# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1891 data_Complex1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H85 B2 Cu2 N9' _chemical_formula_weight 1393.33 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' 'B' 'B' 0.0013 0.0007 '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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M '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 11.0330(10) _cell_length_b 47.147(6) _cell_length_c 14.1930(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.96 _cell_angle_gamma 90.00 _cell_volume 7342.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 4 _cell_measurement_theta_max 12.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10212 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.1602 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 22.50 _reflns_number_total 9601 _reflns_number_gt 5076 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+25.3877P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9601 _refine_ls_number_parameters 893 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1722 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.1444 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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_multiplicit _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.31619(9) 0.12145(2) 0.09793(7) 0.0236(3) Uani 1 1 d . . . Cu2 Cu 0.21017(9) 0.14406(2) -0.18707(7) 0.0262(3) Uani 1 1 d . . . N1 N 0.3635(6) 0.10937(13) 0.2576(4) 0.0243(17) Uani 1 1 d . . . C1A C 0.4488(7) 0.13227(16) 0.2905(5) 0.028(2) Uani 1 1 d . . . H1AA H 0.5335 0.1258 0.2862 0.034 Uiso 1 1 calc R . . H1AB H 0.4400 0.1366 0.3577 0.034 Uiso 1 1 calc R . . C2A C 0.4248(7) 0.15889(15) 0.2316(5) 0.026(2) Uani 1 1 d . . . H2AA H 0.3425 0.1663 0.2397 0.032 Uiso 1 1 calc R . . H2AB H 0.4851 0.1737 0.2534 0.032 Uiso 1 1 calc R . . N3A N 0.4335(6) 0.15245(13) 0.1306(4) 0.0229(16) Uani 1 1 d . . . C3A C 0.5177(7) 0.16464(17) 0.0927(5) 0.024(2) Uani 1 1 d . . . H3A H 0.5617 0.1791 0.1280 0.029 Uiso 1 1 calc R . . C4A C 0.5529(7) 0.15815(16) -0.0019(5) 0.024(2) Uani 1 1 d . . . C5A C 0.6674(8) 0.16725(18) -0.0227(6) 0.035(2) Uani 1 1 d . . . H5A H 0.7145 0.1792 0.0210 0.041 Uiso 1 1 calc R . . C6A C 0.7143(8) 0.15927(19) -0.1060(6) 0.039(2) Uani 1 1 d . . . H6A H 0.7934 0.1651 -0.1186 0.047 Uiso 1 1 calc R . . C7A C 0.6434(7) 0.14261(19) -0.1703(6) 0.036(2) Uani 1 1 d . . . H7A H 0.6753 0.1367 -0.2268 0.043 Uiso 1 1 calc R . . C8A C 0.5264(7) 0.13433(16) -0.1540(5) 0.023(2) Uani 1 1 d . . . C9A C 0.4824(7) 0.14217(16) -0.0695(5) 0.025(2) Uani 1 1 d . . . H9A H 0.4028 0.1365 -0.0577 0.030 Uiso 1 1 calc R . . C10A C 0.4519(7) 0.12008(17) -0.2310(5) 0.029(2) Uani 1 1 d . . . H10A H 0.4926 0.1097 -0.2757 0.035 Uiso 1 1 calc R . . N4A N 0.3360(6) 0.12064(13) -0.2421(4) 0.0247(16) Uani 1 1 d . . . C11A C 0.2757(7) 0.10952(17) -0.3324(5) 0.033(2) Uani 1 1 d . . . H11A H 0.2035 0.0981 -0.3209 0.040 Uiso 1 1 calc R . . H11B H 0.3326 0.0974 -0.3640 0.040 Uiso 1 1 calc R . . C12A C 0.2372(8) 0.13551(17) -0.3947(5) 0.034(2) Uani 1 1 d . . . H12A H 0.3107 0.1460 -0.4095 0.041 Uiso 1 1 calc R . . H12B H 0.1928 0.1291 -0.4551 0.041 Uiso 1 1 calc R . . N2 N 0.1586(6) 0.15442(13) -0.3454(4) 0.0295(18) Uani 1 1 d . . . C1B C 0.2452(7) 0.11013(16) 0.2971(5) 0.028(2) Uani 1 1 d . . . H1BA H 0.2368 0.1284 0.3302 0.033 Uiso 1 1 calc R . . H1BB H 0.2422 0.0947 0.3441 0.033 Uiso 1 1 calc R . . C2B C 0.1400(7) 0.10671(16) 0.2198(5) 0.026(2) Uani 1 1 d . . . H2BA H 0.1411 0.0875 0.1917 0.032 Uiso 1 1 calc R . . H2BB H 0.0613 0.1094 0.2463 0.032 Uiso 1 1 calc R . . N3B N 0.1558(5) 0.12878(13) 0.1460(4) 0.0219(16) Uani 1 1 d . . . C3B C 0.0936(7) 0.15133(17) 0.1500(5) 0.025(2) Uani 1 1 d . . . H3B1 H 0.0311 0.1514 0.1913 0.030 Uiso 1 1 calc R . . C4B C 0.1104(7) 0.17718(17) 0.0964(5) 0.026(2) Uani 1 1 d . . . C5B C 0.0840(8) 0.20268(18) 0.1381(6) 0.043(3) Uani 1 1 d . . . H5B H 0.0486 0.2026 0.1963 0.051 Uiso 1 1 calc R . . C6B C 0.1081(10) 0.2283(2) 0.0966(7) 0.062(3) Uani 1 1 d . . . H6B H 0.0913 0.2456 0.1271 0.075 Uiso 1 1 calc R . . C7B C 0.1572(9) 0.22869(18) 0.0101(6) 0.048(3) Uani 1 1 d . . . H7B H 0.1737 0.2462 -0.0190 0.058 Uiso 1 1 calc R . . C8B C 0.1817(7) 0.20327(17) -0.0333(5) 0.027(2) Uani 1 1 d . . . C9B C 0.1586(7) 0.17774(16) 0.0102(5) 0.024(2) Uani 1 1 d . . . H9B H 0.1761 0.1604 -0.0196 0.029 Uiso 1 1 calc R . . C10B C 0.2307(8) 0.20588(17) -0.1260(6) 0.033(2) Uani 1 1 d . . . H10B H 0.2505 0.2243 -0.1465 0.040 Uiso 1 1 calc R . . N4B N 0.2481(6) 0.18528(13) -0.1800(4) 0.0262(17) Uani 1 1 d . . . C11B C 0.2877(8) 0.19265(17) -0.2735(5) 0.035(2) Uani 1 1 d . . . H11C H 0.3637 0.1823 -0.2829 0.042 Uiso 1 1 calc R . . H11D H 0.3045 0.2132 -0.2762 0.042 Uiso 1 1 calc R . . C12B C 0.1879(8) 0.18465(17) -0.3514(5) 0.038(2) Uani 1 1 d . . . H12C H 0.1140 0.1961 -0.3447 0.045 Uiso 1 1 calc R . . H12D H 0.2155 0.1888 -0.4141 0.045 Uiso 1 1 calc R . . C1C C 0.4180(7) 0.08105(16) 0.2536(5) 0.030(2) Uani 1 1 d . . . H1CA H 0.3560 0.0664 0.2633 0.036 Uiso 1 1 calc R . . H1CB H 0.4855 0.0791 0.3048 0.036 Uiso 1 1 calc R . . C2C C 0.4666(7) 0.07651(16) 0.1569(5) 0.0212(19) Uani 1 1 d . . . H2CA H 0.5346 0.0897 0.1496 0.025 Uiso 1 1 calc R . . H2CB H 0.4970 0.0569 0.1521 0.025 Uiso 1 1 calc R . . N3C N 0.3658(5) 0.08174(13) 0.0824(4) 0.0210(16) Uani 1 1 d . . . C3C C 0.3182(8) 0.06048(17) 0.0396(5) 0.030(2) Uani 1 1 d . . . H3C H 0.3595 0.0429 0.0495 0.035 Uiso 1 1 calc R . . C4C C 0.2054(7) 0.06034(17) -0.0240(5) 0.025(2) Uani 1 1 d . . . C5C C 0.1404(7) 0.03493(16) -0.0318(5) 0.028(2) Uani 1 1 d . . . H5C H 0.1745 0.0184 -0.0015 0.034 Uiso 1 1 calc R . . C6C C 0.0267(8) 0.03352(18) -0.0833(6) 0.035(2) Uani 1 1 d . . . H6C H -0.0175 0.0162 -0.0874 0.042 Uiso 1 1 calc R . . C7C C -0.0210(8) 0.05708(18) -0.1278(6) 0.034(2) Uani 1 1 d . . . H7C H -0.0989 0.0560 -0.1630 0.041 Uiso 1 1 calc R . . C8C C 0.0409(7) 0.08279(16) -0.1233(5) 0.024(2) Uani 1 1 d . . . C9C C 0.1545(7) 0.08423(15) -0.0712(5) 0.0212(19) Uani 1 1 d . . . H9C H 0.1981 0.1016 -0.0675 0.025 Uiso 1 1 calc R . . C10C C -0.0125(8) 0.10631(19) -0.1801(6) 0.035(2) Uani 1 1 d . . . H10C H -0.0950 0.1041 -0.2057 0.042 Uiso 1 1 calc R . . N4C N 0.0395(6) 0.12949(14) -0.1990(4) 0.0250(17) Uani 1 1 d . . . C11C C -0.0283(7) 0.14862(17) -0.2680(5) 0.030(2) Uani 1 1 d . . . H11E H -0.0253 0.1683 -0.2432 0.037 Uiso 1 1 calc R . . H11F H -0.1147 0.1427 -0.2782 0.037 Uiso 1 1 calc R . . C12C C 0.0280(7) 0.14761(18) -0.3612(5) 0.034(2) Uani 1 1 d . . . H12E H 0.0171 0.1284 -0.3893 0.040 Uiso 1 1 calc R . . H12F H -0.0136 0.1614 -0.4062 0.040 Uiso 1 1 calc R . . B1 B 0.3217(8) 0.31063(19) -0.1322(6) 0.025(2) Uani 1 1 d . . . C20 C 0.3142(7) 0.34338(16) -0.1737(5) 0.022(2) Uani 1 1 d . . . C21 C 0.2877(7) 0.34993(17) -0.2696(5) 0.028(2) Uani 1 1 d . . . H21 H 0.2717 0.3349 -0.3136 0.033 Uiso 1 1 calc R . . C22 C 0.2838(7) 0.37778(18) -0.3034(6) 0.030(2) Uani 1 1 d . . . H22 H 0.2646 0.3813 -0.3692 0.036 Uiso 1 1 calc R . . C23 C 0.3078(7) 0.40015(18) -0.2419(6) 0.035(2) Uani 1 1 d . . . H23 H 0.3061 0.4191 -0.2648 0.042 Uiso 1 1 calc R . . C24 C 0.3341(8) 0.39467(17) -0.1471(6) 0.035(2) Uani 1 1 d . . . H24 H 0.3495 0.4099 -0.1038 0.042 Uiso 1 1 calc R . . C25 C 0.3384(8) 0.36688(17) -0.1143(6) 0.034(2) Uani 1 1 d . . . H25 H 0.3588 0.3637 -0.0485 0.040 Uiso 1 1 calc R . . C30 C 0.4650(8) 0.29943(17) -0.1250(5) 0.029(2) Uani 1 1 d . . . C31 C 0.4951(8) 0.27047(17) -0.1292(5) 0.033(2) Uani 1 1 d . . . H31 H 0.4311 0.2569 -0.1381 0.039 Uiso 1 1 calc R . . C32 C 0.6138(8) 0.26100(19) -0.1207(6) 0.041(2) Uani 1 1 d . . . H32 H 0.6295 0.2412 -0.1217 0.049 Uiso 1 1 calc R . . C33 C 0.7101(8) 0.2797(2) -0.1108(6) 0.043(3) Uani 1 1 d . . . H33 H 0.7918 0.2732 -0.1075 0.052 Uiso 1 1 calc R . . C34 C 0.6846(8) 0.3083(2) -0.1059(5) 0.037(2) Uani 1 1 d . . . H34 H 0.7499 0.3215 -0.0974 0.044 Uiso 1 1 calc R . . C35 C 0.5642(8) 0.31822(18) -0.1131(5) 0.031(2) Uani 1 1 d . . . H35 H 0.5495 0.3380 -0.1099 0.038 Uiso 1 1 calc R . . C40 C 0.2744(7) 0.31006(16) -0.0271(5) 0.025(2) Uani 1 1 d . . . C41 C 0.1688(8) 0.32488(18) -0.0052(6) 0.045(3) Uani 1 1 d . . . H41 H 0.1281 0.3369 -0.0522 0.054 Uiso 1 1 calc R . . C42 C 0.1232(9) 0.3226(2) 0.0804(7) 0.050(3) Uani 1 1 d . . . H42 H 0.0509 0.3327 0.0903 0.061 Uiso 1 1 calc R . . C43 C 0.1787(9) 0.30639(19) 0.1519(6) 0.044(3) Uani 1 1 d . . . H43 H 0.1464 0.3051 0.2113 0.053 Uiso 1 1 calc R . . C44 C 0.2826(9) 0.29204(19) 0.1352(6) 0.042(3) Uani 1 1 d . . . H44 H 0.3250 0.2811 0.1844 0.051 Uiso 1 1 calc R . . C45 C 0.3260(8) 0.29331(18) 0.0475(6) 0.037(2) Uani 1 1 d . . . H45 H 0.3950 0.2821 0.0374 0.044 Uiso 1 1 calc R . . C50 C 0.2355(8) 0.28996(16) -0.2044(6) 0.029(2) Uani 1 1 d . . . C51 C 0.1176(8) 0.28137(17) -0.1879(6) 0.037(2) Uani 1 1 d . . . H51 H 0.0886 0.2865 -0.1295 0.045 Uiso 1 1 calc R . . C52 C 0.0405(9) 0.26568(19) -0.2529(8) 0.055(3) Uani 1 1 d . . . H52 H -0.0385 0.2603 -0.2384 0.066 Uiso 1 1 calc R . . C53 C 0.0806(10) 0.2580(2) -0.3384(8) 0.060(3) Uani 1 1 d . . . H53 H 0.0282 0.2480 -0.3843 0.072 Uiso 1 1 calc R . . C54 C 0.1959(10) 0.26496(18) -0.3564(7) 0.051(3) Uani 1 1 d . . . H54 H 0.2249 0.2591 -0.4140 0.061 Uiso 1 1 calc R . . C55 C 0.2713(8) 0.28055(17) -0.2914(6) 0.042(3) Uani 1 1 d . . . H55 H 0.3510 0.2851 -0.3064 0.050 Uiso 1 1 calc R . . B2 B 0.5884(8) 0.02563(19) -0.2750(6) 0.025(2) Uani 1 1 d . . . C60 C 0.4523(7) 0.01045(18) -0.2840(6) 0.031(2) Uani 1 1 d . . . C61 C 0.3536(8) 0.0245(2) -0.2498(6) 0.041(2) Uani 1 1 d . . . H61 H 0.3674 0.0422 -0.2188 0.050 Uiso 1 1 calc R . . C62 C 0.2367(9) 0.0134(3) -0.2596(7) 0.067(3) Uani 1 1 d . . . H62 H 0.1719 0.0238 -0.2372 0.080 Uiso 1 1 calc R . . C63 C 0.2135(9) -0.0126(3) -0.3011(8) 0.067(4) Uani 1 1 d . . . H63 H 0.1342 -0.0206 -0.3043 0.080 Uiso 1 1 calc R . . C64 C 0.3080(9) -0.0270(2) -0.3388(7) 0.056(3) Uani 1 1 d . . . H64 H 0.2934 -0.0445 -0.3715 0.067 Uiso 1 1 calc R . . C65 C 0.4236(8) -0.01520(19) -0.3269(6) 0.040(2) Uani 1 1 d . . . H65 H 0.4879 -0.0256 -0.3502 0.048 Uiso 1 1 calc R . . C70 C 0.6923(7) 0.00230(15) -0.2981(5) 0.023(2) Uani 1 1 d . . . C71 C 0.6938(7) -0.00867(17) -0.3901(6) 0.032(2) Uani 1 1 d . . . H71 H 0.6348 -0.0022 -0.4387 0.038 Uiso 1 1 calc R . . C72 C 0.7786(7) -0.02867(17) -0.4122(6) 0.032(2) Uani 1 1 d . . . H72 H 0.7754 -0.0358 -0.4751 0.038 Uiso 1 1 calc R . . C73 C 0.8677(7) -0.03843(16) -0.3443(6) 0.029(2) Uani 1 1 d . . . H73 H 0.9253 -0.0522 -0.3596 0.035 Uiso 1 1 calc R . . C74 C 0.8711(7) -0.02771(16) -0.2542(6) 0.029(2) Uani 1 1 d . . . H74 H 0.9322 -0.0340 -0.2067 0.035 Uiso 1 1 calc R . . C75 C 0.7863(7) -0.00775(16) -0.2318(5) 0.024(2) Uani 1 1 d . . . H75 H 0.7918 -0.0006 -0.1690 0.028 Uiso 1 1 calc R . . C80 C 0.6154(7) 0.03736(17) -0.1654(5) 0.027(2) Uani 1 1 d . . . C81 C 0.6561(7) 0.06456(17) -0.1387(6) 0.031(2) Uani 1 1 d . . . H81 H 0.6603 0.0785 -0.1866 0.037 Uiso 1 1 calc R . . C82 C 0.6904(8) 0.0720(2) -0.0460(6) 0.045(3) Uani 1 1 d . . . H82 H 0.7174 0.0908 -0.0316 0.054 Uiso 1 1 calc R . . C83 C 0.6863(8) 0.0529(2) 0.0258(6) 0.046(3) Uani 1 1 d . . . H83 H 0.7143 0.0579 0.0891 0.056 Uiso 1 1 calc R . . C84 C 0.6407(8) 0.0260(2) 0.0044(6) 0.039(2) Uani 1 1 d . . . H84 H 0.6334 0.0126 0.0535 0.047 Uiso 1 1 calc R . . C85 C 0.6059(7) 0.01887(17) -0.0891(6) 0.031(2) Uani 1 1 d . . . H85 H 0.5739 0.0004 -0.1023 0.037 Uiso 1 1 calc R . . C90 C 0.5894(7) 0.05101(15) -0.3525(5) 0.0214(19) Uani 1 1 d . . . C91 C 0.4909(7) 0.05775(16) -0.4186(5) 0.023(2) Uani 1 1 d . . . H91 H 0.4177 0.0471 -0.4182 0.027 Uiso 1 1 calc R . . C92 C 0.4955(8) 0.07965(19) -0.4858(6) 0.036(2) Uani 1 1 d . . . H92 H 0.4275 0.0831 -0.5311 0.043 Uiso 1 1 calc R . . C93 C 0.5992(8) 0.09612(18) -0.4856(6) 0.035(2) Uani 1 1 d . . . H93 H 0.6019 0.1116 -0.5283 0.042 Uiso 1 1 calc R . . C94 C 0.6983(8) 0.08971(17) -0.4222(6) 0.035(2) Uani 1 1 d . . . H94 H 0.7707 0.1006 -0.4228 0.042 Uiso 1 1 calc R . . C95 C 0.6950(7) 0.06792(16) -0.3581(5) 0.027(2) Uani 1 1 d . . . H95 H 0.7658 0.0640 -0.3161 0.032 Uiso 1 1 calc R . . N1S N 0.0360(9) 0.0796(2) -0.4464(8) 0.086(4) Uani 1 1 d . . . C1S C -0.0010(9) 0.0575(2) -0.4347(7) 0.053(3) Uani 1 1 d . . . C2S C -0.0486(9) 0.0296(2) -0.4248(8) 0.073(4) Uani 1 1 d . . . H2S1 H -0.0844 0.0282 -0.3646 0.110 Uiso 1 1 calc R . . H2S2 H 0.0174 0.0157 -0.4257 0.110 Uiso 1 1 calc R . . H2S3 H -0.1113 0.0257 -0.4773 0.110 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 Cu1 0.0244(6) 0.0220(6) 0.0241(6) 0.0002(5) 0.0010(4) -0.0009(5) Cu2 0.0311(6) 0.0237(6) 0.0235(6) -0.0003(5) 0.0009(5) 0.0037(5) N1 0.021(4) 0.028(4) 0.024(4) 0.003(3) -0.002(3) -0.002(3) C1A 0.030(5) 0.032(5) 0.022(5) -0.002(4) -0.004(4) -0.003(4) C2A 0.029(5) 0.020(5) 0.030(5) -0.004(4) 0.005(4) -0.005(4) N3A 0.027(4) 0.024(4) 0.019(4) 0.004(3) 0.007(3) -0.001(3) C3A 0.025(5) 0.028(5) 0.018(5) 0.002(4) -0.004(4) -0.005(4) C4A 0.022(5) 0.024(5) 0.027(5) 0.014(4) 0.005(4) 0.001(4) C5A 0.034(6) 0.042(6) 0.028(5) 0.008(4) 0.003(4) -0.013(5) C6A 0.033(6) 0.057(7) 0.029(6) 0.004(5) 0.011(5) -0.013(5) C7A 0.028(5) 0.052(6) 0.029(5) 0.001(5) 0.007(4) 0.000(5) C8A 0.022(5) 0.029(5) 0.018(5) 0.005(4) 0.001(4) 0.001(4) C9A 0.025(5) 0.026(5) 0.023(5) 0.007(4) -0.005(4) -0.005(4) C10A 0.032(6) 0.032(5) 0.025(5) 0.008(4) 0.009(4) 0.004(5) N4A 0.025(4) 0.025(4) 0.023(4) 0.004(3) -0.004(3) 0.008(4) C11A 0.021(5) 0.041(6) 0.036(6) 0.001(5) -0.001(4) -0.001(4) C12A 0.045(6) 0.038(6) 0.018(5) 0.001(4) -0.004(4) 0.006(5) N2 0.036(5) 0.029(4) 0.022(4) -0.004(3) -0.005(3) 0.008(4) C1B 0.035(6) 0.023(5) 0.026(5) 0.006(4) 0.008(4) -0.002(4) C2B 0.031(5) 0.017(5) 0.031(5) 0.016(4) 0.004(4) -0.003(4) N3B 0.018(4) 0.019(4) 0.028(4) 0.001(3) 0.003(3) -0.002(3) C3B 0.020(5) 0.040(6) 0.015(5) 0.000(4) 0.005(4) 0.001(4) C4B 0.039(6) 0.024(5) 0.016(5) -0.007(4) 0.004(4) 0.006(4) C5B 0.070(7) 0.030(6) 0.029(6) -0.004(5) 0.011(5) 0.016(5) C6B 0.115(10) 0.031(6) 0.041(7) -0.008(5) 0.010(6) 0.022(6) C7B 0.093(8) 0.026(6) 0.026(6) 0.006(5) 0.008(5) -0.006(6) C8B 0.042(6) 0.017(5) 0.022(5) -0.007(4) 0.000(4) 0.000(4) C9B 0.029(5) 0.022(5) 0.022(5) 0.000(4) 0.002(4) 0.001(4) C10B 0.052(6) 0.018(5) 0.027(5) 0.001(4) -0.008(5) 0.004(5) N4B 0.037(5) 0.022(4) 0.020(4) 0.003(3) 0.003(3) -0.004(3) C11B 0.050(6) 0.027(5) 0.030(5) -0.001(4) 0.014(5) -0.011(5) C12B 0.059(7) 0.031(6) 0.023(5) 0.003(4) 0.012(5) -0.003(5) C1C 0.022(5) 0.028(5) 0.038(6) 0.003(4) -0.004(4) 0.009(4) C2C 0.018(5) 0.021(5) 0.024(5) -0.008(4) 0.001(4) -0.001(4) N3C 0.015(4) 0.023(4) 0.025(4) -0.002(3) 0.002(3) 0.000(3) C3C 0.041(6) 0.020(5) 0.027(5) -0.001(4) 0.001(4) 0.004(4) C4C 0.030(5) 0.023(5) 0.024(5) -0.002(4) 0.005(4) 0.006(4) C5C 0.041(6) 0.013(5) 0.029(5) -0.001(4) 0.003(4) 0.000(4) C6C 0.039(6) 0.030(6) 0.036(6) -0.002(5) 0.003(5) -0.018(5) C7C 0.027(5) 0.039(6) 0.036(6) 0.006(5) 0.004(4) -0.003(5) C8C 0.032(5) 0.018(5) 0.022(5) 0.005(4) 0.000(4) 0.004(4) C9C 0.026(5) 0.013(5) 0.024(5) -0.005(4) -0.002(4) 0.001(4) C10C 0.024(5) 0.049(6) 0.033(6) 0.000(5) 0.010(4) -0.006(5) N4C 0.029(4) 0.027(4) 0.019(4) 0.005(3) -0.002(3) 0.008(4) C11C 0.034(5) 0.028(5) 0.029(5) 0.008(4) 0.000(4) 0.009(4) C12C 0.036(6) 0.033(5) 0.029(5) -0.008(4) -0.008(4) 0.012(5) B1 0.030(6) 0.017(5) 0.025(6) 0.003(5) -0.004(5) 0.003(5) C20 0.016(5) 0.023(5) 0.028(5) -0.005(4) 0.004(4) 0.005(4) C21 0.033(5) 0.029(5) 0.020(5) -0.002(4) -0.001(4) -0.005(4) C22 0.028(5) 0.040(6) 0.021(5) 0.008(5) -0.002(4) 0.007(5) C23 0.041(6) 0.026(5) 0.039(6) 0.010(5) 0.010(5) 0.014(5) C24 0.047(6) 0.024(5) 0.035(6) -0.001(5) 0.006(5) 0.006(5) C25 0.046(6) 0.033(6) 0.020(5) 0.006(4) -0.003(4) 0.014(5) C30 0.041(6) 0.030(5) 0.015(5) 0.004(4) -0.004(4) 0.005(5) C31 0.045(6) 0.024(5) 0.030(5) 0.009(4) 0.008(4) 0.003(5) C32 0.046(7) 0.032(6) 0.046(6) 0.008(5) 0.006(5) 0.013(5) C33 0.032(6) 0.055(7) 0.042(6) 0.003(5) 0.002(5) 0.012(6) C34 0.045(6) 0.049(7) 0.017(5) 0.009(5) 0.008(4) -0.011(5) C35 0.035(6) 0.039(6) 0.021(5) 0.001(4) 0.003(4) 0.013(5) C40 0.035(5) 0.019(5) 0.021(5) -0.002(4) 0.004(4) -0.002(4) C41 0.058(7) 0.039(6) 0.038(6) 0.000(5) 0.006(5) 0.017(5) C42 0.049(7) 0.052(7) 0.055(7) -0.001(6) 0.024(6) 0.017(6) C43 0.069(8) 0.040(6) 0.026(6) -0.008(5) 0.013(5) -0.004(6) C44 0.059(7) 0.042(6) 0.025(6) 0.003(5) -0.001(5) 0.001(5) C45 0.036(6) 0.035(6) 0.039(6) -0.010(5) 0.005(5) 0.013(5) C50 0.043(6) 0.017(5) 0.027(5) 0.002(4) 0.000(5) 0.008(4) C51 0.050(7) 0.021(5) 0.037(6) 0.006(4) -0.014(5) -0.001(5) C52 0.045(7) 0.034(6) 0.084(9) 0.011(6) -0.004(7) -0.008(5) C53 0.053(8) 0.034(7) 0.085(9) 0.006(6) -0.033(7) -0.007(6) C54 0.079(9) 0.029(6) 0.039(6) -0.021(5) -0.021(6) 0.017(6) C55 0.044(6) 0.033(6) 0.044(6) -0.003(5) -0.015(5) 0.007(5) B2 0.026(6) 0.026(6) 0.023(6) -0.004(5) -0.006(5) 0.005(5) C60 0.032(6) 0.033(6) 0.027(5) 0.010(4) 0.004(4) 0.006(5) C61 0.044(6) 0.049(6) 0.034(6) -0.004(5) 0.014(5) -0.007(5) C62 0.033(7) 0.114(11) 0.054(8) 0.005(8) 0.002(6) -0.006(7) C63 0.034(7) 0.097(10) 0.068(8) 0.034(8) -0.002(6) -0.025(7) C64 0.034(7) 0.042(6) 0.090(9) 0.007(6) -0.002(6) -0.013(5) C65 0.023(6) 0.035(6) 0.062(7) 0.015(5) 0.004(5) 0.002(5) C70 0.026(5) 0.016(5) 0.027(5) 0.002(4) 0.004(4) -0.004(4) C71 0.028(5) 0.031(5) 0.035(6) -0.008(4) -0.004(4) -0.002(4) C72 0.039(6) 0.031(5) 0.025(5) -0.006(4) 0.006(5) -0.005(5) C73 0.028(5) 0.019(5) 0.042(6) -0.003(5) 0.010(5) 0.001(4) C74 0.025(5) 0.026(5) 0.035(6) 0.006(4) 0.001(4) 0.003(4) C75 0.023(5) 0.026(5) 0.022(5) -0.001(4) 0.000(4) -0.006(4) C80 0.022(5) 0.031(5) 0.028(5) 0.001(4) 0.003(4) 0.005(4) C81 0.033(6) 0.027(5) 0.031(6) -0.002(4) -0.002(4) 0.000(4) C82 0.046(7) 0.052(7) 0.035(6) -0.013(6) 0.001(5) 0.001(5) C83 0.038(6) 0.079(8) 0.020(5) -0.016(6) -0.009(5) 0.013(6) C84 0.042(6) 0.050(7) 0.027(6) 0.014(5) 0.013(5) 0.009(5) C85 0.043(6) 0.023(5) 0.027(5) -0.003(4) 0.005(4) 0.016(4) C90 0.024(5) 0.015(5) 0.025(5) -0.006(4) 0.001(4) 0.001(4) C91 0.024(5) 0.024(5) 0.020(5) -0.006(4) 0.004(4) 0.004(4) C92 0.035(6) 0.050(6) 0.022(5) 0.011(5) 0.000(4) 0.008(5) C93 0.044(6) 0.028(5) 0.032(6) 0.010(4) 0.003(5) 0.007(5) C94 0.037(6) 0.033(6) 0.036(6) -0.001(5) 0.011(5) -0.008(5) C95 0.031(5) 0.030(5) 0.019(5) 0.008(4) 0.000(4) 0.006(4) N1S 0.082(8) 0.041(6) 0.129(9) 0.004(6) -0.023(6) -0.007(6) C1S 0.042(7) 0.053(8) 0.061(7) -0.002(7) -0.005(6) 0.025(6) C2S 0.085(9) 0.040(7) 0.104(10) -0.015(7) 0.053(8) 0.000(6) _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 N3C 1.969(6) . y Cu1 N3A 1.975(6) . y Cu1 N3B 1.992(6) . y Cu1 N1 2.342(6) . y Cu1 H9A 2.5946 . ? Cu1 H9C 2.7295 . ? Cu1 H9B 2.8301 . ? Cu1 Cu2 4.2290(14) . y Cu2 N4B 1.988(6) . y Cu2 N4C 1.995(7) . y Cu2 N4A 1.996(6) . y Cu2 N2 2.312(6) . y Cu2 H9B 2.5625 . ? Cu2 H9C 2.6347 . ? Cu2 H9A 2.6842 . ? N1 C1C 1.468(9) . ? N1 C1B 1.473(9) . ? N1 C1A 1.476(9) . ? C1A C2A 1.516(9) . ? C2A N3A 1.479(9) . ? N3A C3A 1.259(9) . ? C3A C4A 1.469(10) . ? C4A C9A 1.392(10) . ? C4A C5A 1.395(10) . ? C5A C6A 1.390(11) . ? C6A C7A 1.383(11) . ? C7A C8A 1.390(10) . ? C8A C9A 1.389(10) . ? C8A C10A 1.462(10) . ? C10A N4A 1.272(9) . ? N4A C11A 1.477(9) . ? C11A C12A 1.545(10) . ? C12A N2 1.470(9) . ? N2 C12B 1.466(9) . ? N2 C12C 1.471(9) . ? C1B C2B 1.521(10) . ? C2B N3B 1.499(8) . ? N3B C3B 1.270(9) . ? C3B C4B 1.459(10) . ? C4B C9B 1.384(10) . ? C4B C5B 1.384(10) . ? C5B C6B 1.381(12) . ? C6B C7B 1.393(11) . ? C7B C8B 1.387(10) . ? C8B C9B 1.388(10) . ? C8B C10B 1.479(10) . ? C10B N4B 1.263(9) . ? N4B C11B 1.482(9) . ? C11B C12B 1.525(10) . ? C1C C2C 1.540(10) . ? C2C N3C 1.473(8) . ? N3C C3C 1.259(9) . ? C3C C4C 1.459(10) . ? C4C C5C 1.395(10) . ? C4C C9C 1.398(10) . ? C5C C6C 1.386(10) . ? C6C C7C 1.357(10) . ? C7C C8C 1.390(10) . ? C8C C9C 1.389(10) . ? C8C C10C 1.459(10) . ? C10C N4C 1.276(9) . ? N4C C11C 1.476(9) . ? C11C C12C 1.519(10) . ? B1 C40 1.632(11) . ? B1 C50 1.643(12) . ? B1 C20 1.651(11) . ? B1 C30 1.660(12) . ? C20 C21 1.396(10) . ? C20 C25 1.401(10) . ? C21 C22 1.397(10) . ? C22 C23 1.377(10) . ? C23 C24 1.371(10) . ? C24 C25 1.389(10) . ? C30 C35 1.405(11) . ? C30 C31 1.408(10) . ? C31 C32 1.376(11) . ? C32 C33 1.378(11) . ? C33 C34 1.377(11) . ? C34 C35 1.402(11) . ? C40 C45 1.394(10) . ? C40 C41 1.420(11) . ? C41 C42 1.366(11) . ? C42 C43 1.365(11) . ? C43 C44 1.373(11) . ? C44 C45 1.381(11) . ? C50 C51 1.405(11) . ? C50 C55 1.407(11) . ? C51 C52 1.399(12) . ? C52 C53 1.383(13) . ? C53 C54 1.363(13) . ? C54 C55 1.387(11) . ? B2 C90 1.627(11) . ? B2 C70 1.646(11) . ? B2 C80 1.648(11) . ? B2 C60 1.656(12) . ? C60 C65 1.376(11) . ? C60 C61 1.404(11) . ? C61 C62 1.386(12) . ? C62 C63 1.370(14) . ? C63 C64 1.397(13) . ? C64 C65 1.386(11) . ? C70 C71 1.406(10) . ? C70 C75 1.408(10) . ? C71 C72 1.387(10) . ? C72 C73 1.383(10) . ? C73 C74 1.372(10) . ? C74 C75 1.387(10) . ? C80 C81 1.398(10) . ? C80 C85 1.403(10) . ? C81 C82 1.377(10) . ? C82 C83 1.364(12) . ? C83 C84 1.385(12) . ? C84 C85 1.384(10) . ? C90 C91 1.397(10) . ? C90 C95 1.421(10) . ? C91 C92 1.411(10) . ? C92 C93 1.382(11) . ? C93 C94 1.375(10) . ? C94 C95 1.376(10) . ? N1S C1S 1.137(12) . ? C1S C2S 1.428(13) . ? 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 N3C Cu1 N3A 123.1(3) . . y N3C Cu1 N3B 118.0(2) . . y N3A Cu1 N3B 112.0(2) . . y N3C Cu1 N1 80.8(2) . . y N3A Cu1 N1 83.0(2) . . y N3B Cu1 N1 80.1(2) . . y N3C Cu1 H9A 92.0 . . ? N3A Cu1 H9A 73.0 . . ? N3B Cu1 H9A 131.5 . . ? N1 Cu1 H9A 145.6 . . ? N3C Cu1 H9C 72.1 . . ? N3A Cu1 H9C 134.2 . . ? N3B Cu1 H9C 89.6 . . ? N1 Cu1 H9C 142.0 . . ? H9A Cu1 H9C 63.0 . . ? N3C Cu1 H9B 133.8 . . ? N3A Cu1 H9B 87.9 . . ? N3B Cu1 H9B 68.8 . . ? N1 Cu1 H9B 141.4 . . ? H9A Cu1 H9B 63.1 . . ? H9C Cu1 H9B 62.1 . . ? N3C Cu1 Cu2 100.67(18) . . ? N3A Cu1 Cu2 98.48(17) . . ? N3B Cu1 Cu2 96.68(17) . . ? N1 Cu1 Cu2 176.76(16) . . ? H9A Cu1 Cu2 37.5 . . ? H9C Cu1 Cu2 37.2 . . ? H9B Cu1 Cu2 36.2 . . ? N4B Cu2 N4C 122.2(3) . . y N4B Cu2 N4A 114.2(3) . . y N4C Cu2 N4A 117.7(3) . . y N4B Cu2 N2 82.6(2) . . y N4C Cu2 N2 81.7(2) . . y N4A Cu2 N2 81.2(2) . . y N4B Cu2 H9B 73.1 . . ? N4C Cu2 H9B 87.4 . . ? N4A Cu2 H9B 134.8 . . ? N2 Cu2 H9B 142.4 . . ? N4B Cu2 H9C 137.2 . . ? N4C Cu2 H9C 71.5 . . ? N4A Cu2 H9C 85.2 . . ? N2 Cu2 H9C 139.7 . . ? H9B Cu2 H9C 67.0 . . ? N4B Cu2 H9A 87.0 . . ? N4C Cu2 H9A 133.3 . . ? N4A Cu2 H9A 70.2 . . ? N2 Cu2 H9A 142.2 . . ? H9B Cu2 H9A 65.6 . . ? H9C Cu2 H9A 63.1 . . ? N4B Cu2 Cu1 99.32(18) . . ? N4C Cu2 Cu1 99.18(17) . . ? N4A Cu2 Cu1 95.75(17) . . ? N2 Cu2 Cu1 176.90(16) . . ? H9B Cu2 Cu1 40.7 . . ? H9C Cu2 Cu1 38.8 . . ? H9A Cu2 Cu1 36.0 . . ? C1C N1 C1B 114.8(6) . . ? C1C N1 C1A 115.3(6) . . ? C1B N1 C1A 115.0(6) . . ? C1C N1 Cu1 103.6(4) . . ? C1B N1 Cu1 104.2(4) . . ? C1A N1 Cu1 101.5(4) . . ? N1 C1A C2A 111.2(6) . . ? N3A C2A C1A 109.8(6) . . ? C3A N3A C2A 116.5(6) . . ? C3A N3A Cu1 137.0(6) . . ? C2A N3A Cu1 105.8(4) . . ? N3A C3A C4A 124.9(7) . . ? C9A C4A C5A 118.3(7) . . ? C9A C4A C3A 124.1(7) . . ? C5A C4A C3A 117.4(7) . . ? C6A C5A C4A 121.4(8) . . ? C7A C6A C5A 118.7(8) . . ? C6A C7A C8A 121.4(8) . . ? C9A C8A C7A 118.8(7) . . ? C9A C8A C10A 123.2(7) . . ? C7A C8A C10A 117.7(7) . . ? C8A C9A C4A 121.2(7) . . ? N4A C10A C8A 124.3(7) . . ? C10A N4A C11A 117.2(7) . . ? C10A N4A Cu2 134.0(6) . . ? C11A N4A Cu2 105.5(5) . . ? N4A C11A C12A 106.7(6) . . ? N2 C12A C11A 110.5(6) . . ? C12B N2 C12A 114.7(7) . . ? C12B N2 C12C 114.9(6) . . ? C12A N2 C12C 114.3(6) . . ? C12B N2 Cu2 103.2(4) . . ? C12A N2 Cu2 103.7(4) . . ? C12C N2 Cu2 103.9(5) . . ? N1 C1B C2B 111.3(6) . . ? N3B C2B C1B 107.2(6) . . ? C3B N3B C2B 116.5(6) . . ? C3B N3B Cu1 131.6(5) . . ? C2B N3B Cu1 106.9(4) . . ? N3B C3B C4B 125.3(7) . . ? C9B C4B C5B 118.6(8) . . ? C9B C4B C3B 124.0(7) . . ? C5B C4B C3B 117.3(7) . . ? C6B C5B C4B 121.2(8) . . ? C5B C6B C7B 119.9(9) . . ? C8B C7B C6B 119.4(8) . . ? C7B C8B C9B 119.9(7) . . ? C7B C8B C10B 115.4(7) . . ? C9B C8B C10B 124.7(7) . . ? C4B C9B C8B 121.0(7) . . ? N4B C10B C8B 124.6(8) . . ? C10B N4B C11B 116.1(7) . . ? C10B N4B Cu2 137.5(6) . . ? C11B N4B Cu2 105.3(5) . . ? N4B C11B C12B 109.5(7) . . ? N2 C12B C11B 110.2(7) . . ? N1 C1C C2C 110.0(6) . . ? N3C C2C C1C 108.0(6) . . ? C3C N3C C2C 117.3(7) . . ? C3C N3C Cu1 134.8(6) . . ? C2C N3C Cu1 106.1(5) . . ? N3C C3C C4C 126.0(8) . . ? C5C C4C C9C 118.5(7) . . ? C5C C4C C3C 116.8(7) . . ? C9C C4C C3C 124.5(7) . . ? C6C C5C C4C 120.8(8) . . ? C7C C6C C5C 119.5(8) . . ? C6C C7C C8C 121.8(8) . . ? C9C C8C C7C 118.7(7) . . ? C9C C8C C10C 123.2(7) . . ? C7C C8C C10C 118.0(7) . . ? C8C C9C C4C 120.7(7) . . ? N4C C10C C8C 127.1(8) . . ? C10C N4C C11C 117.1(7) . . ? C10C N4C Cu2 135.9(6) . . ? C11C N4C Cu2 104.8(5) . . ? N4C C11C C12C 109.5(6) . . ? N2 C12C C11C 110.0(6) . . ? C40 B1 C50 109.9(7) . . ? C40 B1 C20 109.4(7) . . ? C50 B1 C20 109.1(6) . . ? C40 B1 C30 109.3(6) . . ? C50 B1 C30 109.6(7) . . ? C20 B1 C30 109.4(7) . . ? C21 C20 C25 114.8(7) . . ? C21 C20 B1 123.5(7) . . ? C25 C20 B1 121.7(7) . . ? C20 C21 C22 122.6(7) . . ? C23 C22 C21 120.3(7) . . ? C24 C23 C22 119.0(8) . . ? C23 C24 C25 120.2(8) . . ? C24 C25 C20 123.1(8) . . ? C35 C30 C31 115.6(8) . . ? C35 C30 B1 122.2(7) . . ? C31 C30 B1 122.2(8) . . ? C32 C31 C30 122.5(8) . . ? C31 C32 C33 121.1(8) . . ? C34 C33 C32 118.2(9) . . ? C33 C34 C35 121.3(9) . . ? C34 C35 C30 121.2(8) . . ? C45 C40 C41 113.1(7) . . ? C45 C40 B1 124.0(7) . . ? C41 C40 B1 122.6(7) . . ? C42 C41 C40 122.8(9) . . ? C43 C42 C41 121.8(9) . . ? C42 C43 C44 117.8(9) . . ? C43 C44 C45 120.5(9) . . ? C44 C45 C40 123.8(8) . . ? C51 C50 C55 113.9(8) . . ? C51 C50 B1 123.6(7) . . ? C55 C50 B1 122.5(8) . . ? C52 C51 C50 123.5(9) . . ? C53 C52 C51 119.3(10) . . ? C54 C53 C52 119.4(10) . . ? C53 C54 C55 120.7(10) . . ? C54 C55 C50 123.1(9) . . ? C90 B2 C70 107.6(6) . . ? C90 B2 C80 112.2(7) . . ? C70 B2 C80 110.6(6) . . ? C90 B2 C60 109.6(6) . . ? C70 B2 C60 109.9(7) . . ? C80 B2 C60 107.0(7) . . ? C65 C60 C61 114.6(8) . . ? C65 C60 B2 125.4(8) . . ? C61 C60 B2 120.0(8) . . ? C62 C61 C60 122.4(9) . . ? C63 C62 C61 120.7(11) . . ? C62 C63 C64 119.1(10) . . ? C65 C64 C63 118.1(10) . . ? C60 C65 C64 125.0(9) . . ? C71 C70 C75 114.7(7) . . ? C71 C70 B2 120.5(7) . . ? C75 C70 B2 124.8(7) . . ? C72 C71 C70 122.3(8) . . ? C73 C72 C71 121.0(8) . . ? C74 C73 C72 118.4(8) . . ? C73 C74 C75 120.7(8) . . ? C74 C75 C70 122.9(7) . . ? C81 C80 C85 114.1(7) . . ? C81 C80 B2 125.8(7) . . ? C85 C80 B2 120.0(7) . . ? C82 C81 C80 122.7(8) . . ? C83 C82 C81 121.3(9) . . ? C82 C83 C84 118.7(9) . . ? C85 C84 C83 119.3(8) . . ? C84 C85 C80 123.7(8) . . ? C91 C90 C95 114.9(7) . . ? C91 C90 B2 124.2(7) . . ? C95 C90 B2 120.9(7) . . ? C90 C91 C92 122.7(8) . . ? C93 C92 C91 119.9(8) . . ? C94 C93 C92 118.7(8) . . ? C93 C94 C95 121.5(8) . . ? C94 C95 C90 122.3(8) . . ? N1S C1S C2S 177.3(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3A C3A C10A N4A 40.9(7) . . . . ? N3B C3B C10B N4B 32.8(7) . . . . ? N3C C3C C10C N4C 34.8(7) . . . . ? C1A N1 Cu1 N3A 2.1(5) . . . . ? C1B N1 Cu1 N3B 7.9(5) . . . . ? C1C N1 Cu1 N3C 7.5(5) . . . . ? C12A N2 Cu2 N4A 6.4(5) . . . . ? C12B N2 Cu2 N4B 2.4(5) . . . . ? C12C N2 Cu2 N4C 6.3(5) . . . . ? C1A N1 N2 C12A 99.6(6) . . . . ? C1B N1 N2 C12B 99.3(6) . . . . ? C1C N1 N2 C12C 98.2(6) . . . . ? N3A Cu1 Cu2 N4A 91.2(3) . . . . ? N3B Cu1 Cu2 N4B 89.1(3) . . . . ? N3C Cu1 Cu2 N4C 84.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.405 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.092 data_Complex2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H49.50 Cl2 Cu2 N8 O11.69' _chemical_formula_weight 979.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 22.386(4) _cell_length_b 22.386(4) _cell_length_c 45.09(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 19567(10) _cell_formula_units_Z 18 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 21 _cell_measurement_theta_min 5.13 _cell_measurement_theta_max 9.91 _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour brown _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9127 _exptl_absorpt_coefficient_mu 1.168 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.651 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5598 _diffrn_reflns_av_R_equivalents 0.0747 _diffrn_reflns_av_sigmaI/netI 0.1929 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 22.49 _reflns_number_total 5294 _reflns_number_gt 2543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0933P)^2^+59.4822P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5294 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1985 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.2251 _refine_ls_wR_factor_gt 0.1756 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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_multiplicit _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.25236(8) 0.24088(8) 0.28518(4) 0.0279(5) Uani 1 1 d . . . Cu2 Cu 0.44280(8) 0.37896(8) 0.23076(4) 0.0297(5) Uani 1 1 d . . . N1 N 0.1580(5) 0.1648(5) 0.3114(2) 0.030(3) Uani 1 1 d . . . C1A C 0.1738(7) 0.1199(7) 0.3295(3) 0.036(4) Uani 1 1 d . . . H1A1 H 0.1303 0.0841 0.3386 0.044 Uiso 1 1 calc R . . H1A2 H 0.2045 0.1480 0.3458 0.044 Uiso 1 1 calc R . . C2A C 0.2075(7) 0.0834(7) 0.3143(3) 0.038(4) Uani 1 1 d . . . H2A1 H 0.1782 0.0564 0.2974 0.046 Uiso 1 1 calc R . . H2A2 H 0.2091 0.0505 0.3285 0.046 Uiso 1 1 calc R . . C3A C 0.2807(7) 0.1316(7) 0.3028(3) 0.029(3) Uani 1 1 d . . . H3A1 H 0.3084 0.1644 0.3187 0.035 Uiso 1 1 calc R . . H3A2 H 0.3028 0.1041 0.2977 0.035 Uiso 1 1 calc R . . N3A N 0.2799(5) 0.1702(5) 0.2766(2) 0.023(3) Uani 1 1 d . . . C4A C 0.2829(7) 0.1438(7) 0.2519(3) 0.035(4) Uani 1 1 d . . . H4A H 0.2849 0.1024 0.2523 0.041 Uiso 1 1 calc R . . C5A C 0.2836(7) 0.1738(7) 0.2238(3) 0.033(4) Uani 1 1 d . . . C6A C 0.2644(9) 0.1461(8) 0.1962(4) 0.056(5) Uani 1 1 d . . . H6A H 0.2462 0.0990 0.1909 0.067 Uiso 1 1 calc R . . C7A C 0.2772(8) 0.2012(8) 0.1769(3) 0.050(4) Uani 1 1 d . . . H7A H 0.2683 0.1978 0.1562 0.060 Uiso 1 1 calc R . . C8A C 0.3037(7) 0.2583(7) 0.1929(3) 0.032(4) Uani 1 1 d . . . O1A O 0.3104(4) 0.2435(4) 0.22193(18) 0.027(2) Uani 1 1 d . . . C9A C 0.3337(7) 0.3284(7) 0.1849(3) 0.031(4) Uani 1 1 d . . . H9A H 0.3176 0.3381 0.1670 0.038 Uiso 1 1 calc R . . N4A N 0.3801(6) 0.3801(6) 0.1990(2) 0.031(3) Uani 1 1 d . . . C10A C 0.4020(7) 0.4482(7) 0.1866(3) 0.045(4) Uani 1 1 d . . . H10A H 0.4068 0.4801 0.2029 0.054 Uiso 1 1 calc R . . H10B H 0.3659 0.4450 0.1729 0.054 Uiso 1 1 calc R . . C11A C 0.4710(8) 0.4782(9) 0.1697(4) 0.076(6) Uani 1 1 d . . . H11A H 0.4667 0.4438 0.1549 0.091 Uiso 1 1 calc R . . H11B H 0.4780 0.5195 0.1587 0.091 Uiso 1 1 calc R . . C12A C 0.5325(9) 0.4977(10) 0.1873(4) 0.076(6) Uani 1 1 d . . . H12A H 0.5373 0.5334 0.2016 0.091 Uiso 1 1 calc R . . H12B H 0.5727 0.5197 0.1738 0.091 Uiso 1 1 calc R . . N2 N 0.5377(6) 0.4443(7) 0.2041(3) 0.051(4) Uani 1 1 d . . . C1B C 0.1014(6) 0.1214(7) 0.2910(3) 0.040(4) Uani 1 1 d . . . H1B1 H 0.0595 0.0930 0.3030 0.048 Uiso 1 1 calc R . . H1B2 H 0.1132 0.0894 0.2809 0.048 Uiso 1 1 calc R . . C2B C 0.0839(7) 0.1594(8) 0.2673(3) 0.053(5) Uani 1 1 d . . . H2B1 H 0.0402 0.1257 0.2576 0.064 Uiso 1 1 calc R . . H2B2 H 0.0759 0.1941 0.2773 0.064 Uiso 1 1 calc R . . C3B C 0.1377(7) 0.1951(8) 0.2436(3) 0.046(4) Uani 1 1 d . . . H3B1 H 0.1521 0.1628 0.2359 0.056 Uiso 1 1 calc R . . H3B2 H 0.1171 0.2075 0.2270 0.056 Uiso 1 1 calc R . . N3B N 0.1991(6) 0.2580(7) 0.2544(2) 0.035(3) Uani 1 1 d . . . C4B C 0.2055(8) 0.3166(9) 0.2458(3) 0.045(4) Uani 1 1 d . . . H4B H 0.1699 0.3149 0.2337 0.054 Uiso 1 1 calc R . . C5B C 0.2616(8) 0.3829(8) 0.2531(3) 0.040(4) Uani 1 1 d . . . C6B C 0.2663(10) 0.4447(10) 0.2551(4) 0.057(5) Uani 1 1 d . . . H6B H 0.2306 0.4545 0.2507 0.069 Uiso 1 1 calc R . . C7B C 0.3312(12) 0.4913(10) 0.2646(4) 0.071(6) Uani 1 1 d . . . H7B H 0.3483 0.5385 0.2692 0.085 Uiso 1 1 calc R . . C8B C 0.3672(10) 0.4562(8) 0.2661(3) 0.044(4) Uani 1 1 d . . . O1B O 0.3232(5) 0.3887(5) 0.2594(2) 0.036(2) Uani 1 1 d . . . C9B C 0.4375(10) 0.4784(8) 0.2732(4) 0.053(5) Uani 1 1 d . . . H9B H 0.4619 0.5182 0.2852 0.064 Uiso 1 1 calc R . . N4B N 0.4687(6) 0.4482(6) 0.2643(2) 0.037(3) Uani 1 1 d . . . C10B C 0.5404(8) 0.4770(8) 0.2744(3) 0.059(5) Uani 1 1 d . . . H10C H 0.5489 0.5102 0.2906 0.071 Uiso 1 1 calc R . . H10D H 0.5458 0.4391 0.2828 0.071 Uiso 1 1 calc R . . C11B C 0.5925(10) 0.5116(12) 0.2518(5) 0.102(9) Uani 1 1 d . . . H11C H 0.5894 0.5525 0.2456 0.122 Uiso 1 1 calc R . . H11D H 0.6376 0.5295 0.2617 0.122 Uiso 1 1 calc R . . C12B C 0.5960(8) 0.4804(12) 0.2259(5) 0.100(8) Uani 1 1 d . . . H12C H 0.6093 0.4461 0.2319 0.120 Uiso 1 1 calc R . . H12D H 0.6354 0.5164 0.2146 0.120 Uiso 1 1 calc R . . C1C C 0.1346(8) 0.2016(9) 0.3318(3) 0.058(5) Uani 1 1 d . . . H1C1 H 0.0991 0.1674 0.3453 0.070 Uiso 1 1 calc R . . H1C2 H 0.1126 0.2224 0.3198 0.070 Uiso 1 1 calc R . . C2C C 0.1915(8) 0.2578(8) 0.3503(3) 0.049(4) Uani 1 1 d . . . H2C1 H 0.1695 0.2731 0.3653 0.059 Uiso 1 1 calc R . . H2C2 H 0.2150 0.2370 0.3612 0.059 Uiso 1 1 calc R . . C3C C 0.2457(8) 0.3208(7) 0.3345(3) 0.045(4) Uani 1 1 d . . . H3C1 H 0.2234 0.3359 0.3197 0.055 Uiso 1 1 calc R . . H3C2 H 0.2701 0.3587 0.3490 0.055 Uiso 1 1 calc R . . N3C N 0.2961(6) 0.3067(6) 0.3195(2) 0.034(3) Uani 1 1 d . . . C4C C 0.3537(8) 0.3296(7) 0.3322(3) 0.042(4) Uani 1 1 d . . . H4C H 0.3595 0.3534 0.3504 0.051 Uiso 1 1 calc R . . C5C C 0.4131(8) 0.3236(7) 0.3219(3) 0.041(4) Uani 1 1 d . . . C6C C 0.4681(7) 0.3279(7) 0.3355(3) 0.037(4) Uani 1 1 d . . . H6C H 0.4814 0.3410 0.3555 0.044 Uiso 1 1 calc R . . C7C C 0.5025(7) 0.3094(7) 0.3147(3) 0.035(4) Uani 1 1 d . . . H7C H 0.5426 0.3059 0.3181 0.042 Uiso 1 1 calc R . . C8C C 0.4674(7) 0.2974(7) 0.2887(3) 0.033(4) Uani 1 1 d . . . O1C O 0.4107(4) 0.3043(4) 0.29261(19) 0.029(2) Uani 1 1 d . . . C9C C 0.4793(7) 0.2811(7) 0.2599(3) 0.029(3) Uani 1 1 d . . . H9C H 0.4996 0.2528 0.2581 0.035 Uiso 1 1 calc R . . N4C N 0.4647(6) 0.3019(6) 0.2360(3) 0.036(3) Uani 1 1 d . . . C10C C 0.4802(9) 0.2795(9) 0.2076(3) 0.056(5) Uani 1 1 d . . . H10E H 0.4861 0.2392 0.2112 0.067 Uiso 1 1 calc R . . H10F H 0.4407 0.2650 0.1939 0.067 Uiso 1 1 calc R . . C11C C 0.5428(12) 0.3347(14) 0.1936(5) 0.116(9) Uani 1 1 d . . . H11E H 0.5811 0.3476 0.2078 0.139 Uiso 1 1 calc R . . H11F H 0.5527 0.3143 0.1762 0.139 Uiso 1 1 calc R . . C12C C 0.5469(10) 0.3988(13) 0.1837(4) 0.097(9) Uani 1 1 d . . . H12E H 0.5927 0.4269 0.1743 0.117 Uiso 1 1 calc R . . H12F H 0.5122 0.3863 0.1678 0.117 Uiso 1 1 calc R . . Cl1 Cl 0.3333 0.6667 0.05122(16) 0.0451(18) Uani 1 3 d S . . O11 O 0.3333 0.6667 0.0186(4) 0.067(6) Uani 1 3 d S . . O12 O 0.2713(5) 0.6640(5) 0.0612(3) 0.062(3) Uani 1 1 d . . . Cl2 Cl 0.0000 0.0000 0.05692(18) 0.054(3) Uani 0.458(18) 3 d SP . 1 O21 O 0.0000 0.0000 0.0891(8) 0.039(10) Uiso 0.458(18) 3 d SP . 1 O22 O 0.0541(12) 0.0646(11) 0.0455(6) 0.041(7) Uiso 0.458(18) 1 d P . 1 Cl2' Cl 0.0000 0.0000 0.05692(18) 0.054(3) Uani 0.54 3 d SP . 2 O21' O 0.0000 0.0000 0.0189(10) 0.104(16) Uiso 0.542(18) 3 d SP . 2 O22' O 0.0492(10) 0.0679(10) 0.0603(5) 0.038(6) Uiso 0.542(18) 1 d P . 2 Cl3 Cl 0.0000 0.0000 0.2095(2) 0.075(2) Uani 1 3 d S . . O31 O 0.0000 0.0000 0.2430(5) 0.141(11) Uani 1 3 d S . . O32 O 0.0649(8) 0.0471(10) 0.2039(4) 0.169(9) Uani 1 1 d . . . Cl4 Cl 0.2918(3) -0.0198(2) 0.23601(14) 0.0836(18) Uani 1 1 d . . . O41 O 0.3388(6) 0.0402(7) 0.2212(3) 0.087(4) Uani 1 1 d . . . O42 O 0.2969(9) -0.0765(7) 0.2284(4) 0.123(6) Uani 1 1 d . . . O43 O 0.2848(14) -0.0134(10) 0.2638(3) 0.192(11) Uani 1 1 d . . . O44 O 0.2263(9) -0.0269(10) 0.2221(5) 0.170(8) Uani 1 1 d . . . O1W O 0.2155(16) 0.6869(17) 0.1290(7) 0.132(12) Uiso 0.50 1 d P . . O2W O 0.203(3) 0.600(3) 0.1682(12) 0.094(17) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0325(10) 0.0307(10) 0.0245(10) 0.0012(8) 0.0013(8) 0.0189(9) Cu2 0.0291(10) 0.0346(10) 0.0230(10) 0.0010(8) 0.0002(8) 0.0141(9) N1 0.025(7) 0.037(7) 0.023(7) 0.008(6) 0.005(5) 0.011(6) C1A 0.041(9) 0.041(9) 0.022(9) 0.013(7) 0.003(7) 0.017(8) C2A 0.051(10) 0.024(8) 0.040(10) -0.006(7) -0.011(8) 0.020(8) C3A 0.038(9) 0.034(8) 0.025(8) -0.006(7) -0.008(7) 0.025(7) N3A 0.014(6) 0.027(6) 0.028(7) -0.003(6) -0.006(5) 0.010(5) C4A 0.059(10) 0.027(8) 0.031(9) -0.014(7) -0.006(8) 0.031(8) C5A 0.059(10) 0.033(9) 0.021(9) -0.016(7) -0.014(7) 0.033(8) C6A 0.091(14) 0.028(9) 0.042(11) -0.005(8) -0.011(10) 0.025(9) C7A 0.089(13) 0.041(10) 0.013(8) 0.002(8) -0.002(9) 0.027(10) C8A 0.042(9) 0.040(10) 0.016(8) -0.012(8) -0.005(7) 0.022(8) O1A 0.036(6) 0.037(6) 0.015(5) -0.004(4) -0.001(4) 0.025(5) C9A 0.028(9) 0.046(10) 0.028(9) 0.007(8) -0.001(7) 0.025(8) N4A 0.025(7) 0.036(7) 0.025(7) 0.011(6) 0.011(6) 0.009(6) C10A 0.050(10) 0.026(8) 0.052(11) 0.022(8) 0.001(8) 0.013(8) C11A 0.054(12) 0.071(13) 0.067(13) 0.049(11) 0.012(11) 0.005(11) C12A 0.048(12) 0.072(14) 0.076(15) 0.041(12) 0.019(11) 0.007(11) N2 0.030(8) 0.066(10) 0.055(9) 0.012(8) 0.016(7) 0.023(7) C1B 0.007(7) 0.048(10) 0.039(10) 0.010(8) 0.008(7) -0.005(7) C2B 0.030(9) 0.073(12) 0.038(10) 0.012(9) 0.020(8) 0.011(9) C3B 0.046(10) 0.060(11) 0.039(10) 0.018(9) -0.009(8) 0.031(9) N3B 0.036(8) 0.057(9) 0.023(7) 0.002(7) 0.005(6) 0.031(7) C4B 0.053(11) 0.091(14) 0.023(9) 0.014(9) 0.011(8) 0.062(11) C5B 0.043(10) 0.042(11) 0.048(11) 0.018(8) 0.015(8) 0.031(9) C6B 0.076(14) 0.082(14) 0.053(12) 0.036(11) 0.036(11) 0.068(12) C7B 0.131(19) 0.062(13) 0.050(13) 0.018(10) 0.047(13) 0.071(15) C8B 0.090(14) 0.025(9) 0.028(9) -0.001(7) 0.023(9) 0.036(10) O1B 0.054(7) 0.032(6) 0.029(6) 0.006(5) 0.020(5) 0.027(5) C9B 0.072(14) 0.037(10) 0.038(11) -0.005(8) 0.004(10) 0.018(10) N4B 0.054(9) 0.030(7) 0.017(7) 0.011(6) -0.006(6) 0.014(7) C10B 0.066(12) 0.041(10) 0.037(10) 0.016(9) -0.009(10) 0.002(9) C11B 0.064(15) 0.115(19) 0.058(15) 0.013(14) -0.035(13) -0.006(13) C12B 0.014(10) 0.13(2) 0.090(18) 0.033(16) -0.001(11) -0.008(11) C1C 0.058(12) 0.104(15) 0.030(10) 0.011(10) 0.026(9) 0.055(12) C2C 0.055(11) 0.070(12) 0.036(10) -0.005(9) 0.021(9) 0.041(10) C3C 0.070(12) 0.045(10) 0.040(10) -0.006(8) 0.003(9) 0.043(9) N3C 0.040(8) 0.033(7) 0.025(7) 0.002(6) 0.009(6) 0.015(6) C4C 0.055(11) 0.020(8) 0.033(10) -0.005(7) 0.002(9) 0.005(8) C5C 0.060(11) 0.035(9) 0.014(8) 0.002(7) 0.014(8) 0.014(9) C6C 0.028(9) 0.043(9) 0.022(9) 0.006(7) 0.000(8) 0.004(8) C7C 0.022(8) 0.029(8) 0.030(9) 0.024(7) -0.007(7) -0.005(7) C8C 0.017(8) 0.042(9) 0.043(10) 0.001(8) 0.000(7) 0.017(7) O1C 0.027(5) 0.031(5) 0.020(5) 0.005(4) -0.003(4) 0.006(5) C9C 0.032(9) 0.028(8) 0.035(10) -0.003(7) -0.002(7) 0.019(7) N4C 0.039(7) 0.044(8) 0.028(7) -0.006(6) 0.000(6) 0.022(6) C10C 0.076(13) 0.109(15) 0.024(9) -0.009(10) 0.012(9) 0.076(12) C11C 0.13(2) 0.22(3) 0.058(15) 0.010(17) 0.053(15) 0.14(2) C12C 0.078(15) 0.19(2) 0.075(16) 0.083(17) 0.059(12) 0.102(17) Cl1 0.036(2) 0.036(2) 0.063(5) 0.000 0.000 0.0181(12) O11 0.084(9) 0.084(9) 0.031(12) 0.000 0.000 0.042(5) O12 0.041(7) 0.065(8) 0.089(9) 0.007(7) 0.018(6) 0.033(6) Cl2 0.042(3) 0.042(3) 0.077(6) 0.000 0.000 0.0210(17) Cl2' 0.042(3) 0.042(3) 0.077(6) 0.000 0.000 0.0210(17) Cl3 0.071(4) 0.071(4) 0.084(7) 0.000 0.000 0.0353(18) O31 0.191(19) 0.191(19) 0.043(17) 0.000 0.000 0.095(10) O32 0.082(11) 0.176(18) 0.182(19) -0.075(14) 0.054(12) 0.014(12) Cl4 0.059(3) 0.050(3) 0.114(5) -0.031(3) 0.035(3) 0.006(3) O41 0.075(9) 0.100(11) 0.080(10) 0.026(8) 0.006(8) 0.039(9) O42 0.181(16) 0.102(12) 0.139(14) -0.040(11) -0.009(12) 0.110(12) O43 0.48(4) 0.216(19) 0.013(7) 0.020(10) 0.037(13) 0.28(2) O44 0.086(13) 0.168(18) 0.23(2) -0.030(16) 0.014(14) 0.044(13) _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 N3B 1.987(11) . y Cu1 N3A 2.001(10) . y Cu1 N3C 2.020(12) . y Cu1 N1 2.271(10) . y Cu1 O1B 3.094(9) . ? Cu1 O1C 3.108(8) . ? Cu1 O1A 3.122(8) . ? Cu1 Cu2 4.535(2) . y Cu2 N4A 2.015(11) . y Cu2 N4C 2.030(12) . y Cu2 N4B 2.030(12) . y Cu2 N2 2.234(12) . y Cu2 O1A 3.025(9) . ? Cu2 O1B 3.075(9) . ? Cu2 O1C 3.144(8) . ? N1 C1B 1.469(16) . ? N1 C1A 1.470(15) . ? N1 C1C 1.494(17) . ? N1 N2 9.033(15) . ? C1A C2A 1.523(18) . ? C2A C3A 1.532(18) . ? C3A N3A 1.472(15) . ? N3A C4A 1.277(15) . ? C4A C5A 1.433(18) . ? C5A C6A 1.361(19) . ? C5A O1A 1.365(15) . ? C6A C7A 1.417(19) . ? C7A C8A 1.320(18) . ? C8A O1A 1.377(14) . ? C8A C9A 1.412(18) . ? C9A N4A 1.273(16) . ? N4A C10A 1.460(16) . ? C10A C11A 1.54(2) . ? C11A C12A 1.46(2) . ? C12A N2 1.47(2) . ? N2 C12C 1.46(2) . ? N2 C12B 1.51(2) . ? C1B C2B 1.53(2) . ? C2B C3B 1.505(18) . ? C3B N3B 1.473(17) . ? N3B C4B 1.307(17) . ? C4B C5B 1.42(2) . ? C5B C6B 1.34(2) . ? C5B O1B 1.350(16) . ? C6B C7B 1.37(2) . ? C7B C8B 1.38(2) . ? C8B O1B 1.362(16) . ? C8B C9B 1.43(2) . ? C9B N4B 1.258(18) . ? N4B C10B 1.472(18) . ? C10B C11B 1.45(2) . ? C11B C12B 1.38(3) . ? C1C C2C 1.52(2) . ? C2C C3C 1.503(19) . ? C3C N3C 1.479(16) . ? N3C C4C 1.262(17) . ? C4C C5C 1.48(2) . ? C5C C6C 1.333(19) . ? C5C O1C 1.383(15) . ? C6C C7C 1.401(19) . ? C7C C8C 1.361(18) . ? C8C O1C 1.364(14) . ? C8C C9C 1.411(18) . ? C9C N4C 1.279(16) . ? N4C C10C 1.478(16) . ? C10C C11C 1.47(3) . ? C11C C12C 1.46(3) . ? Cl1 O12 1.432(10) . ? Cl1 O12 1.432(10) 3_565 ? Cl1 O12 1.432(10) 2_665 ? Cl1 O11 1.469(19) . ? Cl2 O22 1.44(2) 2 ? Cl2 O22 1.44(2) 3 ? Cl2 O22 1.44(2) . ? Cl2 O21 1.45(4) . ? O21' O21' 1.71(9) 10 ? Cl3 O32 1.325(15) 3 ? Cl3 O32 1.325(15) 2 ? Cl3 O32 1.325(15) . ? Cl3 O31 1.51(2) . ? Cl4 O43 1.281(13) . ? Cl4 O42 1.372(12) . ? Cl4 O41 1.394(13) . ? Cl4 O44 1.53(2) . ? 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 N3B Cu1 N3A 117.9(4) . . y N3B Cu1 N3C 120.9(5) . . y N3A Cu1 N3C 119.8(4) . . y N3B Cu1 N1 94.8(4) . . y N3A Cu1 N1 92.7(4) . . y N3C Cu1 N1 94.5(4) . . y N3B Cu1 O1B 64.4(4) . . ? N3A Cu1 O1B 125.2(3) . . ? N3C Cu1 O1B 72.9(4) . . ? N1 Cu1 O1B 141.7(3) . . ? N3B Cu1 O1C 130.1(4) . . ? N3A Cu1 O1C 69.6(3) . . ? N3C Cu1 O1C 63.8(4) . . ? N1 Cu1 O1C 135.0(3) . . ? O1B Cu1 O1C 72.2(2) . . ? N3B Cu1 O1A 69.1(3) . . ? N3A Cu1 O1A 63.1(3) . . ? N3C Cu1 O1A 129.8(4) . . ? N1 Cu1 O1A 135.3(3) . . ? O1B Cu1 O1A 69.5(2) . . ? O1C Cu1 O1A 73.8(2) . . ? N3B Cu1 Cu2 86.6(3) . . ? N3A Cu1 Cu2 83.0(3) . . ? N3C Cu1 Cu2 88.3(3) . . ? N1 Cu1 Cu2 175.6(3) . . ? O1B Cu1 Cu2 42.52(17) . . ? O1C Cu1 Cu2 43.80(16) . . ? O1A Cu1 Cu2 41.64(16) . . ? N4A Cu2 N4C 124.1(5) . . y N4A Cu2 N4B 117.0(5) . . y N4C Cu2 N4B 117.6(5) . . y N4A Cu2 N2 92.8(5) . . y N4C Cu2 N2 93.7(5) . . y N4B Cu2 N2 95.0(5) . . y N4A Cu2 O1A 65.1(3) . . ? N4C Cu2 O1A 72.3(4) . . ? N4B Cu2 O1A 128.7(4) . . ? N2 Cu2 O1A 136.0(4) . . ? N4A Cu2 O1B 70.1(3) . . ? N4C Cu2 O1B 126.9(4) . . ? N4B Cu2 O1B 63.9(4) . . ? N2 Cu2 O1B 139.1(4) . . ? O1A Cu2 O1B 71.0(2) . . ? N4A Cu2 O1C 131.4(3) . . ? N4C Cu2 O1C 62.2(4) . . ? N4B Cu2 O1C 69.4(3) . . ? N2 Cu2 O1C 135.7(4) . . ? O1A Cu2 O1C 74.6(2) . . ? O1B Cu2 O1C 71.9(2) . . ? N4A Cu2 Cu1 88.2(3) . . ? N4C Cu2 Cu1 84.4(3) . . ? N4B Cu2 Cu1 86.0(3) . . ? N2 Cu2 Cu1 178.1(4) . . ? O1A Cu2 Cu1 43.29(15) . . ? O1B Cu2 Cu1 42.83(16) . . ? O1C Cu2 Cu1 43.17(15) . . ? C1B N1 C1A 108.4(11) . . ? C1B N1 C1C 109.0(11) . . ? C1A N1 C1C 107.9(11) . . ? C1B N1 Cu1 110.1(8) . . ? C1A N1 Cu1 110.5(8) . . ? C1C N1 Cu1 111.0(9) . . ? C1B N1 N2 109.0(7) . . ? C1A N1 N2 107.8(7) . . ? C1C N1 N2 114.6(8) . . ? Cu1 N1 N2 3.7(2) . . ? N1 C1A C2A 118.1(11) . . ? C1A C2A C3A 114.6(11) . . ? N3A C3A C2A 111.2(10) . . ? C4A N3A C3A 114.1(11) . . ? C4A N3A Cu1 130.1(9) . . ? C3A N3A Cu1 114.1(8) . . ? N3A C4A C5A 122.9(12) . . ? C6A C5A O1A 108.9(12) . . ? C6A C5A C4A 132.0(13) . . ? O1A C5A C4A 119.0(11) . . ? C5A C6A C7A 106.4(13) . . ? C8A C7A C6A 107.8(13) . . ? C7A C8A O1A 109.6(12) . . ? C7A C8A C9A 132.1(14) . . ? O1A C8A C9A 117.6(12) . . ? C5A O1A C8A 107.1(10) . . ? C5A O1A Cu2 142.0(8) . . ? C8A O1A Cu2 93.1(7) . . ? C5A O1A Cu1 89.0(7) . . ? C8A O1A Cu1 141.1(7) . . ? Cu2 O1A Cu1 95.1(2) . . ? N4A C9A C8A 127.0(13) . . ? C9A N4A C10A 117.0(12) . . ? C9A N4A Cu2 126.9(9) . . ? C10A N4A Cu2 114.4(9) . . ? N4A C10A C11A 112.6(12) . . ? C12A C11A C10A 117.0(15) . . ? C11A C12A N2 119.0(15) . . ? C12C N2 C12A 109.9(14) . . ? C12C N2 C12B 113.5(15) . . ? C12A N2 C12B 107.4(15) . . ? C12C N2 Cu2 107.6(11) . . ? C12A N2 Cu2 112.0(10) . . ? C12B N2 Cu2 106.5(10) . . ? C12C N2 N1 105.4(10) . . ? C12A N2 N1 114.2(8) . . ? C12B N2 N1 106.5(9) . . ? Cu2 N2 N1 2.5(3) . . ? N1 C1B C2B 116.3(12) . . ? C3B C2B C1B 115.6(12) . . ? N3B C3B C2B 113.0(13) . . ? C4B N3B C3B 116.3(12) . . ? C4B N3B Cu1 128.8(11) . . ? C3B N3B Cu1 114.2(9) . . ? N3B C4B C5B 125.1(14) . . ? C6B C5B O1B 109.8(16) . . ? C6B C5B C4B 131.8(16) . . ? O1B C5B C4B 118.4(13) . . ? C5B C6B C7B 108.3(16) . . ? C6B C7B C8B 106.4(16) . . ? O1B C8B C7B 108.4(16) . . ? O1B C8B C9B 119.7(13) . . ? C7B C8B C9B 131.8(17) . . ? C5B O1B C8B 106.9(12) . . ? C5B O1B Cu2 142.1(9) . . ? C8B O1B Cu2 90.0(8) . . ? C5B O1B Cu1 91.3(8) . . ? C8B O1B Cu1 143.3(8) . . ? Cu2 O1B Cu1 94.6(2) . . ? N4B C9B C8B 123.6(15) . . ? C9B N4B C10B 116.3(14) . . ? C9B N4B Cu2 128.7(11) . . ? C10B N4B Cu2 113.5(11) . . ? C11B C10B N4B 115.1(14) . . ? C12B C11B C10B 123.9(19) . . ? C11B C12B N2 124.7(18) . . ? N1 C1C C2C 114.6(12) . . ? C3C C2C C1C 117.8(13) . . ? N3C C3C C2C 111.2(11) . . ? C4C N3C C3C 116.1(12) . . ? C4C N3C Cu1 131.9(10) . . ? C3C N3C Cu1 111.3(9) . . ? N3C C4C C5C 127.2(14) . . ? C6C C5C O1C 110.6(14) . . ? C6C C5C C4C 133.7(14) . . ? O1C C5C C4C 115.5(14) . . ? C5C C6C C7C 107.3(13) . . ? C8C C7C C6C 106.4(13) . . ? C7C C8C O1C 110.3(13) . . ? C7C C8C C9C 132.6(13) . . ? O1C C8C C9C 117.1(12) . . ? C8C O1C C5C 105.3(11) . . ? C8C O1C Cu1 147.9(8) . . ? C5C O1C Cu1 96.0(8) . . ? C8C O1C Cu2 88.2(7) . . ? C5C O1C Cu2 136.0(8) . . ? Cu1 O1C Cu2 93.0(2) . . ? N4C C9C C8C 124.5(12) . . ? C9C N4C C10C 117.5(12) . . ? C9C N4C Cu2 128.4(10) . . ? C10C N4C Cu2 112.6(9) . . ? C11C C10C N4C 111.9(15) . . ? C12C C11C C10C 121.4(17) . . ? N2 C12C C11C 122.1(16) . . ? O12 Cl1 O12 110.6(5) . 3_565 ? O12 Cl1 O12 110.6(5) . 2_665 ? O12 Cl1 O12 110.6(5) 3_565 2_665 ? O12 Cl1 O11 108.3(5) . . ? O12 Cl1 O11 108.3(5) 3_565 . ? O12 Cl1 O11 108.3(5) 2_665 . ? O22 Cl2 O22 107.9(12) 2 3 ? O22 Cl2 O22 107.9(12) 2 . ? O22 Cl2 O22 107.9(12) 3 . ? O22 Cl2 O21 111.0(11) 2 . ? O22 Cl2 O21 111.0(11) 3 . ? O22 Cl2 O21 111.0(11) . . ? O32 Cl3 O32 116.4(6) 3 2 ? O32 Cl3 O32 116.4(6) 3 . ? O32 Cl3 O32 116.4(6) 2 . ? O32 Cl3 O31 101.0(10) 3 . ? O32 Cl3 O31 101.0(10) 2 . ? O32 Cl3 O31 101.0(10) . . ? O43 Cl4 O42 114.7(11) . . ? O43 Cl4 O41 115.8(12) . . ? O42 Cl4 O41 113.6(10) . . ? O43 Cl4 O44 104.4(13) . . ? O42 Cl4 O44 108.7(10) . . ? O41 Cl4 O44 97.3(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3A C4A C9A N4A 44.2(11) . . . . ? N3B C4B C9B N4B 45.0(13) . . . . ? N3C C4C C9C N4C 45.8(12) . . . . ? C1A N1 Cu1 N3A 39.3(9) . . . . ? C1B N1 Cu1 N3B 37.9(9) . . . . ? C1C N1 Cu1 N3C 38.7(9) . . . . ? C12A N2 Cu2 N4A 37.6(12) . . . . ? C12B N2 Cu2 N4B 37.2(13) . . . . ? C12C N2 Cu2 N4C 41.1(11) . . . . ? N3A Cu1 Cu2 N4A 111.3(4) . . . . ? N3B Cu1 Cu2 N4B 109.9(5) . . . . ? N3C Cu1 Cu2 N4C 107.1(5) . . . . ? C1A N1 N2 C12A -173.4(13) . . . . ? C1B N1 N2 C12B -172.6(14) . . . . ? C1C N1 N2 C12C -174.1(13) . . . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.813 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.115 data_complex3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H57 Ag Cl2 Cu N8 O12.50' _chemical_formula_weight 1080.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Ag' 'Ag' -0.8971 1.1015 '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 15.569(3) _cell_length_b 14.289(4) _cell_length_c 22.001(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.755(11) _cell_angle_gamma 90.00 _cell_volume 4710.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 12.41 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.96 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2228 _exptl_absorpt_coefficient_mu 1.048 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.44 _exptl_absorpt_correction_T_max 0.66 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 7017 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_sigmaI/netI 0.0974 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 22.49 _reflns_number_total 6141 _reflns_number_gt 3888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0929P)^2^+39.8606P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6141 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1395 _refine_ls_R_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.2267 _refine_ls_wR_factor_gt 0.1948 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicit _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.47488(8) 0.75928(9) 0.13993(7) 0.0269(4) Uani 1 1 d . . . Ag Ag 0.50360(6) 0.92308(8) 0.27269(5) 0.0462(4) Uani 1 1 d . . . N1 N 0.4560(6) 0.6633(7) 0.0538(4) 0.032(2) Uani 1 1 d . . . C1A C 0.4317(9) 0.7202(10) -0.0052(6) 0.044(3) Uani 1 1 d . . . H1A1 H 0.3727 0.7492 -0.0091 0.052 Uiso 1 1 calc R . . H1A2 H 0.4251 0.6774 -0.0416 0.052 Uiso 1 1 calc R . . C2A C 0.4963(9) 0.7963(10) -0.0102(6) 0.043(3) Uani 1 1 d . . . H2A1 H 0.4770 0.8231 -0.0532 0.051 Uiso 1 1 calc R . . H2A2 H 0.5557 0.7675 -0.0051 0.051 Uiso 1 1 calc R . . C3A C 0.5062(8) 0.8755(8) 0.0370(6) 0.035(3) Uani 1 1 d . . . H3A1 H 0.5410 0.9265 0.0246 0.042 Uiso 1 1 calc R . . H3A2 H 0.4462 0.9005 0.0351 0.042 Uiso 1 1 calc R . . N3A N 0.5508(6) 0.8477(6) 0.1033(4) 0.027(2) Uani 1 1 d . . . C4A C 0.6310(8) 0.8715(8) 0.1243(6) 0.032(3) Uani 1 1 d . . . H4A H 0.6583 0.9018 0.0958 0.039 Uiso 1 1 calc R . . C5A C 0.6851(7) 0.8569(8) 0.1878(5) 0.027(3) Uani 1 1 d . . . C6A C 0.7746(7) 0.8588(8) 0.2149(6) 0.033(3) Uani 1 1 d . . . H6A H 0.8195 0.8715 0.1942 0.040 Uiso 1 1 calc R . . C7A C 0.7884(8) 0.8385(8) 0.2791(7) 0.038(3) Uani 1 1 d . . . H7A H 0.8442 0.8337 0.3101 0.046 Uiso 1 1 calc R . . C8A C 0.7065(7) 0.8272(9) 0.2882(6) 0.034(3) Uani 1 1 d . . . O1A O 0.6424(5) 0.8374(5) 0.2323(4) 0.0301(19) Uani 1 1 d . . . C9A C 0.6759(8) 0.8142(8) 0.3437(6) 0.033(3) Uani 1 1 d . . . H9A H 0.7163 0.7894 0.3805 0.039 Uiso 1 1 calc R . . N4A N 0.5975(6) 0.8342(8) 0.3457(5) 0.040(3) Uani 1 1 d . . . C10A C 0.5755(9) 0.8155(11) 0.4054(6) 0.050(4) Uani 1 1 d . . . H10A H 0.5396 0.7574 0.4006 0.061 Uiso 1 1 calc R . . H10B H 0.6317 0.8040 0.4387 0.061 Uiso 1 1 calc R . . C11A C 0.5275(13) 0.8886(14) 0.4264(8) 0.086(6) Uani 1 1 d . . . H11A H 0.4642 0.8839 0.4018 0.103 Uiso 1 1 calc R . . H11B H 0.5298 0.8757 0.4711 0.103 Uiso 1 1 calc R . . C12A C 0.5554(13) 0.9836(13) 0.4226(7) 0.081(6) Uani 1 1 d . . . H12A H 0.6213 0.9836 0.4322 0.098 Uiso 1 1 calc R . . H12B H 0.5398 1.0191 0.4568 0.098 Uiso 1 1 calc R . . N2 N 0.5190(6) 1.0381(7) 0.3612(5) 0.036(3) Uani 1 1 d . . . C1B C 0.5398(8) 0.6136(9) 0.0583(6) 0.039(3) Uani 1 1 d . . . H1B1 H 0.5857 0.6601 0.0556 0.047 Uiso 1 1 calc R . . H1B2 H 0.5309 0.5717 0.0212 0.047 Uiso 1 1 calc R . . C2B C 0.5751(8) 0.5563(9) 0.1169(7) 0.044(4) Uani 1 1 d . . . H2B1 H 0.6250 0.5178 0.1109 0.053 Uiso 1 1 calc R . . H2B2 H 0.5274 0.5127 0.1206 0.053 Uiso 1 1 calc R . . C3B C 0.6077(8) 0.6077(9) 0.1789(6) 0.037(3) Uani 1 1 d . . . H3B1 H 0.6387 0.5629 0.2119 0.044 Uiso 1 1 calc R . . H3B2 H 0.6516 0.6557 0.1747 0.044 Uiso 1 1 calc R . . N3B N 0.5356(6) 0.6532(7) 0.1992(5) 0.030(2) Uani 1 1 d . . . C4B C 0.5146(7) 0.6140(9) 0.2444(6) 0.033(3) Uani 1 1 d . . . H4B H 0.5451 0.5582 0.2615 0.039 Uiso 1 1 calc R . . C5B C 0.4461(7) 0.6499(8) 0.2719(6) 0.032(3) Uani 1 1 d . . . C6B C 0.3975(8) 0.6119(8) 0.3078(6) 0.035(3) Uani 1 1 d . . . H6B H 0.4034 0.5503 0.3246 0.043 Uiso 1 1 calc R . . C7B C 0.3363(9) 0.6802(9) 0.3158(6) 0.042(3) Uani 1 1 d . . . H7B H 0.2915 0.6724 0.3373 0.050 Uiso 1 1 calc R . . C8B C 0.3534(7) 0.7590(9) 0.2871(5) 0.032(3) Uani 1 1 d . . . O1B O 0.4204(5) 0.7417(5) 0.2596(4) 0.0316(19) Uani 1 1 d . . . C9B C 0.3180(9) 0.8529(10) 0.2826(6) 0.041(3) Uani 1 1 d . . . H9B H 0.2618 0.8625 0.2908 0.049 Uiso 1 1 calc R . . N4B N 0.3575(7) 0.9220(7) 0.2685(4) 0.032(2) Uani 1 1 d . . . C10B C 0.3127(9) 1.0127(9) 0.2653(7) 0.047(4) Uani 1 1 d . . . H10C H 0.2910 1.0315 0.2204 0.056 Uiso 1 1 calc R . . H10D H 0.2599 1.0050 0.2817 0.056 Uiso 1 1 calc R . . C11B C 0.3674(10) 1.0882(9) 0.3001(8) 0.063(5) Uani 1 1 d . . . H11C H 0.3988 1.1161 0.2709 0.076 Uiso 1 1 calc R . . H11D H 0.3254 1.1364 0.3069 0.076 Uiso 1 1 calc R . . C12B C 0.4341(11) 1.0770(15) 0.3600(9) 0.101(8) Uani 1 1 d . . . H12C H 0.4448 1.1395 0.3801 0.121 Uiso 1 1 calc R . . H12D H 0.4076 1.0374 0.3872 0.121 Uiso 1 1 calc R . . C1C C 0.3845(8) 0.5959(9) 0.0523(6) 0.043(3) Uani 1 1 d . . . H1C1 H 0.4039 0.5545 0.0896 0.052 Uiso 1 1 calc R . . H1C2 H 0.3766 0.5563 0.0143 0.052 Uiso 1 1 calc R . . C2C C 0.2943(8) 0.6372(9) 0.0517(6) 0.043(3) Uani 1 1 d . . . H2C1 H 0.2767 0.6825 0.0165 0.052 Uiso 1 1 calc R . . H2C2 H 0.2495 0.5863 0.0432 0.052 Uiso 1 1 calc R . . C3C C 0.2917(8) 0.6860(9) 0.1120(6) 0.039(3) Uani 1 1 d . . . H3C1 H 0.2288 0.6965 0.1118 0.046 Uiso 1 1 calc R . . H3C2 H 0.3193 0.6450 0.1484 0.046 Uiso 1 1 calc R . . N3C N 0.3394(6) 0.7771(7) 0.1202(4) 0.032(2) Uani 1 1 d . . . C4C C 0.2915(8) 0.8495(10) 0.1040(6) 0.035(3) Uani 1 1 d . . . H4C H 0.2287 0.8416 0.0884 0.043 Uiso 1 1 calc R . . C5C C 0.3266(8) 0.9420(8) 0.1081(6) 0.030(3) Uani 1 1 d . . . C6C C 0.2914(9) 1.0232(9) 0.0792(6) 0.043(3) Uani 1 1 d . . . H6C H 0.2333 1.0314 0.0516 0.052 Uiso 1 1 calc R . . C7C C 0.3574(9) 1.0927(9) 0.0981(6) 0.044(3) Uani 1 1 d . . . H7C H 0.3532 1.1563 0.0850 0.053 Uiso 1 1 calc R . . C8C C 0.4286(8) 1.0503(8) 0.1388(5) 0.031(3) Uani 1 1 d . . . O1C O 0.4096(5) 0.9576(5) 0.1447(3) 0.0263(18) Uani 1 1 d . . . C9C C 0.5102(8) 1.0845(9) 0.1787(6) 0.034(3) Uani 1 1 d . . . H9C H 0.5299 1.1444 0.1693 0.041 Uiso 1 1 calc R . . N4C N 0.5586(6) 1.0413(7) 0.2259(5) 0.030(2) Uani 1 1 d . . . C10C C 0.6418(7) 1.0872(9) 0.2606(5) 0.033(3) Uani 1 1 d . . . H10E H 0.6930 1.0531 0.2525 0.040 Uiso 1 1 calc R . . H10F H 0.6426 1.1518 0.2447 0.040 Uiso 1 1 calc R . . C11C C 0.6525(10) 1.0903(18) 0.3284(8) 0.105(8) Uani 1 1 d . . . H11E H 0.6764 1.0284 0.3450 0.126 Uiso 1 1 calc R . . H11F H 0.7006 1.1362 0.3456 0.126 Uiso 1 1 calc R . . C12C C 0.5828(10) 1.1112(10) 0.3574(7) 0.056(4) Uani 1 1 d . . . H12E H 0.5485 1.1647 0.3344 0.067 Uiso 1 1 calc R . . H12F H 0.6113 1.1328 0.4010 0.067 Uiso 1 1 calc R . . Cl1 Cl 0.4362(2) 0.3488(2) 0.19014(16) 0.0425(8) Uani 1 1 d . . . O11 O 0.3849(7) 0.4335(7) 0.1743(5) 0.064(3) Uani 1 1 d . . . O12 O 0.4786(7) 0.3251(7) 0.1420(5) 0.066(3) Uani 1 1 d . . . O13 O 0.3793(6) 0.2752(7) 0.1979(6) 0.072(3) Uani 1 1 d . . . O14 O 0.5034(8) 0.3640(10) 0.2465(6) 0.098(4) Uani 1 1 d . . . Cl2 Cl 0.2274(3) 0.9250(3) -0.08991(18) 0.0738(14) Uani 1 1 d . . . O21 O 0.2098(8) 1.0201(9) -0.0763(6) 0.089(4) Uani 1 1 d . . . O22 O 0.2203(11) 0.8605(9) -0.0454(6) 0.116(5) Uani 1 1 d . . . O23 O 0.3217(12) 0.9245(11) -0.0848(11) 0.170(8) Uani 1 1 d . . . O24 O 0.1861(15) 0.8995(11) -0.1490(7) 0.191(11) Uani 1 1 d . . . O20 O 0.2103(8) 0.4172(12) 0.0766(8) 0.109(5) Uani 1 1 d . . . H20 H 0.2621 0.4274 0.0995 0.164 Uiso 1 1 calc R . . C21 C 0.2096(15) 0.3331(14) 0.0426(9) 0.098(7) Uani 1 1 d . . . H21A H 0.2239 0.2810 0.0734 0.118 Uiso 1 1 calc R . . H21B H 0.1481 0.3227 0.0159 0.118 Uiso 1 1 calc R . . C22 C 0.2672(10) 0.3275(18) 0.0043(9) 0.113(9) Uani 1 1 d . . . H22A H 0.2588 0.2673 -0.0180 0.169 Uiso 1 1 calc R . . H22B H 0.3290 0.3326 0.0303 0.169 Uiso 1 1 calc R . . H22C H 0.2543 0.3786 -0.0266 0.169 Uiso 1 1 calc R . . O30 O 0.4151(15) 0.3565(17) 0.3601(11) 0.082(7) Uiso 0.50 1 d P . . H30 H 0.4394 0.3599 0.3292 0.123 Uiso 0.50 1 d P . . C31 C 0.501(2) 0.373(3) 0.4102(17) 0.087(12) Uiso 0.50 1 d P . . H31A H 0.5469 0.3290 0.4030 0.105 Uiso 0.50 1 calc PR . . H31B H 0.5221 0.4372 0.4057 0.105 Uiso 0.50 1 calc PR . . C32 C 0.495(3) 0.360(3) 0.474(2) 0.111(14) Uiso 0.50 1 d P . . H32A H 0.5522 0.3748 0.5038 0.500 Uiso 0.50 1 calc PR . . H32B H 0.4782 0.2955 0.4797 0.500 Uiso 0.50 1 calc PR . . H32C H 0.4488 0.4026 0.4812 0.500 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0184(7) 0.0217(8) 0.0419(9) 0.0152(7) 0.0101(6) 0.0021(6) Ag 0.0328(6) 0.0551(7) 0.0546(7) 0.0174(6) 0.0186(5) 0.0071(5) N1 0.039(6) 0.023(6) 0.035(6) 0.001(5) 0.013(5) 0.002(5) C1A 0.049(8) 0.052(9) 0.034(8) -0.003(7) 0.017(6) -0.006(7) C2A 0.049(8) 0.048(9) 0.034(8) 0.005(7) 0.015(6) 0.004(7) C3A 0.043(7) 0.024(7) 0.041(8) 0.010(6) 0.018(6) 0.006(6) N3A 0.032(6) 0.018(5) 0.035(6) 0.004(5) 0.014(5) 0.008(4) C4A 0.036(8) 0.023(7) 0.045(8) 0.006(6) 0.023(6) 0.003(6) C5A 0.027(7) 0.026(7) 0.032(7) -0.004(6) 0.012(6) 0.003(5) C6A 0.029(7) 0.022(7) 0.053(9) 0.003(6) 0.018(6) -0.002(5) C7A 0.026(7) 0.030(7) 0.058(9) -0.008(7) 0.012(6) 0.005(6) C8A 0.026(7) 0.038(8) 0.038(8) -0.004(6) 0.011(6) 0.007(6) O1A 0.027(4) 0.026(5) 0.042(5) -0.006(4) 0.016(4) -0.002(4) C9A 0.031(7) 0.031(7) 0.030(7) -0.004(6) -0.001(6) 0.004(6) N4A 0.026(6) 0.059(8) 0.037(6) -0.017(6) 0.011(5) -0.005(5) C10A 0.044(8) 0.079(11) 0.028(8) -0.013(8) 0.009(6) -0.015(8) C11A 0.116(15) 0.094(15) 0.059(11) 0.009(10) 0.044(11) 0.045(13) C12A 0.128(15) 0.087(14) 0.044(10) -0.054(10) 0.051(10) -0.073(12) N2 0.028(5) 0.044(7) 0.039(6) -0.003(5) 0.015(5) 0.006(5) C1B 0.047(8) 0.026(7) 0.050(8) -0.003(6) 0.021(7) -0.004(6) C2B 0.039(7) 0.026(8) 0.075(10) 0.002(7) 0.031(7) 0.010(6) C3B 0.030(7) 0.027(7) 0.058(9) 0.007(6) 0.019(6) 0.011(6) N3B 0.024(5) 0.025(6) 0.044(7) -0.008(5) 0.015(5) -0.002(4) C4B 0.027(7) 0.025(7) 0.044(8) -0.007(6) 0.005(6) 0.001(6) C5B 0.031(7) 0.029(7) 0.032(7) -0.010(6) 0.003(6) 0.002(6) C6B 0.051(8) 0.015(7) 0.042(8) 0.006(6) 0.016(7) 0.003(6) C7B 0.057(9) 0.031(8) 0.042(8) -0.015(6) 0.022(7) -0.016(7) C8B 0.028(6) 0.035(8) 0.032(7) -0.018(6) 0.004(5) -0.004(6) O1B 0.029(4) 0.027(5) 0.040(5) -0.007(4) 0.011(4) 0.006(4) C9B 0.037(8) 0.050(10) 0.038(8) -0.018(7) 0.013(6) 0.013(7) N4B 0.043(6) 0.024(6) 0.034(6) 0.006(5) 0.016(5) 0.017(5) C10B 0.041(8) 0.042(9) 0.060(9) 0.000(7) 0.019(7) 0.016(7) C11B 0.059(10) 0.019(8) 0.102(13) 0.000(8) 0.006(9) 0.012(7) C12B 0.061(11) 0.122(17) 0.108(15) -0.082(14) 0.002(11) 0.029(11) C1C 0.055(8) 0.036(8) 0.042(8) -0.003(7) 0.020(7) -0.005(7) C2C 0.043(8) 0.041(8) 0.044(8) -0.007(7) 0.009(6) -0.021(7) C3C 0.030(7) 0.040(8) 0.047(8) 0.004(7) 0.012(6) -0.016(6) N3C 0.029(5) 0.038(7) 0.028(6) -0.004(5) 0.007(4) -0.010(5) C4C 0.019(6) 0.052(9) 0.035(8) 0.002(7) 0.005(5) -0.002(6) C5C 0.028(7) 0.026(8) 0.037(7) 0.003(6) 0.010(6) 0.002(6) C6C 0.042(8) 0.041(9) 0.046(8) -0.008(7) 0.012(7) 0.003(7) C7C 0.062(9) 0.027(8) 0.047(8) -0.003(7) 0.019(7) 0.007(7) C8C 0.035(7) 0.033(8) 0.030(7) 0.005(6) 0.017(6) 0.002(6) O1C 0.032(5) 0.019(4) 0.032(5) 0.002(4) 0.014(4) -0.002(3) C9C 0.044(8) 0.029(7) 0.039(8) -0.008(7) 0.028(7) 0.002(6) N4C 0.034(6) 0.021(5) 0.040(6) -0.011(5) 0.020(5) 0.004(5) C10C 0.027(6) 0.032(7) 0.042(8) -0.006(6) 0.013(6) -0.017(6) C11C 0.054(10) 0.19(2) 0.074(12) -0.062(14) 0.030(9) -0.078(13) C12C 0.070(10) 0.044(9) 0.065(10) -0.010(8) 0.037(8) -0.001(8) Cl1 0.0342(17) 0.036(2) 0.058(2) -0.0009(17) 0.0138(16) -0.0025(15) O11 0.065(7) 0.035(6) 0.097(8) 0.011(6) 0.031(6) 0.006(5) O12 0.076(7) 0.052(7) 0.087(8) -0.001(6) 0.051(6) 0.002(6) O13 0.053(6) 0.042(6) 0.140(10) 0.004(6) 0.060(7) -0.006(5) O14 0.072(8) 0.121(11) 0.088(9) -0.027(8) 0.001(7) 0.013(8) Cl2 0.101(3) 0.051(3) 0.049(2) 0.011(2) -0.014(2) -0.038(3) O21 0.102(9) 0.075(9) 0.104(10) 0.026(8) 0.055(8) 0.003(7) O22 0.192(15) 0.082(9) 0.068(8) 0.031(7) 0.024(9) -0.053(10) O23 0.117(13) 0.091(12) 0.28(2) 0.061(14) 0.006(14) 0.001(10) O24 0.30(2) 0.095(12) 0.094(12) 0.019(10) -0.083(14) -0.072(14) O20 0.079(9) 0.119(13) 0.136(13) 0.023(11) 0.038(9) 0.020(9) C21 0.132(19) 0.072(14) 0.080(14) 0.017(12) 0.011(13) 0.045(13) C22 0.043(10) 0.22(3) 0.089(14) 0.081(16) 0.036(10) 0.027(13) _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 Cu N3A 2.041(9) . y Cu N3C 2.051(10) . y Cu N3B 2.054(10) . y Cu N1 2.292(10) . y Cu O1B 2.987(8) . ? Cu O1C 3.021(7) . ? Cu O1A 3.050(7) . ? Cu Ag 3.674(2) . y Ag N4A 2.248(11) . y Ag N4B 2.251(10) . y Ag N4C 2.264(10) . y Ag N2 2.509(10) . y Ag O1A 2.829(7) . ? Ag O1C 2.841(7) . ? Ag O1B 2.876(8) . ? N1 C1B 1.465(15) . ? N1 C1C 1.466(15) . ? N1 C1A 1.492(15) . ? N1 N2 8.471(14) . ? C1A C2A 1.505(18) . ? C2A C3A 1.515(17) . ? C3A N3A 1.487(14) . ? N3A C4A 1.255(14) . ? C4A C5A 1.439(16) . ? C5A O1A 1.353(13) . ? C5A C6A 1.359(15) . ? C6A C7A 1.399(17) . ? C7A C8A 1.353(16) . ? C8A O1A 1.363(13) . ? C8A C9A 1.439(17) . ? C9A N4A 1.266(14) . ? N4A C10A 1.470(16) . ? C10A C11A 1.43(2) . ? C11A C12A 1.43(2) . ? C12A N2 1.53(2) . ? N2 C12B 1.428(17) . ? N2 C12C 1.460(17) . ? C1B C2B 1.500(17) . ? C2B C3B 1.510(18) . ? C3B N3B 1.467(14) . ? N3B C4B 1.261(15) . ? C4B C5B 1.456(17) . ? C5B C6B 1.346(17) . ? C5B O1B 1.377(14) . ? C6B C7B 1.408(17) . ? C7B C8B 1.352(17) . ? C8B O1B 1.365(13) . ? C8B C9B 1.443(18) . ? C9B N4B 1.247(16) . ? N4B C10B 1.464(15) . ? C10B C11B 1.456(19) . ? C11B C12B 1.45(2) . ? C1C C2C 1.519(18) . ? C2C C3C 1.509(17) . ? C3C N3C 1.484(15) . ? N3C C4C 1.269(15) . ? C4C C5C 1.423(17) . ? C5C O1C 1.344(13) . ? C5C C6C 1.365(17) . ? C6C C7C 1.408(18) . ? C7C C8C 1.364(17) . ? C8C O1C 1.372(14) . ? C8C C9C 1.420(17) . ? C9C N4C 1.266(15) . ? N4C C10C 1.467(14) . ? C10C C11C 1.455(19) . ? C11C C12C 1.43(2) . ? Cl1 O14 1.406(12) . ? Cl1 O13 1.414(10) . ? Cl1 O12 1.433(10) . ? Cl1 O11 1.441(10) . ? Cl2 O24 1.336(14) . ? Cl2 O22 1.371(11) . ? Cl2 O21 1.434(13) . ? Cl2 O23 1.442(18) . ? O20 C21 1.41(2) . ? C21 C22 1.39(2) . ? O30 C31 1.50(4) . ? C31 C32 1.44(5) . ? 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 N3A Cu N3C 120.9(4) . . y N3A Cu N3B 119.4(4) . . y N3C Cu N3B 119.7(4) . . y N3A Cu N1 90.1(4) . . y N3C Cu N1 90.3(4) . . y N3B Cu N1 90.9(4) . . y N3A Cu O1B 137.2(3) . . ? N3C Cu O1B 71.0(3) . . ? N3B Cu O1B 64.6(3) . . ? N1 Cu O1B 132.4(3) . . ? N3A Cu O1C 70.7(3) . . ? N3C Cu O1C 63.6(3) . . ? N3B Cu O1C 140.4(3) . . ? N1 Cu O1C 128.4(3) . . ? O1B Cu O1C 82.5(2) . . ? N3A Cu O1A 63.5(3) . . ? N3C Cu O1A 137.7(3) . . ? N3B Cu O1A 71.6(3) . . ? N1 Cu O1A 131.6(3) . . ? O1B Cu O1A 80.8(2) . . ? O1C Cu O1A 82.4(2) . . ? N3A Cu Ag 87.8(3) . . ? N3C Cu Ag 89.2(3) . . ? N3B Cu Ag 91.7(3) . . ? N1 Cu Ag 177.2(2) . . ? O1B Cu Ag 49.87(15) . . ? O1C Cu Ag 49.03(14) . . ? O1A Cu Ag 48.67(14) . . ? N4A Ag N4B 118.6(4) . . y N4A Ag N4C 119.6(4) . . y N4B Ag N4C 119.3(4) . . y N4A Ag N2 84.8(3) . . y N4B Ag N2 85.3(3) . . y N4C Ag N2 84.0(3) . . y N4A Ag O1A 64.9(3) . . ? N4B Ag O1A 146.5(3) . . ? N4C Ag O1A 76.4(3) . . ? N2 Ag O1A 127.4(3) . . ? N4A Ag O1C 150.0(3) . . ? N4B Ag O1C 73.6(3) . . ? N4C Ag O1C 65.0(3) . . ? N2 Ag O1C 124.8(3) . . ? O1A Ag O1C 89.8(2) . . ? N4A Ag O1B 75.5(3) . . ? N4B Ag O1B 64.4(3) . . ? N4C Ag O1B 147.4(3) . . ? N2 Ag O1B 127.8(3) . . ? O1A Ag O1B 86.6(2) . . ? O1C Ag O1B 87.7(2) . . ? N4A Ag Cu 97.1(3) . . ? N4B Ag Cu 93.4(3) . . ? N4C Ag Cu 95.4(2) . . ? N2 Ag Cu 178.1(2) . . ? O1A Ag Cu 54.07(15) . . ? O1C Ag Cu 53.42(15) . . ? O1B Ag Cu 52.55(15) . . ? C1B N1 C1C 109.9(9) . . ? C1B N1 C1A 109.4(9) . . ? C1C N1 C1A 109.0(9) . . ? C1B N1 Cu 108.9(7) . . ? C1C N1 Cu 109.8(7) . . ? C1A N1 Cu 109.8(7) . . ? C1B N1 N2 110.2(7) . . ? C1C N1 N2 110.9(6) . . ? C1A N1 N2 107.3(7) . . ? Cu N1 N2 2.50(19) . . ? N1 C1A C2A 116.1(10) . . ? C1A C2A C3A 115.9(11) . . ? N3A C3A C2A 114.0(10) . . ? C4A N3A C3A 116.2(10) . . ? C4A N3A Cu 130.3(8) . . ? C3A N3A Cu 112.7(7) . . ? N3A C4A C5A 125.4(11) . . ? O1A C5A C6A 109.5(10) . . ? O1A C5A C4A 117.4(10) . . ? C6A C5A C4A 133.1(11) . . ? C5A C6A C7A 107.2(11) . . ? C8A C7A C6A 106.3(11) . . ? C7A C8A O1A 110.0(11) . . ? C7A C8A C9A 133.1(12) . . ? O1A C8A C9A 116.7(10) . . ? C5A O1A C8A 106.9(8) . . ? C5A O1A Ag 134.9(7) . . ? C8A O1A Ag 101.4(6) . . ? C5A O1A Cu 95.3(6) . . ? C8A O1A Cu 147.7(7) . . ? Ag O1A Cu 77.26(18) . . ? N4A C9A C8A 123.0(11) . . ? C9A N4A C10A 116.8(11) . . ? C9A N4A Ag 123.3(9) . . ? C10A N4A Ag 118.5(8) . . ? C11A C10A N4A 115.2(13) . . ? C12A C11A C10A 118.5(17) . . ? C11A C12A N2 119.2(13) . . ? C12B N2 C12C 111.2(13) . . ? C12B N2 C12A 109.5(13) . . ? C12C N2 C12A 108.7(11) . . ? C12B N2 Ag 110.4(8) . . ? C12C N2 Ag 110.4(7) . . ? C12A N2 Ag 106.7(8) . . ? C12B N2 N1 109.0(8) . . ? C12C N2 N1 109.9(7) . . ? C12A N2 N1 108.6(7) . . ? Ag N2 N1 1.97(18) . . ? N1 C1B C2B 115.7(10) . . ? C1B C2B C3B 117.8(11) . . ? N3B C3B C2B 113.1(10) . . ? C4B N3B C3B 115.3(10) . . ? C4B N3B Cu 131.0(8) . . ? C3B N3B Cu 113.1(8) . . ? N3B C4B C5B 123.2(11) . . ? C6B C5B O1B 108.7(10) . . ? C6B C5B C4B 133.9(12) . . ? O1B C5B C4B 117.4(11) . . ? C5B C6B C7B 107.5(11) . . ? C8B C7B C6B 107.0(11) . . ? C7B C8B O1B 109.1(11) . . ? C7B C8B C9B 133.3(12) . . ? O1B C8B C9B 117.5(12) . . ? C8B O1B C5B 107.5(9) . . ? C8B O1B Ag 99.8(6) . . ? C5B O1B Ag 137.8(6) . . ? C8B O1B Cu 144.2(7) . . ? C5B O1B Cu 96.8(6) . . ? Ag O1B Cu 77.6(2) . . ? N4B C9B C8B 123.3(11) . . ? C9B N4B C10B 116.9(10) . . ? C9B N4B Ag 123.8(8) . . ? C10B N4B Ag 117.3(8) . . ? C11B C10B N4B 115.3(11) . . ? C12B C11B C10B 124.7(14) . . ? N2 C12B C11B 119.4(15) . . ? N1 C1C C2C 116.1(11) . . ? C3C C2C C1C 114.6(11) . . ? N3C C3C C2C 112.3(10) . . ? C4C N3C C3C 116.4(10) . . ? C4C N3C Cu 130.7(8) . . ? C3C N3C Cu 111.6(8) . . ? N3C C4C C5C 123.6(10) . . ? O1C C5C C6C 109.7(10) . . ? O1C C5C C4C 118.8(10) . . ? C6C C5C C4C 131.4(11) . . ? C5C C6C C7C 107.1(11) . . ? C8C C7C C6C 106.2(12) . . ? C7C C8C O1C 109.5(11) . . ? C7C C8C C9C 133.2(12) . . ? O1C C8C C9C 116.9(10) . . ? C5C O1C C8C 107.5(9) . . ? C5C O1C Ag 136.0(6) . . ? C8C O1C Ag 101.3(6) . . ? C5C O1C Cu 95.8(6) . . ? C8C O1C Cu 145.0(6) . . ? Ag O1C Cu 77.55(18) . . ? N4C C9C C8C 125.0(12) . . ? C9C N4C C10C 117.0(10) . . ? C9C N4C Ag 121.5(8) . . ? C10C N4C Ag 119.1(8) . . ? C11C C10C N4C 112.7(10) . . ? C12C C11C C10C 125.0(15) . . ? C11C C12C N2 119.1(14) . . ? O14 Cl1 O13 110.4(8) . . ? O14 Cl1 O12 107.9(7) . . ? O13 Cl1 O12 110.1(6) . . ? O14 Cl1 O11 108.3(7) . . ? O13 Cl1 O11 109.2(6) . . ? O12 Cl1 O11 110.9(6) . . ? O24 Cl2 O22 113.7(9) . . ? O24 Cl2 O21 113.1(10) . . ? O22 Cl2 O21 115.5(9) . . ? O24 Cl2 O23 106.6(15) . . ? O22 Cl2 O23 102.7(11) . . ? O21 Cl2 O23 103.6(9) . . ? C22 C21 O20 117(2) . . ? C32 C31 O30 114(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3A C4A C9A N4A -32.8(10) . . . . ? N3B C4B C9B N4B -33.4(10) . . . . ? N3C C4C C9C N4C -31.9(10) . . . . ? C1A N1 Cu N3A -46.7(8) . . . . ? C1B N1 Cu N3B -46.4(8) . . . . ? C1C N1 Cu N3C -45.7(8) . . . . ? C12A N2 Ag N4A -18.2(9) . . . . ? C12B N2 Ag N4B -17.8(12) . . . . ? C12C N2 Ag N4C -20.9(9) . . . . ? N3A Cu Ag N4A -107.8(4) . . . . ? N3B Cu Ag N4B -107.8(4) . . . . ? N3C Cu Ag N4C -108.0(4) . . . . ? C1A N1 N2 C12A -172.9(10) . . . . ? C1B N1 N2 C12B -173.1(13) . . . . ? C1C N1 N2 C12C -173.2(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O20 H20 O11 0.84 2.16 2.982(18) 166.4 . O30 H30 O14 0.87 2.30 3.16(3) 178.2 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.143 _refine_diff_density_min -1.633 _refine_diff_density_rms 0.144