.013(13) -0.123(18) -0.008(14) C48 0.104(14) 0.085(14) 0.117(16) -0.006(15) 0.028(12) -0.002(14) _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 S1 2.318(4) . ? Cu1 I1 2.6307(19) . ? Cu1 Cu7 2.634(2) 5_576 ? Cu1 I9 2.6446(19) . ? Cu1 I3 2.722(2) . ? Cu1 Cu2 2.801(2) . ? Cu2 I2 2.626(2) . ? Cu2 I4 2.695(2) . ? Cu2 I1 2.706(2) . ? Cu2 I3 2.719(2) . ? Cu2 Cu3 2.738(3) . ? Cu2 Cu7 2.984(3) 5_576 ? Cu3 Cu5 2.517(4) . ? Cu3 I4 2.525(2) . ? Cu3 Cu4 2.544(5) . ? Cu3 I5 2.555(2) . ? Cu3 I3 2.579(2) . ? Cu4 I8 2.600(5) 5_566 ? Cu4 Cu6 2.643(5) 5_566 ? Cu4 I5 2.718(4) . ? Cu4 I6 2.718(6) 5_566 ? Cu4 I3 2.838(5) . ? Cu4 I6 3.005(6) . ? Cu5 I5 2.559(4) . ? Cu5 I7 2.581(4) . ? Cu5 Cu6 2.585(5) . ? Cu5 I6 2.733(5) . ? Cu5 I6 3.066(5) 5_566 ? Cu6 I8 2.518(4) . ? Cu6 I7 2.534(4) . ? Cu6 I6 2.580(5) . ? Cu6 Cu4 2.643(5) 5_566 ? Cu7 I2 2.595(2) 5_576 ? Cu7 Cu1 2.634(2) 5_576 ? Cu7 I9 2.6434(19) . ? Cu7 I9 2.717(2) 5_576 ? Cu7 I1 2.774(2) 5_576 ? Cu7 Cu2 2.984(3) 5_576 ? K1 O1 2.657(9) . ? K1 O4 2.705(8) . ? K1 O3 2.768(9) . ? K1 O2 2.858(10) . ? K1 C32 3.149(14) . ? K1 C33 3.187(14) . ? K1 S1 3.193(4) . ? K1 C31 3.254(16) . ? K1 C19 3.261(13) . ? K1 C18 3.301(12) . ? K1 C34 3.415(12) . ? K1 C17 3.435(12) . ? K2 O7 2.744(11) . ? K2 O8 2.767(11) . ? K2 O6 2.790(11) . ? K2 O5 2.810(9) . ? K2 O9 2.822(9) . ? K2 C12 3.160(12) . ? K2 C25 3.203(14) . ? K2 C13 3.225(12) . ? K2 C26 3.249(12) . ? K2 C11 3.289(12) . ? K2 C24 3.389(13) . ? K2 C14 3.490(12) . ? I1 Cu7 2.774(2) 5_576 ? I2 Cu7 2.595(2) 5_576 ? I6 I6 0.689(4) 5_566 ? I6 Cu4 2.718(6) 5_566 ? I6 Cu5 3.066(5) 5_566 ? I8 Cu4 2.600(5) 5_566 ? I9 Cu7 2.717(2) 5_576 ? S1 C5 1.782(19) . ? S1 C4 1.829(19) . ? O1 C28 1.430(14) . ? O1 C1 1.473(15) . ? O2 C2 1.378(18) . ? O2 C3 1.444(16) . ? O3 C7 1.434(15) . ? O3 C6 1.444(14) . ? O4 C9 1.369(14) . ? O4 C8 1.448(14) . ? O5 C35 1.396(15) . ? O5 C37 1.415(15) . ? O6 C38 1.306(18) . ? O6 C39 1.379(19) . ? O7 C40 1.431(19) . ? O7 C41 1.446(19) . ? O8 C42 1.380(19) . ? O8 C43 1.43(2) . ? O9 C21 1.403(13) . ? O9 C44 1.421(15) . ? C1 C2 1.49(2) . ? C3 C4 1.49(2) . ? C5 C6 1.53(2) . ? C7 C8 1.504(18) . ? C9 C14 1.379(18) . ? C9 C10 1.424(17) . ? C10 C11 1.407(16) . ? C10 C36 1.508(17) . ? C11 C12 1.371(19) . ? C12 C13 1.387(19) . ? C13 C14 1.423(17) . ? C14 C15 1.521(17) . ? C15 C16 1.509(17) . ? C16 C17 1.386(17) . ? C16 C21 1.417(16) . ? C17 C18 1.379(18) . ? C18 C19 1.369(18) . ? C19 C20 1.381(18) . ? C20 C21 1.382(18) . ? C20 C22 1.534(18) . ? C22 C23 1.510(19) . ? C23 C24 1.377(17) . ? C23 C28 1.380(18) . ? C24 C25 1.37(2) . ? C25 C26 1.373(19) . ? C26 C27 1.424(17) . ? C27 C28 1.385(18) . ? C27 C29 1.535(18) . ? C29 C30 1.526(17) . ? C30 C31 1.385(19) . ? C30 C35 1.410(18) . ? C31 C32 1.38(2) . ? C32 C33 1.40(2) . ? C33 C34 1.367(19) . ? C34 C35 1.425(17) . ? C34 C36 1.560(18) . ? C37 C38 1.39(2) . ? C39 C40 1.50(2) . ? C41 C42 1.50(2) . ? C43 C44 1.41(2) . ? N1 C45 1.30(3) . ? C45 C46 1.433(9) . ? N2 C47 1.30(3) . ? C47 C48 1.447(9) . ? 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 S1 Cu1 I1 103.62(11) . . ? S1 Cu1 Cu7 149.37(12) . 5_576 ? I1 Cu1 Cu7 63.60(6) . 5_576 ? S1 Cu1 I9 111.05(11) . . ? I1 Cu1 I9 120.64(7) . . ? Cu7 Cu1 I9 61.95(6) 5_576 . ? S1 Cu1 I3 101.51(11) . . ? I1 Cu1 I3 114.26(7) . . ? Cu7 Cu1 I3 109.12(7) 5_576 . ? I9 Cu1 I3 104.26(6) . . ? S1 Cu1 Cu2 133.49(11) . . ? I1 Cu1 Cu2 59.66(6) . . ? Cu7 Cu1 Cu2 66.52(7) 5_576 . ? I9 Cu1 Cu2 114.56(7) . . ? I3 Cu1 Cu2 58.96(6) . . ? I2 Cu2 I4 114.48(7) . . ? I2 Cu2 I1 106.03(7) . . ? I4 Cu2 I1 109.45(7) . . ? I2 Cu2 I3 106.17(7) . . ? I4 Cu2 I3 108.79(7) . . ? I1 Cu2 I3 111.93(7) . . ? I2 Cu2 Cu3 142.03(9) . . ? I4 Cu2 Cu3 55.37(6) . . ? I1 Cu2 Cu3 111.79(8) . . ? I3 Cu2 Cu3 56.40(6) . . ? I2 Cu2 Cu1 100.72(7) . . ? I4 Cu2 Cu1 144.80(8) . . ? I1 Cu2 Cu1 57.03(6) . . ? I3 Cu2 Cu1 59.06(6) . . ? Cu3 Cu2 Cu1 96.94(8) . . ? I2 Cu2 Cu7 54.65(5) . 5_576 ? I4 Cu2 Cu7 151.48(9) . 5_576 ? I1 Cu2 Cu7 58.11(5) . 5_576 ? I3 Cu2 Cu7 99.73(7) . 5_576 ? Cu3 Cu2 Cu7 150.81(9) . 5_576 ? Cu1 Cu2 Cu7 54.05(6) . 5_576 ? Cu5 Cu3 I4 78.55(13) . . ? Cu5 Cu3 Cu4 82.42(17) . . ? I4 Cu3 Cu4 144.12(14) . . ? Cu5 Cu3 I5 60.61(11) . . ? I4 Cu3 I5 127.45(8) . . ? Cu4 Cu3 I5 64.43(11) . . ? Cu5 Cu3 I3 147.21(14) . . ? I4 Cu3 I3 119.19(8) . . ? Cu4 Cu3 I3 67.29(12) . . ? I5 Cu3 I3 112.88(8) . . ? Cu5 Cu3 Cu2 139.30(15) . . ? I4 Cu3 Cu2 61.45(7) . . ? Cu4 Cu3 Cu2 125.99(13) . . ? I5 Cu3 Cu2 153.10(10) . . ? I3 Cu3 Cu2 61.42(6) . . ? Cu3 Cu4 I8 152.5(2) . 5_566 ? Cu3 Cu4 Cu6 127.25(19) . 5_566 ? I8 Cu4 Cu6 57.41(12) 5_566 5_566 ? Cu3 Cu4 I5 57.99(10) . . ? I8 Cu4 I5 128.90(17) 5_566 . ? Cu6 Cu4 I5 160.0(2) 5_566 . ? Cu3 Cu4 I6 86.56(16) . 5_566 ? I8 Cu4 I6 111.75(17) 5_566 5_566 ? Cu6 Cu4 I6 57.50(13) 5_566 5_566 ? I5 Cu4 I6 107.16(17) . 5_566 ? Cu3 Cu4 I3 56.94(10) . . ? I8 Cu4 I3 96.66(16) 5_566 . ? Cu6 Cu4 I3 96.89(16) 5_566 . ? I5 Cu4 I3 100.67(13) . . ? I6 Cu4 I3 109.05(16) 5_566 . ? Cu3 Cu4 I6 85.26(15) . . ? I8 Cu4 I6 117.06(16) 5_566 . ? Cu6 Cu4 I6 67.06(14) 5_566 . ? I5 Cu4 I6 96.06(15) . . ? I6 Cu4 I6 12.57(10) 5_566 . ? I3 Cu4 I6 117.95(16) . . ? Cu3 Cu5 I5 60.44(10) . . ? Cu3 Cu5 I7 155.7(2) . . ? I5 Cu5 I7 119.85(17) . . ? Cu3 Cu5 Cu6 131.7(2) . . ? I5 Cu5 Cu6 156.9(2) . . ? I7 Cu5 Cu6 58.74(12) . . ? Cu3 Cu5 I6 91.82(14) . . ? I5 Cu5 I6 107.15(18) . . ? I7 Cu5 I6 109.83(16) . . ? Cu6 Cu5 I6 57.95(14) . . ? Cu3 Cu5 I6 79.92(13) . 5_566 ? I5 Cu5 I6 101.72(15) . 5_566 ? I7 Cu5 I6 121.26(16) . 5_566 ? Cu6 Cu5 I6 66.75(14) . 5_566 ? I6 Cu5 I6 11.95(10) . 5_566 ? I8 Cu6 I7 124.02(17) . . ? I8 Cu6 I6 119.46(17) . . ? I7 Cu6 I6 116.52(16) . . ? I8 Cu6 Cu5 153.1(2) . . ? I7 Cu6 Cu5 60.54(13) . . ? I6 Cu6 Cu5 63.89(15) . . ? I8 Cu6 Cu4 60.43(13) . 5_566 ? I7 Cu6 Cu4 159.92(19) . 5_566 ? I6 Cu6 Cu4 62.72(16) . 5_566 ? Cu5 Cu6 Cu4 126.0(2) . 5_566 ? I2 Cu7 Cu1 106.18(8) 5_576 5_576 ? I2 Cu7 I9 120.22(7) 5_576 . ? Cu1 Cu7 I9 133.31(8) 5_576 . ? I2 Cu7 I9 112.40(7) 5_576 5_576 ? Cu1 Cu7 I9 59.21(6) 5_576 5_576 ? I9 Cu7 I9 103.77(7) . 5_576 ? I2 Cu7 I1 104.96(7) 5_576 5_576 ? Cu1 Cu7 I1 58.14(5) 5_576 5_576 ? I9 Cu7 I1 102.15(7) . 5_576 ? I9 Cu7 I1 113.15(6) 5_576 5_576 ? I2 Cu7 Cu2 55.63(5) 5_576 5_576 ? Cu1 Cu7 Cu2 59.43(6) 5_576 5_576 ? I9 Cu7 Cu2 147.61(8) . 5_576 ? I9 Cu7 Cu2 106.89(7) 5_576 5_576 ? I1 Cu7 Cu2 55.92(5) 5_576 5_576 ? O1 K1 O4 127.3(3) . . ? O1 K1 O3 170.8(3) . . ? O4 K1 O3 61.9(2) . . ? O1 K1 O2 59.8(3) . . ? O4 K1 O2 168.7(3) . . ? O3 K1 O2 111.0(3) . . ? O1 K1 C32 93.0(3) . . ? O4 K1 C32 95.8(3) . . ? O3 K1 C32 84.5(3) . . ? O2 K1 C32 74.3(4) . . ? O1 K1 C33 107.4(3) . . ? O4 K1 C33 70.3(3) . . ? O3 K1 C33 73.7(3) . . ? O2 K1 C33 99.7(4) . . ? C32 K1 C33 25.5(4) . . ? O1 K1 S1 110.4(2) . . ? O4 K1 S1 117.7(2) . . ? O3 K1 S1 61.83(19) . . ? O2 K1 S1 61.1(2) . . ? C32 K1 S1 103.4(3) . . ? C33 K1 S1 115.6(3) . . ? O1 K1 C31 68.3(3) . . ? O4 K1 C31 108.4(3) . . ? O3 K1 C31 109.3(4) . . ? O2 K1 C31 64.5(4) . . ? C32 K1 C31 24.8(4) . . ? C33 K1 C31 43.3(4) . . ? S1 K1 C31 113.4(3) . . ? O1 K1 C19 68.7(3) . . ? O4 K1 C19 100.6(3) . . ? O3 K1 C19 112.5(3) . . ? O2 K1 C19 90.2(3) . . ? C32 K1 C19 160.5(4) . . ? C33 K1 C19 165.7(4) . . ? S1 K1 C19 78.2(3) . . ? C31 K1 C19 136.8(4) . . ? O1 K1 C18 92.8(3) . . ? O4 K1 C18 85.9(3) . . ? O3 K1 C18 88.8(3) . . ? O2 K1 C18 103.1(4) . . ? C32 K1 C18 171.3(4) . . ? C33 K1 C18 155.1(4) . . ? S1 K1 C18 68.4(3) . . ? C31 K1 C18 160.6(4) . . ? C19 K1 C18 24.1(3) . . ? O1 K1 C34 97.2(3) . . ? O4 K1 C34 59.1(3) . . ? O3 K1 C34 87.0(3) . . ? O2 K1 C34 113.5(4) . . ? C32 K1 C34 43.2(3) . . ? C33 K1 C34 23.6(3) . . ? S1 K1 C34 138.6(2) . . ? C31 K1 C34 49.3(3) . . ? C19 K1 C34 142.1(3) . . ? C18 K1 C34 142.1(3) . . ? O1 K1 C17 105.6(3) . . ? O4 K1 C17 62.5(3) . . ? O3 K1 C17 79.1(3) . . ? O2 K1 C17 126.6(3) . . ? C32 K1 C17 157.2(3) . . ? C33 K1 C17 132.4(4) . . ? S1 K1 C17 82.8(2) . . ? C31 K1 C17 163.7(3) . . ? C19 K1 C17 41.9(3) . . ? C18 K1 C17 23.5(3) . . ? C34 K1 C17 119.4(3) . . ? O7 K2 O8 59.6(3) . . ? O7 K2 O6 60.7(3) . . ? O8 K2 O6 120.0(3) . . ? O7 K2 O5 119.3(3) . . ? O8 K2 O5 177.7(3) . . ? O6 K2 O5 58.7(3) . . ? O7 K2 O9 119.6(3) . . ? O8 K2 O9 60.1(3) . . ? O6 K2 O9 177.7(3) . . ? O5 K2 O9 121.1(3) . . ? O7 K2 C12 85.0(4) . . ? O8 K2 C12 86.8(4) . . ? O6 K2 C12 83.6(4) . . ? O5 K2 C12 91.1(3) . . ? O9 K2 C12 94.2(3) . . ? O7 K2 C25 93.7(4) . . ? O8 K2 C25 92.0(4) . . ? O6 K2 C25 96.3(4) . . ? O5 K2 C25 90.1(3) . . ? O9 K2 C25 85.9(3) . . ? C12 K2 C25 178.6(4) . . ? O7 K2 C13 96.1(4) . . ? O8 K2 C13 73.4(4) . . ? O6 K2 C13 108.6(4) . . ? O5 K2 C13 105.0(3) . . ? O9 K2 C13 69.2(3) . . ? C12 K2 C13 25.1(3) . . ? C25 K2 C13 154.9(4) . . ? O7 K2 C26 104.4(4) . . ? O8 K2 C26 116.6(4) . . ? O6 K2 C26 82.6(4) . . ? O5 K2 C26 65.5(3) . . ? O9 K2 C26 99.4(3) . . ? C12 K2 C26 156.6(4) . . ? C25 K2 C26 24.6(3) . . ? C13 K2 C26 159.5(3) . . ? O7 K2 C11 97.7(3) . . ? O8 K2 C11 111.2(4) . . ? O6 K2 C11 72.1(4) . . ? O5 K2 C11 66.7(3) . . ? O9 K2 C11 105.7(3) . . ? C12 K2 C11 24.4(3) . . ? C25 K2 C11 156.7(4) . . ? C13 K2 C11 43.2(3) . . ? C26 K2 C11 132.2(4) . . ? O7 K2 C24 105.6(3) . . ? O8 K2 C24 80.9(4) . . ? O6 K2 C24 120.2(4) . . ? O5 K2 C24 101.4(3) . . ? O9 K2 C24 62.0(3) . . ? C12 K2 C24 156.2(4) . . ? C25 K2 C24 23.9(3) . . ? C13 K2 C24 131.2(3) . . ? C26 K2 C24 41.9(4) . . ? C11 K2 C24 156.7(3) . . ? O7 K2 C14 120.0(3) . . ? O8 K2 C14 85.7(3) . . ? O6 K2 C14 120.7(4) . . ? O5 K2 C14 93.3(3) . . ? O9 K2 C14 57.1(3) . . ? C12 K2 C14 42.5(3) . . ? C25 K2 C14 138.2(3) . . ? C13 K2 C14 24.1(3) . . ? C26 K2 C14 135.5(3) . . ? C11 K2 C14 48.6(3) . . ? C24 K2 C14 115.8(3) . . ? Cu1 I1 Cu2 63.30(6) . . ? Cu1 I1 Cu7 58.26(5) . 5_576 ? Cu2 I1 Cu7 65.97(6) . 5_576 ? Cu7 I2 Cu2 69.71(6) 5_576 . ? Cu3 I3 Cu2 62.19(6) . . ? Cu3 I3 Cu1 102.94(7) . . ? Cu2 I3 Cu1 61.99(6) . . ? Cu3 I3 Cu4 55.76(10) . . ? Cu2 I3 Cu4 115.76(10) . . ? Cu1 I3 Cu4 144.98(10) . . ? Cu3 I4 Cu2 63.19(6) . . ? Cu3 I5 Cu5 58.95(11) . . ? Cu3 I5 Cu4 57.58(10) . . ? Cu5 I5 Cu4 78.29(14) . . ? I6 I6 Cu6 139.4(7) 5_566 . ? I6 I6 Cu4 108.2(7) 5_566 5_566 ? Cu6 I6 Cu4 59.78(14) . 5_566 ? I6 I6 Cu5 112.8(6) 5_566 . ? Cu6 I6 Cu5 58.16(13) . . ? Cu4 I6 Cu5 117.42(16) 5_566 . ? I6 I6 Cu4 59.3(6) 5_566 . ? Cu6 I6 Cu4 128.98(17) . . ? Cu4 I6 Cu4 167.43(10) 5_566 . ? Cu5 I6 Cu4 70.86(14) . . ? I6 I6 Cu5 55.3(6) 5_566 5_566 ? Cu6 I6 Cu5 129.84(17) . 5_566 ? Cu4 I6 Cu5 70.10(14) 5_566 5_566 ? Cu5 I6 Cu5 168.05(10) . 5_566 ? Cu4 I6 Cu5 100.22(12) . 5_566 ? Cu6 I7 Cu5 60.72(13) . . ? Cu6 I8 Cu4 62.16(13) . 5_566 ? Cu7 I9 Cu1 116.02(7) . . ? Cu7 I9 Cu7 76.23(7) . 5_576 ? Cu1 I9 Cu7 58.83(5) . 5_576 ? C5 S1 C4 102.2(8) . . ? C5 S1 Cu1 108.6(6) . . ? C4 S1 Cu1 104.7(5) . . ? C5 S1 K1 91.4(6) . . ? C4 S1 K1 106.3(5) . . ? Cu1 S1 K1 138.22(15) . . ? C28 O1 C1 111.6(9) . . ? C28 O1 K1 124.5(6) . . ? C1 O1 K1 123.5(7) . . ? C2 O2 C3 115.7(12) . . ? C2 O2 K1 107.8(9) . . ? C3 O2 K1 122.0(7) . . ? C7 O3 C6 111.2(10) . . ? C7 O3 K1 110.7(7) . . ? C6 O3 K1 126.5(7) . . ? C9 O4 C8 113.1(9) . . ? C9 O4 K1 126.3(7) . . ? C8 O4 K1 118.8(7) . . ? C35 O5 C37 116.0(10) . . ? C35 O5 K2 125.6(7) . . ? C37 O5 K2 118.0(8) . . ? C38 O6 C39 118.3(13) . . ? C38 O6 K2 118.5(9) . . ? C39 O6 K2 115.8(10) . . ? C40 O7 C41 109.1(12) . . ? C40 O7 K2 115.1(9) . . ? C41 O7 K2 117.0(10) . . ? C42 O8 C43 115.5(14) . . ? C42 O8 K2 118.1(9) . . ? C43 O8 K2 115.5(8) . . ? C21 O9 C44 112.4(10) . . ? C21 O9 K2 128.4(7) . . ? C44 O9 K2 118.8(7) . . ? O1 C1 C2 107.8(12) . . ? O2 C2 C1 112.9(14) . . ? O2 C2 K1 50.4(7) . . ? C1 C2 K1 83.8(8) . . ? O2 C3 C4 113.2(13) . . ? C3 C4 S1 113.3(11) . . ? C6 C5 S1 110.4(12) . . ? O3 C6 C5 107.9(12) . . ? O3 C7 C8 110.2(10) . . ? O3 C7 K1 47.0(5) . . ? C8 C7 K1 81.4(7) . . ? O4 C8 C7 108.5(10) . . ? O4 C9 C14 119.5(11) . . ? O4 C9 C10 119.9(11) . . ? C14 C9 C10 120.5(11) . . ? C11 C10 C9 118.5(12) . . ? C11 C10 C36 119.2(11) . . ? C9 C10 C36 122.2(10) . . ? C11 C10 K2 68.6(7) . . ? C9 C10 K2 83.4(7) . . ? C36 C10 K2 120.2(7) . . ? C12 C11 C10 120.7(12) . . ? C12 C11 K2 72.5(7) . . ? C10 C11 K2 87.9(7) . . ? C11 C12 C13 120.9(12) . . ? C11 C12 K2 83.0(7) . . ? C13 C12 K2 80.1(7) . . ? C12 C13 C14 119.7(12) . . ? C12 C13 K2 74.9(7) . . ? C14 C13 K2 88.5(7) . . ? C9 C14 C13 119.4(12) . . ? C9 C14 C15 120.7(11) . . ? C13 C14 C15 119.9(11) . . ? C9 C14 K2 85.6(7) . . ? C13 C14 K2 67.5(7) . . ? C15 C14 K2 118.8(8) . . ? C16 C15 C14 115.6(10) . . ? C17 C16 C21 116.0(12) . . ? C17 C16 C15 120.9(11) . . ? C21 C16 C15 123.1(11) . . ? C18 C17 C16 120.8(12) . . ? C18 C17 K1 72.8(7) . . ? C16 C17 K1 86.2(7) . . ? C19 C18 C17 121.6(13) . . ? C19 C18 K1 76.3(7) . . ? C17 C18 K1 83.7(7) . . ? C18 C19 C20 119.8(13) . . ? C18 C19 K1 79.6(7) . . ? C20 C19 K1 87.0(8) . . ? C19 C20 C21 118.3(12) . . ? C19 C20 C22 120.3(12) . . ? C21 C20 C22 121.4(11) . . ? C19 C20 K1 69.6(8) . . ? C21 C20 K1 86.3(8) . . ? C22 C20 K1 114.2(9) . . ? C20 C21 O9 120.0(11) . . ? C20 C21 C16 122.9(11) . . ? O9 C21 C16 117.1(11) . . ? C23 C22 C20 115.1(11) . . ? C24 C23 C28 116.6(12) . . ? C24 C23 C22 121.2(12) . . ? C28 C23 C22 122.0(12) . . ? C25 C24 C23 122.1(13) . . ? C25 C24 K2 70.5(8) . . ? C23 C24 K2 91.1(7) . . ? C26 C25 C24 119.8(13) . . ? C26 C25 K2 79.6(8) . . ? C24 C25 K2 85.7(8) . . ? C25 C26 C27 120.7(13) . . ? C25 C26 K2 75.9(8) . . ? C27 C26 K2 93.8(7) . . ? C28 C27 C26 115.7(12) . . ? C28 C27 C29 125.0(11) . . ? C26 C27 C29 119.3(12) . . ? C23 C28 C27 124.5(12) . . ? C23 C28 O1 117.3(11) . . ? C27 C28 O1 118.0(11) . . ? C30 C29 C27 113.5(10) . . ? C31 C30 C35 118.5(12) . . ? C31 C30 C29 121.4(12) . . ? C35 C30 C29 120.0(12) . . ? C31 C30 K1 70.4(8) . . ? C35 C30 K1 83.1(8) . . ? C29 C30 K1 118.4(8) . . ? C32 C31 C30 122.5(14) . . ? C32 C31 K1 73.3(9) . . ? C30 C31 K1 86.0(9) . . ? C31 C32 C33 117.6(14) . . ? C31 C32 K1 81.8(9) . . ? C33 C32 K1 78.8(8) . . ? C34 C33 C32 123.2(13) . . ? C34 C33 K1 87.6(8) . . ? C32 C33 K1 75.7(8) . . ? C33 C34 C35 118.0(12) . . ? C33 C34 C36 121.6(12) . . ? C35 C34 C36 120.3(11) . . ? C33 C34 K1 68.8(7) . . ? C35 C34 K1 84.1(7) . . ? C36 C34 K1 117.9(8) . . ? O5 C35 C30 119.7(11) . . ? O5 C35 C34 120.3(11) . . ? C30 C35 C34 119.9(12) . . ? C10 C36 C34 114.9(9) . . ? C38 C37 O5 116.0(13) . . ? O6 C38 C37 118.9(15) . . ? O6 C39 C40 112.5(14) . . ? O7 C40 C39 107.4(14) . . ? O7 C41 C42 106.3(14) . . ? O8 C42 C41 110.5(17) . . ? C44 C43 O8 117.0(14) . . ? C43 C44 O9 114.7(12) . . ? N1 C45 C46 178(3) . . ? N2 C47 C48 180.000(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.587 _refine_diff_density_min -3.484 _refine_diff_density_rms 0.529 #=====================================================END data_2 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H62 Cu3 I4 K N2 O9 S2' _chemical_formula_weight 1636.46 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' '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' 'I' 'I' -0.4742 1.8119 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.442(3) _cell_length_b 30.738(6) _cell_length_c 14.288(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.43(3) _cell_angle_gamma 90.00 _cell_volume 5903(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10752 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 27.00 _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3192 _exptl_absorpt_coefficient_mu 3.355 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4326 _exptl_absorpt_correction_T_max 0.7302 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.75000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Fixed gap multipole wiggler beamline' _diffrn_radiation_monochromator 'Pt coated Si double crystal' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20119 _diffrn_reflns_av_R_equivalents 0.1008 _diffrn_reflns_av_sigmaI/netI 0.0984 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.00 _reflns_number_total 10752 _reflns_number_gt 7889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PAL ADSC Quantum-210' _computing_cell_refinement 'HKL2000' _computing_data_reduction 'HKL2000' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.1178P)^2^+46.0997P] 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 SHELXL _refine_ls_extinction_coef 0.00128(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10752 _refine_ls_number_parameters 642 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_gt 0.0817 _refine_ls_wR_factor_ref 0.2548 _refine_ls_wR_factor_gt 0.2347 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.001 _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 K1 K 0.44908(19) 0.33345(9) 0.35599(18) 0.0551(6) Uani 1 1 d . . . Cu1 Cu 0.84710(13) 0.09206(5) 0.32361(12) 0.0668(4) Uani 1 1 d . . . Cu2 Cu 1.04065(13) 0.09001(5) 0.37222(11) 0.0657(4) Uani 1 1 d . . . Cu3 Cu 0.91969(13) 0.02549(5) 0.43064(12) 0.0652(4) Uani 1 1 d . . . I1 I 0.94358(6) 0.16447(3) 0.36484(6) 0.0596(3) Uani 1 1 d . . . I2 I 1.05477(7) 0.05973(3) 0.54640(6) 0.0609(3) Uani 1 1 d . . . I3 I 0.96789(8) 0.03253(3) 0.24570(6) 0.0722(3) Uani 1 1 d . . . I4 I 0.73774(7) 0.05300(3) 0.45078(6) 0.0646(3) Uani 1 1 d . . . S1 S 0.7374(3) 0.10938(11) 0.2007(2) 0.0665(8) Uani 1 1 d . . . S2 S 0.2056(3) 0.09771(12) 0.3293(3) 0.0847(12) Uani 1 1 d . . . O1 O 0.6029(6) 0.2196(3) 0.2799(5) 0.0526(18) Uani 1 1 d . . . O2 O 0.5157(13) 0.0332(7) 0.1142(12) 0.147(6) Uani 1 1 d . . . O3 O 0.316(3) 0.0320(14) 0.181(3) 0.86(10) Uani 1 1 d D . . O4 O 0.3072(5) 0.1946(3) 0.4092(6) 0.0560(19) Uani 1 1 d . . . O5 O 0.3772(6) 0.2921(3) 0.2015(5) 0.0542(18) Uani 1 1 d . . . O6 O 0.3241(7) 0.3788(3) 0.2356(6) 0.070(2) Uani 1 1 d . . . O7 O 0.4176(11) 0.4216(4) 0.3812(8) 0.101(4) Uani 1 1 d . . . O8 O 0.5570(10) 0.3774(3) 0.4994(7) 0.090(3) Uani 1 1 d . . . O9 O 0.5185(6) 0.2901(3) 0.5097(5) 0.0539(18) Uani 1 1 d . . . C1 C 0.6768(10) 0.1918(4) 0.2380(9) 0.060(3) Uani 1 1 d . . . H1A H 0.7411 0.1965 0.2676 0.071 Uiso 1 1 calc R . . H1B H 0.6826 0.1983 0.1718 0.071 Uiso 1 1 calc R . . C2 C 0.6441(10) 0.1451(4) 0.2514(8) 0.060(3) Uani 1 1 d . . . H2A H 0.5802 0.1404 0.2210 0.072 Uiso 1 1 calc R . . H2B H 0.6371 0.1389 0.3176 0.072 Uiso 1 1 calc R . . C3 C 0.6615(13) 0.0609(5) 0.1844(12) 0.082(4) Uani 1 1 d . . . H3A H 0.7045 0.0361 0.1733 0.099 Uiso 1 1 calc R . . H3B H 0.6243 0.0553 0.2410 0.099 Uiso 1 1 calc R . . C4 C 0.5936(14) 0.0656(7) 0.1072(12) 0.096(5) Uani 1 1 d . . . H4A H 0.6289 0.0619 0.0487 0.115 Uiso 1 1 calc R . . H4B H 0.5647 0.0945 0.1077 0.115 Uiso 1 1 calc R . . C5 C 0.4318(17) 0.0400(9) 0.0519(19) 0.141(9) Uani 1 1 d D . . H5A H 0.4473 0.0298 -0.0106 0.169 Uiso 1 1 calc R . . H5B H 0.4156 0.0707 0.0484 0.169 Uiso 1 1 calc R . . C6 C 0.346(4) 0.0150(17) 0.091(4) 0.47(7) Uani 1 1 d D . . H6A H 0.2902 0.0166 0.0475 0.569 Uiso 1 1 calc R . . H6B H 0.3647 -0.0153 0.0974 0.569 Uiso 1 1 calc R . . C7 C 0.344(2) 0.0391(11) 0.278(3) 0.68(11) Uani 1 1 d D . . H7A H 0.3806 0.0663 0.2844 0.816 Uiso 1 1 calc R . . H7B H 0.3867 0.0157 0.3001 0.816 Uiso 1 1 calc R . . C8 C 0.2506(14) 0.0408(5) 0.3340(18) 0.117(8) Uani 1 1 d D . . H8A H 0.2637 0.0322 0.3983 0.140 Uiso 1 1 calc R . . H8B H 0.2012 0.0212 0.3076 0.140 Uiso 1 1 calc R . . C9 C 0.2714(11) 0.1184(6) 0.4344(15) 0.098(6) Uani 1 1 d . . . H9A H 0.2560 0.0999 0.4874 0.117 Uiso 1 1 calc R . . H9B H 0.3426 0.1169 0.4242 0.117 Uiso 1 1 calc R . . C10 C 0.2431(10) 0.1644(4) 0.4569(10) 0.068(3) Uani 1 1 d . . . H10A H 0.1746 0.1694 0.4381 0.081 Uiso 1 1 calc R . . H10B H 0.2482 0.1690 0.5239 0.081 Uiso 1 1 calc R . . C11 C 0.2814(8) 0.2375(4) 0.4206(8) 0.054(3) Uani 1 1 d . . . C12 C 0.2359(8) 0.2589(4) 0.3447(9) 0.058(3) Uani 1 1 d . . . C13 C 0.2072(9) 0.3029(5) 0.3550(9) 0.062(3) Uani 1 1 d . . . H13A H 0.1609 0.3160 0.3097 0.074 Uiso 1 1 calc R . . C14 C 0.2282(9) 0.3248(5) 0.4397(9) 0.065(3) Uani 1 1 d . . . H14A H 0.1910 0.3512 0.4554 0.078 Uiso 1 1 calc R . . C15 C 0.2789(9) 0.3037(4) 0.5076(8) 0.059(3) Uani 1 1 d . . . H15A H 0.2814 0.3175 0.5693 0.071 Uiso 1 1 calc R . . C16 C 0.3067(8) 0.2599(4) 0.5032(8) 0.056(3) Uani 1 1 d . . . C17 C 0.3637(9) 0.2389(4) 0.5826(8) 0.061(3) Uani 1 1 d . . . H17A H 0.3760 0.2606 0.6307 0.073 Uiso 1 1 calc R . . H17B H 0.3225 0.2163 0.6098 0.073 Uiso 1 1 calc R . . C18 C 0.4607(10) 0.2193(4) 0.5548(9) 0.061(3) Uani 1 1 d . . . C19 C 0.4800(12) 0.1741(5) 0.5632(10) 0.072(4) Uani 1 1 d . . . H19A H 0.4332 0.1559 0.5905 0.087 Uiso 1 1 calc R . . C20 C 0.5678(10) 0.1573(5) 0.5309(9) 0.067(3) Uani 1 1 d . . . H20A H 0.5800 0.1277 0.5373 0.081 Uiso 1 1 calc R . . C21 C 0.6392(10) 0.1836(4) 0.4888(9) 0.061(3) Uani 1 1 d . . . H21A H 0.6975 0.1713 0.4663 0.074 Uiso 1 1 calc R . . C22 C 0.6239(9) 0.2275(5) 0.4803(8) 0.060(3) Uani 1 1 d . . . C23 C 0.5356(8) 0.2448(4) 0.5149(7) 0.050(2) Uani 1 1 d . . . C24 C 0.7030(9) 0.2563(4) 0.4362(9) 0.059(3) Uani 1 1 d . . . H24A H 0.7267 0.2765 0.4835 0.071 Uiso 1 1 calc R . . H24B H 0.7587 0.2381 0.4189 0.071 Uiso 1 1 calc R . . C25 C 0.6723(8) 0.2819(4) 0.3524(9) 0.057(3) Uani 1 1 d . . . C26 C 0.6901(9) 0.3274(4) 0.3464(9) 0.062(3) Uani 1 1 d . . . H26A H 0.7296 0.3414 0.3958 0.074 Uiso 1 1 calc R . . C27 C 0.6659(10) 0.3512(4) 0.2678(11) 0.069(3) Uani 1 1 d . . . H27A H 0.6903 0.3810 0.2609 0.083 Uiso 1 1 calc R . . C28 C 0.6204(9) 0.3304(4) 0.1934(10) 0.063(3) Uani 1 1 d . . . H28A H 0.6091 0.3469 0.1356 0.075 Uiso 1 1 calc R . . C29 C 0.5987(9) 0.2865(4) 0.1937(8) 0.057(3) Uani 1 1 d . . . C30 C 0.6255(8) 0.2628(4) 0.2743(8) 0.051(3) Uani 1 1 d . . . C31 C 0.5502(9) 0.2653(5) 0.1066(9) 0.063(3) Uani 1 1 d . . . H31A H 0.5273 0.2882 0.0651 0.076 Uiso 1 1 calc R . . H31B H 0.6008 0.2489 0.0737 0.076 Uiso 1 1 calc R . . C32 C 0.4645(9) 0.2355(4) 0.1261(7) 0.056(3) Uani 1 1 d . . . C33 C 0.4680(11) 0.1929(5) 0.0931(9) 0.067(3) Uani 1 1 d . . . H33A H 0.5219 0.1836 0.0578 0.081 Uiso 1 1 calc R . . C34 C 0.3909(10) 0.1644(5) 0.1128(9) 0.066(3) Uani 1 1 d . . . H34A H 0.3919 0.1363 0.0884 0.079 Uiso 1 1 calc R . . C35 C 0.3098(10) 0.1778(4) 0.1704(8) 0.063(3) Uani 1 1 d . . . H35A H 0.2604 0.1580 0.1861 0.075 Uiso 1 1 calc R . . C36 C 0.3050(8) 0.2198(4) 0.2025(8) 0.055(3) Uani 1 1 d . . . C37 C 0.3809(8) 0.2483(4) 0.1761(8) 0.053(3) Uani 1 1 d . . . C38 C 0.2146(9) 0.2350(5) 0.2559(9) 0.061(3) Uani 1 1 d . . . H38A H 0.1756 0.2538 0.2153 0.073 Uiso 1 1 calc R . . H38B H 0.1741 0.2099 0.2704 0.073 Uiso 1 1 calc R . . C39 C 0.3233(12) 0.3169(5) 0.1336(10) 0.075(4) Uani 1 1 d . . . H39A H 0.2529 0.3106 0.1393 0.090 Uiso 1 1 calc R . . H39B H 0.3439 0.3082 0.0715 0.090 Uiso 1 1 calc R . . C40 C 0.3389(12) 0.3630(5) 0.1444(10) 0.072(4) Uani 1 1 d . . . H40A H 0.4063 0.3699 0.1257 0.087 Uiso 1 1 calc R . . H40B H 0.2940 0.3783 0.1021 0.087 Uiso 1 1 calc R . . C41 C 0.3251(11) 0.4256(5) 0.2450(10) 0.070(3) Uani 1 1 d . . . H41A H 0.2636 0.4374 0.2197 0.084 Uiso 1 1 calc R . . H41B H 0.3797 0.4374 0.2091 0.084 Uiso 1 1 calc R . . C42 C 0.3360(15) 0.4388(6) 0.3423(12) 0.093(5) Uani 1 1 d . . . H42A H 0.3397 0.4703 0.3458 0.111 Uiso 1 1 calc R . . H42B H 0.2780 0.4296 0.3771 0.111 Uiso 1 1 calc R . . C43 C 0.4474(19) 0.4387(6) 0.4706(14) 0.111(7) Uani 1 1 d . . . H43A H 0.4010 0.4294 0.5182 0.133 Uiso 1 1 calc R . . H43B H 0.4471 0.4703 0.4686 0.133 Uiso 1 1 calc R . . C44 C 0.5472(16) 0.4231(5) 0.4939(12) 0.091(5) Uani 1 1 d . . . H44A H 0.5929 0.4339 0.4470 0.110 Uiso 1 1 calc R . . H44B H 0.5671 0.4356 0.5535 0.110 Uiso 1 1 calc R . . C45 C 0.5261(13) 0.3588(5) 0.5835(10) 0.083(4) Uani 1 1 d . . . H45A H 0.4542 0.3606 0.5880 0.100 Uiso 1 1 calc R . . H45B H 0.5548 0.3747 0.6357 0.100 Uiso 1 1 calc R . . C46 C 0.5562(10) 0.3140(4) 0.5886(8) 0.062(3) Uani 1 1 d . . . H46A H 0.6283 0.3123 0.5898 0.074 Uiso 1 1 calc R . . H46B H 0.5316 0.3011 0.6459 0.074 Uiso 1 1 calc R . . N1 N 0.9513(10) 0.2924(8) 0.3263(11) 0.112(6) Uani 1 1 d . . . C47 C 0.995(2) 0.3821(8) 0.3774(19) 0.142(12) Uani 1 1 d . . . H47A H 0.9739 0.4032 0.3320 0.213 Uiso 1 1 calc R . . H47B H 1.0657 0.3839 0.3860 0.213 Uiso 1 1 calc R . . H47C H 0.9626 0.3877 0.4359 0.213 Uiso 1 1 calc R . . C48 C 0.972(2) 0.3449(18) 0.349(3) 0.20(2) Uani 1 1 d . . . N2 N 0.6587(15) 0.9269(8) 0.3164(17) 0.134(7) Uani 1 1 d . . . C49 C 0.493(2) 0.9510(9) 0.3897(19) 0.154(11) Uani 1 1 d . . . H49A H 0.4937 0.9806 0.4115 0.231 Uiso 1 1 calc R . . H49B H 0.4808 0.9318 0.4413 0.231 Uiso 1 1 calc R . . H49C H 0.4417 0.9475 0.3434 0.231 Uiso 1 1 calc R . . C50 C 0.592(2) 0.9403(10) 0.347(2) 0.154(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0606(14) 0.0562(15) 0.0484(12) -0.0006(11) 0.0011(11) -0.0031(11) Cu1 0.0823(11) 0.0547(9) 0.0636(9) 0.0031(7) 0.0006(8) 0.0019(8) Cu2 0.0849(11) 0.0504(8) 0.0620(9) 0.0040(7) 0.0147(8) 0.0063(7) Cu3 0.0832(11) 0.0500(8) 0.0624(9) 0.0018(7) 0.0086(8) 0.0021(7) I1 0.0729(5) 0.0474(4) 0.0587(5) 0.0011(3) 0.0056(4) 0.0042(3) I2 0.0793(6) 0.0449(4) 0.0585(5) 0.0016(3) 0.0041(4) 0.0002(4) I3 0.1097(7) 0.0518(5) 0.0553(5) 0.0009(4) 0.0154(4) 0.0063(4) I4 0.0766(6) 0.0546(5) 0.0628(5) -0.0026(4) 0.0066(4) 0.0004(4) S1 0.085(2) 0.0564(18) 0.0584(17) -0.0013(14) -0.0023(16) 0.0018(16) S2 0.100(3) 0.0515(19) 0.103(3) -0.0049(19) 0.045(2) -0.0054(18) O1 0.056(4) 0.055(5) 0.046(4) 0.003(3) 0.000(3) -0.005(4) O2 0.128(12) 0.188(18) 0.125(12) 0.014(12) -0.011(10) -0.055(12) O3 0.73(10) 0.58(9) 1.30(17) -0.76(11) 0.85(12) -0.54(8) O4 0.049(4) 0.061(5) 0.058(4) -0.005(4) 0.007(3) -0.005(4) O5 0.056(4) 0.056(5) 0.051(4) 0.004(4) -0.006(3) -0.003(4) O6 0.097(6) 0.062(5) 0.052(5) 0.005(4) 0.011(4) 0.012(5) O7 0.158(11) 0.072(7) 0.072(7) -0.008(6) -0.019(7) 0.012(7) O8 0.145(10) 0.061(6) 0.063(6) -0.002(5) -0.006(6) -0.021(6) O9 0.061(5) 0.056(5) 0.044(4) -0.005(3) -0.004(3) 0.002(4) C1 0.070(7) 0.056(7) 0.053(6) 0.005(5) 0.010(6) 0.005(6) C2 0.079(8) 0.057(7) 0.043(6) -0.007(5) 0.002(5) -0.003(6) C3 0.101(11) 0.064(9) 0.083(10) -0.010(8) -0.012(9) -0.007(8) C4 0.107(13) 0.104(13) 0.075(10) -0.022(9) 0.017(9) -0.021(11) C5 0.122(17) 0.15(2) 0.15(2) -0.062(19) -0.011(16) -0.018(16) C6 0.42(7) 0.44(8) 0.58(10) -0.41(8) 0.40(8) -0.31(7) C7 0.41(7) 0.12(3) 1.5(3) -0.20(8) 0.71(13) -0.04(4) C8 0.110(13) 0.057(9) 0.18(2) -0.041(12) 0.052(14) -0.012(9) C9 0.064(9) 0.080(11) 0.149(17) 0.028(11) 0.014(9) 0.011(8) C10 0.069(8) 0.065(8) 0.069(8) 0.002(6) 0.019(6) -0.004(6) C11 0.041(5) 0.069(8) 0.052(6) 0.001(6) -0.001(5) -0.005(5) C12 0.046(6) 0.070(8) 0.058(7) -0.008(6) 0.009(5) -0.013(5) C13 0.057(7) 0.068(8) 0.061(7) 0.004(6) -0.004(6) -0.001(6) C14 0.062(7) 0.073(8) 0.060(7) -0.009(6) 0.024(6) -0.008(6) C15 0.064(7) 0.068(8) 0.044(6) -0.001(6) 0.016(5) -0.007(6) C16 0.054(6) 0.067(8) 0.046(6) -0.003(5) 0.011(5) -0.006(6) C17 0.071(7) 0.065(8) 0.046(6) 0.009(6) 0.016(5) 0.002(6) C18 0.067(7) 0.056(7) 0.061(7) 0.003(6) -0.007(6) 0.001(6) C19 0.095(10) 0.059(8) 0.063(8) 0.015(6) -0.014(7) -0.006(7) C20 0.073(8) 0.068(8) 0.060(7) 0.006(6) -0.010(6) 0.010(7) C21 0.064(7) 0.064(8) 0.057(7) -0.009(6) -0.012(6) 0.011(6) C22 0.060(7) 0.073(8) 0.046(6) 0.004(6) -0.003(5) 0.002(6) C23 0.058(6) 0.050(6) 0.042(5) -0.006(5) -0.004(5) 0.005(5) C24 0.057(6) 0.067(8) 0.055(6) -0.003(6) -0.008(5) 0.003(6) C25 0.048(6) 0.057(7) 0.065(7) 0.007(6) 0.006(5) -0.002(5) C26 0.058(7) 0.064(8) 0.065(7) -0.012(6) 0.008(6) -0.009(6) C27 0.065(8) 0.051(7) 0.091(10) 0.002(7) 0.005(7) -0.009(6) C28 0.066(7) 0.059(7) 0.064(7) 0.006(6) 0.016(6) -0.001(6) C29 0.056(6) 0.060(7) 0.055(6) 0.012(5) 0.016(5) 0.000(5) C30 0.049(6) 0.058(7) 0.047(6) -0.006(5) 0.008(5) -0.005(5) C31 0.068(7) 0.068(8) 0.054(7) -0.003(6) 0.008(6) 0.010(6) C32 0.068(7) 0.062(7) 0.037(5) -0.001(5) 0.002(5) 0.004(6) C33 0.080(9) 0.071(8) 0.051(7) -0.002(6) -0.007(6) 0.007(7) C34 0.081(9) 0.068(8) 0.048(6) -0.008(6) -0.013(6) 0.012(7) C35 0.076(8) 0.063(8) 0.048(6) 0.004(6) -0.018(6) -0.005(6) C36 0.052(6) 0.070(8) 0.042(5) -0.002(5) -0.008(5) -0.002(6) C37 0.056(6) 0.052(6) 0.050(6) -0.001(5) -0.013(5) 0.004(5) C38 0.056(7) 0.072(8) 0.055(6) 0.003(6) -0.011(5) -0.009(6) C39 0.098(10) 0.068(9) 0.059(7) 0.001(7) -0.014(7) 0.023(8) C40 0.096(10) 0.063(8) 0.058(7) 0.000(6) -0.010(7) 0.005(7) C41 0.082(9) 0.056(7) 0.073(8) 0.010(7) 0.008(7) 0.004(7) C42 0.127(14) 0.068(10) 0.083(11) -0.013(8) 0.019(10) 0.013(10) C43 0.17(2) 0.067(11) 0.096(13) -0.027(10) 0.028(13) -0.011(12) C44 0.143(16) 0.062(9) 0.069(9) -0.012(8) 0.000(10) -0.013(10) C45 0.118(12) 0.072(9) 0.060(8) -0.008(7) -0.025(8) 0.004(9) C46 0.075(8) 0.067(8) 0.043(6) -0.009(6) -0.008(5) -0.004(6) N1 0.073(9) 0.18(2) 0.078(9) -0.001(11) 0.005(7) 0.013(10) C47 0.19(3) 0.111(17) 0.121(18) -0.027(15) -0.054(18) 0.078(19) C48 0.12(2) 0.30(5) 0.18(3) 0.10(4) 0.06(2) 0.12(3) N2 0.104(13) 0.154(19) 0.144(18) 0.035(15) -0.033(13) 0.023(13) C49 0.16(2) 0.15(2) 0.15(2) 0.08(2) 0.047(18) -0.021(18) C50 0.14(2) 0.15(2) 0.18(3) -0.07(2) -0.03(2) 0.013(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 K1 O5 2.718(8) . ? K1 O9 2.727(8) . ? K1 O7 2.766(12) . ? K1 O6 2.771(9) . ? K1 O8 2.843(11) . ? K1 C14 3.220(12) . ? K1 C27 3.230(14) . ? K1 C26 3.249(13) . ? K1 C28 3.285(12) . ? K1 C15 3.292(11) . ? K1 C13 3.384(13) . ? K1 C25 3.394(12) . ? Cu1 S1 2.346(4) . ? Cu1 I4 2.635(2) . ? Cu1 I1 2.6401(19) . ? Cu1 Cu2 2.688(3) . ? Cu1 I3 2.693(2) . ? Cu1 Cu3 2.730(2) . ? Cu2 S2 2.317(4) 1_655 ? Cu2 I1 2.6362(18) . ? Cu2 I2 2.6624(19) . ? Cu2 Cu3 2.701(2) . ? Cu2 I3 2.705(2) . ? Cu3 I4 2.606(2) . ? Cu3 I2 2.6618(18) 3_756 ? Cu3 I2 2.664(2) . ? Cu3 I3 2.7339(19) . ? I2 Cu3 2.6618(18) 3_756 ? S1 C3 1.821(15) . ? S1 C2 1.822(13) . ? S2 C9 1.85(2) . ? S2 C8 1.853(18) . ? S2 Cu2 2.317(4) 1_455 ? O1 C30 1.366(14) . ? O1 C1 1.443(14) . ? O2 C5 1.45(3) . ? O2 C4 1.45(2) . ? O3 C7 1.450(7) . ? O3 C6 1.453(10) . ? O4 C11 1.375(15) . ? O4 C10 1.442(15) . ? O5 C37 1.397(14) . ? O5 C39 1.427(15) . ? O6 C40 1.406(16) . ? O6 C41 1.446(17) . ? O7 C42 1.34(2) . ? O7 C43 1.44(2) . ? O8 C45 1.398(19) . ? O8 C44 1.414(19) . ? O9 C23 1.413(14) . ? O9 C46 1.435(13) . ? C1 C2 1.515(18) . ? C3 C4 1.43(2) . ? C5 C6 1.496(7) . ? C7 C8 1.498(7) . ? C9 C10 1.50(2) . ? C11 C16 1.405(17) . ? C11 C12 1.405(18) . ? C12 C13 1.415(19) . ? C12 C38 1.491(17) . ? C13 C14 1.411(18) . ? C14 C15 1.347(19) . ? C15 C16 1.398(18) . ? C16 C17 1.510(17) . ? C17 C18 1.493(17) . ? C18 C23 1.401(17) . ? C18 C19 1.418(19) . ? C19 C20 1.37(2) . ? C20 C21 1.40(2) . ? C21 C22 1.369(19) . ? C22 C23 1.395(17) . ? C22 C24 1.525(18) . ? C24 C25 1.488(17) . ? C25 C30 1.404(17) . ? C25 C26 1.423(18) . ? C26 C27 1.38(2) . ? C27 C28 1.38(2) . ? C28 C29 1.383(18) . ? C29 C30 1.406(17) . ? C29 C31 1.544(18) . ? C31 C32 1.498(18) . ? C32 C37 1.392(17) . ? C32 C33 1.393(18) . ? C33 C34 1.39(2) . ? C34 C35 1.430(19) . ? C35 C36 1.373(18) . ? C36 C37 1.399(17) . ? C36 C38 1.514(17) . ? C39 C40 1.44(2) . ? C41 C42 1.45(2) . ? C43 C44 1.46(3) . ? C45 C46 1.44(2) . ? N1 C48 1.67(6) . ? C47 C48 1.25(6) . ? N2 C50 1.08(3) . ? C49 C50 1.50(4) . ? 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 K1 O9 122.9(3) . . ? O5 K1 O7 120.7(3) . . ? O9 K1 O7 115.2(3) . . ? O5 K1 O6 61.4(3) . . ? O9 K1 O6 161.4(3) . . ? O7 K1 O6 59.7(3) . . ? O5 K1 O8 169.7(3) . . ? O9 K1 O8 58.8(3) . . ? O7 K1 O8 61.2(3) . . ? O6 K1 O8 120.8(3) . . ? O5 K1 C14 86.6(3) . . ? O9 K1 C14 88.3(3) . . ? O7 K1 C14 83.7(4) . . ? O6 K1 C14 73.5(3) . . ? O8 K1 C14 103.8(4) . . ? O5 K1 C27 94.5(3) . . ? O9 K1 C27 95.3(3) . . ? O7 K1 C27 91.4(4) . . ? O6 K1 C27 102.6(3) . . ? O8 K1 C27 75.2(4) . . ? C14 K1 C27 174.8(4) . . ? O5 K1 C26 106.7(3) . . ? O9 K1 C26 70.8(3) . . ? O7 K1 C26 102.4(4) . . ? O6 K1 C26 127.1(3) . . ? O8 K1 C26 63.5(4) . . ? C14 K1 C26 159.0(4) . . ? C27 K1 C26 24.5(3) . . ? O5 K1 C28 70.1(3) . . ? O9 K1 C28 108.5(3) . . ? O7 K1 C28 103.2(4) . . ? O6 K1 C28 90.0(3) . . ? O8 K1 C28 99.6(4) . . ? C14 K1 C28 156.0(4) . . ? C27 K1 C28 24.4(4) . . ? C26 K1 C28 42.6(3) . . ? O5 K1 C15 99.2(3) . . ? O9 K1 C15 64.5(3) . . ? O7 K1 C15 94.5(4) . . ? O6 K1 C15 97.3(3) . . ? O8 K1 C15 90.7(3) . . ? C14 K1 C15 23.8(3) . . ? C27 K1 C15 159.6(4) . . ? C26 K1 C15 135.2(3) . . ? C28 K1 C15 162.1(3) . . ? O5 K1 C13 62.0(3) . . ? O9 K1 C13 101.0(3) . . ? O7 K1 C13 97.1(4) . . ? O6 K1 C13 63.8(3) . . ? O8 K1 C13 128.3(4) . . ? C14 K1 C13 24.5(3) . . ? C27 K1 C13 156.2(4) . . ? C26 K1 C13 160.5(3) . . ? C28 K1 C13 131.9(3) . . ? C15 K1 C13 41.7(3) . . ? O5 K1 C25 94.5(3) . . ? O9 K1 C25 59.1(3) . . ? O7 K1 C25 126.5(4) . . ? O6 K1 C25 139.2(3) . . ? O8 K1 C25 77.7(3) . . ? C14 K1 C25 141.7(4) . . ? C27 K1 C25 43.3(3) . . ? C26 K1 C25 24.6(3) . . ? C28 K1 C25 49.6(3) . . ? C15 K1 C25 119.9(3) . . ? C13 K1 C25 136.1(3) . . ? S1 Cu1 I4 105.60(11) . . ? S1 Cu1 I1 106.30(11) . . ? I4 Cu1 I1 120.38(7) . . ? S1 Cu1 Cu2 143.16(12) . . ? I4 Cu1 Cu2 110.79(7) . . ? I1 Cu1 Cu2 59.30(5) . . ? S1 Cu1 I3 102.84(11) . . ? I4 Cu1 I3 108.46(7) . . ? I1 Cu1 I3 111.62(7) . . ? Cu2 Cu1 I3 60.36(6) . . ? S1 Cu1 Cu3 144.03(12) . . ? I4 Cu1 Cu3 58.08(5) . . ? I1 Cu1 Cu3 109.51(8) . . ? Cu2 Cu1 Cu3 59.78(6) . . ? I3 Cu1 Cu3 60.54(5) . . ? S2 Cu2 I1 112.03(12) 1_655 . ? S2 Cu2 I2 102.79(14) 1_655 . ? I1 Cu2 I2 111.88(6) . . ? S2 Cu2 Cu1 148.80(15) 1_655 . ? I1 Cu2 Cu1 59.44(5) . . ? I2 Cu2 Cu1 108.17(7) . . ? S2 Cu2 Cu3 137.42(12) 1_655 . ? I1 Cu2 Cu3 110.54(7) . . ? I2 Cu2 Cu3 59.55(6) . . ? Cu1 Cu2 Cu3 60.88(6) . . ? S2 Cu2 I3 103.40(13) 1_655 . ? I1 Cu2 I3 111.34(7) . . ? I2 Cu2 I3 114.78(6) . . ? Cu1 Cu2 I3 59.90(6) . . ? Cu3 Cu2 I3 60.76(6) . . ? I4 Cu3 I2 115.22(7) . 3_756 ? I4 Cu3 I2 116.05(7) . . ? I2 Cu3 I2 103.03(6) 3_756 . ? I4 Cu3 Cu2 111.32(7) . . ? I2 Cu3 Cu2 133.11(8) 3_756 . ? I2 Cu3 Cu2 59.51(6) . . ? I4 Cu3 Cu1 59.13(6) . . ? I2 Cu3 Cu1 148.40(8) 3_756 . ? I2 Cu3 Cu1 106.90(7) . . ? Cu2 Cu3 Cu1 59.34(6) . . ? I4 Cu3 I3 108.09(7) . . ? I2 Cu3 I3 99.54(6) 3_756 . ? I2 Cu3 I3 113.79(7) . . ? Cu2 Cu3 I3 59.71(6) . . ? Cu1 Cu3 I3 59.05(5) . . ? Cu2 I1 Cu1 61.26(6) . . ? Cu3 I2 Cu2 117.87(6) 3_756 . ? Cu3 I2 Cu3 76.97(6) 3_756 . ? Cu2 I2 Cu3 60.94(6) . . ? Cu1 I3 Cu2 59.74(6) . . ? Cu1 I3 Cu3 60.41(5) . . ? Cu2 I3 Cu3 59.53(5) . . ? Cu3 I4 Cu1 62.79(6) . . ? C3 S1 C2 99.1(7) . . ? C3 S1 Cu1 105.0(5) . . ? C2 S1 Cu1 105.6(4) . . ? C9 S2 C8 98.1(10) . . ? C9 S2 Cu2 105.9(6) . 1_455 ? C8 S2 Cu2 101.9(5) . 1_455 ? C30 O1 C1 113.4(8) . . ? C5 O2 C4 114.7(18) . . ? C7 O3 C6 146(5) . . ? C11 O4 C10 114.2(9) . . ? C37 O5 C39 111.0(9) . . ? C37 O5 K1 130.4(6) . . ? C39 O5 K1 118.5(7) . . ? C40 O6 C41 115.3(10) . . ? C40 O6 K1 108.2(8) . . ? C41 O6 K1 115.9(8) . . ? C42 O7 C43 116.6(15) . . ? C42 O7 K1 117.4(10) . . ? C43 O7 K1 115.7(11) . . ? C45 O8 C44 115.3(12) . . ? C45 O8 K1 105.8(8) . . ? C44 O8 K1 112.7(9) . . ? C23 O9 C46 114.0(9) . . ? C23 O9 K1 125.3(6) . . ? C46 O9 K1 119.9(7) . . ? O1 C1 C2 107.9(10) . . ? C1 C2 S1 108.7(9) . . ? C4 C3 S1 111.7(13) . . ? C3 C4 O2 109.5(17) . . ? O2 C5 C6 107(3) . . ? O3 C6 C5 111(3) . . ? O3 C7 C8 107(3) . . ? C7 C8 S2 106.7(16) . . ? C10 C9 S2 112.2(12) . . ? O4 C10 C9 110.6(11) . . ? O4 C11 C16 120.7(11) . . ? O4 C11 C12 117.8(11) . . ? C16 C11 C12 121.3(12) . . ? C11 C12 C13 119.0(11) . . ? C11 C12 C38 120.4(12) . . ? C13 C12 C38 120.6(12) . . ? C14 C13 C12 119.4(12) . . ? C14 C13 K1 71.2(7) . . ? C12 C13 K1 90.1(7) . . ? C15 C14 C13 119.0(13) . . ? C15 C14 K1 81.1(7) . . ? C13 C14 K1 84.3(7) . . ? C14 C15 C16 124.4(12) . . ? C14 C15 K1 75.1(7) . . ? C16 C15 K1 92.9(7) . . ? C15 C16 C11 116.5(11) . . ? C15 C16 C17 120.8(11) . . ? C11 C16 C17 122.6(12) . . ? C18 C17 C16 114.3(10) . . ? C23 C18 C19 116.8(12) . . ? C23 C18 C17 121.0(11) . . ? C19 C18 C17 122.2(13) . . ? C20 C19 C18 119.9(14) . . ? C19 C20 C21 121.6(13) . . ? C22 C21 C20 120.3(13) . . ? C21 C22 C23 118.2(12) . . ? C21 C22 C24 120.3(12) . . ? C23 C22 C24 121.4(12) . . ? C22 C23 C18 123.1(11) . . ? C22 C23 O9 119.8(11) . . ? C18 C23 O9 117.1(10) . . ? C25 C24 C22 116.8(10) . . ? C30 C25 C26 115.9(12) . . ? C30 C25 C24 122.6(11) . . ? C26 C25 C24 121.5(12) . . ? C30 C25 K1 79.4(7) . . ? C26 C25 K1 72.0(7) . . ? C24 C25 K1 118.3(8) . . ? C27 C26 C25 122.1(12) . . ? C27 C26 K1 77.0(8) . . ? C25 C26 K1 83.4(7) . . ? C26 C27 C28 119.0(13) . . ? C26 C27 K1 78.5(8) . . ? C28 C27 K1 80.0(7) . . ? C27 C28 C29 122.8(13) . . ? C27 C28 K1 75.6(8) . . ? C29 C28 K1 82.9(7) . . ? C28 C29 C30 117.0(12) . . ? C28 C29 C31 119.8(11) . . ? C30 C29 C31 123.1(11) . . ? C28 C29 K1 73.3(7) . . ? C30 C29 K1 79.1(7) . . ? C31 C29 K1 118.7(7) . . ? O1 C30 C25 117.2(10) . . ? O1 C30 C29 119.7(10) . . ? C25 C30 C29 123.1(11) . . ? O1 C30 K1 116.2(6) . . ? C25 C30 K1 76.9(7) . . ? C29 C30 K1 77.2(7) . . ? C32 C31 C29 115.3(10) . . ? C37 C32 C33 117.9(12) . . ? C37 C32 C31 123.3(11) . . ? C33 C32 C31 118.9(11) . . ? C34 C33 C32 119.8(13) . . ? C33 C34 C35 120.6(13) . . ? C36 C35 C34 120.1(13) . . ? C35 C36 C37 117.5(11) . . ? C35 C36 C38 120.0(12) . . ? C37 C36 C38 122.2(11) . . ? C32 C37 O5 115.8(11) . . ? C32 C37 C36 123.8(11) . . ? O5 C37 C36 120.4(10) . . ? C12 C38 C36 115.6(9) . . ? O5 C39 C40 112.4(12) . . ? O6 C40 C39 114.6(12) . . ? O6 C40 K1 49.2(6) . . ? C39 C40 K1 84.0(8) . . ? O6 C41 C42 111.6(12) . . ? O7 C42 C41 111.3(14) . . ? O7 C43 C44 109.4(15) . . ? O8 C44 C43 115.1(15) . . ? O8 C45 C46 110.5(13) . . ? O8 C45 K1 51.6(6) . . ? C46 C45 K1 85.1(8) . . ? O9 C46 C45 110.7(11) . . ? C47 C48 N1 171(3) . . ? N2 C50 C49 170(4) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 3.091 _refine_diff_density_min -1.952 _refine_diff_density_rms 0.249 #=================================================END data_3 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H62 Cu Hg I4 K N2 O11 S2' _chemical_formula_weight 1741.97 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' '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 19.0690(11) _cell_length_b 20.4124(12) _cell_length_c 15.6455(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6089.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8854 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.24 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.900 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 5.085 _exptl_absorpt_correction_type 'empirical (SADABS)' _exptl_absorpt_correction_T_min 0.2355 _exptl_absorpt_correction_T_max 0.4295 _exptl_absorpt_process_details 'SADABS, sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35320 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.1033 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.00 _reflns_number_total 12701 _reflns_number_gt 8910 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0643P)^2^+7.3347P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.015(7) _refine_ls_number_reflns 12701 _refine_ls_number_parameters 592 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1485 _refine_ls_wR_factor_gt 0.1296 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.018 _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 Cu1 Cu 0.66868(8) 0.24949(7) 0.04083(9) 0.0347(4) Uani 1 1 d . . . Hg1 Hg 0.66423(2) 0.25619(2) -0.18698(3) 0.03774(13) Uani 1 1 d . . . K1 K 0.41612(12) 0.33521(14) 0.50784(16) 0.0306(5) Uiso 1 1 d . . . I1 I 0.76969(4) 0.20869(5) -0.06989(5) 0.0444(2) Uani 1 1 d . . . I2 I 0.56295(4) 0.29310(4) -0.05883(4) 0.03594(19) Uani 1 1 d . . . I3 I 0.61363(6) 0.14734(5) -0.26501(6) 0.0590(3) Uani 1 1 d . . . I4 I 0.70921(5) 0.36885(5) -0.25979(6) 0.0483(2) Uani 1 1 d . . . S1 S 0.63363(16) 0.15467(15) 0.10388(18) 0.0337(7) Uani 1 1 d . . . S2 S 0.20974(16) 0.15615(15) 0.10218(18) 0.0324(6) Uani 1 1 d . . . O1 O 0.5244(4) 0.2269(4) 0.2979(5) 0.0299(18) Uani 1 1 d . . . O2 O 0.4956(5) 0.0546(5) 0.0570(7) 0.055(3) Uani 1 1 d . . . O3 O 0.3496(5) 0.0568(5) 0.0629(5) 0.044(2) Uani 1 1 d . . . O4 O 0.3037(4) 0.2335(4) 0.3047(5) 0.0315(18) Uani 1 1 d . . . O5 O 0.4070(4) 0.2005(4) 0.5222(5) 0.0289(18) Uani 1 1 d . . . O6 O 0.4337(5) 0.2726(5) 0.6650(5) 0.052(3) Uani 1 1 d . . . O7 O 0.4434(6) 0.4088(5) 0.6571(6) 0.063(3) Uani 1 1 d . . . O8 O 0.4400(8) 0.4731(5) 0.4998(6) 0.085(4) Uani 1 1 d . . . O9 O 0.4147(4) 0.4031(4) 0.3558(5) 0.0256(17) Uani 1 1 d . . . C1 C 0.5822(6) 0.2090(7) 0.2458(9) 0.042(2) Uani 1 1 d . . . H1A H 0.6156 0.1822 0.2793 0.050 Uiso 1 1 calc R . . H1B H 0.6069 0.2488 0.2261 0.050 Uiso 1 1 calc R . . C2 C 0.5564(6) 0.1704(7) 0.1699(7) 0.036(3) Uani 1 1 d . . . H2A H 0.5211 0.1959 0.1375 0.043 Uiso 1 1 calc R . . H2B H 0.5348 0.1287 0.1886 0.043 Uiso 1 1 calc R . . C3 C 0.6028(8) 0.1046(8) 0.0171(10) 0.059(4) Uani 1 1 d . . . H3A H 0.5697 0.1307 -0.0179 0.071 Uiso 1 1 calc R . . H3B H 0.6432 0.0930 -0.0197 0.071 Uiso 1 1 calc R . . C4 C 0.5658(8) 0.0409(7) 0.0457(9) 0.050(4) Uani 1 1 d . . . H4A H 0.5718 0.0065 0.0017 0.060 Uiso 1 1 calc R . . H4B H 0.5865 0.0250 0.0999 0.060 Uiso 1 1 calc R . . C5 C 0.4550(7) 0.0069(6) 0.1003(8) 0.041(3) Uani 1 1 d . . . H5A H 0.4484 0.0209 0.1604 0.049 Uiso 1 1 calc R . . H5B H 0.4809 -0.0351 0.1008 0.049 Uiso 1 1 calc R . . C6 C 0.3851(9) -0.0035(8) 0.0603(12) 0.067(5) Uani 1 1 d . . . H6A H 0.3906 -0.0184 0.0005 0.080 Uiso 1 1 calc R . . H6B H 0.3584 -0.0372 0.0922 0.080 Uiso 1 1 calc R . . C7 C 0.2849(9) 0.0503(8) 0.0264(12) 0.070(5) Uani 1 1 d . . . H7A H 0.2539 0.0242 0.0640 0.083 Uiso 1 1 calc R . . H7B H 0.2890 0.0274 -0.0292 0.083 Uiso 1 1 calc R . . C8 C 0.2540(6) 0.1195(7) 0.0131(8) 0.042(2) Uani 1 1 d . . . H8A H 0.2206 0.1175 -0.0352 0.050 Uiso 1 1 calc R . . H8B H 0.2927 0.1491 -0.0041 0.050 Uiso 1 1 calc R . . C9 C 0.2818(6) 0.1755(6) 0.1756(7) 0.033(3) Uani 1 1 d . . . H9A H 0.3036 0.1348 0.1977 0.040 Uiso 1 1 calc R . . H9B H 0.3183 0.2017 0.1463 0.040 Uiso 1 1 calc R . . C10 C 0.2492(5) 0.2139(7) 0.2468(8) 0.040(3) Uani 1 1 d . . . H10A H 0.2251 0.2531 0.2237 0.048 Uiso 1 1 calc R . . H10B H 0.2142 0.1867 0.2772 0.048 Uiso 1 1 calc R . . C11 C 0.2791(5) 0.2697(7) 0.3735(7) 0.032(2) Uani 1 1 d . . . C12 C 0.2704(6) 0.3393(7) 0.3662(7) 0.032(3) Uani 1 1 d . . . C13 C 0.2480(5) 0.3732(6) 0.4355(9) 0.040(3) Uani 1 1 d . . . H13A H 0.2345 0.4202 0.4287 0.048 Uiso 1 1 calc R . . C14 C 0.2354(6) 0.3420(7) 0.5136(8) 0.040(3) Uani 1 1 d . . . H14A H 0.2110 0.3659 0.5608 0.048 Uiso 1 1 calc R . . C15 C 0.2455(6) 0.2749(7) 0.5187(8) 0.037(3) Uani 1 1 d . . . H15A H 0.2307 0.2521 0.5723 0.045 Uiso 1 1 calc R . . C16 C 0.2671(5) 0.2368(6) 0.4505(7) 0.029(3) Uani 1 1 d . . . C17 C 0.2748(6) 0.1638(6) 0.4582(7) 0.033(3) Uani 1 1 d . . . H17A H 0.2687 0.1522 0.5192 0.040 Uiso 1 1 calc R . . H17B H 0.2355 0.1434 0.4265 0.040 Uiso 1 1 calc R . . C18 C 0.3409(6) 0.1327(6) 0.4281(8) 0.036(3) Uani 1 1 d . . . C19 C 0.3388(7) 0.0850(7) 0.3658(8) 0.045(3) Uani 1 1 d . . . H19A H 0.2947 0.0714 0.3439 0.053 Uiso 1 1 calc R . . C20 C 0.3998(9) 0.0563(7) 0.3341(8) 0.056(4) Uani 1 1 d . . . H20A H 0.3976 0.0208 0.2950 0.068 Uiso 1 1 calc R . . C21 C 0.4635(7) 0.0808(6) 0.3611(8) 0.041(3) Uani 1 1 d . . . H21A H 0.5053 0.0637 0.3366 0.049 Uiso 1 1 calc R . . C22 C 0.4689(6) 0.1299(6) 0.4230(8) 0.034(3) Uani 1 1 d . . . C23 C 0.4053(5) 0.1535(6) 0.4576(7) 0.028(3) Uani 1 1 d . . . C24 C 0.5390(6) 0.1557(7) 0.4523(8) 0.043(3) Uani 1 1 d . . . H24A H 0.5458 0.1420 0.5124 0.051 Uiso 1 1 calc R . . H24B H 0.5758 0.1339 0.4180 0.051 Uiso 1 1 calc R . . C25 C 0.5513(5) 0.2280(6) 0.4475(7) 0.030(3) Uani 1 1 d . . . C26 C 0.5723(6) 0.2649(8) 0.5196(8) 0.040(3) Uani 1 1 d . . . H26A H 0.5861 0.2415 0.5732 0.048 Uiso 1 1 calc R . . C27 C 0.5829(6) 0.3280(7) 0.5134(8) 0.034(3) Uani 1 1 d . . . H27A H 0.6071 0.3502 0.5622 0.041 Uiso 1 1 calc R . . C28 C 0.5761(5) 0.3624(6) 0.4395(8) 0.033(3) Uani 1 1 d . . . H28A H 0.5940 0.4084 0.4368 0.040 Uiso 1 1 calc R . . C29 C 0.5551(5) 0.3306(7) 0.3626(7) 0.032(2) Uani 1 1 d . . . C30 C 0.5440(5) 0.2616(6) 0.3691(7) 0.027(3) Uani 1 1 d . . . C31 C 0.5478(6) 0.3678(6) 0.2825(7) 0.030(3) Uani 1 1 d . . . H31A H 0.5859 0.3545 0.2432 0.036 Uiso 1 1 calc R . . H31B H 0.5541 0.4149 0.2952 0.036 Uiso 1 1 calc R . . C32 C 0.4782(5) 0.3588(6) 0.2368(6) 0.027(2) Uani 1 1 d . . . C33 C 0.4771(6) 0.3342(6) 0.1516(6) 0.033(3) Uani 1 1 d . . . H33A H 0.5198 0.3252 0.1224 0.039 Uiso 1 1 calc R . . C34 C 0.4147(6) 0.3237(7) 0.1126(7) 0.037(3) Uani 1 1 d . . . H34A H 0.4143 0.3082 0.0553 0.044 Uiso 1 1 calc R . . C35 C 0.3523(7) 0.3345(7) 0.1530(8) 0.042(3) Uani 1 1 d . . . H35A H 0.3098 0.3237 0.1245 0.050 Uiso 1 1 calc R . . C36 C 0.3492(6) 0.3615(6) 0.2363(8) 0.035(3) Uani 1 1 d . . . C37 C 0.4143(6) 0.3747(6) 0.2741(7) 0.029(3) Uani 1 1 d . . . C38 C 0.2823(6) 0.3737(7) 0.2798(7) 0.040(3) Uani 1 1 d . . . H38A H 0.2440 0.3606 0.2407 0.048 Uiso 1 1 calc R . . H38B H 0.2780 0.4215 0.2890 0.048 Uiso 1 1 calc R . . C39 C 0.4119(7) 0.1689(7) 0.6057(8) 0.046(3) Uani 1 1 d . . . H39A H 0.4605 0.1540 0.6161 0.055 Uiso 1 1 calc R . . H39B H 0.3805 0.1303 0.6078 0.055 Uiso 1 1 calc R . . C40 C 0.3903(10) 0.2186(9) 0.6738(9) 0.061(4) Uani 1 1 d . . . H40A H 0.3407 0.2316 0.6657 0.074 Uiso 1 1 calc R . . H40B H 0.3955 0.1994 0.7315 0.074 Uiso 1 1 calc R . . C41 C 0.4326(10) 0.3178(10) 0.7375(11) 0.072(5) Uani 1 1 d . . . H41A H 0.3838 0.3326 0.7474 0.087 Uiso 1 1 calc R . . H41B H 0.4485 0.2944 0.7894 0.087 Uiso 1 1 calc R . . C42 C 0.4737(9) 0.3703(9) 0.7247(10) 0.073(5) Uani 1 1 d . . . H42A H 0.5216 0.3561 0.7086 0.088 Uiso 1 1 calc R . . H42B H 0.4769 0.3966 0.7777 0.088 Uiso 1 1 calc R . . C43 C 0.4771(12) 0.4696(9) 0.6397(12) 0.089(6) Uani 1 1 d . . . H43A H 0.5246 0.4614 0.6165 0.107 Uiso 1 1 calc R . . H43B H 0.4821 0.4948 0.6934 0.107 Uiso 1 1 calc R . . C44 C 0.4373(13) 0.5070(9) 0.5795(10) 0.089(7) Uani 1 1 d . . . H44A H 0.3881 0.5112 0.5990 0.107 Uiso 1 1 calc R . . H44B H 0.4575 0.5514 0.5734 0.107 Uiso 1 1 calc R . . C45 C 0.4075(8) 0.5000(7) 0.4348(13) 0.064(4) Uani 1 1 d . . . H45A H 0.4205 0.5469 0.4326 0.076 Uiso 1 1 calc R . . H45B H 0.3564 0.4976 0.4454 0.076 Uiso 1 1 calc R . . C46 C 0.4212(9) 0.4724(7) 0.3556(9) 0.059(5) Uani 1 1 d . . . H46A H 0.4693 0.4843 0.3377 0.071 Uiso 1 1 calc R . . H46B H 0.3882 0.4909 0.3131 0.071 Uiso 1 1 calc R . . N1 N 0.4445(17) 0.1038(14) -0.161(2) 0.219(14) Uiso 1 1 d D . . C47 C 0.4138(15) 0.0630(13) -0.193(2) 0.162(13) Uiso 1 1 d D . . C48 C 0.3749(12) 0.0010(11) -0.2181(15) 0.115(8) Uiso 1 1 d D . . H48A H 0.4088 -0.0339 -0.2302 0.172 Uiso 1 1 calc R . . H48B H 0.3467 0.0095 -0.2693 0.172 Uiso 1 1 calc R . . H48C H 0.3441 -0.0127 -0.1712 0.172 Uiso 1 1 calc R . . N2 N 0.8637(8) 0.0058(11) 0.0840(12) 0.116(6) Uiso 1 1 d D . . C49 C 0.8114(8) 0.0004(10) 0.0500(12) 0.078(5) Uiso 1 1 d D . . C50 C 0.7355(7) -0.0088(10) 0.0228(12) 0.083(6) Uiso 1 1 d D . . H50A H 0.7133 -0.0419 0.0591 0.124 Uiso 1 1 calc R . . H50B H 0.7339 -0.0231 -0.0370 0.124 Uiso 1 1 calc R . . H50C H 0.7103 0.0329 0.0286 0.124 Uiso 1 1 calc R . . O10W O 0.2176(8) 0.0009(8) 0.2251(11) 0.124(5) Uiso 1 1 d . . . O11W O 0.8497(5) 0.0306(5) -0.1371(6) 0.056(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0417(9) 0.0351(10) 0.0274(7) 0.0012(6) -0.0019(6) -0.0102(7) Hg1 0.0478(3) 0.0411(3) 0.0243(2) -0.0022(3) 0.0008(2) 0.0005(2) I1 0.0464(4) 0.0594(6) 0.0274(4) -0.0013(4) -0.0022(3) 0.0171(4) I2 0.0363(4) 0.0501(5) 0.0215(3) -0.0024(4) 0.0011(3) 0.0040(3) I3 0.1017(8) 0.0424(6) 0.0327(4) -0.0082(4) -0.0092(5) -0.0061(5) I4 0.0547(5) 0.0493(6) 0.0409(4) 0.0070(4) 0.0077(4) -0.0040(4) S1 0.0479(17) 0.0293(17) 0.0238(13) -0.0039(13) 0.0016(12) -0.0046(13) S2 0.0410(16) 0.0288(17) 0.0275(13) -0.0017(13) -0.0023(12) 0.0017(13) O1 0.024(4) 0.037(5) 0.028(4) -0.005(4) 0.003(3) -0.005(3) O2 0.062(7) 0.037(6) 0.067(6) 0.017(5) -0.009(5) -0.013(5) O3 0.047(5) 0.048(6) 0.038(5) -0.002(4) -0.002(4) 0.010(4) O4 0.023(4) 0.051(5) 0.020(4) -0.008(4) -0.001(3) 0.010(3) O5 0.031(4) 0.025(5) 0.031(4) -0.002(4) 0.001(3) 0.002(3) O6 0.070(6) 0.061(7) 0.025(4) 0.008(4) -0.005(4) -0.020(5) O7 0.096(8) 0.035(6) 0.058(6) -0.027(5) -0.031(6) 0.010(5) O8 0.190(13) 0.028(6) 0.036(6) -0.012(5) -0.031(7) -0.011(7) O9 0.033(4) 0.022(5) 0.021(3) -0.002(3) 0.003(3) -0.002(3) C1 0.030(4) 0.044(6) 0.051(5) -0.021(5) 0.000(4) 0.005(4) C2 0.032(6) 0.043(8) 0.034(6) -0.006(6) -0.003(5) -0.011(6) C3 0.078(10) 0.044(9) 0.055(9) -0.019(8) -0.004(7) -0.031(8) C4 0.063(9) 0.043(9) 0.044(8) -0.023(7) 0.013(6) -0.018(7) C5 0.047(8) 0.028(8) 0.048(7) 0.012(6) 0.000(6) 0.000(6) C6 0.080(11) 0.043(10) 0.077(11) 0.033(9) 0.005(9) 0.024(9) C7 0.080(11) 0.050(10) 0.079(11) -0.041(9) -0.015(9) 0.022(8) C8 0.030(4) 0.044(6) 0.051(5) -0.021(5) 0.000(4) 0.005(4) C9 0.039(7) 0.030(7) 0.031(6) -0.010(5) -0.008(5) 0.009(5) C10 0.021(6) 0.047(8) 0.051(7) -0.025(7) -0.002(5) 0.009(5) C11 0.009(4) 0.054(6) 0.033(4) -0.002(4) 0.001(3) 0.005(3) C12 0.023(6) 0.050(9) 0.024(5) -0.004(5) 0.002(4) 0.004(5) C13 0.019(5) 0.042(8) 0.060(8) -0.013(7) -0.009(6) 0.008(5) C14 0.026(6) 0.059(10) 0.036(6) -0.015(7) 0.007(5) 0.000(6) C15 0.026(6) 0.057(9) 0.030(6) -0.008(6) 0.001(5) 0.001(6) C16 0.021(5) 0.044(8) 0.022(5) -0.007(5) -0.002(4) 0.001(4) C17 0.041(7) 0.031(7) 0.028(6) -0.001(5) 0.005(4) -0.012(5) C18 0.033(6) 0.036(7) 0.040(6) 0.004(6) -0.006(5) -0.009(5) C19 0.050(8) 0.039(8) 0.045(7) -0.010(6) 0.009(6) -0.005(6) C20 0.108(13) 0.029(8) 0.032(8) -0.008(6) 0.011(7) 0.005(8) C21 0.042(7) 0.029(8) 0.050(7) 0.005(6) 0.020(6) 0.000(6) C22 0.042(6) 0.025(7) 0.037(6) 0.012(6) 0.007(5) 0.007(5) C23 0.033(6) 0.027(7) 0.023(5) 0.010(5) 0.004(4) 0.001(5) C24 0.035(6) 0.046(8) 0.048(7) 0.025(7) 0.009(5) 0.012(6) C25 0.021(5) 0.036(7) 0.033(6) 0.011(5) 0.000(4) 0.008(4) C26 0.034(7) 0.064(11) 0.023(6) -0.002(6) -0.001(4) 0.004(6) C27 0.028(6) 0.034(8) 0.040(7) 0.000(6) -0.002(5) 0.008(5) C28 0.022(5) 0.047(8) 0.030(6) -0.013(6) -0.005(4) -0.002(5) C29 0.009(4) 0.054(6) 0.033(4) -0.002(4) 0.001(3) 0.005(3) C30 0.015(5) 0.036(7) 0.031(6) 0.004(5) 0.007(4) 0.001(5) C31 0.029(6) 0.032(7) 0.030(5) -0.001(5) 0.007(4) 0.001(5) C32 0.038(6) 0.029(7) 0.014(4) 0.003(5) 0.004(4) -0.004(5) C33 0.036(6) 0.044(8) 0.019(5) 0.004(5) 0.007(4) 0.007(5) C34 0.039(7) 0.054(9) 0.017(5) -0.002(6) 0.001(4) -0.001(6) C35 0.055(8) 0.044(9) 0.027(6) -0.001(6) -0.006(5) -0.006(6) C36 0.035(6) 0.040(8) 0.029(6) -0.001(6) -0.007(5) 0.010(5) C37 0.041(6) 0.025(7) 0.020(5) -0.003(5) 0.000(4) 0.000(5) C38 0.045(7) 0.048(9) 0.029(6) 0.004(6) -0.004(5) 0.005(6) C39 0.067(9) 0.045(9) 0.026(6) 0.015(6) -0.001(6) -0.006(7) C40 0.088(11) 0.069(12) 0.026(7) 0.009(7) 0.002(7) -0.001(9) C41 0.093(13) 0.080(13) 0.044(9) -0.022(9) -0.022(9) 0.001(10) C42 0.090(12) 0.082(14) 0.048(9) -0.023(9) -0.036(9) 0.003(11) C43 0.142(18) 0.065(13) 0.060(10) -0.030(10) -0.017(11) -0.040(12) C44 0.18(2) 0.036(10) 0.052(10) -0.032(9) -0.033(11) -0.017(12) C45 0.091(11) 0.022(8) 0.078(11) -0.007(9) 0.008(10) 0.007(7) C46 0.129(15) 0.020(8) 0.028(6) 0.011(6) -0.002(7) -0.016(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 S1 2.273(3) . ? Cu1 S2 2.290(3) 3 ? Cu1 I2 2.6997(17) . ? Cu1 I1 2.7212(17) . ? Hg1 I4 2.7058(10) . ? Hg1 I3 2.7125(11) . ? Hg1 I2 2.8840(8) . ? Hg1 I1 2.8880(9) . ? K1 O9 2.754(8) . ? K1 O5 2.765(8) . ? K1 O6 2.792(9) . ? K1 O7 2.824(9) . ? K1 O8 2.854(11) . ? K1 C27 3.186(11) . ? K1 C28 3.281(10) . ? K1 C26 3.311(13) . ? K1 C14 3.450(12) . ? K1 C15 3.482(12) . ? K1 C13 3.486(11) . ? K1 C29 3.492(11) . ? S1 C3 1.798(14) . ? S1 C2 1.827(12) . ? S2 C8 1.792(12) . ? S2 C9 1.834(11) . ? S2 Cu1 2.290(3) 3_455 ? O1 C30 1.372(13) . ? O1 C1 1.418(13) . ? O2 C4 1.379(17) . ? O2 C5 1.417(15) . ? O3 C7 1.366(17) . ? O3 C6 1.406(18) . ? O4 C11 1.388(13) . ? O4 C10 1.435(13) . ? O5 C23 1.393(14) . ? O5 C39 1.459(14) . ? O6 C40 1.386(19) . ? O6 C41 1.461(19) . ? O7 C43 1.42(2) . ? O7 C42 1.439(18) . ? O8 C45 1.311(19) . ? O8 C44 1.426(17) . ? O9 C37 1.403(12) . ? O9 C46 1.419(16) . ? C1 C2 1.508(17) . ? C3 C4 1.55(2) . ? C5 C6 1.49(2) . ? C7 C8 1.55(2) . ? C9 C10 1.499(15) . ? C11 C16 1.399(16) . ? C11 C12 1.435(19) . ? C12 C13 1.354(17) . ? C12 C38 1.540(16) . ? C13 C14 1.399(19) . ? C14 C15 1.384(19) . ? C15 C16 1.383(16) . ? C16 C17 1.503(17) . ? C17 C18 1.487(17) . ? C18 C19 1.379(18) . ? C18 C23 1.379(15) . ? C19 C20 1.394(19) . ? C20 C21 1.38(2) . ? C21 C22 1.397(18) . ? C22 C23 1.414(15) . ? C22 C24 1.508(17) . ? C24 C25 1.496(18) . ? C25 C30 1.413(15) . ? C25 C26 1.414(17) . ? C26 C27 1.309(19) . ? C27 C28 1.358(18) . ? C28 C29 1.424(16) . ? C29 C30 1.428(18) . ? C29 C31 1.473(15) . ? C31 C32 1.518(15) . ? C32 C37 1.388(14) . ? C32 C33 1.426(15) . ? C33 C34 1.354(15) . ? C34 C35 1.367(17) . ? C35 C36 1.416(17) . ? C36 C37 1.401(15) . ? C36 C38 1.468(16) . ? C39 C40 1.53(2) . ? C41 C42 1.34(2) . ? C43 C44 1.43(3) . ? C45 C46 1.39(2) . ? N1 C47 1.131(9) . ? C47 C48 1.521(9) . ? N2 C49 1.135(8) . ? C49 C50 1.520(8) . ? 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 S1 Cu1 S2 129.41(12) . 3 ? S1 Cu1 I2 108.17(10) . . ? S2 Cu1 I2 102.71(10) 3 . ? S1 Cu1 I1 102.93(10) . . ? S2 Cu1 I1 106.39(9) 3 . ? I2 Cu1 I1 105.18(6) . . ? I4 Hg1 I3 128.27(4) . . ? I4 Hg1 I2 106.43(3) . . ? I3 Hg1 I2 106.78(3) . . ? I4 Hg1 I1 109.37(3) . . ? I3 Hg1 I1 104.96(3) . . ? I2 Hg1 I1 96.49(3) . . ? O9 K1 O5 124.8(2) . . ? O9 K1 O6 173.1(3) . . ? O5 K1 O6 58.7(3) . . ? O9 K1 O7 116.6(3) . . ? O5 K1 O7 118.2(3) . . ? O6 K1 O7 59.5(3) . . ? O9 K1 O8 57.8(3) . . ? O5 K1 O8 174.0(3) . . ? O6 K1 O8 118.1(3) . . ? O7 K1 O8 58.8(3) . . ? O9 K1 C27 93.2(3) . . ? O5 K1 C27 90.8(3) . . ? O6 K1 C27 80.5(3) . . ? O7 K1 C27 79.5(3) . . ? O8 K1 C27 83.5(4) . . ? O9 K1 C28 69.0(3) . . ? O5 K1 C28 104.6(3) . . ? O6 K1 C28 104.6(3) . . ? O7 K1 C28 90.5(3) . . ? O8 K1 C28 70.8(4) . . ? C27 K1 C28 24.2(3) . . ? O9 K1 C26 106.0(3) . . ? O5 K1 C26 67.7(3) . . ? O6 K1 C26 69.2(3) . . ? O7 K1 C26 91.1(3) . . ? O8 K1 C26 106.7(4) . . ? C27 K1 C26 23.1(3) . . ? C28 K1 C26 41.8(3) . . ? O9 K1 C14 89.6(3) . . ? O5 K1 C14 88.6(3) . . ? O6 K1 C14 96.6(3) . . ? O7 K1 C14 98.1(3) . . ? O8 K1 C14 96.9(4) . . ? C27 K1 C14 176.9(3) . . ? C28 K1 C14 158.6(3) . . ? C26 K1 C14 156.1(4) . . ? O9 K1 C15 102.2(3) . . ? O5 K1 C15 65.5(3) . . ? O6 K1 C15 84.7(3) . . ? O7 K1 C15 108.6(3) . . ? O8 K1 C15 120.0(4) . . ? C27 K1 C15 156.2(3) . . ? C28 K1 C15 160.8(3) . . ? C26 K1 C15 133.2(4) . . ? C14 K1 C15 23.0(3) . . ? O9 K1 C13 66.3(3) . . ? O5 K1 C13 100.9(3) . . ? O6 K1 C13 119.9(3) . . ? O7 K1 C13 108.6(3) . . ? O8 K1 C13 85.0(4) . . ? C27 K1 C13 159.6(3) . . ? C28 K1 C13 135.4(4) . . ? C26 K1 C13 160.3(3) . . ? C14 K1 C13 23.3(3) . . ? C15 K1 C13 40.1(3) . . ? O9 K1 C29 57.2(2) . . ? O5 K1 C29 94.2(3) . . ? O6 K1 C29 118.0(3) . . ? O7 K1 C29 114.4(3) . . ? O8 K1 C29 82.9(4) . . ? C27 K1 C29 42.2(3) . . ? C28 K1 C29 24.0(3) . . ? C26 K1 C29 48.9(3) . . ? C14 K1 C29 140.9(3) . . ? C15 K1 C29 137.0(3) . . ? C13 K1 C29 119.5(3) . . ? Cu1 I1 Hg1 78.94(4) . . ? Cu1 I2 Hg1 79.36(4) . . ? C3 S1 C2 105.3(6) . . ? C3 S1 Cu1 104.6(5) . . ? C2 S1 Cu1 109.4(5) . . ? C8 S2 C9 102.9(5) . . ? C8 S2 Cu1 100.7(5) . 3_455 ? C9 S2 Cu1 109.7(4) . 3_455 ? C30 O1 C1 112.8(8) . . ? C4 O2 C5 116.9(11) . . ? C7 O3 C6 109.7(12) . . ? C11 O4 C10 113.1(8) . . ? C23 O5 C39 110.3(9) . . ? C23 O5 K1 128.8(6) . . ? C39 O5 K1 120.5(7) . . ? C40 O6 C41 114.7(12) . . ? C40 O6 K1 112.3(8) . . ? C41 O6 K1 113.1(10) . . ? C43 O7 C42 115.8(13) . . ? C43 O7 K1 112.9(9) . . ? C42 O7 K1 113.0(8) . . ? C45 O8 C44 117.3(14) . . ? C45 O8 K1 111.8(9) . . ? C44 O8 K1 115.7(10) . . ? C37 O9 C46 114.2(9) . . ? C37 O9 K1 125.3(6) . . ? C46 O9 K1 120.2(7) . . ? O1 C1 C2 109.5(9) . . ? C1 C2 S1 105.9(8) . . ? C4 C3 S1 114.1(11) . . ? O2 C4 C3 108.1(14) . . ? O2 C5 C6 112.7(11) . . ? O3 C6 C5 107.1(14) . . ? O3 C7 C8 108.2(12) . . ? C7 C8 S2 117.2(11) . . ? C10 C9 S2 105.5(8) . . ? O4 C10 C9 108.2(8) . . ? O4 C11 C16 117.9(11) . . ? O4 C11 C12 120.4(10) . . ? C16 C11 C12 121.6(10) . . ? C13 C12 C11 118.6(11) . . ? C13 C12 C38 121.1(12) . . ? C11 C12 C38 120.2(10) . . ? C12 C13 C14 121.5(12) . . ? C12 C13 K1 81.8(6) . . ? C14 C13 K1 76.9(7) . . ? C15 C14 C13 118.4(11) . . ? C15 C14 K1 79.8(7) . . ? C13 C14 K1 79.8(6) . . ? C16 C15 C14 123.6(12) . . ? C16 C15 K1 83.3(7) . . ? C14 C15 K1 77.2(7) . . ? C15 C16 C11 116.3(12) . . ? C15 C16 C17 121.7(11) . . ? C11 C16 C17 121.9(10) . . ? C18 C17 C16 118.8(9) . . ? C19 C18 C23 118.7(11) . . ? C19 C18 C17 120.1(10) . . ? C23 C18 C17 121.1(11) . . ? C18 C19 C20 121.6(13) . . ? C21 C20 C19 118.3(13) . . ? C20 C21 C22 122.5(12) . . ? C21 C22 C23 116.5(11) . . ? C21 C22 C24 121.8(11) . . ? C23 C22 C24 121.7(11) . . ? C18 C23 O5 118.4(10) . . ? C18 C23 C22 122.1(12) . . ? O5 C23 C22 119.4(10) . . ? C25 C24 C22 117.9(10) . . ? C30 C25 C26 117.5(11) . . ? C30 C25 C24 120.5(11) . . ? C26 C25 C24 122.0(11) . . ? C30 C25 K1 81.9(6) . . ? C26 C25 K1 70.3(7) . . ? C24 C25 K1 119.1(7) . . ? C27 C26 C25 120.6(12) . . ? C27 C26 K1 73.0(7) . . ? C25 C26 K1 86.1(7) . . ? C26 C27 C28 123.9(13) . . ? C26 C27 K1 83.8(7) . . ? C28 C27 K1 81.8(6) . . ? C27 C28 C29 120.7(12) . . ? C27 C28 K1 74.0(6) . . ? C29 C28 K1 86.3(6) . . ? C28 C29 C30 115.5(11) . . ? C28 C29 C31 120.7(11) . . ? C30 C29 C31 123.7(10) . . ? C28 C29 K1 69.7(6) . . ? C30 C29 K1 82.5(6) . . ? C31 C29 K1 117.9(7) . . ? O1 C30 C25 118.7(10) . . ? O1 C30 C29 119.5(10) . . ? C25 C30 C29 121.7(11) . . ? C29 C31 C32 114.9(9) . . ? C37 C32 C33 117.6(9) . . ? C37 C32 C31 122.8(9) . . ? C33 C32 C31 119.7(9) . . ? C34 C33 C32 119.3(10) . . ? C33 C34 C35 122.1(11) . . ? C34 C35 C36 121.6(11) . . ? C37 C36 C35 115.3(10) . . ? C37 C36 C38 122.8(10) . . ? C35 C36 C38 121.9(11) . . ? C32 C37 C36 123.7(10) . . ? C32 C37 O9 118.3(9) . . ? C36 C37 O9 118.0(9) . . ? C36 C38 C12 117.2(10) . . ? O5 C39 C40 108.3(11) . . ? O6 C40 C39 107.4(12) . . ? C42 C41 O6 112.3(16) . . ? C41 C42 O7 108.1(13) . . ? O7 C43 C44 110.6(15) . . ? O8 C44 C43 107.4(15) . . ? O8 C45 C46 115.8(13) . . ? C45 C46 O9 112.7(11) . . ? N1 C47 C48 168(4) . . ? N2 C49 C50 168(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.036 _refine_diff_density_min -1.333 _refine_diff_density_rms 0.194 #=====================================================END