# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_mo_sam _database_code_depnum_ccdc_archive 'CCDC 918502' #TrackingRef 'Co4L4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C142.65 H116.31 B8 Cl19.31 Co4 F32 N25 O17 S8' _chemical_formula_weight 4324.00 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.9775(15) _cell_length_b 21.8535(18) _cell_length_c 24.415(2) _cell_angle_alpha 105.483(2) _cell_angle_beta 95.760(2) _cell_angle_gamma 103.275(2) _cell_volume 8862.2(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4351 _exptl_absorpt_coefficient_mu 0.854 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4299 _exptl_absorpt_correction_T_max 0.8567 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 164320 _diffrn_reflns_av_R_equivalents 0.0802 _diffrn_reflns_av_sigmaI/netI 0.1083 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.50 _reflns_number_total 39488 _reflns_number_gt 21115 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1748P)^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 39488 _refine_ls_number_parameters 2357 _refine_ls_number_restraints 401 _refine_ls_R_factor_all 0.1574 _refine_ls_R_factor_gt 0.0925 _refine_ls_wR_factor_ref 0.3036 _refine_ls_wR_factor_gt 0.2724 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.084 _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_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.19474(5) 0.43518(4) 1.00449(4) 0.0227(2) Uani 1 1 d . . . Co2 Co -0.13497(5) 0.13563(4) 0.47359(4) 0.0251(2) Uani 1 1 d . . . Co3 Co 0.26806(5) 0.52206(4) 0.66572(4) 0.0242(2) Uani 1 1 d . . . Co4 Co -0.21212(5) 0.06997(4) 0.82796(4) 0.0253(2) Uani 1 1 d . . . S1 S -0.24720(10) 0.23756(8) 0.76170(8) 0.0300(4) Uani 1 1 d . . . S2 S 0.26499(10) 0.30192(9) 0.85207(7) 0.0331(4) Uani 1 1 d . . . S3 S -0.04422(9) 0.41989(8) 0.91206(7) 0.0289(4) Uani 1 1 d . . . S4 S 0.26028(10) 0.30980(8) 0.64872(8) 0.0321(4) Uani 1 1 d . . . S5 S 0.04411(10) 0.51261(8) 0.73721(8) 0.0306(4) Uani 1 1 d . . . S6 S 0.03112(11) 0.08406(9) 0.59510(8) 0.0372(4) Uani 1 1 d . . . S7 S -0.15213(12) 0.32643(8) 0.59578(8) 0.0369(4) Uani 1 1 d . . . S8 S 0.04114(10) 0.09746(9) 0.80486(8) 0.0343(4) Uani 1 1 d . . . B1 B 0.4720(6) 0.4519(5) 0.7694(4) 0.0481(10) Uani 1 1 d U . . B2 B 0.8553(4) 0.4111(4) 0.7529(3) 0.0269(9) Uani 1 1 d U . . B3 B 0.6282(6) 0.1886(6) 0.2921(5) 0.0581(11) Uani 1 1 d U . . B4 B 0.0339(8) 0.3276(6) 0.2767(5) 0.0655(12) Uani 1 1 d U . . B5 B 0.2021(5) 0.1607(4) 0.7190(4) 0.0518(11) Uani 1 1 d DU . . B6 B 0.4909(8) 0.8152(7) 0.9754(7) 0.0774(13) Uani 1 1 d U . . B7 B 0.3954(13) 0.2222(9) 0.5186(10) 0.1176(19) Uani 1 1 d U . . B8 B 0.8085(10) 0.8164(10) 0.9360(9) 0.1089(17) Uani 1 1 d U . . F1 F 0.5097(3) 0.4985(3) 0.8214(2) 0.0603(12) Uani 1 1 d U . . F2 F 0.5266(3) 0.4253(2) 0.74029(19) 0.0527(10) Uani 1 1 d U . . F3 F 0.4324(3) 0.4777(2) 0.7351(2) 0.0576(11) Uani 1 1 d U . . F4 F 0.4205(3) 0.3992(2) 0.78108(19) 0.0520(10) Uani 1 1 d U . . F5 F 0.8679(2) 0.45151(19) 0.81176(16) 0.0362(8) Uani 1 1 d U . . F6 F 0.9075(2) 0.37428(18) 0.74834(17) 0.0337(8) Uani 1 1 d U . . F7 F 0.7788(2) 0.36905(19) 0.74150(18) 0.0411(9) Uani 1 1 d U . . F8 F 0.8619(2) 0.4505(2) 0.71722(17) 0.0397(9) Uani 1 1 d U . . F9 F 0.5976(3) 0.2369(3) 0.2861(2) 0.0621(11) Uani 1 1 d U . . F10 F 0.6291(3) 0.1472(3) 0.2380(3) 0.0847(15) Uani 1 1 d U . . F11 F 0.5812(3) 0.1507(2) 0.3205(2) 0.0620(11) Uani 1 1 d U . . F12 F 0.7020(3) 0.2126(2) 0.3241(2) 0.0586(11) Uani 1 1 d U . . F13 F 0.0356(3) 0.2700(3) 0.2892(2) 0.0697(12) Uani 1 1 d U . . F14 F -0.0113(3) 0.3604(2) 0.3095(2) 0.0576(11) Uani 1 1 d U . . F15 F 0.0066(4) 0.3170(3) 0.2189(2) 0.0763(13) Uani 1 1 d U . . F16 F 0.1103(4) 0.3674(3) 0.2889(3) 0.0827(14) Uani 1 1 d U . . F19 F 0.1544(3) 0.2019(2) 0.72944(19) 0.0470(9) Uani 1 1 d U D . F21 F 0.5669(4) 0.8299(3) 1.0087(3) 0.0920(15) Uani 1 1 d U A . F22 F 0.5251(9) 0.8152(7) 0.9279(7) 0.087(2) Uani 0.50 1 d PU A 1 F22' F 0.4934(8) 0.8285(7) 0.9240(6) 0.0776(18) Uani 0.50 1 d PU A 2 F23 F 0.4545(4) 0.7542(3) 0.9763(3) 0.0902(15) Uani 1 1 d U A . F24 F 0.4601(4) 0.8620(3) 1.0040(3) 0.0899(15) Uani 1 1 d U A . F25 F 0.4517(15) 0.2773(12) 0.5395(9) 0.115(3) Uani 0.50 1 d PU B 1 F25' F 0.4431(15) 0.2712(12) 0.5169(9) 0.116(2) Uani 0.50 1 d PU B 2 F26 F 0.3437(4) 0.2196(3) 0.5532(4) 0.1071(18) Uani 1 1 d U B . F27 F 0.3351(6) 0.2190(4) 0.4662(4) 0.138(2) Uani 1 1 d U B . F28 F 0.8430(4) 0.7662(4) 0.9180(4) 0.1154(18) Uani 1 1 d U C . F29 F 0.4121(5) 0.1655(4) 0.4943(4) 0.137(2) Uani 1 1 d U B . F30 F 0.7342(12) 0.8106(10) 0.9205(9) 0.107(2) Uani 0.50 1 d PU C 1 F30' F 0.7387(12) 0.7888(10) 0.9009(8) 0.107(2) Uani 0.50 1 d PU C 2 F31 F 0.8198(4) 0.8381(4) 0.9938(4) 0.1215(19) Uani 1 1 d U C . F32 F 0.8514(4) 0.8722(4) 0.9176(4) 0.1178(19) Uani 1 1 d U C . F20 F 0.2111(8) 0.1365(6) 0.7675(5) 0.0531(16) Uani 0.345(4) 1 d PDU D 1 F17 F 0.2742(7) 0.1911(7) 0.7151(7) 0.0565(16) Uani 0.345(4) 1 d PDU D 1 F18 F 0.1710(10) 0.1012(8) 0.6701(7) 0.0506(19) Uani 0.345(4) 1 d PU D 1 F20' F 0.1618(5) 0.0993(4) 0.6963(4) 0.0541(15) Uani 0.655(4) 1 d PDU D 2 F18' F 0.2355(4) 0.1767(3) 0.6675(3) 0.0542(13) Uani 0.655(4) 1 d PU D 2 F17' F 0.2662(4) 0.1781(4) 0.7574(4) 0.0628(14) Uani 0.655(4) 1 d PDU D 2 C8S C 0.7549(11) 0.9128(7) 0.0992(7) 0.086(6) Uani 0.655(4) 1 d P D 2 H8SA H 0.7650 0.8795 0.0665 0.103 Uiso 0.655(4) 1 calc PR D 2 H8SB H 0.7066 0.9222 0.0848 0.103 Uiso 0.655(4) 1 calc PR D 2 Cl15 Cl 0.81966(19) 0.97634(15) 0.10731(13) 0.0500(9) Uani 0.655(4) 1 d P D 2 Cl16 Cl 0.7317(2) 0.87461(19) 0.14486(16) 0.0689(12) Uani 0.655(4) 1 d P D 2 N1 N -0.3049(3) -0.0638(3) 0.7973(3) 0.0347(14) Uani 1 1 d . . . N2 N -0.3192(3) 0.0573(3) 0.7749(2) 0.0289(12) Uani 1 1 d . . . N3 N -0.2034(3) 0.1669(2) 0.8201(2) 0.0240(11) Uani 1 1 d . . . N4 N 0.1948(3) 0.3545(2) 0.9308(2) 0.0246(11) Uani 1 1 d . . . N5 N 0.3075(3) 0.4658(2) 0.9827(2) 0.0223(11) Uani 1 1 d . . . N6 N 0.2846(3) 0.5622(2) 1.0841(2) 0.0262(12) Uani 1 1 d . . . N7 N 0.2395(3) 0.4116(3) 1.1122(2) 0.0286(12) Uani 1 1 d . . . N8 N 0.0968(3) 0.4164(2) 1.0468(2) 0.0222(11) Uani 1 1 d . . . N9 N 0.1012(3) 0.4430(2) 0.9464(2) 0.0230(11) Uani 1 1 d . . . N10 N 0.2662(3) 0.4320(3) 0.6851(2) 0.0267(12) Uani 1 1 d . . . N11 N 0.2943(3) 0.4644(3) 0.5895(2) 0.0251(11) Uani 1 1 d . . . N12 N 0.2809(3) 0.5915(3) 0.5814(2) 0.0288(12) Uani 1 1 d . . . N13 N 0.4249(3) 0.6145(3) 0.7230(2) 0.0297(12) Uani 1 1 d . . . N14 N 0.2602(3) 0.5992(2) 0.7376(2) 0.0268(12) Uani 1 1 d . . . N15 N 0.1451(3) 0.4904(2) 0.6730(2) 0.0232(11) Uani 1 1 d . . . N16 N -0.0365(3) 0.1393(2) 0.5328(2) 0.0256(12) Uani 1 1 d . . . N17 N -0.1598(3) 0.0373(2) 0.4785(2) 0.0292(12) Uani 1 1 d . . . N18 N -0.2791(3) 0.0573(3) 0.4012(3) 0.0327(13) Uani 1 1 d . . . N19 N -0.1091(3) 0.1048(3) 0.3566(2) 0.0308(13) Uani 1 1 d . . . N20 N -0.1279(3) 0.2185(2) 0.4428(2) 0.0262(12) Uani 1 1 d . . . N21 N -0.1521(3) 0.2075(2) 0.5466(2) 0.0267(12) Uani 1 1 d . . . N22 N -0.1059(3) 0.0813(2) 0.7908(2) 0.0250(11) Uani 1 1 d . . . N23 N -0.1307(3) 0.0577(3) 0.8903(2) 0.0276(12) Uani 1 1 d . . . N24 N -0.2825(3) 0.0516(3) 0.9259(2) 0.0354(14) Uani 1 1 d . . . O1 O -0.2375(3) -0.0284(2) 0.7881(2) 0.0391(12) Uani 1 1 d . . . O2 O 0.2183(2) 0.5327(2) 1.04713(19) 0.0282(10) Uani 1 1 d . . . O3 O 0.2388(3) 0.3899(2) 1.05577(19) 0.0310(10) Uani 1 1 d . . . O4 O 0.2259(2) 0.5642(2) 0.60719(19) 0.0287(10) Uani 1 1 d . . . O5 O 0.3768(3) 0.5786(2) 0.67269(19) 0.0332(11) Uani 1 1 d . . . O6 O -0.0752(3) 0.1095(2) 0.40904(19) 0.0331(11) Uani 1 1 d . . . O7 O -0.2507(3) 0.1098(2) 0.4470(2) 0.0365(12) Uani 1 1 d . . . O8 O -0.2619(3) 0.0979(2) 0.9001(2) 0.0353(11) Uani 1 1 d . . . O9 O 0.0089(3) 0.2719(2) 0.8150(2) 0.0340(11) Uani 1 1 d . . . H9 H 0.0498 0.3016 0.8193 0.051 Uiso 1 1 calc R . . O10 O 0.1126(3) 0.3685(2) 0.78346(19) 0.0329(11) Uani 1 1 d . . . H10 H 0.1099 0.3586 0.7475 0.049 Uiso 1 1 calc R . . O11 O 0.0457(3) 0.3012(2) 0.66372(19) 0.0313(10) Uani 1 1 d . . . H11 H 0.0267 0.2611 0.6597 0.047 Uiso 1 1 calc R . . O12 O -0.0591(3) 0.2077(2) 0.6975(2) 0.0330(11) Uani 1 1 d . . . H12 H -0.0489 0.2127 0.7330 0.050 Uiso 1 1 calc R . . C1 C -0.2999(5) -0.1124(4) 0.8204(4) 0.047(2) Uani 1 1 d . . . H1 H -0.2506 -0.1192 0.8305 0.057 Uiso 1 1 calc R . . C2 C -0.3662(5) -0.1526(4) 0.8295(4) 0.058(2) Uani 1 1 d . . . H2 H -0.3627 -0.1866 0.8463 0.070 Uiso 1 1 calc R . . C3 C -0.4380(5) -0.1425(4) 0.8137(4) 0.057(2) Uani 1 1 d . . . H3 H -0.4845 -0.1704 0.8182 0.069 Uiso 1 1 calc R . . C4 C -0.4398(4) -0.0916(3) 0.7915(3) 0.0393(18) Uani 1 1 d . . . H4 H -0.4881 -0.0827 0.7825 0.047 Uiso 1 1 calc R . . C5 C -0.3727(4) -0.0526(3) 0.7820(3) 0.0324(15) Uani 1 1 d . . . C6 C -0.3766(4) 0.0025(3) 0.7560(3) 0.0289(14) Uani 1 1 d . . . C7 C -0.4417(4) -0.0042(3) 0.7169(3) 0.0343(16) Uani 1 1 d . . . H7 H -0.4819 -0.0441 0.7040 0.041 Uiso 1 1 calc R . . C8 C -0.4467(4) 0.0483(3) 0.6971(3) 0.0360(16) Uani 1 1 d . . . H8 H -0.4897 0.0442 0.6691 0.043 Uiso 1 1 calc R . . C9 C -0.3902(4) 0.1059(3) 0.7177(3) 0.0317(15) Uani 1 1 d . . . H9A H -0.3944 0.1430 0.7055 0.038 Uiso 1 1 calc R . . C10 C -0.3262(4) 0.1100(3) 0.7569(3) 0.0266(14) Uani 1 1 d . . . C11 C -0.2606(4) 0.1676(3) 0.7820(3) 0.0257(14) Uani 1 1 d . . . C12 C -0.1581(4) 0.2679(3) 0.8059(3) 0.0306(15) Uani 1 1 d . . . H12A H -0.1234 0.3095 0.8102 0.037 Uiso 1 1 calc R . . C13 C -0.1439(4) 0.2252(3) 0.8337(3) 0.0267(14) Uani 1 1 d . . . C14 C -0.0747(3) 0.2358(3) 0.8772(3) 0.0240(13) Uani 1 1 d . . . C15 C -0.0001(4) 0.2608(3) 0.8674(3) 0.0258(14) Uani 1 1 d . . . C16 C 0.0641(4) 0.2720(3) 0.9103(3) 0.0268(14) Uani 1 1 d . . . C17 C 0.0538(4) 0.2604(3) 0.9615(3) 0.0281(14) Uani 1 1 d . . . H17 H 0.0975 0.2698 0.9907 0.034 Uiso 1 1 calc R . . C18 C -0.0212(4) 0.2346(3) 0.9717(3) 0.0297(15) Uani 1 1 d . . . C19 C -0.0830(4) 0.2233(3) 0.9301(3) 0.0285(14) Uani 1 1 d . . . H19 H -0.1336 0.2065 0.9370 0.034 Uiso 1 1 calc R . . C20 C -0.0330(4) 0.2201(4) 1.0284(3) 0.0355(16) Uani 1 1 d . . . H20A H -0.0350 0.2604 1.0573 0.053 Uiso 1 1 calc R . . H20B H 0.0102 0.2046 1.0421 0.053 Uiso 1 1 calc R . . H20C H -0.0818 0.1861 1.0224 0.053 Uiso 1 1 calc R . . C21 C 0.1432(4) 0.2939(3) 0.8979(3) 0.0274(14) Uani 1 1 d . . . C22 C 0.1725(4) 0.2597(3) 0.8541(3) 0.0347(16) Uani 1 1 d . . . H22 H 0.1454 0.2178 0.8280 0.042 Uiso 1 1 calc R . . C23 C 0.2593(3) 0.3644(3) 0.9093(3) 0.0235(13) Uani 1 1 d . . . C24 C 0.3202(4) 0.4268(3) 0.9343(3) 0.0257(13) Uani 1 1 d . . . C25 C 0.3834(4) 0.4432(3) 0.9076(3) 0.0313(15) Uani 1 1 d . . . H25 H 0.3904 0.4137 0.8734 0.038 Uiso 1 1 calc R . . C26 C 0.4361(4) 0.5048(3) 0.9332(3) 0.0317(15) Uani 1 1 d . . . H26 H 0.4789 0.5193 0.9156 0.038 Uiso 1 1 calc R . . C27 C 0.4249(4) 0.5444(3) 0.9845(3) 0.0321(15) Uani 1 1 d . . . H27 H 0.4611 0.5857 1.0035 0.039 Uiso 1 1 calc R . . C28 C 0.3599(4) 0.5228(3) 1.0079(3) 0.0267(14) Uani 1 1 d . . . C29 C 0.3541(4) 0.5617(3) 1.0671(3) 0.0264(14) Uani 1 1 d . . . C30 C 0.4206(4) 0.5973(3) 1.1075(3) 0.0328(15) Uani 1 1 d . . . H30 H 0.4696 0.5981 1.0959 0.039 Uiso 1 1 calc R . . C31 C 0.4187(4) 0.6307(4) 1.1624(3) 0.0383(17) Uani 1 1 d . . . H31 H 0.4650 0.6549 1.1891 0.046 Uiso 1 1 calc R . . C32 C 0.3449(4) 0.6281(4) 1.1784(3) 0.0403(18) Uani 1 1 d . . . H32 H 0.3401 0.6501 1.2165 0.048 Uiso 1 1 calc R . . C33 C 0.2806(4) 0.5930(3) 1.1376(3) 0.0334(16) Uani 1 1 d . . . H33 H 0.2309 0.5907 1.1484 0.040 Uiso 1 1 calc R . . C34 C 0.3085(4) 0.4276(4) 1.1467(3) 0.0394(17) Uani 1 1 d . . . H34 H 0.3530 0.4231 1.1297 0.047 Uiso 1 1 calc R . . C35 C 0.3167(5) 0.4501(4) 1.2048(3) 0.0418(18) Uani 1 1 d . . . H35 H 0.3666 0.4644 1.2283 0.050 Uiso 1 1 calc R . . C36 C 0.2513(5) 0.4518(4) 1.2293(3) 0.0409(18) Uani 1 1 d . . . H36 H 0.2549 0.4655 1.2700 0.049 Uiso 1 1 calc R . . C37 C 0.1804(4) 0.4334(3) 1.1936(3) 0.0363(16) Uani 1 1 d . . . H37 H 0.1350 0.4337 1.2103 0.044 Uiso 1 1 calc R . . C38 C 0.1736(4) 0.4149(3) 1.1349(3) 0.0305(15) Uani 1 1 d . . . C39 C 0.0981(4) 0.4043(3) 1.0981(3) 0.0275(14) Uani 1 1 d . . . C40 C 0.0294(4) 0.3876(3) 1.1205(3) 0.0362(17) Uani 1 1 d . . . H40 H 0.0309 0.3776 1.1560 0.043 Uiso 1 1 calc R . . C41 C -0.0403(4) 0.3861(3) 1.0895(3) 0.0361(17) Uani 1 1 d . . . H41 H -0.0869 0.3760 1.1044 0.043 Uiso 1 1 calc R . . C42 C -0.0424(4) 0.3991(3) 1.0365(3) 0.0301(15) Uani 1 1 d . . . H42 H -0.0898 0.3973 1.0142 0.036 Uiso 1 1 calc R . . C43 C 0.0281(3) 0.4150(3) 1.0178(3) 0.0235(13) Uani 1 1 d . . . C44 C 0.0339(3) 0.4276(3) 0.9619(3) 0.0243(13) Uani 1 1 d . . . C45 C 0.0183(4) 0.4365(3) 0.8656(3) 0.0322(15) Uani 1 1 d . . . H45 H 0.0026 0.4379 0.8277 0.039 Uiso 1 1 calc R . . C46 C 0.0932(4) 0.4474(3) 0.8905(3) 0.0249(13) Uani 1 1 d . . . C47 C 0.1607(4) 0.4659(3) 0.8625(3) 0.0247(13) Uani 1 1 d . . . C48 C 0.1685(4) 0.4274(3) 0.8093(3) 0.0256(13) Uani 1 1 d . . . C49 C 0.2327(4) 0.4478(3) 0.7844(3) 0.0265(14) Uani 1 1 d . . . C50 C 0.2884(4) 0.5073(3) 0.8141(3) 0.0285(14) Uani 1 1 d . . . H50 H 0.3325 0.5209 0.7975 0.034 Uiso 1 1 calc R . . C51 C 0.2812(4) 0.5470(3) 0.8670(3) 0.0268(14) Uani 1 1 d . . . C52 C 0.2180(4) 0.5246(3) 0.8912(3) 0.0281(14) Uani 1 1 d . . . H52 H 0.2133 0.5497 0.9284 0.034 Uiso 1 1 calc R . . C53 C 0.3393(4) 0.6119(3) 0.8975(3) 0.0393(17) Uani 1 1 d . . . H53A H 0.3899 0.6108 0.8864 0.059 Uiso 1 1 calc R . . H53B H 0.3435 0.6201 0.9393 0.059 Uiso 1 1 calc R . . H53C H 0.3222 0.6473 0.8867 0.059 Uiso 1 1 calc R . . C54 C 0.2445(4) 0.4055(3) 0.7289(3) 0.0251(13) Uani 1 1 d . . . C55 C 0.2381(4) 0.3395(3) 0.7154(3) 0.0317(15) Uani 1 1 d . . . H55 H 0.2231 0.3135 0.7400 0.038 Uiso 1 1 calc R . . C56 C 0.2760(3) 0.3863(3) 0.6405(3) 0.0252(13) Uani 1 1 d . . . C57 C 0.2929(4) 0.4018(3) 0.5874(3) 0.0263(14) Uani 1 1 d . . . C58 C 0.3038(4) 0.3563(3) 0.5397(3) 0.0351(16) Uani 1 1 d . . . H58 H 0.3027 0.3127 0.5400 0.042 Uiso 1 1 calc R . . C59 C 0.3165(4) 0.3765(4) 0.4911(3) 0.0392(17) Uani 1 1 d . . . H59 H 0.3227 0.3464 0.4568 0.047 Uiso 1 1 calc R . . C60 C 0.3199(4) 0.4404(3) 0.4936(3) 0.0346(16) Uani 1 1 d . . . H60 H 0.3296 0.4552 0.4612 0.041 Uiso 1 1 calc R . . C61 C 0.3092(4) 0.4837(3) 0.5433(3) 0.0298(15) Uani 1 1 d . . . C62 C 0.3221(4) 0.5555(3) 0.5492(3) 0.0290(14) Uani 1 1 d . . . C63 C 0.3783(4) 0.5875(4) 0.5225(3) 0.0386(17) Uani 1 1 d . . . H63 H 0.4076 0.5629 0.4998 0.046 Uiso 1 1 calc R . . C64 C 0.3913(5) 0.6526(4) 0.5284(3) 0.0419(18) Uani 1 1 d . . . H64 H 0.4284 0.6735 0.5095 0.050 Uiso 1 1 calc R . . C65 C 0.3491(5) 0.6884(4) 0.5631(4) 0.047(2) Uani 1 1 d . . . H65 H 0.3575 0.7342 0.5683 0.056 Uiso 1 1 calc R . . C66 C 0.2962(4) 0.6572(3) 0.5894(3) 0.0340(16) Uani 1 1 d . . . H66 H 0.2691 0.6821 0.6141 0.041 Uiso 1 1 calc R . . C67 C 0.5003(4) 0.6151(4) 0.7252(4) 0.0411(18) Uani 1 1 d . . . H67 H 0.5167 0.5904 0.6926 0.049 Uiso 1 1 calc R . . C68 C 0.5534(4) 0.6507(4) 0.7738(4) 0.0431(19) Uani 1 1 d . . . H68 H 0.6062 0.6502 0.7748 0.052 Uiso 1 1 calc R . . C69 C 0.5315(5) 0.6865(4) 0.8200(4) 0.049(2) Uani 1 1 d . . . H69 H 0.5684 0.7104 0.8540 0.058 Uiso 1 1 calc R . . C70 C 0.4557(4) 0.6881(3) 0.8176(3) 0.0355(16) Uani 1 1 d . . . H70 H 0.4403 0.7139 0.8502 0.043 Uiso 1 1 calc R . . C71 C 0.4001(4) 0.6521(3) 0.7677(3) 0.0303(15) Uani 1 1 d . . . C72 C 0.3178(4) 0.6534(3) 0.7656(3) 0.0287(14) Uani 1 1 d . . . C73 C 0.3021(4) 0.7104(3) 0.7972(3) 0.0387(17) Uani 1 1 d . . . H73 H 0.3433 0.7488 0.8159 0.046 Uiso 1 1 calc R . . C74 C 0.2254(5) 0.7111(4) 0.8013(3) 0.0430(19) Uani 1 1 d . . . H74 H 0.2138 0.7501 0.8221 0.052 Uiso 1 1 calc R . . C75 C 0.1671(4) 0.6546(3) 0.7750(3) 0.0346(16) Uani 1 1 d . . . H75 H 0.1146 0.6533 0.7781 0.042 Uiso 1 1 calc R . . C76 C 0.1872(4) 0.5993(3) 0.7436(3) 0.0245(13) Uani 1 1 d . . . C77 C 0.1297(4) 0.5361(3) 0.7145(3) 0.0278(14) Uani 1 1 d . . . C78 C 0.0274(4) 0.4361(3) 0.6882(3) 0.0299(15) Uani 1 1 d . . . H78 H -0.0170 0.4006 0.6835 0.036 Uiso 1 1 calc R . . C79 C 0.0858(3) 0.4326(3) 0.6569(3) 0.0250(13) Uani 1 1 d . . . C80 C 0.0828(4) 0.3753(3) 0.6086(3) 0.0267(14) Uani 1 1 d . . . C81 C 0.0581(4) 0.3092(3) 0.6117(3) 0.0280(14) Uani 1 1 d . . . C82 C 0.0485(4) 0.2560(3) 0.5632(3) 0.0281(14) Uani 1 1 d . . . C83 C 0.0625(4) 0.2664(3) 0.5108(3) 0.0301(15) Uani 1 1 d . . . H83 H 0.0545 0.2297 0.4774 0.036 Uiso 1 1 calc R . . C84 C 0.0884(4) 0.3310(3) 0.5067(3) 0.0289(14) Uani 1 1 d . . . C85 C 0.0992(4) 0.3840(3) 0.5556(3) 0.0301(15) Uani 1 1 d . . . H85 H 0.1183 0.4274 0.5534 0.036 Uiso 1 1 calc R . . C86 C 0.1030(5) 0.3406(4) 0.4491(3) 0.0388(17) Uani 1 1 d . . . H86A H 0.0683 0.3040 0.4178 0.058 Uiso 1 1 calc R . . H86B H 0.1570 0.3419 0.4453 0.058 Uiso 1 1 calc R . . H86C H 0.0929 0.3822 0.4469 0.058 Uiso 1 1 calc R . . C87 C 0.0290(4) 0.1877(3) 0.5677(3) 0.0286(14) Uani 1 1 d . . . C88 C 0.0706(4) 0.1649(3) 0.6021(3) 0.0329(16) Uani 1 1 d . . . H88 H 0.1172 0.1910 0.6277 0.040 Uiso 1 1 calc R . . C89 C -0.0418(4) 0.0836(3) 0.5449(3) 0.0287(14) Uani 1 1 d . . . C90 C -0.1094(4) 0.0266(3) 0.5177(3) 0.0307(15) Uani 1 1 d . . . C91 C -0.1218(5) -0.0323(3) 0.5308(3) 0.0392(18) Uani 1 1 d . . . H91 H -0.0854 -0.0392 0.5579 0.047 Uiso 1 1 calc R . . C92 C -0.1888(6) -0.0806(4) 0.5030(4) 0.053(2) Uani 1 1 d . . . H92 H -0.2001 -0.1208 0.5126 0.064 Uiso 1 1 calc R . . C93 C -0.2395(5) -0.0717(3) 0.4618(4) 0.044(2) Uani 1 1 d . . . H93 H -0.2850 -0.1055 0.4420 0.053 Uiso 1 1 calc R . . C94 C -0.2223(4) -0.0110(3) 0.4497(3) 0.0365(17) Uani 1 1 d . . . C95 C -0.2704(4) -0.0033(3) 0.4013(3) 0.0328(16) Uani 1 1 d . . . C96 C -0.3048(4) -0.0554(3) 0.3525(3) 0.0410(18) Uani 1 1 d . . . H96 H -0.3011 -0.0983 0.3517 0.049 Uiso 1 1 calc R . . C97 C -0.3448(5) -0.0468(4) 0.3045(4) 0.053(2) Uani 1 1 d . . . H97 H -0.3684 -0.0835 0.2715 0.064 Uiso 1 1 calc R . . C98 C -0.3497(5) 0.0137(5) 0.3051(4) 0.055(2) Uani 1 1 d . . . H98 H -0.3752 0.0202 0.2720 0.066 Uiso 1 1 calc R . . C99 C -0.3173(4) 0.0672(4) 0.3547(3) 0.0417(18) Uani 1 1 d . . . H99 H -0.3218 0.1100 0.3558 0.050 Uiso 1 1 calc R . . C100 C -0.1228(5) 0.0456(4) 0.3155(3) 0.0433(18) Uani 1 1 d . . . H100 H -0.1093 0.0099 0.3256 0.052 Uiso 1 1 calc R . . C101 C -0.1557(5) 0.0364(4) 0.2596(4) 0.052(2) Uani 1 1 d . . . H101 H -0.1647 -0.0050 0.2311 0.062 Uiso 1 1 calc R . . C102 C -0.1754(5) 0.0880(4) 0.2454(3) 0.050(2) Uani 1 1 d . . . H102 H -0.1976 0.0827 0.2069 0.060 Uiso 1 1 calc R . . C103 C -0.1628(4) 0.1484(4) 0.2879(3) 0.0409(18) Uani 1 1 d . . . H103 H -0.1770 0.1840 0.2784 0.049 Uiso 1 1 calc R . . C104 C -0.1302(4) 0.1562(3) 0.3428(3) 0.0294(14) Uani 1 1 d . . . C105 C -0.1188(4) 0.2202(3) 0.3893(3) 0.0290(14) Uani 1 1 d . . . C106 C -0.1054(4) 0.2787(4) 0.3749(3) 0.0390(17) Uani 1 1 d . . . H106 H -0.0965 0.2792 0.3373 0.047 Uiso 1 1 calc R . . C107 C -0.1051(4) 0.3355(3) 0.4156(3) 0.0381(17) Uani 1 1 d . . . H107 H -0.0949 0.3760 0.4066 0.046 Uiso 1 1 calc R . . C108 C -0.1197(4) 0.3341(3) 0.4696(3) 0.0340(16) Uani 1 1 d . . . H108 H -0.1221 0.3728 0.4977 0.041 Uiso 1 1 calc R . . C109 C -0.1308(4) 0.2736(3) 0.4818(3) 0.0277(14) Uani 1 1 d . . . C110 C -0.1458(4) 0.2648(3) 0.5373(3) 0.0274(14) Uani 1 1 d . . . C111 C -0.1630(4) 0.2723(3) 0.6341(3) 0.0352(16) Uani 1 1 d . . . H111 H -0.1696 0.2832 0.6734 0.042 Uiso 1 1 calc R . . C112 C -0.1611(4) 0.2110(3) 0.6025(3) 0.0258(14) Uani 1 1 d . . . C113 C -0.1723(4) 0.1527(3) 0.6242(3) 0.0272(14) Uani 1 1 d . . . C114 C -0.1228(4) 0.1538(3) 0.6725(3) 0.0252(13) Uani 1 1 d . . . C115 C -0.1376(4) 0.1004(3) 0.6952(3) 0.0268(14) Uani 1 1 d . . . C116 C -0.2016(4) 0.0476(3) 0.6697(3) 0.0302(15) Uani 1 1 d . . . H116 H -0.2118 0.0118 0.6855 0.036 Uiso 1 1 calc R . . C117 C -0.2510(4) 0.0457(3) 0.6219(3) 0.0352(16) Uani 1 1 d . . . C118 C -0.2335(4) 0.0988(3) 0.5988(3) 0.0324(15) Uani 1 1 d . . . H118 H -0.2653 0.0970 0.5645 0.039 Uiso 1 1 calc R . . C119 C -0.3223(4) -0.0131(3) 0.5937(3) 0.0439(19) Uani 1 1 d . . . H11A H -0.3090 -0.0541 0.5942 0.066 Uiso 1 1 calc R . . H11B H -0.3385 -0.0145 0.5538 0.066 Uiso 1 1 calc R . . H11C H -0.3648 -0.0083 0.6153 0.066 Uiso 1 1 calc R . . C120 C -0.0810(4) 0.0988(3) 0.7437(3) 0.0279(14) Uani 1 1 d . . . C121 C -0.0033(4) 0.1095(3) 0.7442(3) 0.0341(16) Uani 1 1 d . . . H121 H 0.0228 0.1218 0.7153 0.041 Uiso 1 1 calc R . . C122 C -0.0467(4) 0.0807(3) 0.8273(3) 0.0288(14) Uani 1 1 d . . . C123 C -0.0570(4) 0.0696(3) 0.8822(3) 0.0295(15) Uani 1 1 d . . . C124 C 0.0051(4) 0.0742(3) 0.9239(3) 0.0381(17) Uani 1 1 d . . . H124 H 0.0570 0.0839 0.9171 0.046 Uiso 1 1 calc R . . C125 C -0.0117(4) 0.0642(4) 0.9756(3) 0.0386(17) Uani 1 1 d . . . H125 H 0.0289 0.0697 1.0059 0.046 Uiso 1 1 calc R . . C126 C -0.0885(5) 0.0463(4) 0.9824(3) 0.0410(18) Uani 1 1 d . . . H126 H -0.1010 0.0360 1.0164 0.049 Uiso 1 1 calc R . . C127 C -0.1476(4) 0.0435(3) 0.9389(3) 0.0332(16) Uani 1 1 d . . . C128 C -0.2299(4) 0.0227(3) 0.9451(3) 0.0383(17) Uani 1 1 d . . . C129 C -0.2553(5) -0.0279(4) 0.9703(4) 0.049(2) Uani 1 1 d . . . H129 H -0.2192 -0.0478 0.9848 0.059 Uiso 1 1 calc R . . C130 C -0.3316(7) -0.0479(5) 0.9737(4) 0.069(3) Uani 1 1 d . . . H130 H -0.3497 -0.0845 0.9874 0.083 Uiso 1 1 calc R . . C131 C -0.3845(6) -0.0141(5) 0.9569(4) 0.061(3) Uani 1 1 d . . . H131 H -0.4370 -0.0250 0.9623 0.074 Uiso 1 1 calc R . . C132 C -0.3573(4) 0.0347(4) 0.9324(4) 0.051(2) Uani 1 1 d . . . H132 H -0.3920 0.0569 0.9198 0.061 Uiso 1 1 calc R . . C133 C 0.1062(5) 0.4889(4) 0.3888(4) 0.052(2) Uani 1 1 d . . . H13A H 0.1010 0.4412 0.3724 0.063 Uiso 1 1 calc R . . H13B H 0.0998 0.5073 0.3562 0.063 Uiso 1 1 calc R . . C2S1 C 0.1424(8) 0.1322(4) 0.32385(18) 0.157(13) Uani 0.50 1 d PGDU E 1 H2SA H 0.1878 0.1211 0.3080 0.188 Uiso 0.50 1 calc PR E 1 H2SB H 0.1185 0.1544 0.2992 0.188 Uiso 0.50 1 calc PR E 1 C2S2 C 0.0752(2) 0.1381(3) 0.3687(6) 0.057(4) Uani 0.50 1 d PGDU E 2 H2SC H 0.0479 0.1606 0.3464 0.069 Uiso 0.50 1 calc PR E 2 H2SD H 0.0479 0.1334 0.4012 0.069 Uiso 0.50 1 calc PR E 2 Cl3 Cl 0.0738(2) 0.05874(14) 0.32353(15) 0.1009(10) Uani 1 1 d GD . . Cl4 Cl 0.1728(2) 0.18596(16) 0.39584(18) 0.1354(15) Uani 1 1 d GD . . C3S C 0.2930(5) 0.7599(4) 0.0247(4) 0.048(2) Uani 1 1 d . . . H3S1 H 0.2947 0.8024 0.0531 0.058 Uiso 1 1 calc R . . H3S2 H 0.3461 0.7612 0.0168 0.058 Uiso 1 1 calc R . . Cl5 Cl 0.2596(2) 0.69467(17) 0.05333(18) 0.1036(12) Uani 1 1 d . . . Cl6 Cl 0.23127(18) 0.74892(19) -0.03853(12) 0.0935(10) Uani 1 1 d . . . C4S C 0.2440(7) 0.3043(7) 0.3066(7) 0.106(5) Uani 1 1 d . . . H4S1 H 0.1927 0.3065 0.3170 0.127 Uiso 1 1 calc R . . H4S2 H 0.2623 0.2736 0.3245 0.127 Uiso 1 1 calc R . . Cl7 Cl 0.3035(2) 0.37616(16) 0.33302(13) 0.0962(10) Uani 1 1 d . . . Cl8 Cl 0.2325(2) 0.27123(16) 0.22846(17) 0.1093(12) Uani 1 1 d . . . C5S C 0.0170(7) 0.1591(5) 0.1666(5) 0.087(4) Uani 1 1 d . . . H5S1 H 0.0496 0.1722 0.1391 0.105 Uiso 1 1 calc R . . H5S2 H 0.0296 0.1972 0.2020 0.105 Uiso 1 1 calc R . . Cl9 Cl 0.0442(6) 0.0951(2) 0.1843(3) 0.267(5) Uani 1 1 d . . . Cl10 Cl -0.0788(3) 0.1457(3) 0.13675(17) 0.193(3) Uani 1 1 d . . . C7S C 0.6229(6) 0.0938(5) 0.1052(5) 0.077(3) Uani 1 1 d . . . H7S1 H 0.5962 0.1014 0.0710 0.092 Uiso 1 1 calc R . . H7S2 H 0.6166 0.1265 0.1401 0.092 Uiso 1 1 calc R . . Cl13 Cl 0.72204(19) 0.10512(14) 0.10165(14) 0.0898(9) Uani 1 1 d . . . Cl14 Cl 0.5796(2) 0.01365(14) 0.10733(16) 0.0939(10) Uani 1 1 d . . . C9S C 0.5152(5) 0.4316(5) 0.6137(4) 0.066(3) Uani 1 1 d . . . H9S1 H 0.4859 0.3877 0.5874 0.079 Uiso 1 1 calc R . . H9S2 H 0.4936 0.4389 0.6499 0.079 Uiso 1 1 calc R . . Cl17 Cl 0.61500(18) 0.4345(2) 0.62874(12) 0.1065(13) Uani 1 1 d . . . Cl18 Cl 0.50560(15) 0.49328(14) 0.58117(11) 0.0697(7) Uani 1 1 d . . . C10S C 0.4416(8) 0.2183(6) 0.3665(5) 0.099(4) Uani 1 1 d . . . H10A H 0.4556 0.2171 0.4064 0.119 Uiso 1 1 calc R . . H10B H 0.4827 0.2073 0.3446 0.119 Uiso 1 1 calc R . . Cl19 Cl 0.3494(3) 0.1598(2) 0.33274(17) 0.1343(15) Uani 1 1 d . . . Cl20 Cl 0.4332(3) 0.2986(3) 0.3673(3) 0.168(2) Uani 1 1 d . . . C11S C 0.6760(5) 0.7287(4) 0.9970(4) 0.054(2) Uani 1 1 d . . . H11D H 0.7159 0.7073 0.9835 0.081 Uiso 1 1 calc R . . H11E H 0.6949 0.7576 1.0367 0.081 Uiso 1 1 calc R . . H11F H 0.6644 0.7548 0.9719 0.081 Uiso 1 1 calc R . . Cl21 Cl 0.19898(13) 0.52712(11) 0.42963(12) 0.0642(6) Uani 1 1 d . . . Cl22 Cl 0.03227(14) 0.49957(11) 0.42966(11) 0.0620(6) Uani 1 1 d . . . N25 N 0.6047(4) 0.6778(3) 0.9954(3) 0.0451(16) Uani 1 1 d . . . O13 O 0.5801(4) 0.6789(3) 1.0412(3) 0.0591(16) Uani 1 1 d . . . O14 O 0.5728(4) 0.6388(3) 0.9493(3) 0.075(2) Uani 1 1 d . . . O1W O 0.5560(2) 0.0050(2) 0.45861(17) 0.0259(9) Uani 1 1 d U . . H1O1 H 0.5954 0.0229 0.4463 0.031 Uiso 1 1 d R . . H2O1 H 0.5173 0.0158 0.4449 0.031 Uiso 1 1 d R . . O2W O 0.3523(3) 0.8045(3) 0.4770(3) 0.0604(18) Uani 1 1 d . . . H1O2 H 0.3133 0.8172 0.4875 0.072 Uiso 1 1 d R . . H2O2 H 0.3499 0.7680 0.4836 0.072 Uiso 1 1 d R . . O3W O 0.6339(3) 0.2472(4) 0.6362(3) 0.074(2) Uani 1 1 d . . . H1O3 H 0.6025 0.2712 0.6407 0.089 Uiso 1 1 d R . . H2O3 H 0.6714 0.2641 0.6645 0.089 Uiso 1 1 d 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 Co1 0.0178(4) 0.0257(4) 0.0235(4) 0.0060(3) 0.0052(3) 0.0046(3) Co2 0.0255(5) 0.0205(4) 0.0263(4) 0.0051(3) 0.0040(4) 0.0028(3) Co3 0.0208(5) 0.0251(4) 0.0252(4) 0.0059(4) 0.0056(3) 0.0044(3) Co4 0.0206(5) 0.0241(4) 0.0305(5) 0.0090(4) 0.0023(4) 0.0044(3) S1 0.0261(9) 0.0267(8) 0.0373(9) 0.0138(7) 0.0010(7) 0.0043(7) S2 0.0246(9) 0.0367(9) 0.0318(9) 0.0001(7) 0.0064(7) 0.0074(7) S3 0.0186(8) 0.0346(8) 0.0312(9) 0.0063(7) 0.0034(7) 0.0072(7) S4 0.0329(10) 0.0284(8) 0.0358(9) 0.0081(7) 0.0104(7) 0.0096(7) S5 0.0244(9) 0.0312(8) 0.0343(9) 0.0058(7) 0.0116(7) 0.0056(7) S6 0.0405(11) 0.0342(9) 0.0392(10) 0.0116(8) 0.0039(8) 0.0148(8) S7 0.0545(12) 0.0252(8) 0.0303(9) 0.0048(7) 0.0067(8) 0.0137(8) S8 0.0233(9) 0.0392(9) 0.0439(10) 0.0156(8) 0.0078(8) 0.0109(7) B1 0.039(2) 0.064(2) 0.042(2) 0.0150(17) 0.0131(17) 0.0125(17) B2 0.0233(18) 0.0297(19) 0.0305(18) 0.0119(14) 0.0094(18) 0.0072(14) B3 0.040(2) 0.061(2) 0.071(2) 0.0174(19) 0.0083(19) 0.0111(18) B4 0.074(3) 0.067(2) 0.064(2) 0.024(2) 0.027(2) 0.023(2) B5 0.049(2) 0.0469(19) 0.062(3) 0.014(2) 0.0095(19) 0.0199(17) B6 0.080(3) 0.071(3) 0.094(3) 0.034(2) 0.029(2) 0.027(2) B7 0.119(4) 0.082(3) 0.156(5) 0.026(4) 0.047(3) 0.037(3) B8 0.078(3) 0.143(4) 0.131(4) 0.076(4) 0.021(3) 0.039(3) F1 0.051(3) 0.073(3) 0.044(2) 0.0046(19) 0.0129(18) 0.004(2) F2 0.039(2) 0.070(3) 0.046(2) 0.011(2) 0.0140(18) 0.0147(18) F3 0.045(2) 0.070(3) 0.060(2) 0.025(2) 0.0079(19) 0.014(2) F4 0.042(2) 0.066(2) 0.046(2) 0.0155(19) 0.0151(18) 0.0076(18) F5 0.032(2) 0.0399(19) 0.0335(17) 0.0047(15) 0.0054(15) 0.0110(15) F6 0.0258(18) 0.0356(18) 0.039(2) 0.0096(15) 0.0065(16) 0.0087(14) F7 0.0262(17) 0.041(2) 0.046(2) 0.0047(17) 0.0050(16) 0.0008(15) F8 0.042(2) 0.045(2) 0.0393(19) 0.0219(16) 0.0108(17) 0.0130(16) F9 0.045(2) 0.070(2) 0.078(3) 0.037(2) 0.007(2) 0.013(2) F10 0.060(3) 0.090(3) 0.078(3) -0.006(2) 0.007(2) 0.007(2) F11 0.044(2) 0.060(2) 0.083(3) 0.029(2) 0.006(2) 0.0093(19) F12 0.036(2) 0.052(2) 0.077(3) 0.003(2) 0.0056(19) 0.0116(18) F13 0.085(3) 0.067(2) 0.066(3) 0.024(2) 0.024(2) 0.028(2) F14 0.063(3) 0.054(2) 0.059(2) 0.021(2) 0.024(2) 0.012(2) F15 0.093(3) 0.084(3) 0.062(2) 0.027(2) 0.026(2) 0.032(3) F16 0.074(3) 0.079(3) 0.091(3) 0.016(3) 0.032(2) 0.018(2) F19 0.050(2) 0.043(2) 0.051(2) 0.0128(18) 0.0114(18) 0.0193(17) F21 0.082(3) 0.091(3) 0.106(3) 0.037(3) 0.016(3) 0.019(3) F22 0.089(4) 0.082(4) 0.094(3) 0.029(3) 0.033(3) 0.018(3) F22' 0.082(4) 0.074(4) 0.092(3) 0.033(3) 0.028(3) 0.034(3) F23 0.089(3) 0.072(3) 0.113(4) 0.033(3) 0.033(3) 0.013(2) F24 0.099(4) 0.079(3) 0.095(3) 0.017(3) 0.022(3) 0.036(3) F25 0.114(4) 0.081(3) 0.157(6) 0.030(5) 0.052(4) 0.035(3) F25' 0.114(4) 0.085(3) 0.155(6) 0.028(5) 0.054(4) 0.037(3) F26 0.113(4) 0.067(3) 0.152(5) 0.036(3) 0.042(4) 0.032(3) F27 0.139(5) 0.116(4) 0.155(5) 0.025(4) 0.035(4) 0.038(3) F28 0.088(4) 0.148(4) 0.133(4) 0.070(4) 0.013(3) 0.047(3) F29 0.134(5) 0.089(3) 0.176(5) 0.003(4) 0.038(4) 0.042(3) F30 0.078(3) 0.141(5) 0.133(5) 0.081(4) 0.021(4) 0.039(3) F30' 0.077(4) 0.143(5) 0.131(5) 0.082(4) 0.020(4) 0.039(3) F31 0.086(4) 0.155(5) 0.131(4) 0.062(4) 0.024(3) 0.024(3) F32 0.084(4) 0.145(4) 0.144(4) 0.073(4) 0.030(3) 0.030(3) F20 0.052(3) 0.050(3) 0.062(3) 0.015(3) 0.008(3) 0.026(3) F17 0.050(3) 0.054(3) 0.066(3) 0.014(3) 0.012(3) 0.019(2) F18 0.049(3) 0.043(3) 0.064(3) 0.015(3) 0.009(3) 0.020(3) F20' 0.048(3) 0.043(2) 0.072(4) 0.012(3) 0.012(3) 0.018(2) F18' 0.049(3) 0.054(3) 0.067(3) 0.021(2) 0.015(2) 0.024(2) F17' 0.057(3) 0.059(3) 0.067(3) 0.011(3) 0.000(2) 0.021(2) C8S 0.127(15) 0.058(9) 0.066(10) 0.003(8) 0.078(11) 0.002(9) Cl15 0.055(2) 0.0468(17) 0.0399(17) 0.0026(13) 0.0044(14) 0.0123(15) Cl16 0.075(3) 0.063(2) 0.059(2) 0.0167(18) 0.0107(19) 0.0035(19) N1 0.028(3) 0.023(3) 0.045(4) 0.006(3) -0.009(3) 0.002(2) N2 0.028(3) 0.026(3) 0.033(3) 0.009(2) 0.005(2) 0.007(2) N3 0.017(3) 0.022(2) 0.029(3) 0.005(2) 0.005(2) 0.000(2) N4 0.020(3) 0.025(3) 0.023(3) 0.002(2) -0.003(2) 0.004(2) N5 0.016(3) 0.026(3) 0.022(3) 0.007(2) -0.001(2) 0.005(2) N6 0.023(3) 0.025(3) 0.030(3) 0.006(2) 0.008(2) 0.005(2) N7 0.032(3) 0.028(3) 0.031(3) 0.012(2) 0.013(2) 0.012(2) N8 0.021(3) 0.019(2) 0.022(3) 0.003(2) 0.003(2) 0.000(2) N9 0.024(3) 0.021(2) 0.020(3) 0.000(2) 0.001(2) 0.008(2) N10 0.019(3) 0.028(3) 0.031(3) 0.008(2) 0.005(2) 0.004(2) N11 0.017(3) 0.032(3) 0.026(3) 0.010(2) 0.009(2) 0.004(2) N12 0.024(3) 0.037(3) 0.029(3) 0.015(3) 0.004(2) 0.008(2) N13 0.023(3) 0.028(3) 0.034(3) 0.010(2) -0.003(2) 0.000(2) N14 0.032(3) 0.023(3) 0.025(3) 0.007(2) 0.004(2) 0.006(2) N15 0.019(3) 0.023(2) 0.025(3) 0.005(2) 0.003(2) 0.002(2) N16 0.030(3) 0.021(2) 0.023(3) 0.006(2) 0.004(2) 0.004(2) N17 0.032(3) 0.020(3) 0.033(3) 0.005(2) 0.015(3) 0.001(2) N18 0.017(3) 0.030(3) 0.042(3) 0.000(3) 0.002(2) 0.002(2) N19 0.028(3) 0.034(3) 0.031(3) 0.009(3) 0.012(2) 0.008(2) N20 0.023(3) 0.023(3) 0.029(3) 0.006(2) 0.003(2) 0.001(2) N21 0.027(3) 0.024(3) 0.027(3) 0.005(2) 0.004(2) 0.007(2) N22 0.022(3) 0.018(2) 0.033(3) 0.004(2) 0.004(2) 0.005(2) N23 0.027(3) 0.027(3) 0.029(3) 0.007(2) 0.003(2) 0.008(2) N24 0.031(3) 0.044(3) 0.029(3) 0.010(3) 0.007(3) 0.004(3) O1 0.027(3) 0.029(2) 0.055(3) 0.010(2) -0.001(2) 0.003(2) O2 0.015(2) 0.030(2) 0.035(3) 0.005(2) 0.0041(19) 0.0026(18) O3 0.030(3) 0.042(3) 0.026(2) 0.011(2) 0.008(2) 0.018(2) O4 0.023(2) 0.031(2) 0.033(2) 0.010(2) 0.011(2) 0.0066(19) O5 0.026(3) 0.038(3) 0.029(2) 0.005(2) 0.006(2) 0.004(2) O6 0.033(3) 0.041(3) 0.027(2) 0.011(2) 0.005(2) 0.013(2) O7 0.028(3) 0.025(2) 0.049(3) 0.000(2) 0.007(2) 0.005(2) O8 0.035(3) 0.038(3) 0.040(3) 0.017(2) 0.013(2) 0.015(2) O9 0.023(3) 0.045(3) 0.035(3) 0.014(2) 0.005(2) 0.007(2) O10 0.029(3) 0.037(3) 0.027(2) 0.004(2) 0.002(2) 0.004(2) O11 0.035(3) 0.025(2) 0.033(3) 0.012(2) 0.006(2) 0.003(2) O12 0.029(3) 0.033(2) 0.032(3) 0.008(2) -0.001(2) 0.003(2) C1 0.034(4) 0.032(4) 0.071(6) 0.023(4) -0.010(4) -0.002(3) C2 0.062(6) 0.034(4) 0.075(6) 0.028(4) -0.005(5) -0.002(4) C3 0.041(5) 0.046(5) 0.072(6) 0.030(5) -0.014(4) -0.018(4) C4 0.023(4) 0.033(4) 0.051(5) 0.011(3) -0.009(3) -0.007(3) C5 0.027(4) 0.027(3) 0.037(4) 0.010(3) -0.002(3) -0.001(3) C6 0.024(3) 0.024(3) 0.034(4) 0.006(3) 0.001(3) 0.001(3) C7 0.027(4) 0.035(4) 0.038(4) 0.014(3) -0.001(3) 0.002(3) C8 0.025(4) 0.036(4) 0.042(4) 0.014(3) -0.007(3) 0.002(3) C9 0.017(3) 0.035(4) 0.046(4) 0.020(3) 0.001(3) 0.004(3) C10 0.021(3) 0.023(3) 0.032(3) 0.008(3) 0.001(3) 0.001(3) C11 0.017(3) 0.024(3) 0.036(4) 0.008(3) 0.007(3) 0.004(2) C12 0.027(4) 0.025(3) 0.039(4) 0.010(3) 0.008(3) 0.004(3) C13 0.017(3) 0.029(3) 0.034(4) 0.006(3) 0.004(3) 0.010(3) C14 0.018(3) 0.024(3) 0.028(3) 0.003(3) 0.003(3) 0.007(2) C15 0.024(3) 0.022(3) 0.029(3) 0.009(3) 0.002(3) 0.001(3) C16 0.017(3) 0.024(3) 0.034(4) 0.002(3) 0.006(3) 0.002(2) C17 0.023(3) 0.028(3) 0.032(4) 0.006(3) 0.002(3) 0.008(3) C18 0.028(4) 0.032(3) 0.025(3) 0.003(3) -0.001(3) 0.008(3) C19 0.020(3) 0.023(3) 0.037(4) 0.004(3) 0.001(3) 0.005(3) C20 0.035(4) 0.043(4) 0.027(4) 0.013(3) 0.004(3) 0.007(3) C21 0.023(3) 0.026(3) 0.029(3) 0.006(3) -0.003(3) 0.004(3) C22 0.025(4) 0.031(3) 0.040(4) 0.001(3) 0.000(3) 0.005(3) C23 0.019(3) 0.029(3) 0.025(3) 0.010(3) 0.004(3) 0.008(3) C24 0.022(3) 0.032(3) 0.026(3) 0.012(3) 0.005(3) 0.008(3) C25 0.024(4) 0.040(4) 0.030(4) 0.008(3) 0.006(3) 0.012(3) C26 0.024(4) 0.034(3) 0.037(4) 0.010(3) 0.013(3) 0.006(3) C27 0.023(4) 0.035(4) 0.037(4) 0.014(3) 0.006(3) 0.000(3) C28 0.022(3) 0.034(3) 0.026(3) 0.008(3) 0.004(3) 0.011(3) C29 0.020(3) 0.026(3) 0.033(3) 0.009(3) 0.006(3) 0.003(3) C30 0.021(3) 0.041(4) 0.035(4) 0.005(3) 0.003(3) 0.012(3) C31 0.031(4) 0.044(4) 0.033(4) 0.004(3) -0.003(3) 0.011(3) C32 0.038(4) 0.043(4) 0.032(4) 0.000(3) 0.007(3) 0.008(3) C33 0.032(4) 0.031(3) 0.036(4) 0.005(3) 0.011(3) 0.010(3) C34 0.030(4) 0.047(4) 0.046(4) 0.022(4) 0.000(3) 0.012(3) C35 0.038(4) 0.053(5) 0.036(4) 0.013(4) 0.002(3) 0.016(4) C36 0.050(5) 0.043(4) 0.031(4) 0.011(3) 0.003(3) 0.017(4) C37 0.040(4) 0.041(4) 0.035(4) 0.016(3) 0.006(3) 0.017(3) C38 0.035(4) 0.023(3) 0.036(4) 0.009(3) 0.013(3) 0.009(3) C39 0.027(4) 0.026(3) 0.029(3) 0.009(3) 0.008(3) 0.005(3) C40 0.033(4) 0.037(4) 0.039(4) 0.017(3) 0.015(3) 0.002(3) C41 0.029(4) 0.036(4) 0.043(4) 0.012(3) 0.017(3) 0.004(3) C42 0.027(4) 0.033(3) 0.028(3) 0.005(3) 0.013(3) 0.004(3) C43 0.020(3) 0.023(3) 0.023(3) 0.000(3) 0.004(3) 0.004(2) C44 0.013(3) 0.026(3) 0.028(3) 0.003(3) 0.003(2) 0.001(2) C45 0.036(4) 0.030(3) 0.027(3) 0.003(3) 0.000(3) 0.009(3) C46 0.026(3) 0.026(3) 0.022(3) 0.004(3) 0.005(3) 0.011(3) C47 0.024(3) 0.025(3) 0.028(3) 0.012(3) 0.001(3) 0.008(3) C48 0.021(3) 0.028(3) 0.028(3) 0.012(3) 0.000(3) 0.005(3) C49 0.022(3) 0.033(3) 0.029(3) 0.013(3) 0.007(3) 0.013(3) C50 0.022(3) 0.029(3) 0.032(4) 0.010(3) 0.001(3) 0.002(3) C51 0.021(3) 0.034(3) 0.027(3) 0.016(3) 0.001(3) 0.005(3) C52 0.029(4) 0.030(3) 0.025(3) 0.006(3) 0.002(3) 0.011(3) C53 0.036(4) 0.029(3) 0.045(4) 0.010(3) 0.008(3) -0.004(3) C54 0.020(3) 0.027(3) 0.025(3) 0.005(3) 0.003(3) 0.005(3) C55 0.034(4) 0.030(3) 0.030(4) 0.010(3) 0.009(3) 0.003(3) C56 0.016(3) 0.033(3) 0.026(3) 0.010(3) 0.002(3) 0.006(3) C57 0.025(3) 0.032(3) 0.020(3) 0.005(3) 0.008(3) 0.006(3) C58 0.036(4) 0.036(4) 0.035(4) 0.006(3) 0.011(3) 0.015(3) C59 0.044(5) 0.043(4) 0.031(4) 0.007(3) 0.013(3) 0.014(3) C60 0.042(4) 0.044(4) 0.023(3) 0.013(3) 0.011(3) 0.013(3) C61 0.024(4) 0.032(3) 0.032(4) 0.007(3) 0.007(3) 0.007(3) C62 0.025(4) 0.037(4) 0.028(3) 0.012(3) 0.008(3) 0.011(3) C63 0.043(5) 0.050(4) 0.030(4) 0.019(3) 0.011(3) 0.017(4) C64 0.047(5) 0.044(4) 0.031(4) 0.015(3) 0.011(3) 0.001(4) C65 0.051(5) 0.038(4) 0.051(5) 0.016(4) 0.009(4) 0.009(4) C66 0.043(4) 0.032(3) 0.029(4) 0.008(3) 0.002(3) 0.015(3) C67 0.022(4) 0.039(4) 0.061(5) 0.018(4) 0.007(3) 0.004(3) C68 0.022(4) 0.042(4) 0.060(5) 0.018(4) -0.006(4) 0.003(3) C69 0.044(5) 0.036(4) 0.056(5) 0.021(4) -0.013(4) -0.008(4) C70 0.030(4) 0.030(3) 0.037(4) 0.007(3) -0.001(3) -0.004(3) C71 0.031(4) 0.025(3) 0.034(4) 0.014(3) 0.004(3) -0.001(3) C72 0.025(4) 0.028(3) 0.030(3) 0.009(3) 0.003(3) 0.000(3) C73 0.038(4) 0.031(4) 0.042(4) 0.008(3) 0.012(3) 0.001(3) C74 0.049(5) 0.032(4) 0.043(4) 0.000(3) 0.011(4) 0.012(3) C75 0.036(4) 0.028(3) 0.035(4) 0.000(3) 0.009(3) 0.009(3) C76 0.019(3) 0.029(3) 0.025(3) 0.007(3) 0.004(3) 0.006(3) C77 0.025(3) 0.031(3) 0.029(3) 0.013(3) 0.008(3) 0.005(3) C78 0.023(3) 0.026(3) 0.040(4) 0.012(3) 0.005(3) 0.003(3) C79 0.013(3) 0.029(3) 0.030(3) 0.008(3) 0.004(3) 0.000(2) C80 0.016(3) 0.029(3) 0.032(4) 0.009(3) 0.005(3) 0.002(3) C81 0.024(3) 0.035(3) 0.027(3) 0.010(3) 0.006(3) 0.011(3) C82 0.015(3) 0.032(3) 0.033(4) 0.012(3) -0.004(3) -0.002(3) C83 0.027(4) 0.033(3) 0.027(3) 0.005(3) 0.005(3) 0.007(3) C84 0.028(4) 0.031(3) 0.028(3) 0.009(3) 0.006(3) 0.007(3) C85 0.019(3) 0.032(3) 0.038(4) 0.012(3) 0.004(3) 0.003(3) C86 0.045(5) 0.039(4) 0.027(4) 0.011(3) 0.002(3) 0.002(3) C87 0.024(3) 0.026(3) 0.029(3) -0.001(3) 0.005(3) 0.006(3) C88 0.034(4) 0.031(3) 0.030(4) 0.005(3) -0.002(3) 0.010(3) C89 0.033(4) 0.029(3) 0.026(3) 0.004(3) 0.009(3) 0.015(3) C90 0.035(4) 0.027(3) 0.030(4) 0.007(3) 0.009(3) 0.009(3) C91 0.052(5) 0.024(3) 0.043(4) 0.013(3) 0.016(4) 0.006(3) C92 0.083(7) 0.032(4) 0.053(5) 0.021(4) 0.022(5) 0.015(4) C93 0.047(5) 0.019(3) 0.056(5) 0.001(3) 0.018(4) -0.002(3) C94 0.033(4) 0.032(4) 0.043(4) 0.008(3) 0.018(3) 0.006(3) C95 0.021(3) 0.027(3) 0.045(4) 0.007(3) 0.008(3) 0.001(3) C96 0.029(4) 0.028(3) 0.052(5) -0.003(3) 0.002(3) 0.001(3) C97 0.035(5) 0.044(5) 0.060(5) -0.012(4) -0.002(4) 0.005(4) C98 0.034(5) 0.068(6) 0.054(5) 0.007(5) -0.007(4) 0.015(4) C99 0.030(4) 0.044(4) 0.049(5) 0.012(4) -0.001(3) 0.011(3) C100 0.049(5) 0.039(4) 0.040(4) 0.007(3) 0.009(4) 0.012(4) C101 0.054(5) 0.047(5) 0.042(5) -0.003(4) 0.001(4) 0.014(4) C102 0.056(5) 0.060(5) 0.027(4) -0.001(4) -0.001(4) 0.021(4) C103 0.043(5) 0.045(4) 0.037(4) 0.013(3) 0.008(3) 0.015(4) C104 0.026(4) 0.034(3) 0.027(3) 0.007(3) 0.009(3) 0.005(3) C105 0.027(4) 0.027(3) 0.032(4) 0.007(3) 0.005(3) 0.007(3) C106 0.033(4) 0.049(4) 0.038(4) 0.021(4) 0.011(3) 0.007(3) C107 0.045(5) 0.024(3) 0.046(4) 0.017(3) 0.003(4) 0.003(3) C108 0.033(4) 0.024(3) 0.042(4) 0.008(3) 0.001(3) 0.005(3) C109 0.024(3) 0.026(3) 0.030(3) 0.008(3) 0.005(3) 0.004(3) C110 0.023(3) 0.021(3) 0.033(4) 0.000(3) 0.005(3) 0.007(3) C111 0.046(4) 0.027(3) 0.026(3) 0.006(3) -0.004(3) 0.005(3) C112 0.027(4) 0.034(3) 0.017(3) 0.010(3) 0.004(3) 0.007(3) C113 0.025(4) 0.026(3) 0.029(3) 0.005(3) 0.007(3) 0.007(3) C114 0.024(3) 0.021(3) 0.027(3) 0.003(3) 0.004(3) 0.002(2) C115 0.027(4) 0.029(3) 0.026(3) 0.008(3) 0.007(3) 0.010(3) C116 0.030(4) 0.027(3) 0.033(4) 0.012(3) 0.007(3) 0.002(3) C117 0.028(4) 0.034(4) 0.037(4) 0.007(3) 0.007(3) 0.001(3) C118 0.034(4) 0.030(3) 0.027(3) 0.001(3) 0.002(3) 0.008(3) C119 0.038(4) 0.034(4) 0.045(4) 0.007(3) -0.005(4) -0.008(3) C120 0.024(3) 0.029(3) 0.033(4) 0.011(3) 0.007(3) 0.008(3) C121 0.028(4) 0.039(4) 0.037(4) 0.015(3) 0.008(3) 0.006(3) C122 0.022(3) 0.028(3) 0.040(4) 0.014(3) 0.003(3) 0.009(3) C123 0.032(4) 0.028(3) 0.031(4) 0.011(3) 0.007(3) 0.010(3) C124 0.027(4) 0.038(4) 0.054(5) 0.018(4) 0.004(3) 0.015(3) C125 0.038(4) 0.044(4) 0.035(4) 0.012(3) -0.007(3) 0.018(3) C126 0.047(5) 0.044(4) 0.040(4) 0.021(4) 0.006(4) 0.019(4) C127 0.037(4) 0.028(3) 0.036(4) 0.010(3) 0.006(3) 0.011(3) C128 0.041(4) 0.031(4) 0.041(4) 0.014(3) 0.007(3) 0.001(3) C129 0.047(5) 0.041(4) 0.061(5) 0.023(4) 0.016(4) 0.002(4) C130 0.088(8) 0.048(5) 0.048(5) 0.014(4) 0.017(5) -0.028(5) C131 0.045(5) 0.074(6) 0.059(6) 0.031(5) 0.010(4) -0.010(5) C132 0.024(4) 0.072(6) 0.047(5) 0.016(4) -0.001(3) 0.001(4) C133 0.049(5) 0.052(5) 0.047(5) 0.020(4) -0.004(4) -0.004(4) C2S1 0.157(13) 0.157(13) 0.157(13) 0.047(4) 0.027(2) 0.042(4) C2S2 0.057(5) 0.057(5) 0.058(5) 0.0168(17) 0.0097(13) 0.0153(16) Cl3 0.108(3) 0.083(2) 0.116(3) 0.0333(19) 0.027(2) 0.0265(18) Cl4 0.151(4) 0.114(3) 0.144(4) 0.044(3) 0.036(3) 0.031(3) C3S 0.045(5) 0.043(4) 0.058(5) 0.012(4) 0.015(4) 0.015(4) Cl5 0.096(2) 0.111(2) 0.165(3) 0.102(3) 0.069(2) 0.0562(19) Cl6 0.0702(19) 0.154(3) 0.0641(17) 0.0363(19) 0.0075(14) 0.0420(19) C4S 0.074(9) 0.130(12) 0.153(14) 0.076(11) 0.032(9) 0.058(8) Cl7 0.130(3) 0.084(2) 0.0712(18) 0.0201(16) 0.0051(18) 0.031(2) Cl8 0.089(2) 0.081(2) 0.125(3) -0.009(2) 0.002(2) 0.0125(17) C5S 0.117(10) 0.056(6) 0.062(7) -0.003(5) 0.015(7) -0.006(6) Cl9 0.528(14) 0.094(3) 0.277(8) 0.109(4) 0.242(9) 0.134(5) Cl10 0.159(4) 0.256(6) 0.076(2) 0.058(3) -0.014(3) -0.113(4) C7S 0.080(8) 0.063(6) 0.081(8) 0.008(6) -0.007(6) 0.031(6) Cl13 0.085(2) 0.0697(17) 0.095(2) 0.0055(16) -0.0093(17) 0.0155(15) Cl14 0.098(2) 0.0678(17) 0.120(3) 0.0224(17) 0.028(2) 0.0319(16) C9S 0.047(6) 0.102(8) 0.042(5) 0.014(5) 0.009(4) 0.017(5) Cl17 0.0666(19) 0.213(4) 0.0519(15) 0.045(2) 0.0115(13) 0.053(2) Cl18 0.0565(15) 0.0865(17) 0.0664(15) 0.0142(14) 0.0237(12) 0.0246(13) C10S 0.141(13) 0.112(10) 0.076(8) 0.044(8) 0.056(8) 0.062(9) Cl19 0.122(3) 0.170(4) 0.092(3) 0.000(3) 0.017(2) 0.048(3) Cl20 0.135(4) 0.186(5) 0.223(6) 0.123(5) 0.019(4) 0.053(4) C11S 0.037(5) 0.039(4) 0.080(6) 0.014(4) 0.018(4) 0.001(4) Cl21 0.0452(13) 0.0567(13) 0.0845(17) 0.0185(12) -0.0133(12) 0.0153(10) Cl22 0.0539(14) 0.0454(11) 0.0775(16) 0.0103(11) 0.0166(12) 0.0029(10) N25 0.034(4) 0.039(4) 0.060(5) 0.012(3) 0.006(3) 0.010(3) O13 0.050(4) 0.072(4) 0.056(4) 0.026(3) 0.008(3) 0.008(3) O14 0.055(4) 0.063(4) 0.074(5) -0.011(4) 0.016(4) -0.012(3) O1W 0.0230(13) 0.0317(12) 0.0225(12) 0.0111(9) 0.0040(9) 0.0030(9) O2W 0.029(3) 0.093(4) 0.106(5) 0.082(4) 0.025(3) 0.038(3) O3W 0.021(3) 0.129(6) 0.084(5) 0.056(5) 0.001(3) 0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.000(4) . ? Co1 O2 2.029(4) . ? Co1 N8 2.144(5) . ? Co1 N5 2.151(5) . ? Co1 N9 2.156(5) . ? Co1 N4 2.157(5) . ? Co2 O7 2.016(5) . ? Co2 O6 2.026(5) . ? Co2 N20 2.120(5) . ? Co2 N17 2.130(5) . ? Co2 N21 2.138(5) . ? Co2 N16 2.143(5) . ? Co3 O5 2.022(5) . ? Co3 O4 2.067(5) . ? Co3 N11 2.115(5) . ? Co3 N14 2.125(5) . ? Co3 N10 2.137(5) . ? Co3 N15 2.200(5) . ? Co4 O1 2.030(5) . ? Co4 O8 2.067(5) . ? Co4 N23 2.116(5) . ? Co4 N2 2.128(6) . ? Co4 N3 2.150(5) . ? Co4 N22 2.188(5) . ? S1 C11 1.703(6) . ? S1 C12 1.718(7) . ? S2 C23 1.703(6) . ? S2 C22 1.719(7) . ? S3 C44 1.709(6) . ? S3 C45 1.722(7) . ? S4 C56 1.701(7) . ? S4 C55 1.708(7) . ? S5 C77 1.702(6) . ? S5 C78 1.717(7) . ? S6 C89 1.698(7) . ? S6 C88 1.702(7) . ? S7 C111 1.684(7) . ? S7 C110 1.715(6) . ? S8 C122 1.715(7) . ? S8 C121 1.722(7) . ? B1 F3 1.359(11) . ? B1 F1 1.387(11) . ? B1 F2 1.409(10) . ? B1 F4 1.415(11) . ? B2 F6 1.364(8) . ? B2 F8 1.375(8) . ? B2 F7 1.422(8) . ? B2 F5 1.435(8) . ? B3 F9 1.329(12) . ? B3 F12 1.380(12) . ? B3 F10 1.392(13) . ? B3 F11 1.409(12) . ? B4 F13 1.379(13) . ? B4 F14 1.379(12) . ? B4 F15 1.387(13) . ? B4 F16 1.400(14) . ? B5 F20' 1.307(10) . ? B5 F17' 1.318(10) . ? B5 F17 1.339(12) . ? B5 F19 1.373(10) . ? B5 F20 1.428(13) . ? B5 F18 1.462(19) . ? B5 F18' 1.535(12) . ? B6 F24 1.340(14) . ? B6 F23 1.351(14) . ? B6 F22' 1.363(19) . ? B6 F22 1.36(2) . ? B6 F21 1.438(16) . ? B7 F25' 1.22(3) . ? B7 F26 1.32(2) . ? B7 F25 1.32(3) . ? B7 F29 1.338(18) . ? B7 F27 1.57(2) . ? B8 F30 1.32(3) . ? B8 F31 1.34(2) . ? B8 F30' 1.35(3) . ? B8 F28 1.37(2) . ? B8 F32 1.488(19) . ? C8S Cl15 1.545(15) . ? C8S Cl16 1.595(15) . ? C8S H8SA 0.9900 . ? C8S H8SB 0.9900 . ? N1 C5 1.334(9) . ? N1 C1 1.345(9) . ? N1 O1 1.354(7) . ? N2 C6 1.325(8) . ? N2 C10 1.364(8) . ? N3 C11 1.321(8) . ? N3 C13 1.398(8) . ? N4 C23 1.316(8) . ? N4 C21 1.407(8) . ? N5 C28 1.324(8) . ? N5 C24 1.335(8) . ? N6 C33 1.319(8) . ? N6 O2 1.331(7) . ? N6 C29 1.356(8) . ? N7 O3 1.330(7) . ? N7 C34 1.343(9) . ? N7 C38 1.365(8) . ? N8 C39 1.346(8) . ? N8 C43 1.350(8) . ? N9 C44 1.302(8) . ? N9 C46 1.389(8) . ? N10 C56 1.325(8) . ? N10 C54 1.392(8) . ? N11 C61 1.336(8) . ? N11 C57 1.349(8) . ? N12 O4 1.335(7) . ? N12 C66 1.353(8) . ? N12 C62 1.357(8) . ? N13 C67 1.348(9) . ? N13 O5 1.353(7) . ? N13 C71 1.361(9) . ? N14 C76 1.335(8) . ? N14 C72 1.344(8) . ? N15 C77 1.321(8) . ? N15 C79 1.385(7) . ? N16 C89 1.312(8) . ? N16 C87 1.405(8) . ? N17 C94 1.331(9) . ? N17 C90 1.354(9) . ? N18 O7 1.327(7) . ? N18 C99 1.362(9) . ? N18 C95 1.367(9) . ? N19 O6 1.329(7) . ? N19 C100 1.361(9) . ? N19 C104 1.377(9) . ? N20 C109 1.336(8) . ? N20 C105 1.343(8) . ? N21 C110 1.314(8) . ? N21 C112 1.376(8) . ? N22 C122 1.323(8) . ? N22 C120 1.389(8) . ? N23 C123 1.335(8) . ? N23 C127 1.351(9) . ? N24 O8 1.330(7) . ? N24 C132 1.348(9) . ? N24 C128 1.363(10) . ? O9 C15 1.380(8) . ? O9 H9 0.8400 . ? O10 C48 1.381(7) . ? O10 H10 0.8400 . ? O11 C81 1.361(8) . ? O11 H11 0.8400 . ? O12 C114 1.389(7) . ? O12 H12 0.8400 . ? C1 C2 1.386(11) . ? C1 H1 0.9500 . ? C2 C3 1.393(13) . ? C2 H2 0.9500 . ? C3 C4 1.367(11) . ? C3 H3 0.9500 . ? C4 C5 1.387(10) . ? C4 H4 0.9500 . ? C5 C6 1.514(9) . ? C6 C7 1.390(9) . ? C7 C8 1.373(10) . ? C7 H7 0.9500 . ? C8 C9 1.358(9) . ? C8 H8 0.9500 . ? C9 C10 1.390(9) . ? C9 H9A 0.9500 . ? C10 C11 1.453(8) . ? C12 C13 1.345(9) . ? C12 H12A 0.9500 . ? C13 C14 1.484(9) . ? C14 C15 1.398(9) . ? C14 C19 1.405(9) . ? C15 C16 1.408(9) . ? C16 C17 1.363(9) . ? C16 C21 1.480(9) . ? C17 C18 1.411(9) . ? C17 H17 0.9500 . ? C18 C19 1.356(9) . ? C18 C20 1.524(9) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.359(9) . ? C22 H22 0.9500 . ? C23 C24 1.472(9) . ? C24 C25 1.388(9) . ? C25 C26 1.395(9) . ? C25 H25 0.9500 . ? C26 C27 1.381(9) . ? C26 H26 0.9500 . ? C27 C28 1.393(9) . ? C27 H27 0.9500 . ? C28 C29 1.498(9) . ? C29 C30 1.389(9) . ? C30 C31 1.353(10) . ? C30 H30 0.9500 . ? C31 C32 1.413(10) . ? C31 H31 0.9500 . ? C32 C33 1.367(10) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.353(10) . ? C34 H34 0.9500 . ? C35 C36 1.374(11) . ? C35 H35 0.9500 . ? C36 C37 1.379(10) . ? C36 H36 0.9500 . ? C37 C38 1.365(10) . ? C37 H37 0.9500 . ? C38 C39 1.483(10) . ? C39 C40 1.412(9) . ? C40 C41 1.385(10) . ? C40 H40 0.9500 . ? C41 C42 1.397(10) . ? C41 H41 0.9500 . ? C42 C43 1.391(9) . ? C42 H42 0.9500 . ? C43 C44 1.472(9) . ? C45 C46 1.361(9) . ? C45 H45 0.9500 . ? C46 C47 1.481(9) . ? C47 C48 1.386(9) . ? C47 C52 1.402(9) . ? C48 C49 1.396(9) . ? C49 C50 1.405(9) . ? C49 C54 1.490(8) . ? C50 C51 1.386(9) . ? C50 H50 0.9500 . ? C51 C52 1.384(9) . ? C51 C53 1.502(9) . ? C52 H52 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.365(9) . ? C55 H55 0.9500 . ? C56 C57 1.466(9) . ? C57 C58 1.378(9) . ? C58 C59 1.396(10) . ? C58 H58 0.9500 . ? C59 C60 1.368(10) . ? C59 H59 0.9500 . ? C60 C61 1.386(9) . ? C60 H60 0.9500 . ? C61 C62 1.497(9) . ? C62 C63 1.411(10) . ? C63 C64 1.351(10) . ? C63 H63 0.9500 . ? C64 C65 1.397(11) . ? C64 H64 0.9500 . ? C65 C66 1.356(10) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C68 1.364(11) . ? C67 H67 0.9500 . ? C68 C69 1.341(12) . ? C68 H68 0.9500 . ? C69 C70 1.367(11) . ? C69 H69 0.9500 . ? C70 C71 1.410(9) . ? C70 H70 0.9500 . ? C71 C72 1.484(10) . ? C72 C73 1.385(9) . ? C73 C74 1.395(11) . ? C73 H73 0.9500 . ? C74 C75 1.372(10) . ? C74 H74 0.9500 . ? C75 C76 1.393(9) . ? C75 H75 0.9500 . ? C76 C77 1.468(9) . ? C78 C79 1.363(9) . ? C78 H78 0.9500 . ? C79 C80 1.460(9) . ? C80 C85 1.407(9) . ? C80 C81 1.434(9) . ? C81 C82 1.384(9) . ? C82 C83 1.396(9) . ? C82 C87 1.487(9) . ? C83 C84 1.414(9) . ? C83 H83 0.9500 . ? C84 C85 1.386(9) . ? C84 C86 1.516(9) . ? C85 H85 0.9500 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 C88 1.336(9) . ? C88 H88 0.9500 . ? C89 C90 1.474(9) . ? C90 C91 1.382(9) . ? C91 C92 1.375(11) . ? C91 H91 0.9500 . ? C92 C93 1.373(12) . ? C92 H92 0.9500 . ? C93 C94 1.408(10) . ? C93 H93 0.9500 . ? C94 C95 1.464(11) . ? C95 C96 1.379(10) . ? C96 C97 1.393(12) . ? C96 H96 0.9500 . ? C97 C98 1.341(12) . ? C97 H97 0.9500 . ? C98 C99 1.401(11) . ? C98 H98 0.9500 . ? C99 H99 0.9500 . ? C100 C101 1.375(11) . ? C100 H100 0.9500 . ? C101 C102 1.372(12) . ? C101 H101 0.9500 . ? C102 C103 1.397(10) . ? C102 H102 0.9500 . ? C103 C104 1.357(10) . ? C103 H103 0.9500 . ? C104 C105 1.503(9) . ? C105 C106 1.392(10) . ? C106 C107 1.365(10) . ? C106 H106 0.9500 . ? C107 C108 1.376(10) . ? C107 H107 0.9500 . ? C108 C109 1.407(9) . ? C108 H108 0.9500 . ? C109 C110 1.462(9) . ? C111 C112 1.366(9) . ? C111 H111 0.9500 . ? C112 C113 1.484(9) . ? C113 C118 1.365(9) . ? C113 C114 1.395(9) . ? C114 C115 1.406(9) . ? C115 C116 1.380(9) . ? C115 C120 1.494(9) . ? C116 C117 1.379(10) . ? C116 H116 0.9500 . ? C117 C118 1.409(10) . ? C117 C119 1.536(9) . ? C118 H118 0.9500 . ? C119 H11A 0.9800 . ? C119 H11B 0.9800 . ? C119 H11C 0.9800 . ? C120 C121 1.361(9) . ? C121 H121 0.9500 . ? C122 C123 1.445(9) . ? C123 C124 1.400(10) . ? C124 C125 1.388(11) . ? C124 H124 0.9500 . ? C125 C126 1.385(11) . ? C125 H125 0.9500 . ? C126 C127 1.404(10) . ? C126 H126 0.9500 . ? C127 C128 1.480(10) . ? C128 C129 1.412(10) . ? C129 C130 1.360(13) . ? C129 H129 0.9500 . ? C130 C131 1.422(15) . ? C130 H130 0.9500 . ? C131 C132 1.375(12) . ? C131 H131 0.9500 . ? C132 H132 0.9500 . ? C133 Cl21 1.748(8) . ? C133 Cl22 1.762(9) . ? C133 H13A 0.9900 . ? C133 H13B 0.9900 . ? C2S1 Cl4 1.7828 . ? C2S1 Cl3 1.7833 . ? C2S1 H2SA 0.9900 . ? C2S1 H2SB 0.9900 . ? C2S2 Cl4 1.7790 . ? C2S2 Cl3 1.7829 . ? C2S2 H2SC 0.9900 . ? C2S2 H2SD 0.9900 . ? C3S Cl6 1.735(9) . ? C3S Cl5 1.762(8) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S Cl7 1.605(14) . ? C4S Cl8 1.822(15) . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C5S Cl9 1.725(13) . ? C5S Cl10 1.727(14) . ? C5S H5S1 0.9900 . ? C5S H5S2 0.9900 . ? C7S Cl13 1.757(11) . ? C7S Cl14 1.763(11) . ? C7S H7S1 0.9900 . ? C7S H7S2 0.9900 . ? C9S Cl18 1.768(11) . ? C9S Cl17 1.779(10) . ? C9S H9S1 0.9900 . ? C9S H9S2 0.9900 . ? C10S Cl20 1.791(13) . ? C10S Cl19 1.804(15) . ? C10S H10A 0.9900 . ? C10S H10B 0.9900 . ? C11S N25 1.481(10) . ? C11S H11D 0.9800 . ? C11S H11E 0.9800 . ? C11S H11F 0.9800 . ? N25 O14 1.208(9) . ? N25 O13 1.239(9) . ? O1W H1O1 0.8502 . ? O1W H2O1 0.8500 . ? O2W H1O2 0.8499 . ? O2W H2O2 0.8501 . ? O3W H1O3 0.8500 . ? O3W H2O3 0.8501 . ? 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 O3 Co1 O2 109.22(19) . . ? O3 Co1 N8 82.90(19) . . ? O2 Co1 N8 89.68(17) . . ? O3 Co1 N5 89.46(19) . . ? O2 Co1 N5 82.09(18) . . ? N8 Co1 N5 166.30(19) . . ? O3 Co1 N9 151.7(2) . . ? O2 Co1 N9 90.33(18) . . ? N8 Co1 N9 76.8(2) . . ? N5 Co1 N9 114.01(19) . . ? O3 Co1 N4 89.08(19) . . ? O2 Co1 N4 152.1(2) . . ? N8 Co1 N4 114.01(19) . . ? N5 Co1 N4 77.06(19) . . ? N9 Co1 N4 81.58(18) . . ? O7 Co2 O6 113.4(2) . . ? O7 Co2 N20 88.2(2) . . ? O6 Co2 N20 81.9(2) . . ? O7 Co2 N17 81.7(2) . . ? O6 Co2 N17 89.19(19) . . ? N20 Co2 N17 162.7(2) . . ? O7 Co2 N21 87.31(19) . . ? O6 Co2 N21 150.5(2) . . ? N20 Co2 N21 77.8(2) . . ? N17 Co2 N21 115.4(2) . . ? O7 Co2 N16 150.3(2) . . ? O6 Co2 N16 87.77(19) . . ? N20 Co2 N16 116.4(2) . . ? N17 Co2 N16 77.8(2) . . ? N21 Co2 N16 82.4(2) . . ? O5 Co3 O4 90.83(18) . . ? O5 Co3 N11 83.20(19) . . ? O4 Co3 N11 80.46(19) . . ? O5 Co3 N14 84.8(2) . . ? O4 Co3 N14 92.60(19) . . ? N11 Co3 N14 166.0(2) . . ? O5 Co3 N10 112.9(2) . . ? O4 Co3 N10 145.43(19) . . ? N11 Co3 N10 78.0(2) . . ? N14 Co3 N10 113.5(2) . . ? O5 Co3 N15 162.08(19) . . ? O4 Co3 N15 83.45(18) . . ? N11 Co3 N15 112.37(19) . . ? N14 Co3 N15 78.6(2) . . ? N10 Co3 N15 80.19(19) . . ? O1 Co4 O8 115.9(2) . . ? O1 Co4 N23 88.1(2) . . ? O8 Co4 N23 80.8(2) . . ? O1 Co4 N2 80.8(2) . . ? O8 Co4 N2 89.4(2) . . ? N23 Co4 N2 160.3(2) . . ? O1 Co4 N3 147.8(2) . . ? O8 Co4 N3 87.21(19) . . ? N23 Co4 N3 118.9(2) . . ? N2 Co4 N3 77.2(2) . . ? O1 Co4 N22 88.24(19) . . ? O8 Co4 N22 146.3(2) . . ? N23 Co4 N22 76.7(2) . . ? N2 Co4 N22 118.9(2) . . ? N3 Co4 N22 82.19(19) . . ? C11 S1 C12 89.4(3) . . ? C23 S2 C22 89.3(3) . . ? C44 S3 C45 89.0(3) . . ? C56 S4 C55 89.8(3) . . ? C77 S5 C78 89.0(3) . . ? C89 S6 C88 88.7(3) . . ? C111 S7 C110 89.0(3) . . ? C122 S8 C121 89.9(3) . . ? F3 B1 F1 112.0(8) . . ? F3 B1 F2 109.7(7) . . ? F1 B1 F2 109.6(7) . . ? F3 B1 F4 109.9(7) . . ? F1 B1 F4 108.8(7) . . ? F2 B1 F4 106.8(7) . . ? F6 B2 F8 112.8(5) . . ? F6 B2 F7 109.6(5) . . ? F8 B2 F7 110.4(6) . . ? F6 B2 F5 108.0(6) . . ? F8 B2 F5 109.5(5) . . ? F7 B2 F5 106.4(5) . . ? F9 B3 F12 111.8(8) . . ? F9 B3 F10 109.7(9) . . ? F12 B3 F10 110.2(8) . . ? F9 B3 F11 109.2(8) . . ? F12 B3 F11 108.2(9) . . ? F10 B3 F11 107.6(8) . . ? F13 B4 F14 111.3(9) . . ? F13 B4 F15 112.4(9) . . ? F14 B4 F15 108.8(10) . . ? F13 B4 F16 107.6(10) . . ? F14 B4 F16 109.5(9) . . ? F15 B4 F16 107.1(9) . . ? F20' B5 F17' 122.4(9) . . ? F20' B5 F17 130.6(10) . . ? F17' B5 F17 51.6(8) . . ? F20' B5 F19 111.0(8) . . ? F17' B5 F19 115.2(8) . . ? F17 B5 F19 113.7(9) . . ? F20' B5 F20 79.6(8) . . ? F17' B5 F20 55.1(7) . . ? F17 B5 F20 105.1(11) . . ? F19 B5 F20 107.9(8) . . ? F20' B5 F18 28.0(7) . . ? F17' B5 F18 129.6(10) . . ? F17 B5 F18 110.1(11) . . ? F19 B5 F18 115.0(9) . . ? F20 B5 F18 104.1(10) . . ? F20' B5 F18' 102.1(8) . . ? F17' B5 F18' 100.5(7) . . ? F17 B5 F18' 49.4(8) . . ? F19 B5 F18' 101.5(7) . . ? F20 B5 F18' 147.8(9) . . ? F18 B5 F18' 74.1(8) . . ? F24 B6 F23 113.1(11) . . ? F24 B6 F22' 101.5(11) . . ? F23 B6 F22' 119.9(13) . . ? F24 B6 F22 126.5(13) . . ? F23 B6 F22 113.3(12) . . ? F22' B6 F22 30.0(8) . . ? F24 B6 F21 104.2(11) . . ? F23 B6 F21 104.9(10) . . ? F22' B6 F21 112.4(12) . . ? F22 B6 F21 88.3(11) . . ? F25' B7 F26 127.1(19) . . ? F25' B7 F25 23.7(17) . . ? F26 B7 F25 110.5(19) . . ? F25' B7 F29 114(2) . . ? F26 B7 F29 116.2(16) . . ? F25 B7 F29 119.9(19) . . ? F25' B7 F27 96.1(18) . . ? F26 B7 F27 93.6(14) . . ? F25 B7 F27 116.3(19) . . ? F29 B7 F27 96.7(15) . . ? F30 B8 F31 103.7(16) . . ? F30 B8 F30' 26.2(13) . . ? F31 B8 F30' 125.5(17) . . ? F30 B8 F28 124(2) . . ? F31 B8 F28 110.3(14) . . ? F30' B8 F28 99.1(17) . . ? F30 B8 F32 106.0(16) . . ? F31 B8 F32 105.8(16) . . ? F30' B8 F32 108.6(16) . . ? F28 B8 F32 106.1(13) . . ? Cl15 C8S Cl16 129.2(12) . . ? Cl15 C8S H8SA 105.0 . . ? Cl16 C8S H8SA 105.0 . . ? Cl15 C8S H8SB 105.0 . . ? Cl16 C8S H8SB 105.0 . . ? H8SA C8S H8SB 105.8 . . ? C5 N1 C1 122.1(6) . . ? C5 N1 O1 121.6(6) . . ? C1 N1 O1 116.2(6) . . ? C6 N2 C10 118.5(6) . . ? C6 N2 Co4 125.7(4) . . ? C10 N2 Co4 115.7(4) . . ? C11 N3 C13 110.4(5) . . ? C11 N3 Co4 112.1(4) . . ? C13 N3 Co4 135.1(4) . . ? C23 N4 C21 110.1(5) . . ? C23 N4 Co1 112.8(4) . . ? C21 N4 Co1 137.1(4) . . ? C28 N5 C24 117.8(5) . . ? C28 N5 Co1 126.2(4) . . ? C24 N5 Co1 115.3(4) . . ? C33 N6 O2 117.8(5) . . ? C33 N6 C29 120.9(6) . . ? O2 N6 C29 121.3(5) . . ? O3 N7 C34 116.5(5) . . ? O3 N7 C38 122.6(6) . . ? C34 N7 C38 120.9(6) . . ? C39 N8 C43 118.4(5) . . ? C39 N8 Co1 125.7(4) . . ? C43 N8 Co1 115.8(4) . . ? C44 N9 C46 111.1(5) . . ? C44 N9 Co1 113.2(4) . . ? C46 N9 Co1 134.1(4) . . ? C56 N10 C54 111.2(5) . . ? C56 N10 Co3 111.9(4) . . ? C54 N10 Co3 135.8(4) . . ? C61 N11 C57 118.1(5) . . ? C61 N11 Co3 125.9(4) . . ? C57 N11 Co3 116.0(4) . . ? O4 N12 C66 118.1(5) . . ? O4 N12 C62 121.7(5) . . ? C66 N12 C62 120.2(6) . . ? C67 N13 O5 116.5(6) . . ? C67 N13 C71 121.2(6) . . ? O5 N13 C71 122.1(5) . . ? C76 N14 C72 119.0(6) . . ? C76 N14 Co3 113.3(4) . . ? C72 N14 Co3 125.4(4) . . ? C77 N15 C79 111.0(5) . . ? C77 N15 Co3 108.7(4) . . ? C79 N15 Co3 138.2(4) . . ? C89 N16 C87 110.0(6) . . ? C89 N16 Co2 112.6(4) . . ? C87 N16 Co2 136.9(4) . . ? C94 N17 C90 119.5(6) . . ? C94 N17 Co2 125.2(5) . . ? C90 N17 Co2 115.2(4) . . ? O7 N18 C99 116.1(6) . . ? O7 N18 C95 121.5(6) . . ? C99 N18 C95 122.4(6) . . ? O6 N19 C100 116.9(6) . . ? O6 N19 C104 123.1(5) . . ? C100 N19 C104 119.9(6) . . ? C109 N20 C105 118.7(5) . . ? C109 N20 Co2 115.4(4) . . ? C105 N20 Co2 125.9(4) . . ? C110 N21 C112 111.3(5) . . ? C110 N21 Co2 111.9(4) . . ? C112 N21 Co2 136.4(4) . . ? C122 N22 C120 111.0(5) . . ? C122 N22 Co4 110.8(4) . . ? C120 N22 Co4 137.2(4) . . ? C123 N23 C127 118.8(6) . . ? C123 N23 Co4 116.7(4) . . ? C127 N23 Co4 124.3(5) . . ? O8 N24 C132 117.4(6) . . ? O8 N24 C128 121.2(6) . . ? C132 N24 C128 121.4(7) . . ? N1 O1 Co4 114.4(4) . . ? N6 O2 Co1 119.2(3) . . ? N7 O3 Co1 118.6(4) . . ? N12 O4 Co3 112.9(4) . . ? N13 O5 Co3 125.2(4) . . ? N19 O6 Co2 115.8(4) . . ? N18 O7 Co2 116.3(4) . . ? N24 O8 Co4 115.0(4) . . ? C15 O9 H9 109.5 . . ? C48 O10 H10 109.5 . . ? C81 O11 H11 109.5 . . ? C114 O12 H12 109.5 . . ? N1 C1 C2 120.3(7) . . ? N1 C1 H1 119.9 . . ? C2 C1 H1 119.9 . . ? C1 C2 C3 119.1(8) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 118.3(8) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 121.5(7) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? N1 C5 C4 118.6(6) . . ? N1 C5 C6 120.9(6) . . ? C4 C5 C6 120.4(6) . . ? N2 C6 C7 122.4(6) . . ? N2 C6 C5 117.9(6) . . ? C7 C6 C5 119.5(6) . . ? C8 C7 C6 118.6(6) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C9 C8 C7 120.0(7) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 119.1(6) . . ? C8 C9 H9A 120.4 . . ? C10 C9 H9A 120.4 . . ? N2 C10 C9 121.3(6) . . ? N2 C10 C11 113.0(6) . . ? C9 C10 C11 125.7(6) . . ? N3 C11 C10 121.0(6) . . ? N3 C11 S1 114.9(4) . . ? C10 C11 S1 123.9(5) . . ? C13 C12 S1 111.3(5) . . ? C13 C12 H12A 124.3 . . ? S1 C12 H12A 124.3 . . ? C12 C13 N3 114.0(6) . . ? C12 C13 C14 126.5(6) . . ? N3 C13 C14 119.4(6) . . ? C15 C14 C19 118.7(6) . . ? C15 C14 C13 120.6(6) . . ? C19 C14 C13 120.6(6) . . ? O9 C15 C14 119.1(6) . . ? O9 C15 C16 121.7(6) . . ? C14 C15 C16 119.1(6) . . ? C17 C16 C15 120.5(6) . . ? C17 C16 C21 120.6(6) . . ? C15 C16 C21 118.8(6) . . ? C16 C17 C18 120.7(6) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 118.6(6) . . ? C19 C18 C20 120.4(6) . . ? C17 C18 C20 120.9(6) . . ? C18 C19 C14 122.2(6) . . ? C18 C19 H19 118.9 . . ? C14 C19 H19 118.9 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N4 113.6(6) . . ? C22 C21 C16 124.8(6) . . ? N4 C21 C16 121.6(6) . . ? C21 C22 S2 111.3(5) . . ? C21 C22 H22 124.4 . . ? S2 C22 H22 124.4 . . ? N4 C23 C24 120.0(6) . . ? N4 C23 S2 115.7(5) . . ? C24 C23 S2 124.3(5) . . ? N5 C24 C25 124.2(6) . . ? N5 C24 C23 114.2(5) . . ? C25 C24 C23 121.6(6) . . ? C24 C25 C26 117.3(6) . . ? C24 C25 H25 121.3 . . ? C26 C25 H25 121.3 . . ? C27 C26 C25 118.8(6) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C26 C27 C28 119.2(6) . . ? C26 C27 H27 120.4 . . ? C28 C27 H27 120.4 . . ? N5 C28 C27 122.6(6) . . ? N5 C28 C29 118.5(6) . . ? C27 C28 C29 118.4(6) . . ? N6 C29 C30 117.6(6) . . ? N6 C29 C28 121.8(6) . . ? C30 C29 C28 120.6(6) . . ? C31 C30 C29 123.1(6) . . ? C31 C30 H30 118.5 . . ? C29 C30 H30 118.5 . . ? C30 C31 C32 117.1(7) . . ? C30 C31 H31 121.4 . . ? C32 C31 H31 121.4 . . ? C33 C32 C31 118.4(7) . . ? C33 C32 H32 120.8 . . ? C31 C32 H32 120.8 . . ? N6 C33 C32 122.8(7) . . ? N6 C33 H33 118.6 . . ? C32 C33 H33 118.6 . . ? N7 C34 C35 122.1(7) . . ? N7 C34 H34 118.9 . . ? C35 C34 H34 118.9 . . ? C34 C35 C36 118.6(7) . . ? C34 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? C35 C36 C37 118.7(7) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? C38 C37 C36 122.0(7) . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 119.0 . . ? N7 C38 C37 117.4(7) . . ? N7 C38 C39 122.0(6) . . ? C37 C38 C39 120.4(6) . . ? N8 C39 C40 121.5(6) . . ? N8 C39 C38 119.7(6) . . ? C40 C39 C38 118.5(6) . . ? C41 C40 C39 118.7(7) . . ? C41 C40 H40 120.7 . . ? C39 C40 H40 120.7 . . ? C40 C41 C42 120.5(6) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C43 C42 C41 116.8(7) . . ? C43 C42 H42 121.6 . . ? C41 C42 H42 121.6 . . ? N8 C43 C42 124.1(6) . . ? N8 C43 C44 113.4(5) . . ? C42 C43 C44 122.4(6) . . ? N9 C44 C43 120.4(6) . . ? N9 C44 S3 115.4(5) . . ? C43 C44 S3 124.1(5) . . ? C46 C45 S3 110.8(5) . . ? C46 C45 H45 124.6 . . ? S3 C45 H45 124.6 . . ? C45 C46 N9 113.7(6) . . ? C45 C46 C47 123.7(6) . . ? N9 C46 C47 122.5(6) . . ? C48 C47 C52 119.6(6) . . ? C48 C47 C46 122.2(6) . . ? C52 C47 C46 118.2(6) . . ? O10 C48 C47 118.0(6) . . ? O10 C48 C49 122.2(6) . . ? C47 C48 C49 119.8(6) . . ? C48 C49 C50 119.0(6) . . ? C48 C49 C54 120.7(6) . . ? C50 C49 C54 120.2(6) . . ? C51 C50 C49 122.1(6) . . ? C51 C50 H50 118.9 . . ? C49 C50 H50 118.9 . . ? C52 C51 C50 117.4(6) . . ? C52 C51 C53 120.6(6) . . ? C50 C51 C53 122.0(6) . . ? C51 C52 C47 121.9(6) . . ? C51 C52 H52 119.0 . . ? C47 C52 H52 119.0 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 N10 113.1(6) . . ? C55 C54 C49 125.7(6) . . ? N10 C54 C49 121.2(5) . . ? C54 C55 S4 111.4(5) . . ? C54 C55 H55 124.3 . . ? S4 C55 H55 124.3 . . ? N10 C56 C57 120.8(6) . . ? N10 C56 S4 114.5(5) . . ? C57 C56 S4 124.5(5) . . ? N11 C57 C58 123.6(6) . . ? N11 C57 C56 113.1(5) . . ? C58 C57 C56 123.2(6) . . ? C57 C58 C59 117.7(6) . . ? C57 C58 H58 121.1 . . ? C59 C58 H58 121.1 . . ? C60 C59 C58 118.7(7) . . ? C60 C59 H59 120.7 . . ? C58 C59 H59 120.7 . . ? C59 C60 C61 120.5(6) . . ? C59 C60 H60 119.8 . . ? C61 C60 H60 119.8 . . ? N11 C61 C60 121.4(6) . . ? N11 C61 C62 117.4(6) . . ? C60 C61 C62 120.9(6) . . ? N12 C62 C63 118.5(6) . . ? N12 C62 C61 120.6(6) . . ? C63 C62 C61 120.9(6) . . ? C64 C63 C62 121.3(7) . . ? C64 C63 H63 119.4 . . ? C62 C63 H63 119.4 . . ? C63 C64 C65 118.6(7) . . ? C63 C64 H64 120.7 . . ? C65 C64 H64 120.7 . . ? C66 C65 C64 119.5(7) . . ? C66 C65 H65 120.3 . . ? C64 C65 H65 120.3 . . ? N12 C66 C65 121.8(7) . . ? N12 C66 H66 119.1 . . ? C65 C66 H66 119.1 . . ? N13 C67 C68 120.8(8) . . ? N13 C67 H67 119.6 . . ? C68 C67 H67 119.6 . . ? C69 C68 C67 120.4(7) . . ? C69 C68 H68 119.8 . . ? C67 C68 H68 119.8 . . ? C68 C69 C70 119.4(7) . . ? C68 C69 H69 120.3 . . ? C70 C69 H69 120.3 . . ? C69 C70 C71 121.0(7) . . ? C69 C70 H70 119.5 . . ? C71 C70 H70 119.5 . . ? N13 C71 C70 117.0(6) . . ? N13 C71 C72 122.1(6) . . ? C70 C71 C72 120.8(6) . . ? N14 C72 C73 121.1(6) . . ? N14 C72 C71 120.7(6) . . ? C73 C72 C71 118.0(6) . . ? C72 C73 C74 119.5(7) . . ? C72 C73 H73 120.2 . . ? C74 C73 H73 120.2 . . ? C75 C74 C73 119.2(7) . . ? C75 C74 H74 120.4 . . ? C73 C74 H74 120.4 . . ? C74 C75 C76 118.1(7) . . ? C74 C75 H75 121.0 . . ? C76 C75 H75 121.0 . . ? N14 C76 C75 123.0(6) . . ? N14 C76 C77 114.4(5) . . ? C75 C76 C77 122.6(6) . . ? N15 C77 C76 121.6(6) . . ? N15 C77 S5 115.2(5) . . ? C76 C77 S5 122.8(5) . . ? C79 C78 S5 111.6(5) . . ? C79 C78 H78 124.2 . . ? S5 C78 H78 124.2 . . ? C78 C79 N15 113.2(6) . . ? C78 C79 C80 122.9(6) . . ? N15 C79 C80 123.7(5) . . ? C85 C80 C81 118.0(6) . . ? C85 C80 C79 119.6(6) . . ? C81 C80 C79 122.3(6) . . ? O11 C81 C82 121.8(6) . . ? O11 C81 C80 117.6(6) . . ? C82 C81 C80 120.6(6) . . ? C81 C82 C83 119.9(6) . . ? C81 C82 C87 120.3(6) . . ? C83 C82 C87 119.7(6) . . ? C82 C83 C84 120.9(6) . . ? C82 C83 H83 119.6 . . ? C84 C83 H83 119.6 . . ? C85 C84 C83 118.8(6) . . ? C85 C84 C86 121.6(6) . . ? C83 C84 C86 119.6(6) . . ? C84 C85 C80 121.8(6) . . ? C84 C85 H85 119.1 . . ? C80 C85 H85 119.1 . . ? C84 C86 H86A 109.5 . . ? C84 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C84 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C88 C87 N16 113.0(6) . . ? C88 C87 C82 125.6(6) . . ? N16 C87 C82 121.3(6) . . ? C87 C88 S6 112.6(5) . . ? C87 C88 H88 123.7 . . ? S6 C88 H88 123.7 . . ? N16 C89 C90 120.5(6) . . ? N16 C89 S6 115.5(5) . . ? C90 C89 S6 123.9(5) . . ? N17 C90 C91 122.4(6) . . ? N17 C90 C89 113.5(6) . . ? C91 C90 C89 124.1(7) . . ? C92 C91 C90 117.6(8) . . ? C92 C91 H91 121.2 . . ? C90 C91 H91 121.2 . . ? C93 C92 C91 121.1(7) . . ? C93 C92 H92 119.5 . . ? C91 C92 H92 119.5 . . ? C92 C93 C94 118.2(7) . . ? C92 C93 H93 120.9 . . ? C94 C93 H93 120.9 . . ? N17 C94 C93 121.1(7) . . ? N17 C94 C95 119.7(6) . . ? C93 C94 C95 119.0(7) . . ? N18 C95 C96 117.2(7) . . ? N18 C95 C94 120.9(6) . . ? C96 C95 C94 121.8(6) . . ? C95 C96 C97 121.7(7) . . ? C95 C96 H96 119.1 . . ? C97 C96 H96 119.1 . . ? C98 C97 C96 119.5(8) . . ? C98 C97 H97 120.3 . . ? C96 C97 H97 120.3 . . ? C97 C98 C99 120.0(8) . . ? C97 C98 H98 120.0 . . ? C99 C98 H98 120.0 . . ? N18 C99 C98 119.2(7) . . ? N18 C99 H99 120.4 . . ? C98 C99 H99 120.4 . . ? N19 C100 C101 121.1(7) . . ? N19 C100 H100 119.4 . . ? C101 C100 H100 119.4 . . ? C102 C101 C100 119.0(8) . . ? C102 C101 H101 120.5 . . ? C100 C101 H101 120.5 . . ? C101 C102 C103 119.7(7) . . ? C101 C102 H102 120.1 . . ? C103 C102 H102 120.1 . . ? C104 C103 C102 120.2(7) . . ? C104 C103 H103 119.9 . . ? C102 C103 H103 119.9 . . ? C103 C104 N19 119.9(6) . . ? C103 C104 C105 120.7(6) . . ? N19 C104 C105 119.4(6) . . ? N20 C105 C106 121.8(6) . . ? N20 C105 C104 118.7(6) . . ? C106 C105 C104 119.3(6) . . ? C107 C106 C105 119.0(7) . . ? C107 C106 H106 120.5 . . ? C105 C106 H106 120.5 . . ? C106 C107 C108 120.1(6) . . ? C106 C107 H107 119.9 . . ? C108 C107 H107 119.9 . . ? C107 C108 C109 117.9(6) . . ? C107 C108 H108 121.1 . . ? C109 C108 H108 121.1 . . ? N20 C109 C108 122.2(6) . . ? N20 C109 C110 113.9(5) . . ? C108 C109 C110 124.0(6) . . ? N21 C110 C109 120.7(6) . . ? N21 C110 S7 114.5(5) . . ? C109 C110 S7 124.7(5) . . ? C112 C111 S7 112.5(5) . . ? C112 C111 H111 123.8 . . ? S7 C111 H111 123.8 . . ? C111 C112 N21 112.7(6) . . ? C111 C112 C113 124.5(6) . . ? N21 C112 C113 122.7(5) . . ? C118 C113 C114 119.3(6) . . ? C118 C113 C112 120.2(6) . . ? C114 C113 C112 120.4(6) . . ? O12 C114 C113 119.6(5) . . ? O12 C114 C115 120.6(6) . . ? C113 C114 C115 119.9(6) . . ? C116 C115 C114 119.4(6) . . ? C116 C115 C120 120.6(6) . . ? C114 C115 C120 119.9(6) . . ? C117 C116 C115 121.6(6) . . ? C117 C116 H116 119.2 . . ? C115 C116 H116 119.2 . . ? C116 C117 C118 118.0(6) . . ? C116 C117 C119 121.4(6) . . ? C118 C117 C119 120.6(7) . . ? C113 C118 C117 121.8(7) . . ? C113 C118 H118 119.1 . . ? C117 C118 H118 119.1 . . ? C117 C119 H11A 109.5 . . ? C117 C119 H11B 109.5 . . ? H11A C119 H11B 109.5 . . ? C117 C119 H11C 109.5 . . ? H11A C119 H11C 109.5 . . ? H11B C119 H11C 109.5 . . ? C121 C120 N22 114.5(6) . . ? C121 C120 C115 124.3(6) . . ? N22 C120 C115 121.1(6) . . ? C120 C121 S8 110.4(5) . . ? C120 C121 H121 124.8 . . ? S8 C121 H121 124.8 . . ? N22 C122 C123 121.3(6) . . ? N22 C122 S8 114.2(5) . . ? C123 C122 S8 124.4(5) . . ? N23 C123 C124 123.4(6) . . ? N23 C123 C122 113.7(6) . . ? C124 C123 C122 122.8(6) . . ? C125 C124 C123 117.7(7) . . ? C125 C124 H124 121.2 . . ? C123 C124 H124 121.2 . . ? C126 C125 C124 119.3(7) . . ? C126 C125 H125 120.4 . . ? C124 C125 H125 120.4 . . ? C125 C126 C127 119.6(7) . . ? C125 C126 H126 120.2 . . ? C127 C126 H126 120.2 . . ? N23 C127 C126 120.9(7) . . ? N23 C127 C128 119.1(6) . . ? C126 C127 C128 120.0(7) . . ? N24 C128 C129 119.0(7) . . ? N24 C128 C127 120.3(6) . . ? C129 C128 C127 120.6(7) . . ? C130 C129 C128 119.7(9) . . ? C130 C129 H129 120.2 . . ? C128 C129 H129 120.2 . . ? C129 C130 C131 120.2(8) . . ? C129 C130 H130 119.9 . . ? C131 C130 H130 119.9 . . ? C132 C131 C130 117.8(8) . . ? C132 C131 H131 121.1 . . ? C130 C131 H131 121.1 . . ? N24 C132 C131 121.6(8) . . ? N24 C132 H132 119.2 . . ? C131 C132 H132 119.2 . . ? Cl21 C133 Cl22 112.5(5) . . ? Cl21 C133 H13A 109.1 . . ? Cl22 C133 H13A 109.1 . . ? Cl21 C133 H13B 109.1 . . ? Cl22 C133 H13B 109.1 . . ? H13A C133 H13B 107.8 . . ? Cl4 C2S1 Cl3 109.6 . . ? Cl4 C2S1 H2SA 109.8 . . ? Cl3 C2S1 H2SA 109.8 . . ? Cl4 C2S1 H2SB 109.8 . . ? Cl3 C2S1 H2SB 109.8 . . ? H2SA C2S1 H2SB 108.2 . . ? Cl4 C2S2 Cl3 109.8 . . ? Cl4 C2S2 H2SC 109.7 . . ? Cl3 C2S2 H2SC 109.7 . . ? Cl4 C2S2 H2SD 109.7 . . ? Cl3 C2S2 H2SD 109.7 . . ? H2SC C2S2 H2SD 108.2 . . ? C2S2 Cl3 C2S1 57.4 . . ? C2S2 Cl4 C2S1 57.5 . . ? Cl6 C3S Cl5 109.6(5) . . ? Cl6 C3S H3S1 109.8 . . ? Cl5 C3S H3S1 109.8 . . ? Cl6 C3S H3S2 109.8 . . ? Cl5 C3S H3S2 109.8 . . ? H3S1 C3S H3S2 108.2 . . ? Cl7 C4S Cl8 114.1(8) . . ? Cl7 C4S H4S1 108.7 . . ? Cl8 C4S H4S1 108.7 . . ? Cl7 C4S H4S2 108.7 . . ? Cl8 C4S H4S2 108.7 . . ? H4S1 C4S H4S2 107.6 . . ? Cl9 C5S Cl10 117.8(7) . . ? Cl9 C5S H5S1 107.8 . . ? Cl10 C5S H5S1 107.8 . . ? Cl9 C5S H5S2 107.8 . . ? Cl10 C5S H5S2 107.8 . . ? H5S1 C5S H5S2 107.2 . . ? Cl13 C7S Cl14 111.2(6) . . ? Cl13 C7S H7S1 109.4 . . ? Cl14 C7S H7S1 109.4 . . ? Cl13 C7S H7S2 109.4 . . ? Cl14 C7S H7S2 109.4 . . ? H7S1 C7S H7S2 108.0 . . ? Cl18 C9S Cl17 109.2(5) . . ? Cl18 C9S H9S1 109.8 . . ? Cl17 C9S H9S1 109.8 . . ? Cl18 C9S H9S2 109.8 . . ? Cl17 C9S H9S2 109.8 . . ? H9S1 C9S H9S2 108.3 . . ? Cl20 C10S Cl19 108.0(8) . . ? Cl20 C10S H10A 110.1 . . ? Cl19 C10S H10A 110.1 . . ? Cl20 C10S H10B 110.1 . . ? Cl19 C10S H10B 110.1 . . ? H10A C10S H10B 108.4 . . ? N25 C11S H11D 109.5 . . ? N25 C11S H11E 109.5 . . ? H11D C11S H11E 109.5 . . ? N25 C11S H11F 109.5 . . ? H11D C11S H11F 109.5 . . ? H11E C11S H11F 109.5 . . ? O14 N25 O13 124.0(7) . . ? O14 N25 C11S 117.9(7) . . ? O13 N25 C11S 118.1(7) . . ? H1O1 O1W H2O1 107.7 . . ? H1O2 O2W H2O2 107.7 . . ? H1O3 O3W H2O3 107.7 . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 2.617 _refine_diff_density_min -1.162 _refine_diff_density_rms 0.138 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.492 0.190 0.757 215 67 ' ' 2 0.508 0.810 0.243 215 67 ' ' 3 0.482 0.879 0.584 17 5 ' ' 4 0.518 0.121 0.416 17 5 ' ' data_cu2lph2 _database_code_depnum_ccdc_archive 'CCDC 918503' #TrackingRef 'Cu2LPh2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55.38 H37.83 Cl4.60 Cu2 N11.08 O20.16 S4' _chemical_formula_weight 1599.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0799(12) _cell_length_b 14.7340(15) _cell_length_c 17.2067(17) _cell_angle_alpha 95.609(2) _cell_angle_beta 94.864(2) _cell_angle_gamma 90.453(2) _cell_volume 3036.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4466 _cell_measurement_theta_min 2.332 _cell_measurement_theta_max 23.332 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1618.7 _exptl_absorpt_coefficient_mu 1.129 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4299 _exptl_absorpt_correction_T_max 0.8955 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 52841 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.88 _reflns_number_total 14250 _reflns_number_gt 11126 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0488P)^2^+7.7009P] 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 14250 _refine_ls_number_parameters 978 _refine_ls_number_restraints 135 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O6 O 0.3882(2) 0.57338(17) 0.20125(13) 0.0298(5) Uani 1 1 d . . . O7 O 1.1504(2) 0.67978(17) 0.08818(13) 0.0287(5) Uani 1 1 d . . . Cu1 Cu 0.99390(3) 0.76194(2) 0.169195(19) 0.01526(8) Uani 1 1 d . . . Cu2 Cu 0.57690(3) 0.66308(2) 0.27332(2) 0.01852(9) Uani 1 1 d . . . S1 S 0.98533(8) 0.98868(6) 0.37526(5) 0.0339(2) Uani 1 1 d . . . S2 S 0.67885(8) 0.88458(6) 0.47479(5) 0.03181(19) Uani 1 1 d . . . S3 S 0.90807(7) 0.48196(5) 0.07495(4) 0.02069(15) Uani 1 1 d . . . S4 S 0.61806(7) 0.55685(5) 0.03149(4) 0.02325(16) Uani 1 1 d . . . N1 N 0.5752(2) 0.5897(2) 0.41955(15) 0.0263(6) Uani 1 1 d . . . N2 N 0.6314(2) 0.53628(17) 0.26104(15) 0.0223(5) Uani 1 1 d . . . N3 N 0.6125(2) 0.65773(17) 0.15999(14) 0.0182(5) Uani 1 1 d . . . N4 N 0.9138(2) 0.86815(17) 0.26536(14) 0.0192(5) Uani 1 1 d . . . N5 N 1.0984(2) 0.76103(17) 0.26553(14) 0.0190(5) Uani 1 1 d . . . N6 N 0.9833(2) 0.93413(16) 0.11187(14) 0.0188(5) Uani 1 1 d . . . N7 N 0.9160(2) 0.74892(16) 0.06126(13) 0.0154(5) Uani 1 1 d . . . N8 N 0.9399(2) 0.62978(16) 0.16455(13) 0.0156(5) Uani 1 1 d . . . N9 N 0.6946(2) 0.75664(17) 0.36534(14) 0.0190(5) Uani 1 1 d . . . N10 N 0.4972(2) 0.78082(18) 0.28030(14) 0.0200(5) Uani 1 1 d . . . O1 O 0.50897(17) 0.62834(15) 0.36612(12) 0.0220(4) Uani 1 1 d . . . O2 O 1.05722(17) 0.87545(14) 0.13977(12) 0.0199(4) Uani 1 1 d . . . C1 C 0.5689(3) 0.6253(3) 0.4946(2) 0.0401(10) Uani 1 1 d . . . H1 H 0.5233 0.6765 0.5057 0.048 Uiso 1 1 calc R . . C2 C 0.6287(4) 0.5873(4) 0.5552(2) 0.0623(16) Uani 1 1 d . . . H2 H 0.6246 0.6121 0.6079 0.075 Uiso 1 1 calc R . . C3 C 0.6942(4) 0.5132(4) 0.5381(3) 0.0593(15) Uani 1 1 d . . . H3 H 0.7346 0.4857 0.5791 0.071 Uiso 1 1 calc R . . C4 C 0.7010(3) 0.4791(3) 0.4610(2) 0.0455(11) Uani 1 1 d . . . H4 H 0.7476 0.4289 0.4491 0.055 Uiso 1 1 calc R . . C5 C 0.6402(3) 0.5175(3) 0.4005(2) 0.0314(8) Uani 1 1 d . . . C6 C 0.6455(3) 0.4802(2) 0.3180(2) 0.0320(8) Uani 1 1 d . . . C7 C 0.6675(4) 0.3883(3) 0.2993(3) 0.0513(12) Uani 1 1 d . . . H7 H 0.6787 0.3489 0.3397 0.062 Uiso 1 1 calc R . . C8 C 0.6731(5) 0.3544(3) 0.2220(3) 0.0599(15) Uani 1 1 d . . . H8 H 0.6881 0.2918 0.2091 0.072 Uiso 1 1 calc R . . C9 C 0.6568(4) 0.4118(2) 0.1636(3) 0.0439(11) Uani 1 1 d . . . H9 H 0.6598 0.3897 0.1101 0.053 Uiso 1 1 calc R . . C10 C 0.6359(3) 0.5021(2) 0.1852(2) 0.0265(7) Uani 1 1 d . . . C11 C 0.6039(3) 0.6715(2) 0.02790(17) 0.0215(6) Uani 1 1 d . . . H11 H 0.5964 0.7007 -0.0191 0.026 Uiso 1 1 calc R . . C12 C 0.6047(2) 0.7157(2) 0.10131(16) 0.0179(6) Uani 1 1 d . . . C13 C 0.6212(2) 0.8138(2) 0.12519(16) 0.0182(6) Uani 1 1 d . . . C14 C 0.5589(3) 0.8842(2) 0.09609(19) 0.0255(7) Uani 1 1 d . . . H14 H 0.4996 0.8714 0.0565 0.031 Uiso 1 1 calc R . . C15 C 0.5851(3) 0.9733(2) 0.1261(2) 0.0300(7) Uani 1 1 d . . . H15 H 0.5419 1.0215 0.1074 0.036 Uiso 1 1 calc R . . C16 C 0.6730(3) 0.9939(2) 0.1829(2) 0.0265(7) Uani 1 1 d . . . H16 H 0.6889 1.0555 0.2030 0.032 Uiso 1 1 calc R . . C17 C 0.7379(2) 0.9235(2) 0.21041(17) 0.0197(6) Uani 1 1 d . . . C18 C 0.7100(2) 0.8347(2) 0.18135(16) 0.0182(6) Uani 1 1 d . . . H18 H 0.7528 0.7864 0.2003 0.022 Uiso 1 1 calc R . . C19 C 0.8363(3) 0.9366(2) 0.26763(17) 0.0211(6) Uani 1 1 d . . . C20 C 0.8621(3) 1.0074(2) 0.3235(2) 0.0296(7) Uani 1 1 d . . . H20 H 0.8178 1.0597 0.3324 0.036 Uiso 1 1 calc R . . C21 C 0.9963(3) 0.8864(2) 0.31938(17) 0.0229(6) Uani 1 1 d . . . C22 C 1.0894(3) 0.8240(2) 0.32771(17) 0.0238(6) Uani 1 1 d . . . C23 C 1.1630(3) 0.8257(3) 0.39447(19) 0.0318(8) Uani 1 1 d . . . H23 H 1.1569 0.8711 0.4371 0.038 Uiso 1 1 calc R . . C24 C 1.2453(3) 0.7612(3) 0.39865(19) 0.0333(8) Uani 1 1 d . . . H24 H 1.2958 0.7615 0.4441 0.040 Uiso 1 1 calc R . . C25 C 1.2529(3) 0.6964(2) 0.33581(19) 0.0271(7) Uani 1 1 d . . . H25 H 1.3084 0.6511 0.3375 0.032 Uiso 1 1 calc R . . C26 C 1.1783(3) 0.6985(2) 0.27016(18) 0.0217(6) Uani 1 1 d . . . H26 H 1.1839 0.6540 0.2269 0.026 Uiso 1 1 calc R . . C27 C 0.9882(3) 1.0205(2) 0.14761(18) 0.0237(6) Uani 1 1 d . . . H27 H 1.0390 1.0355 0.1924 0.028 Uiso 1 1 calc R . . C28 C 0.9201(3) 1.0866(2) 0.1196(2) 0.0280(7) Uani 1 1 d . . . H28 H 0.9239 1.1469 0.1451 0.034 Uiso 1 1 calc R . . C29 C 0.8464(3) 1.0654(2) 0.0545(2) 0.0290(7) Uani 1 1 d . . . H29 H 0.8001 1.1108 0.0342 0.035 Uiso 1 1 calc R . . C30 C 0.8410(3) 0.9770(2) 0.01951(19) 0.0245(6) Uani 1 1 d . . . H30 H 0.7899 0.9614 -0.0250 0.029 Uiso 1 1 calc R . . C31 C 0.9094(3) 0.9105(2) 0.04850(17) 0.0192(6) Uani 1 1 d . . . C32 C 0.9007(2) 0.81518(19) 0.01359(16) 0.0175(5) Uani 1 1 d . . . C33 C 0.8708(3) 0.7944(2) -0.06669(17) 0.0212(6) Uani 1 1 d . . . H33 H 0.8619 0.8419 -0.1001 0.025 Uiso 1 1 calc R . . C34 C 0.8544(3) 0.7049(2) -0.09694(17) 0.0209(6) Uani 1 1 d . . . H34 H 0.8352 0.6902 -0.1514 0.025 Uiso 1 1 calc R . . C35 C 0.8662(2) 0.6366(2) -0.04737(16) 0.0188(6) Uani 1 1 d . . . H35 H 0.8520 0.5745 -0.0665 0.023 Uiso 1 1 calc R . . C36 C 0.8994(2) 0.66109(19) 0.03100(16) 0.0160(5) Uani 1 1 d . . . C37 C 0.9168(2) 0.59750(19) 0.09037(16) 0.0159(5) Uani 1 1 d . . . C38 C 0.9365(3) 0.4753(2) 0.17349(18) 0.0223(6) Uani 1 1 d . . . H38 H 0.9429 0.4199 0.1973 0.027 Uiso 1 1 calc R . . C39 C 0.9485(2) 0.55947(19) 0.21288(16) 0.0170(5) Uani 1 1 d . . . C40 C 0.9504(2) 0.5845(2) 0.29795(17) 0.0190(6) Uani 1 1 d . . . C41 C 1.0200(3) 0.5455(2) 0.35394(18) 0.0241(6) Uani 1 1 d . . . H41 H 1.0701 0.4989 0.3388 0.029 Uiso 1 1 calc R . . C42 C 1.0143(3) 0.5765(2) 0.43241(19) 0.0284(7) Uani 1 1 d . . . H42 H 1.0624 0.5511 0.4710 0.034 Uiso 1 1 calc R . . C43 C 0.9407(3) 0.6432(2) 0.45615(17) 0.0251(7) Uani 1 1 d . . . H43 H 0.9391 0.6636 0.5102 0.030 Uiso 1 1 calc R . . C44 C 0.8683(2) 0.6805(2) 0.39971(16) 0.0192(6) Uani 1 1 d . . . C45 C 0.8758(2) 0.6507(2) 0.32104(16) 0.0190(6) Uani 1 1 d . . . H45 H 0.8286 0.6764 0.2822 0.023 Uiso 1 1 calc R . . C46 C 0.7861(3) 0.7500(2) 0.41819(16) 0.0207(6) Uani 1 1 d . . . C47 C 0.7899(3) 0.8139(2) 0.48149(18) 0.0278(7) Uani 1 1 d . . . H47 H 0.8466 0.8185 0.5235 0.033 Uiso 1 1 calc R . . C48 C 0.6309(3) 0.8243(2) 0.38766(17) 0.0222(6) Uani 1 1 d . . . C49 C 0.5290(3) 0.8449(2) 0.34024(17) 0.0215(6) Uani 1 1 d . . . C50 C 0.4713(3) 0.9251(2) 0.35269(19) 0.0280(7) Uani 1 1 d . . . H50 H 0.4932 0.9683 0.3960 0.034 Uiso 1 1 calc R . . C51 C 0.3810(3) 0.9414(2) 0.3010(2) 0.0304(7) Uani 1 1 d . . . H51 H 0.3411 0.9964 0.3081 0.037 Uiso 1 1 calc R . . C52 C 0.3494(3) 0.8771(2) 0.23906(19) 0.0279(7) Uani 1 1 d . . . H52 H 0.2879 0.8871 0.2029 0.033 Uiso 1 1 calc R . . C53 C 0.4095(3) 0.7975(2) 0.23083(17) 0.0228(6) Uani 1 1 d . . . H53 H 0.3877 0.7529 0.1885 0.027 Uiso 1 1 calc R . . C54 C 0.6215(3) 0.5720(2) 0.13098(17) 0.0209(6) Uani 1 1 d . . . Cl1 Cl 0.34361(7) 0.48309(6) 0.20404(4) 0.02877(18) Uani 1 1 d . . . Cl2 Cl 1.22412(6) 0.70834(5) 0.03287(4) 0.01919(14) Uani 1 1 d . . . Cl3 Cl 0.60410(9) 0.16576(6) 0.39557(6) 0.0392(2) Uani 1 1 d U . . O3 O 0.3912(3) 0.4460(2) 0.27291(15) 0.0634(11) Uani 1 1 d . . . O4 O 0.2240(2) 0.4875(2) 0.20400(19) 0.0525(9) Uani 1 1 d . . . O5 O 0.3714(2) 0.42491(18) 0.13635(13) 0.0336(6) Uani 1 1 d . . . O8 O 1.3073(2) 0.64039(17) 0.02193(14) 0.0331(6) Uani 1 1 d . . . O9 O 1.1599(2) 0.71774(16) -0.04066(13) 0.0324(6) Uani 1 1 d . . . O10 O 1.2755(2) 0.79413(16) 0.06192(14) 0.0318(5) Uani 1 1 d . . . O12 O 0.6162(4) 0.25588(19) 0.43068(17) 0.0619(10) Uani 1 1 d U A . O13 O 0.6577(5) 0.1035(3) 0.4377(2) 0.0849(14) Uani 1 1 d U A . O16 O 1.0049(3) 0.21040(19) 0.37089(15) 0.0441(7) Uani 1 1 d U . . O18 O 0.9683(4) 0.2838(3) 0.2553(2) 0.0804(12) Uani 1 1 d U . . O11 O 0.6505(5) 0.1667(3) 0.3214(2) 0.0699(18) Uani 0.791(7) 1 d PU A 1 O14' O 0.4883(4) 0.1495(4) 0.3830(5) 0.122(3) Uani 0.791(7) 1 d PU A 1 O11' O 0.5995(13) 0.1115(11) 0.3328(8) 0.043(4) Uani 0.209(7) 1 d PU A 2 O14 O 0.571(2) 0.1066(10) 0.4672(8) 0.068(4) Uani 0.209(7) 1 d PU A 2 Cl4 Cl 1.04887(13) 0.24741(9) 0.30400(7) 0.0338(4) Uani 0.622(2) 1 d PU B 1 O15 O 1.1231(5) 0.3207(3) 0.3319(3) 0.0594(15) Uani 0.622(2) 1 d PU B 1 O17 O 1.1054(5) 0.1763(3) 0.2598(3) 0.0441(12) Uani 0.622(2) 1 d PU B 1 Cl4A Cl 0.9390(2) 0.26942(16) 0.32685(16) 0.0396(7) Uani 0.378(2) 1 d PU B 2 O15A O 0.8955(8) 0.3412(6) 0.3754(5) 0.062(3) Uani 0.378(2) 1 d PU B 2 O17A O 0.8485(8) 0.2173(6) 0.2848(5) 0.063(2) Uani 0.378(2) 1 d PU B 2 N1SA N 1.2123(7) 0.1626(6) 0.3022(5) 0.037(2) Uani 0.378(2) 1 d P B 2 O1SA O 1.2170(7) 0.1042(5) 0.3478(4) 0.0428(18) Uani 0.378(2) 1 d P B 2 C1SA C 1.2586(10) 0.2527(8) 0.3271(7) 0.046(3) Uani 0.378(2) 1 d P B 2 H1S1 H 1.3356 0.2557 0.3134 0.069 Uiso 0.378(2) 1 calc PR B 2 H1S2 H 1.2570 0.2652 0.3840 0.069 Uiso 0.378(2) 1 calc PR B 2 H1S3 H 1.2146 0.2982 0.3008 0.069 Uiso 0.378(2) 1 calc PR B 2 O2SA O 1.1731(11) 0.1467(9) 0.2352(5) 0.081(4) Uani 0.378(2) 1 d P B 2 Cl1S Cl 0.3771(9) 0.1534(12) 0.1378(14) 0.072(5) Uani 0.298(3) 1 d P C 1 Cl2S Cl 0.5926(3) 0.20417(19) 0.09481(15) 0.0320(9) Uani 0.298(3) 1 d P C 1 C1S C 0.5022(11) 0.2104(9) 0.1704(7) 0.036(3) Uani 0.298(3) 1 d P C 1 H1S4 H 0.5375 0.1825 0.2162 0.043 Uiso 0.298(3) 1 calc PR C 1 H1S5 H 0.4875 0.2751 0.1872 0.043 Uiso 0.298(3) 1 calc PR C 1 C2S C 0.3781(7) 0.2208(5) 0.2342(4) 0.0573(19) Uani 0.702(3) 1 d P C 2 H2S1 H 0.4425 0.2080 0.2699 0.086 Uiso 0.702(3) 1 calc PR C 2 H2S2 H 0.3097 0.2109 0.2593 0.086 Uiso 0.702(3) 1 calc PR C 2 H2S3 H 0.3823 0.2843 0.2221 0.086 Uiso 0.702(3) 1 calc PR C 2 O2S O 0.4288(9) 0.1794(4) 0.1124(4) 0.083(3) Uani 0.702(3) 1 d P C 2 N1S N 0.3780(15) 0.1571(13) 0.1585(14) 0.057(5) Uani 0.702(3) 1 d P C 2 O1S O 0.3231(5) 0.0860(4) 0.1630(3) 0.0672(16) Uani 0.702(3) 1 d P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O6 0.0261(13) 0.0395(14) 0.0233(11) 0.0020(10) 0.0007(9) -0.0103(10) O7 0.0245(13) 0.0383(13) 0.0259(11) 0.0103(10) 0.0078(9) 0.0053(10) Cu1 0.01452(17) 0.01651(17) 0.01420(16) 0.00009(12) -0.00025(12) -0.00111(13) Cu2 0.01745(19) 0.02335(19) 0.01613(17) 0.00547(13) 0.00512(13) 0.00410(14) S1 0.0291(5) 0.0381(5) 0.0301(4) -0.0176(4) 0.0008(3) -0.0022(4) S2 0.0354(5) 0.0388(5) 0.0193(4) -0.0064(3) 0.0008(3) 0.0101(4) S3 0.0252(4) 0.0160(3) 0.0207(3) -0.0006(3) 0.0037(3) 0.0005(3) S4 0.0197(4) 0.0264(4) 0.0226(4) -0.0044(3) 0.0038(3) -0.0036(3) N1 0.0154(13) 0.0453(17) 0.0219(13) 0.0184(12) 0.0050(10) 0.0054(11) N2 0.0196(13) 0.0231(13) 0.0269(13) 0.0094(10) 0.0100(10) 0.0025(10) N3 0.0151(12) 0.0221(12) 0.0181(11) 0.0035(9) 0.0046(9) -0.0007(9) N4 0.0173(13) 0.0218(12) 0.0182(11) -0.0016(9) 0.0041(9) -0.0034(10) N5 0.0166(12) 0.0241(13) 0.0158(11) 0.0006(9) 0.0008(9) -0.0035(10) N6 0.0177(13) 0.0171(12) 0.0226(12) 0.0031(9) 0.0071(10) 0.0003(9) N7 0.0132(12) 0.0174(11) 0.0157(11) 0.0001(9) 0.0035(9) 0.0001(9) N8 0.0124(12) 0.0194(12) 0.0151(11) 0.0021(9) 0.0006(9) 0.0015(9) N9 0.0150(12) 0.0273(13) 0.0156(11) 0.0048(10) 0.0038(9) 0.0018(10) N10 0.0187(13) 0.0271(13) 0.0155(11) 0.0050(10) 0.0054(9) 0.0048(10) O1 0.0139(10) 0.0359(12) 0.0180(10) 0.0100(9) 0.0024(8) 0.0035(9) O2 0.0178(11) 0.0186(10) 0.0231(10) 0.0018(8) 0.0015(8) -0.0009(8) C1 0.0232(19) 0.080(3) 0.0213(16) 0.0192(17) 0.0094(13) 0.0137(18) C2 0.034(2) 0.135(5) 0.0256(19) 0.037(2) 0.0093(16) 0.023(3) C3 0.028(2) 0.112(4) 0.049(2) 0.058(3) 0.0080(18) 0.019(2) C4 0.025(2) 0.070(3) 0.051(2) 0.042(2) 0.0110(17) 0.0126(18) C5 0.0228(17) 0.042(2) 0.0348(18) 0.0243(16) 0.0100(14) 0.0050(14) C6 0.0297(19) 0.0315(18) 0.0402(19) 0.0186(15) 0.0166(15) 0.0078(14) C7 0.065(3) 0.037(2) 0.062(3) 0.029(2) 0.034(2) 0.020(2) C8 0.089(4) 0.027(2) 0.075(3) 0.021(2) 0.055(3) 0.020(2) C9 0.061(3) 0.0245(18) 0.053(2) 0.0068(16) 0.038(2) 0.0076(17) C10 0.0258(17) 0.0250(16) 0.0310(16) 0.0055(13) 0.0136(13) 0.0003(13) C11 0.0172(15) 0.0277(16) 0.0194(14) 0.0022(12) 0.0009(11) -0.0004(12) C12 0.0113(13) 0.0240(14) 0.0186(13) 0.0031(11) 0.0025(10) -0.0006(11) C13 0.0156(14) 0.0228(14) 0.0174(13) 0.0033(11) 0.0056(10) 0.0003(11) C14 0.0212(16) 0.0325(17) 0.0242(15) 0.0083(13) 0.0032(12) 0.0033(13) C15 0.0234(17) 0.0293(17) 0.0397(19) 0.0112(14) 0.0065(14) 0.0066(13) C16 0.0257(17) 0.0207(15) 0.0346(17) 0.0014(13) 0.0128(13) 0.0029(12) C17 0.0161(14) 0.0243(15) 0.0198(13) 0.0006(11) 0.0093(11) -0.0002(11) C18 0.0177(14) 0.0217(14) 0.0164(13) 0.0039(11) 0.0056(11) 0.0019(11) C19 0.0179(15) 0.0228(15) 0.0230(14) -0.0021(11) 0.0091(11) -0.0022(11) C20 0.0258(18) 0.0308(17) 0.0304(17) -0.0098(14) 0.0060(13) 0.0009(13) C21 0.0216(16) 0.0305(16) 0.0154(13) -0.0052(12) 0.0045(11) -0.0037(12) C22 0.0199(16) 0.0323(17) 0.0176(14) -0.0045(12) 0.0014(11) -0.0067(13) C23 0.0254(18) 0.047(2) 0.0208(15) -0.0042(14) -0.0010(13) -0.0042(15) C24 0.0262(18) 0.053(2) 0.0197(15) 0.0057(15) -0.0067(13) -0.0066(16) C25 0.0181(16) 0.0365(18) 0.0275(16) 0.0106(14) -0.0014(12) -0.0025(13) C26 0.0169(15) 0.0271(15) 0.0218(14) 0.0060(12) 0.0015(11) -0.0020(12) C27 0.0259(17) 0.0223(15) 0.0233(15) -0.0007(12) 0.0090(12) -0.0047(12) C28 0.0325(19) 0.0188(15) 0.0349(17) 0.0023(13) 0.0158(14) -0.0002(13) C29 0.0312(19) 0.0238(16) 0.0344(17) 0.0085(13) 0.0108(14) 0.0041(13) C30 0.0260(17) 0.0231(15) 0.0263(15) 0.0082(12) 0.0067(12) 0.0013(12) C31 0.0186(15) 0.0200(14) 0.0201(13) 0.0035(11) 0.0058(11) 0.0010(11) C32 0.0141(14) 0.0199(14) 0.0191(13) 0.0027(11) 0.0046(10) 0.0006(10) C33 0.0194(15) 0.0255(15) 0.0195(14) 0.0058(11) 0.0017(11) -0.0003(12) C34 0.0181(15) 0.0295(16) 0.0147(13) 0.0012(11) 0.0009(11) 0.0013(12) C35 0.0170(14) 0.0227(14) 0.0158(13) -0.0017(11) 0.0005(10) -0.0003(11) C36 0.0126(13) 0.0199(13) 0.0151(12) -0.0006(10) 0.0019(10) 0.0000(10) C37 0.0119(13) 0.0172(13) 0.0184(13) 0.0004(10) 0.0016(10) 0.0008(10) C38 0.0222(16) 0.0226(15) 0.0235(14) 0.0071(12) 0.0044(12) 0.0038(12) C39 0.0117(13) 0.0212(14) 0.0191(13) 0.0071(11) 0.0007(10) 0.0016(10) C40 0.0159(14) 0.0219(14) 0.0199(13) 0.0063(11) 0.0001(11) -0.0005(11) C41 0.0200(16) 0.0287(16) 0.0246(15) 0.0097(12) -0.0002(12) 0.0060(12) C42 0.0235(17) 0.0408(19) 0.0220(15) 0.0133(13) -0.0036(12) 0.0068(14) C43 0.0246(17) 0.0367(18) 0.0145(13) 0.0078(12) -0.0022(11) 0.0010(13) C44 0.0168(14) 0.0250(15) 0.0165(13) 0.0065(11) 0.0002(11) -0.0006(11) C45 0.0178(15) 0.0242(14) 0.0155(13) 0.0069(11) -0.0011(10) 0.0006(11) C46 0.0198(15) 0.0294(16) 0.0136(12) 0.0050(11) 0.0020(11) 0.0004(12) C47 0.0258(17) 0.0395(19) 0.0171(14) -0.0010(13) 0.0008(12) 0.0031(14) C48 0.0230(16) 0.0283(16) 0.0160(13) 0.0017(11) 0.0064(11) 0.0013(12) C49 0.0213(16) 0.0275(15) 0.0166(13) 0.0032(11) 0.0060(11) 0.0039(12) C50 0.0298(18) 0.0300(17) 0.0256(16) 0.0036(13) 0.0087(13) 0.0064(14) C51 0.0301(19) 0.0309(17) 0.0328(17) 0.0096(14) 0.0089(14) 0.0128(14) C52 0.0221(17) 0.0369(18) 0.0269(16) 0.0114(14) 0.0048(13) 0.0071(13) C53 0.0201(16) 0.0319(17) 0.0181(13) 0.0080(12) 0.0041(11) 0.0021(12) C54 0.0180(15) 0.0236(15) 0.0218(14) 0.0017(11) 0.0066(11) -0.0012(11) Cl1 0.0275(4) 0.0438(5) 0.0138(3) -0.0024(3) 0.0021(3) -0.0154(3) Cl2 0.0214(4) 0.0220(3) 0.0140(3) 0.0020(2) 0.0005(2) 0.0024(3) Cl3 0.0454(6) 0.0324(4) 0.0387(5) -0.0106(4) 0.0133(4) 0.0008(4) O3 0.093(3) 0.074(2) 0.0220(13) 0.0247(14) -0.0215(14) -0.053(2) O4 0.0291(15) 0.0630(19) 0.0608(19) -0.0293(15) 0.0201(13) -0.0222(14) O5 0.0337(14) 0.0448(15) 0.0209(11) -0.0037(10) 0.0022(10) 0.0032(11) O8 0.0368(15) 0.0336(13) 0.0322(13) 0.0085(10) 0.0149(11) 0.0166(11) O9 0.0497(16) 0.0250(12) 0.0200(11) 0.0047(9) -0.0138(10) -0.0022(11) O10 0.0304(14) 0.0310(13) 0.0313(12) -0.0044(10) -0.0046(10) -0.0061(10) O12 0.126(3) 0.0301(14) 0.0329(15) 0.0040(12) 0.0213(17) 0.0217(17) O13 0.151(5) 0.052(2) 0.048(2) -0.0016(17) -0.005(2) 0.024(2) O16 0.060(2) 0.0421(15) 0.0290(13) 0.0066(11) -0.0040(12) -0.0035(13) O18 0.118(3) 0.074(3) 0.055(2) 0.0332(19) 0.013(2) 0.040(2) O11 0.133(5) 0.048(3) 0.035(2) 0.0032(18) 0.039(2) 0.036(3) O14' 0.037(3) 0.059(3) 0.272(10) 0.043(4) 0.006(4) -0.002(2) O11' 0.055(9) 0.044(8) 0.027(5) -0.009(5) 0.010(5) 0.004(7) O14 0.154(12) 0.026(6) 0.023(6) -0.006(5) 0.009(8) -0.007(8) Cl4 0.0527(10) 0.0248(7) 0.0221(6) 0.0016(5) -0.0061(6) -0.0086(6) O15 0.083(4) 0.030(2) 0.061(3) -0.009(2) 0.000(3) -0.023(2) O17 0.058(3) 0.035(2) 0.036(3) -0.0078(19) -0.002(2) 0.000(2) Cl4A 0.0399(15) 0.0320(12) 0.0474(14) 0.0094(10) 0.0005(11) 0.0103(10) O15A 0.060(6) 0.047(5) 0.068(5) -0.022(4) -0.033(4) 0.022(4) O17A 0.074(6) 0.048(5) 0.058(5) -0.014(4) -0.030(4) 0.018(4) N1SA 0.036(5) 0.053(5) 0.022(4) -0.004(4) 0.001(3) -0.004(4) O1SA 0.045(5) 0.040(4) 0.045(4) 0.001(3) 0.013(3) 0.007(3) C1SA 0.048(7) 0.045(6) 0.044(6) 0.011(5) -0.008(5) -0.008(5) O2SA 0.101(10) 0.108(9) 0.029(5) 0.001(5) -0.009(5) -0.034(8) Cl1S 0.022(4) 0.065(6) 0.121(13) -0.020(6) -0.018(4) 0.005(3) Cl2S 0.0474(19) 0.0252(14) 0.0236(14) 0.0020(10) 0.0049(11) -0.0009(12) C1S 0.035(7) 0.041(7) 0.030(6) 0.004(5) -0.007(5) 0.005(5) C2S 0.073(5) 0.050(4) 0.044(3) 0.000(3) -0.020(3) 0.005(3) O2S 0.129(7) 0.058(4) 0.076(4) 0.038(3) 0.051(5) 0.052(4) N1S 0.058(8) 0.038(7) 0.074(9) 0.012(7) -0.008(5) 0.021(5) O1S 0.075(4) 0.053(3) 0.068(3) 0.000(2) -0.026(3) 0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O6 Cl1 1.438(2) . ? O6 Cu2 2.763(2) . ? O7 Cl2 1.446(2) . ? O7 Cu1 2.671(2) . ? Cu1 O2 1.962(2) . ? Cu1 N5 1.998(2) . ? Cu1 N7 2.001(2) . ? Cu1 N8 2.041(2) . ? Cu1 N4 2.431(2) . ? Cu2 O1 1.965(2) . ? Cu2 N2 1.983(3) . ? Cu2 N10 1.989(3) . ? Cu2 N3 2.026(2) . ? Cu2 N9 2.364(3) . ? S1 C20 1.707(4) . ? S1 C21 1.719(3) . ? S2 C47 1.708(4) . ? S2 C48 1.720(3) . ? S3 C37 1.698(3) . ? S3 C38 1.713(3) . ? S4 C54 1.702(3) . ? S4 C11 1.706(3) . ? N1 O1 1.340(3) . ? N1 C1 1.354(5) . ? N1 C5 1.358(5) . ? N2 C6 1.343(4) . ? N2 C10 1.357(4) . ? N3 C54 1.321(4) . ? N3 C12 1.383(4) . ? N4 C21 1.311(4) . ? N4 C19 1.381(4) . ? N5 C26 1.343(4) . ? N5 C22 1.358(4) . ? N6 O2 1.340(3) . ? N6 C27 1.357(4) . ? N6 C31 1.365(4) . ? N7 C32 1.339(4) . ? N7 C36 1.354(4) . ? N8 C37 1.324(3) . ? N8 C39 1.390(4) . ? N9 C48 1.311(4) . ? N9 C46 1.382(4) . ? N10 C53 1.341(4) . ? N10 C49 1.356(4) . ? C1 C2 1.383(5) . ? C1 H1 0.9500 . ? C2 C3 1.377(7) . ? C2 H2 0.9500 . ? C3 C4 1.382(7) . ? C3 H3 0.9500 . ? C4 C5 1.391(5) . ? C4 H4 0.9500 . ? C5 C6 1.478(5) . ? C6 C7 1.395(5) . ? C7 C8 1.382(7) . ? C7 H7 0.9500 . ? C8 C9 1.377(6) . ? C8 H8 0.9500 . ? C9 C10 1.377(5) . ? C9 H9 0.9500 . ? C10 C54 1.458(4) . ? C11 C12 1.363(4) . ? C11 H11 0.9500 . ? C12 C13 1.470(4) . ? C13 C18 1.393(4) . ? C13 C14 1.394(4) . ? C14 C15 1.387(5) . ? C14 H14 0.9500 . ? C15 C16 1.392(5) . ? C15 H15 0.9500 . ? C16 C17 1.400(4) . ? C16 H16 0.9500 . ? C17 C18 1.382(4) . ? C17 C19 1.477(4) . ? C18 H18 0.9500 . ? C19 C20 1.364(4) . ? C20 H20 0.9500 . ? C21 C22 1.465(5) . ? C22 C23 1.390(4) . ? C23 C24 1.383(5) . ? C23 H23 0.9500 . ? C24 C25 1.381(5) . ? C24 H24 0.9500 . ? C25 C26 1.387(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.376(5) . ? C27 H27 0.9500 . ? C28 C29 1.380(5) . ? C28 H28 0.9500 . ? C29 C30 1.379(5) . ? C29 H29 0.9500 . ? C30 C31 1.389(4) . ? C30 H30 0.9500 . ? C31 C32 1.472(4) . ? C32 C33 1.401(4) . ? C33 C34 1.375(4) . ? C33 H33 0.9500 . ? C34 C35 1.383(4) . ? C34 H34 0.9500 . ? C35 C36 1.386(4) . ? C35 H35 0.9500 . ? C36 C37 1.456(4) . ? C38 C39 1.355(4) . ? C38 H38 0.9500 . ? C39 C40 1.472(4) . ? C40 C45 1.386(4) . ? C40 C41 1.395(4) . ? C41 C42 1.390(4) . ? C41 H41 0.9500 . ? C42 C43 1.387(5) . ? C42 H42 0.9500 . ? C43 C44 1.406(4) . ? C43 H43 0.9500 . ? C44 C45 1.392(4) . ? C44 C46 1.463(4) . ? C45 H45 0.9500 . ? C46 C47 1.366(4) . ? C47 H47 0.9500 . ? C48 C49 1.469(4) . ? C49 C50 1.385(4) . ? C50 C51 1.385(5) . ? C50 H50 0.9500 . ? C51 C52 1.381(5) . ? C51 H51 0.9500 . ? C52 C53 1.386(5) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? Cl1 O3 1.432(3) . ? Cl1 O5 1.442(2) . ? Cl1 O4 1.447(3) . ? Cl2 O10 1.430(2) . ? Cl2 O8 1.434(2) . ? Cl2 O9 1.446(2) . ? Cl3 O11' 1.276(12) . ? Cl3 O13 1.358(4) . ? Cl3 O12 1.405(3) . ? Cl3 O14' 1.412(5) . ? Cl3 O11 1.438(4) . ? Cl3 O14 1.650(16) . ? O13 O14 1.20(2) . ? O16 Cl4A 1.415(4) . ? O16 Cl4 1.458(3) . ? O18 Cl4A 1.346(4) . ? O18 Cl4 1.377(4) . ? Cl4 O15 1.418(5) . ? Cl4 O17 1.445(5) . ? Cl4A O15A 1.416(8) . ? Cl4A O17A 1.432(9) . ? N1SA O2SA 1.208(12) . ? N1SA O1SA 1.218(11) . ? N1SA C1SA 1.448(14) . ? C1SA H1S1 0.9800 . ? C1SA H1S2 0.9800 . ? C1SA H1S3 0.9800 . ? Cl1S C1S 1.746(18) . ? Cl2S C1S 1.765(14) . ? C1S H1S4 0.9900 . ? C1S H1S5 0.9900 . ? C2S N1S 1.53(3) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? O2S N1S 1.11(2) . ? N1S O1S 1.25(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 Cl1 O6 Cu2 132.72(14) . . ? Cl2 O7 Cu1 134.45(14) . . ? O2 Cu1 N5 93.47(9) . . ? O2 Cu1 N7 85.80(9) . . ? N5 Cu1 N7 167.50(10) . . ? O2 Cu1 N8 161.69(9) . . ? N5 Cu1 N8 96.98(10) . . ? N7 Cu1 N8 80.74(9) . . ? O2 Cu1 N4 81.55(8) . . ? N5 Cu1 N4 75.79(10) . . ? N7 Cu1 N4 116.34(9) . . ? N8 Cu1 N4 115.59(9) . . ? O2 Cu1 O7 85.08(8) . . ? N5 Cu1 O7 88.04(9) . . ? N7 Cu1 O7 79.47(8) . . ? N8 Cu1 O7 80.30(8) . . ? N4 Cu1 O7 158.25(8) . . ? O1 Cu2 N2 86.37(10) . . ? O1 Cu2 N10 90.36(9) . . ? N2 Cu2 N10 170.36(11) . . ? O1 Cu2 N3 158.48(10) . . ? N2 Cu2 N3 81.30(10) . . ? N10 Cu2 N3 98.89(10) . . ? O1 Cu2 N9 84.40(9) . . ? N2 Cu2 N9 111.34(10) . . ? N10 Cu2 N9 77.30(10) . . ? N3 Cu2 N9 116.49(9) . . ? O1 Cu2 O6 80.30(8) . . ? N2 Cu2 O6 79.70(10) . . ? N10 Cu2 O6 90.81(10) . . ? N3 Cu2 O6 80.20(9) . . ? N9 Cu2 O6 160.56(8) . . ? C20 S1 C21 89.83(16) . . ? C47 S2 C48 89.72(16) . . ? C37 S3 C38 89.77(14) . . ? C54 S4 C11 89.87(15) . . ? O1 N1 C1 115.0(3) . . ? O1 N1 C5 122.6(3) . . ? C1 N1 C5 122.3(3) . . ? C6 N2 C10 119.4(3) . . ? C6 N2 Cu2 126.0(2) . . ? C10 N2 Cu2 113.7(2) . . ? C54 N3 C12 111.4(2) . . ? C54 N3 Cu2 109.99(19) . . ? C12 N3 Cu2 136.6(2) . . ? C21 N4 C19 111.1(3) . . ? C21 N4 Cu1 103.36(19) . . ? C19 N4 Cu1 138.9(2) . . ? C26 N5 C22 118.9(3) . . ? C26 N5 Cu1 120.9(2) . . ? C22 N5 Cu1 120.2(2) . . ? O2 N6 C27 116.7(2) . . ? O2 N6 C31 122.4(2) . . ? C27 N6 C31 120.8(3) . . ? C32 N7 C36 118.9(2) . . ? C32 N7 Cu1 126.25(19) . . ? C36 N7 Cu1 113.41(18) . . ? C37 N8 C39 111.0(2) . . ? C37 N8 Cu1 109.10(18) . . ? C39 N8 Cu1 137.05(19) . . ? C48 N9 C46 111.7(3) . . ? C48 N9 Cu2 103.75(19) . . ? C46 N9 Cu2 140.0(2) . . ? C53 N10 C49 118.7(3) . . ? C53 N10 Cu2 122.7(2) . . ? C49 N10 Cu2 118.5(2) . . ? N1 O1 Cu2 116.95(17) . . ? N6 O2 Cu1 115.39(16) . . ? N1 C1 C2 120.0(4) . . ? N1 C1 H1 120.0 . . ? C2 C1 H1 120.0 . . ? C3 C2 C1 119.2(4) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 119.7(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 120.6(4) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? N1 C5 C4 118.0(4) . . ? N1 C5 C6 121.1(3) . . ? C4 C5 C6 120.9(4) . . ? N2 C6 C7 120.1(3) . . ? N2 C6 C5 119.3(3) . . ? C7 C6 C5 120.6(3) . . ? C8 C7 C6 120.0(4) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 119.7(4) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 118.0(4) . . ? C8 C9 H9 121.0 . . ? C10 C9 H9 121.0 . . ? N2 C10 C9 122.8(3) . . ? N2 C10 C54 112.5(3) . . ? C9 C10 C54 124.6(3) . . ? C12 C11 S4 111.1(2) . . ? C12 C11 H11 124.5 . . ? S4 C11 H11 124.5 . . ? C11 C12 N3 113.4(3) . . ? C11 C12 C13 128.1(3) . . ? N3 C12 C13 117.2(2) . . ? C18 C13 C14 119.4(3) . . ? C18 C13 C12 114.2(3) . . ? C14 C13 C12 126.3(3) . . ? C15 C14 C13 118.7(3) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 C16 121.7(3) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C15 C16 C17 119.6(3) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 118.4(3) . . ? C18 C17 C19 116.7(3) . . ? C16 C17 C19 124.9(3) . . ? C17 C18 C13 122.1(3) . . ? C17 C18 H18 118.9 . . ? C13 C18 H18 118.9 . . ? C20 C19 N4 114.4(3) . . ? C20 C19 C17 129.0(3) . . ? N4 C19 C17 116.6(3) . . ? C19 C20 S1 110.4(3) . . ? C19 C20 H20 124.8 . . ? S1 C20 H20 124.8 . . ? N4 C21 C22 121.0(3) . . ? N4 C21 S1 114.2(2) . . ? C22 C21 S1 124.8(2) . . ? N5 C22 C23 121.0(3) . . ? N5 C22 C21 115.3(3) . . ? C23 C22 C21 123.7(3) . . ? C24 C23 C22 119.7(3) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 119.1(3) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C24 C25 C26 118.9(3) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? N5 C26 C25 122.4(3) . . ? N5 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? N6 C27 C28 120.6(3) . . ? N6 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C27 C28 C29 120.0(3) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 118.9(3) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C29 C30 C31 120.8(3) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? N6 C31 C30 119.0(3) . . ? N6 C31 C32 120.0(3) . . ? C30 C31 C32 121.0(3) . . ? N7 C32 C33 120.9(3) . . ? N7 C32 C31 118.2(2) . . ? C33 C32 C31 120.8(3) . . ? C34 C33 C32 119.8(3) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 119.5(3) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C34 C35 C36 118.1(3) . . ? C34 C35 H35 120.9 . . ? C36 C35 H35 120.9 . . ? N7 C36 C35 122.8(3) . . ? N7 C36 C37 112.3(2) . . ? C35 C36 C37 124.9(3) . . ? N8 C37 C36 119.2(2) . . ? N8 C37 S3 114.5(2) . . ? C36 C37 S3 126.3(2) . . ? C39 C38 S3 111.1(2) . . ? C39 C38 H38 124.5 . . ? S3 C38 H38 124.5 . . ? C38 C39 N8 113.6(3) . . ? C38 C39 C40 128.1(3) . . ? N8 C39 C40 117.4(2) . . ? C45 C40 C41 120.2(3) . . ? C45 C40 C39 115.6(2) . . ? C41 C40 C39 124.3(3) . . ? C42 C41 C40 118.3(3) . . ? C42 C41 H41 120.9 . . ? C40 C41 H41 120.9 . . ? C43 C42 C41 122.0(3) . . ? C43 C42 H42 119.0 . . ? C41 C42 H42 119.0 . . ? C42 C43 C44 119.5(3) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C45 C44 C43 118.3(3) . . ? C45 C44 C46 117.5(3) . . ? C43 C44 C46 124.1(3) . . ? C40 C45 C44 121.6(3) . . ? C40 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? C47 C46 N9 113.8(3) . . ? C47 C46 C44 127.8(3) . . ? N9 C46 C44 118.4(3) . . ? C46 C47 S2 110.8(2) . . ? C46 C47 H47 124.6 . . ? S2 C47 H47 124.6 . . ? N9 C48 C49 121.4(3) . . ? N9 C48 S2 114.0(2) . . ? C49 C48 S2 124.6(2) . . ? N10 C49 C50 121.6(3) . . ? N10 C49 C48 115.0(3) . . ? C50 C49 C48 123.4(3) . . ? C51 C50 C49 119.0(3) . . ? C51 C50 H50 120.5 . . ? C49 C50 H50 120.5 . . ? C52 C51 C50 119.6(3) . . ? C52 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? C51 C52 C53 118.5(3) . . ? C51 C52 H52 120.8 . . ? C53 C52 H52 120.8 . . ? N10 C53 C52 122.6(3) . . ? N10 C53 H53 118.7 . . ? C52 C53 H53 118.7 . . ? N3 C54 C10 118.5(3) . . ? N3 C54 S4 114.2(2) . . ? C10 C54 S4 127.2(2) . . ? O3 Cl1 O6 109.48(15) . . ? O3 Cl1 O5 108.4(2) . . ? O6 Cl1 O5 109.77(15) . . ? O3 Cl1 O4 110.8(2) . . ? O6 Cl1 O4 109.16(18) . . ? O5 Cl1 O4 109.17(16) . . ? O10 Cl2 O8 109.99(16) . . ? O10 Cl2 O9 109.29(14) . . ? O8 Cl2 O9 110.08(15) . . ? O10 Cl2 O7 110.02(15) . . ? O8 Cl2 O7 108.72(14) . . ? O9 Cl2 O7 108.72(15) . . ? O11' Cl3 O13 91.9(7) . . ? O11' Cl3 O12 147.8(8) . . ? O13 Cl3 O12 113.9(2) . . ? O11' Cl3 O14' 79.7(8) . . ? O13 Cl3 O14' 113.2(4) . . ? O12 Cl3 O14' 105.2(3) . . ? O11' Cl3 O11 45.5(7) . . ? O13 Cl3 O11 109.4(3) . . ? O12 Cl3 O11 105.1(3) . . ? O14' Cl3 O11 109.6(5) . . ? O11' Cl3 O14 107.7(9) . . ? O13 Cl3 O14 45.8(8) . . ? O12 Cl3 O14 104.2(5) . . ? O14' Cl3 O14 74.0(9) . . ? O11 Cl3 O14 148.2(6) . . ? O14 O13 Cl3 80.1(8) . . ? Cl4A O16 Cl4 60.45(17) . . ? Cl4A O18 Cl4 64.17(19) . . ? O13 O14 Cl3 54.1(7) . . ? O18 Cl4 O15 105.6(3) . . ? O18 Cl4 O17 109.4(3) . . ? O15 Cl4 O17 110.7(4) . . ? O18 Cl4 O16 113.2(2) . . ? O15 Cl4 O16 108.8(3) . . ? O17 Cl4 O16 109.2(3) . . ? O18 Cl4A O16 118.0(3) . . ? O18 Cl4A O15A 120.4(5) . . ? O16 Cl4A O15A 111.8(4) . . ? O18 Cl4A O17A 84.8(5) . . ? O16 Cl4A O17A 108.4(4) . . ? O15A Cl4A O17A 108.8(6) . . ? O2SA N1SA O1SA 121.8(10) . . ? O2SA N1SA C1SA 118.4(10) . . ? O1SA N1SA C1SA 119.7(8) . . ? N1SA C1SA H1S1 109.5 . . ? N1SA C1SA H1S2 109.5 . . ? H1S1 C1SA H1S2 109.5 . . ? N1SA C1SA H1S3 109.5 . . ? H1S1 C1SA H1S3 109.5 . . ? H1S2 C1SA H1S3 109.5 . . ? Cl1S C1S Cl2S 110.2(11) . . ? Cl1S C1S H1S4 109.6 . . ? Cl2S C1S H1S4 109.6 . . ? Cl1S C1S H1S5 109.6 . . ? Cl2S C1S H1S5 109.6 . . ? H1S4 C1S H1S5 108.1 . . ? N1S C2S H2S1 109.5 . . ? N1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? N1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? O2S N1S O1S 132(2) . . ? O2S N1S C2S 116.7(16) . . ? O1S N1S C2S 110.8(17) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.630 _refine_diff_density_min -1.276 _refine_diff_density_rms 0.094 data_mo_alexcul4no_0m _database_code_depnum_ccdc_archive 'CCDC 918504' #TrackingRef 'CuL.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H29 Cl6 Cu2 N9 O27 S2' _chemical_formula_weight 1447.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4086(8) _cell_length_b 16.9828(14) _cell_length_c 18.2559(16) _cell_angle_alpha 67.070(2) _cell_angle_beta 82.993(2) _cell_angle_gamma 74.439(2) _cell_volume 2587.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9350 _cell_measurement_theta_min 3.1988 _cell_measurement_theta_max 30.5986 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 1.314 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15306 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.1404 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 26.02 _reflns_number_total 10037 _reflns_number_gt 5604 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0409P)^2^+3.0244P] 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 10037 _refine_ls_number_parameters 777 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.1326 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.988 _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 Cu1 Cu 0.67016(9) 0.88578(5) 0.22503(5) 0.0178(2) Uani 1 1 d . A 4 Cl3 Cl 0.80470(18) 1.06112(10) 0.11609(9) 0.0202(4) Uani 1 1 d . A 4 S5 S 0.23999(18) 0.98139(11) 0.11391(10) 0.0197(4) Uani 1 1 d . A 4 Cu2 Cu 0.40598(9) 0.44448(5) 0.28012(5) 0.0203(2) Uani 1 1 d . B 4 S7 S 0.61732(19) 0.31444(11) 0.11568(10) 0.0241(4) Uani 1 1 d . B 4 Cl4 Cl 0.1994(2) 0.34408(11) 0.44131(10) 0.0292(4) Uani 1 1 d . B 4 Cl6 Cl 0.88752(18) 0.00572(11) 0.36966(9) 0.0213(4) Uani 1 1 d . C 4 Cl1 Cl 0.58883(19) 0.60202(11) 0.12275(10) 0.0226(4) Uani 1 1 d . D 4 C13 C 0.1521(7) 0.5248(4) 0.1713(4) 0.0186(15) Uani 1 1 d . B 4 C8 C 0.4955(7) 0.3703(4) 0.1668(4) 0.0182(14) Uani 1 1 d . B 4 C11 C 0.1738(7) 0.5188(4) 0.0406(4) 0.0220(15) Uani 1 1 d . B 4 H11 H 0.1370 0.5382 -0.0113 0.026 Uiso 1 1 calc R B 4 C9 C 0.3575(7) 0.4342(4) 0.1364(4) 0.0193(15) Uani 1 1 d . B 4 C6 C 0.6727(7) 0.2946(4) 0.2546(4) 0.0172(14) Uani 1 1 d . B 4 C15 C -0.0877(8) 0.5724(4) 0.2343(4) 0.0260(16) Uani 1 1 d . B 4 H15 H -0.1365 0.5654 0.1954 0.031 Uiso 1 1 calc R B 4 C10 C 0.3055(8) 0.4578(4) 0.0613(4) 0.0255(16) Uani 1 1 d . B 4 H10 H 0.3595 0.4323 0.0252 0.031 Uiso 1 1 calc R B 4 C5 C 0.7416(8) 0.2651(4) 0.3321(4) 0.0231(16) Uani 1 1 d . B 4 C1 C 0.6671(9) 0.2413(4) 0.4042(4) 0.0326(19) Uani 1 1 d . B 4 H1 H 0.5640 0.2455 0.4064 0.039 Uiso 1 1 calc R B 4 C17 C -0.0968(8) 0.6067(4) 0.3498(4) 0.0292(18) Uani 1 1 d . B 4 H17 H -0.1507 0.6255 0.3899 0.035 Uiso 1 1 calc R B 4 C18 C 0.0523(9) 0.5854(4) 0.3492(4) 0.0295(18) Uani 1 1 d . B 4 H18 H 0.1023 0.5881 0.3901 0.035 Uiso 1 1 calc R B 4 C12 C 0.0935(8) 0.5526(4) 0.0959(4) 0.0250(16) Uani 1 1 d . B 4 H12 H 0.0007 0.5938 0.0826 0.030 Uiso 1 1 calc R B 4 C7 C 0.7308(7) 0.2675(4) 0.1946(4) 0.0232(16) Uani 1 1 d . B 4 H7 H 0.8237 0.2272 0.1963 0.028 Uiso 1 1 calc R B 4 C14 C 0.0656(7) 0.5537(4) 0.2330(4) 0.0190(15) Uani 1 1 d . B 4 C3 C 0.8943(13) 0.2064(5) 0.4710(5) 0.058(3) Uani 1 1 d . B 4 H3 H 0.9475 0.1866 0.5184 0.069 Uiso 1 1 calc R B 4 C16 C -0.1708(8) 0.6010(4) 0.2915(4) 0.0301(18) Uani 1 1 d . B 4 H16 H -0.2755 0.6163 0.2907 0.036 Uiso 1 1 calc R B 4 C4 C 0.9636(10) 0.2307(5) 0.3985(5) 0.054(3) Uani 1 1 d . B 4 H4 H 1.0666 0.2270 0.3954 0.065 Uiso 1 1 calc R B 4 C2 C 0.7459(12) 0.2111(5) 0.4740(4) 0.050(3) Uani 1 1 d . B 4 H2 H 0.6962 0.1936 0.5241 0.059 Uiso 1 1 calc R B 4 C25 C 0.7592(7) 0.7994(4) 0.0311(4) 0.0185(15) Uani 1 1 d . A 4 H25 H 0.8383 0.7651 0.0106 0.022 Uiso 1 1 calc R A 4 C24 C 0.7832(7) 0.8223(4) 0.0939(4) 0.0169(14) Uani 1 1 d . A 4 C28 C 0.4248(7) 0.9438(4) 0.1327(4) 0.0164(14) Uani 1 1 d . A 4 C26 C 0.6201(8) 0.8269(4) -0.0008(4) 0.0223(16) Uani 1 1 d . A 4 H26 H 0.6031 0.8123 -0.0436 0.027 Uiso 1 1 calc R A 4 C23 C 0.9346(7) 0.7997(4) 0.1233(4) 0.0172(14) Uani 1 1 d . A 4 C27 C 0.5058(7) 0.8761(4) 0.0308(4) 0.0189(15) Uani 1 1 d . A 4 H27 H 0.4095 0.8965 0.0096 0.023 Uiso 1 1 calc R A 4 C35 C 0.2642(8) 1.0447(4) 0.4082(4) 0.0269(17) Uani 1 1 d . A 4 H35 H 0.1928 1.0334 0.4501 0.032 Uiso 1 1 calc R A 4 C19 C 1.0963(7) 0.7738(4) 0.2245(4) 0.0232(16) Uani 1 1 d . A 4 H19 H 1.1097 0.7725 0.2757 0.028 Uiso 1 1 calc R A 4 C30 C 0.3455(7) 1.0061(4) 0.2219(4) 0.0201(15) Uani 1 1 d . A 4 C33 C 0.4720(8) 1.1018(4) 0.3497(4) 0.0274(17) Uani 1 1 d . A 4 H33 H 0.5455 1.1303 0.3506 0.033 Uiso 1 1 calc R A 4 C31 C 0.3638(7) 1.0337(4) 0.2865(4) 0.0148(14) Uani 1 1 d . A 4 C29 C 0.2156(7) 1.0224(4) 0.1875(4) 0.0185(15) Uani 1 1 d . A 4 H29 H 0.1233 1.0525 0.2024 0.022 Uiso 1 1 calc R A 4 C32 C 0.4698(7) 1.0750(4) 0.2872(4) 0.0246(16) Uani 1 1 d . A 4 H32 H 0.5414 1.0851 0.2453 0.030 Uiso 1 1 calc R A 4 C22 C 1.0562(7) 0.7856(4) 0.0755(4) 0.0242(16) Uani 1 1 d . A 4 H22 H 1.0424 0.7921 0.0225 0.029 Uiso 1 1 calc R A 4 C34 C 0.3684(8) 1.0872(5) 0.4100(4) 0.0280(17) Uani 1 1 d . A 4 H34 H 0.3686 1.1063 0.4525 0.034 Uiso 1 1 calc R A 4 C20 C 1.2161(8) 0.7571(4) 0.1785(4) 0.0289(17) Uani 1 1 d . A 4 H20 H 1.3126 0.7420 0.1983 0.035 Uiso 1 1 calc R A 4 C21 C 1.1971(8) 0.7621(4) 0.1031(4) 0.0246(16) Uani 1 1 d . A 4 H21 H 1.2800 0.7495 0.0706 0.030 Uiso 1 1 calc R A 4 N3 N 0.4662(5) 0.9607(3) 0.1910(3) 0.0147(11) Uani 1 1 d . A 4 N7 N 0.2845(6) 0.4678(3) 0.1898(3) 0.0182(12) Uani 1 1 d . B 4 N2 N 0.6702(6) 0.8681(3) 0.1249(3) 0.0171(12) Uani 1 1 d . A 4 N1 N 0.9580(6) 0.7922(3) 0.1987(3) 0.0181(12) Uani 1 1 d . A 4 N4 N 0.2627(6) 1.0189(3) 0.3473(3) 0.0179(12) Uani 1 1 d . A 4 N6 N 0.5366(6) 0.3536(3) 0.2385(3) 0.0186(12) Uani 1 1 d . B 4 N8 N 0.1323(6) 0.5601(3) 0.2914(3) 0.0234(13) Uani 1 1 d . B 4 N5 N 0.8877(7) 0.2599(4) 0.3309(4) 0.0330(16) Uani 1 1 d . B 4 O13 O 0.2787(5) 0.5477(3) 0.2930(3) 0.0284(12) Uani 1 1 d . B 4 O8 O 0.8504(5) 0.7965(3) 0.2530(2) 0.0220(10) Uani 1 1 d . A 4 O4 O 0.9140(5) 1.1061(3) 0.1149(3) 0.0302(12) Uani 1 1 d . A 4 O3 O 1.0196(5) -0.0447(3) 0.3438(3) 0.0343(13) Uani 1 1 d . C 4 O1 O 0.7914(5) -0.0527(3) 0.4099(3) 0.0284(12) Uani 1 1 d . C 4 O15 O 0.2812(5) 0.2581(3) 0.1508(3) 0.0391(14) Uani 1 1 d . E 4 O10 O 0.7256(5) 0.6030(3) 0.0779(3) 0.0333(12) Uani 1 1 d . D 4 O6 O 0.6605(5) 1.1192(3) 0.1122(3) 0.0340(13) Uani 1 1 d . A 4 O2 O 0.8156(6) 0.0776(3) 0.3032(3) 0.0340(12) Uani 1 1 d . C 4 O17 O 0.0903(6) 0.1918(3) 0.2225(3) 0.0391(14) Uani 1 1 d . E 4 O12 O 0.5201(6) 0.7653(3) 0.2735(3) 0.0330(13) Uani 1 1 d . F 4 O9 O 0.5572(6) 0.6692(3) 0.1548(3) 0.0369(13) Uani 1 1 d . D 4 O14 O 0.2403(7) 0.4022(3) 0.4695(3) 0.0510(16) Uani 1 1 d . B 4 O11 O 0.6028(6) 0.5181(3) 0.1865(3) 0.0452(15) Uani 1 1 d . D 4 O16 O 0.0663(6) 0.3404(3) 0.1931(3) 0.0402(14) Uani 1 1 d . E 4 O5 O 0.8266(5) 1.0326(3) 0.0505(3) 0.0328(12) Uani 1 1 d . A 4 O21 O 0.8134(6) 0.9848(3) 0.1899(3) 0.0314(12) Uani 1 1 d . A 4 O22 O 0.9270(5) 0.0377(3) 0.4245(3) 0.0337(13) Uani 1 1 d . C 4 O23 O 0.0535(6) 0.2911(3) 0.0917(3) 0.0450(15) Uani 1 1 d . E 4 O20 O 0.5217(6) 0.7290(4) 0.4109(3) 0.0520(16) Uani 1 1 d . F 4 O24 O 0.2930(7) 0.3380(3) 0.3751(3) 0.0484(16) Uani 1 1 d . B 4 O25 O 0.2154(7) 0.2578(3) 0.4997(3) 0.0576(18) Uani 1 1 d . B 4 O26 O 0.0508(7) 0.3792(4) 0.4143(5) 0.086(3) Uani 1 1 d . B 4 O27 O 0.4728(6) 0.6156(4) 0.0715(3) 0.0436(14) Uani 1 1 d . D 4 N9 N 0.5375(6) 0.4402(3) 0.3590(3) 0.0231(13) Uani 1 1 d . B 4 C36 C 0.6011(8) 0.4495(4) 0.4032(4) 0.0238(16) Uani 1 1 d . B 4 C37 C 0.5357(7) 0.8943(4) 0.0931(4) 0.0143(14) Uani 1 1 d . A 4 C38 C 0.6825(9) 0.4582(5) 0.4609(4) 0.043(2) Uani 1 1 d . B 4 H38A H 0.6547 0.4223 0.5146 0.064 Uiso 1 1 calc R B 4 H38B H 0.6595 0.5201 0.4551 0.064 Uiso 1 1 calc R B 4 H38C H 0.7886 0.4380 0.4519 0.064 Uiso 1 1 calc R B 4 O7 O 0.6451(5) 0.8784(3) 0.3367(2) 0.0228(11) Uani 1 1 d . . . H7A H 0.7104 0.8985 0.3470 0.027 Uiso 1 1 d R A . H7B H 0.5948 0.8420 0.3651 0.027 Uiso 1 1 d R . . Cl5 Cl 0.12453(19) 0.27056(11) 0.16359(10) 0.0260(4) Uani 1 1 d . . . Cl2 Cl 0.4373(2) 0.74164(11) 0.34622(10) 0.0281(4) Uani 1 1 d D . . O18 O 0.3123(6) 0.8165(4) 0.3380(4) 0.039(2) Uani 0.811(8) 1 d PDU F 1 O19 O 0.3817(10) 0.6669(5) 0.3564(4) 0.050(2) Uani 0.811(8) 1 d PDU F 1 O18A O 0.2836(14) 0.745(2) 0.3685(17) 0.049(4) Uani 0.189(8) 1 d PDU F 2 O19A O 0.482(4) 0.6458(6) 0.3760(19) 0.054(5) Uani 0.189(8) 1 d PDU F 2 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 0.0135(4) 0.0214(4) 0.0195(4) -0.0101(3) -0.0006(4) -0.0021(3) Cl3 0.0187(9) 0.0227(9) 0.0213(8) -0.0089(7) -0.0020(7) -0.0064(7) S5 0.0132(9) 0.0230(9) 0.0240(9) -0.0106(7) -0.0028(7) -0.0022(7) Cu2 0.0179(5) 0.0206(4) 0.0244(4) -0.0118(4) -0.0033(4) -0.0016(4) S7 0.0214(10) 0.0287(10) 0.0223(9) -0.0142(8) 0.0013(8) 0.0001(8) Cl4 0.0265(10) 0.0299(10) 0.0251(9) -0.0054(8) 0.0027(8) -0.0059(8) Cl6 0.0166(9) 0.0314(9) 0.0209(8) -0.0127(7) 0.0016(7) -0.0102(7) Cl1 0.0190(9) 0.0284(9) 0.0234(9) -0.0115(7) 0.0017(7) -0.0084(7) C13 0.018(4) 0.013(3) 0.025(4) -0.007(3) -0.006(3) -0.001(3) C8 0.018(4) 0.017(3) 0.021(4) -0.009(3) 0.007(3) -0.008(3) C11 0.025(4) 0.028(4) 0.015(3) -0.010(3) -0.001(3) -0.007(3) C9 0.020(4) 0.019(3) 0.020(3) -0.007(3) 0.002(3) -0.008(3) C6 0.011(3) 0.015(3) 0.021(3) -0.004(3) 0.000(3) 0.000(3) C15 0.020(4) 0.027(4) 0.030(4) -0.012(3) -0.005(3) -0.001(3) C10 0.019(4) 0.031(4) 0.033(4) -0.019(3) -0.001(3) -0.006(3) C5 0.023(4) 0.024(4) 0.023(4) -0.015(3) 0.004(3) 0.000(3) C1 0.040(5) 0.021(4) 0.036(4) -0.015(3) 0.002(4) -0.001(4) C17 0.037(5) 0.021(4) 0.022(4) -0.008(3) 0.004(4) 0.002(3) C18 0.044(5) 0.024(4) 0.022(4) -0.013(3) 0.001(4) -0.005(4) C12 0.023(4) 0.024(4) 0.025(4) -0.008(3) -0.007(3) -0.001(3) C7 0.018(4) 0.025(4) 0.021(4) -0.009(3) 0.001(3) 0.003(3) C14 0.021(4) 0.013(3) 0.025(4) -0.011(3) 0.002(3) -0.004(3) C3 0.086(8) 0.040(5) 0.046(6) -0.030(5) -0.033(6) 0.021(5) C16 0.026(4) 0.024(4) 0.032(4) -0.007(3) 0.006(4) 0.000(3) C4 0.051(6) 0.057(6) 0.058(6) -0.044(5) -0.035(5) 0.030(5) C2 0.101(9) 0.021(4) 0.022(4) -0.016(3) -0.003(5) 0.004(5) C25 0.025(4) 0.012(3) 0.017(3) -0.007(3) 0.004(3) -0.002(3) C24 0.013(4) 0.019(3) 0.020(3) -0.006(3) 0.005(3) -0.008(3) C28 0.015(4) 0.016(3) 0.017(3) -0.003(3) -0.002(3) -0.005(3) C26 0.027(4) 0.024(4) 0.020(4) -0.010(3) 0.002(3) -0.010(3) C23 0.015(4) 0.012(3) 0.022(3) -0.005(3) 0.000(3) -0.003(3) C27 0.019(4) 0.019(3) 0.021(3) -0.007(3) -0.005(3) -0.007(3) C35 0.024(4) 0.036(4) 0.024(4) -0.017(3) 0.001(3) -0.004(3) C19 0.013(4) 0.025(4) 0.030(4) -0.008(3) -0.006(3) -0.002(3) C30 0.019(4) 0.018(3) 0.024(4) -0.011(3) -0.002(3) 0.001(3) C33 0.021(4) 0.032(4) 0.036(4) -0.017(3) 0.000(3) -0.010(3) C31 0.013(3) 0.011(3) 0.018(3) -0.005(3) 0.000(3) 0.000(3) C29 0.018(4) 0.013(3) 0.022(4) -0.007(3) -0.003(3) 0.000(3) C32 0.015(4) 0.039(4) 0.028(4) -0.018(3) 0.007(3) -0.013(3) C22 0.021(4) 0.026(4) 0.023(4) -0.008(3) 0.003(3) -0.003(3) C34 0.021(4) 0.042(4) 0.029(4) -0.021(4) 0.006(3) -0.010(4) C20 0.015(4) 0.024(4) 0.045(5) -0.009(3) -0.006(4) -0.003(3) C21 0.017(4) 0.023(4) 0.031(4) -0.006(3) 0.008(3) -0.011(3) N3 0.008(3) 0.016(3) 0.022(3) -0.010(2) 0.003(2) -0.002(2) N7 0.015(3) 0.018(3) 0.023(3) -0.012(2) 0.003(2) -0.001(2) N2 0.017(3) 0.013(3) 0.021(3) -0.007(2) 0.000(2) -0.002(2) N1 0.014(3) 0.018(3) 0.023(3) -0.008(2) 0.001(3) -0.004(2) N4 0.016(3) 0.024(3) 0.015(3) -0.012(2) 0.003(2) 0.000(2) N6 0.016(3) 0.022(3) 0.019(3) -0.009(2) 0.003(3) -0.006(2) N8 0.019(3) 0.022(3) 0.029(3) -0.012(3) -0.004(3) 0.001(3) N5 0.025(4) 0.045(4) 0.033(4) -0.027(3) -0.006(3) 0.006(3) O13 0.024(3) 0.025(3) 0.044(3) -0.024(2) -0.007(2) 0.001(2) O8 0.017(3) 0.027(3) 0.018(2) -0.006(2) 0.000(2) -0.003(2) O4 0.033(3) 0.034(3) 0.023(3) -0.001(2) -0.001(2) -0.023(2) O3 0.016(3) 0.046(3) 0.050(3) -0.029(3) 0.007(3) -0.008(2) O1 0.025(3) 0.041(3) 0.027(3) -0.013(2) 0.009(2) -0.024(2) O15 0.024(3) 0.042(3) 0.055(4) -0.024(3) 0.008(3) -0.009(3) O10 0.026(3) 0.049(3) 0.030(3) -0.019(3) 0.009(2) -0.014(3) O6 0.026(3) 0.037(3) 0.042(3) -0.022(3) -0.004(3) 0.000(2) O2 0.034(3) 0.038(3) 0.027(3) -0.006(2) -0.004(2) -0.010(3) O17 0.037(3) 0.024(3) 0.045(3) -0.003(2) 0.005(3) -0.007(2) O12 0.046(3) 0.027(3) 0.028(3) -0.009(2) 0.010(3) -0.017(3) O9 0.043(3) 0.034(3) 0.047(3) -0.030(3) 0.013(3) -0.014(3) O14 0.086(5) 0.039(3) 0.037(3) -0.025(3) -0.006(3) -0.011(3) O11 0.045(4) 0.029(3) 0.046(3) 0.006(3) -0.006(3) -0.012(3) O16 0.043(4) 0.032(3) 0.060(4) -0.032(3) 0.020(3) -0.017(3) O5 0.028(3) 0.051(3) 0.029(3) -0.026(3) -0.002(2) -0.008(3) O21 0.041(3) 0.026(3) 0.026(3) 0.001(2) -0.012(2) -0.017(2) O22 0.027(3) 0.059(3) 0.035(3) -0.033(3) 0.006(2) -0.023(3) O23 0.041(4) 0.061(4) 0.028(3) -0.020(3) 0.004(3) -0.001(3) O20 0.045(4) 0.077(4) 0.028(3) -0.004(3) -0.009(3) -0.024(3) O24 0.077(5) 0.047(3) 0.041(3) -0.030(3) 0.033(3) -0.041(3) O25 0.093(5) 0.033(3) 0.032(3) 0.008(3) -0.008(3) -0.017(3) O26 0.024(4) 0.050(4) 0.168(8) -0.019(4) -0.024(4) -0.003(3) O27 0.028(3) 0.062(4) 0.049(3) -0.034(3) -0.009(3) -0.002(3) N9 0.024(3) 0.021(3) 0.026(3) -0.011(3) 0.001(3) -0.007(3) C36 0.025(4) 0.024(4) 0.026(4) -0.011(3) 0.011(3) -0.014(3) C37 0.013(3) 0.013(3) 0.016(3) -0.004(3) 0.001(3) -0.004(3) C38 0.051(6) 0.059(6) 0.026(4) -0.012(4) -0.003(4) -0.030(5) O7 0.016(3) 0.032(3) 0.027(3) -0.013(2) 0.002(2) -0.013(2) Cl5 0.0230(10) 0.0244(9) 0.0327(10) -0.0140(8) 0.0042(8) -0.0061(8) Cl2 0.0274(10) 0.0333(10) 0.0294(9) -0.0153(8) 0.0080(8) -0.0151(8) O18 0.025(4) 0.052(4) 0.028(3) -0.013(3) 0.005(3) 0.003(3) O19 0.067(6) 0.060(4) 0.042(4) -0.015(3) 0.004(4) -0.054(4) O18A 0.046(6) 0.062(6) 0.037(6) -0.011(6) 0.002(6) -0.024(6) O19A 0.068(10) 0.058(8) 0.046(8) -0.008(7) 0.010(9) -0.052(9) _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 O8 1.914(4) . ? Cu1 N2 1.965(5) . ? Cu1 O7 1.981(4) . ? Cu1 N3 2.013(5) . ? Cu1 O21 2.285(5) . ? Cl3 O4 1.429(5) . ? Cl3 O5 1.432(4) . ? Cl3 O6 1.438(5) . ? Cl3 O21 1.452(5) . ? S5 C29 1.706(6) . ? S5 C28 1.711(7) . ? Cu2 O13 1.920(4) . ? Cu2 N7 1.972(5) . ? Cu2 N9 1.979(6) . ? Cu2 N6 2.034(5) . ? Cu2 O24 2.355(5) . ? S7 C7 1.695(7) . ? S7 C8 1.711(6) . ? Cl4 O25 1.417(5) . ? Cl4 O14 1.427(5) . ? Cl4 O24 1.427(5) . ? Cl4 O26 1.431(6) . ? Cl6 O2 1.423(5) . ? Cl6 O22 1.435(4) . ? Cl6 O1 1.447(4) . ? Cl6 O3 1.449(5) . ? Cl1 O9 1.425(4) . ? Cl1 O11 1.431(5) . ? Cl1 O27 1.437(5) . ? Cl1 O10 1.440(5) . ? C13 N7 1.343(8) . ? C13 C12 1.399(8) . ? C13 C14 1.472(8) . ? C8 N6 1.312(8) . ? C8 C9 1.456(9) . ? C11 C10 1.369(9) . ? C11 C12 1.396(8) . ? C11 H11 0.9500 . ? C9 N7 1.345(7) . ? C9 C10 1.382(9) . ? C6 C7 1.350(8) . ? C6 N6 1.380(8) . ? C6 C5 1.474(9) . ? C15 C16 1.390(9) . ? C15 C14 1.391(9) . ? C15 H15 0.9500 . ? C10 H10 0.9500 . ? C5 N5 1.351(9) . ? C5 C1 1.378(9) . ? C1 C2 1.397(10) . ? C1 H1 0.9500 . ? C17 C18 1.351(10) . ? C17 C16 1.386(10) . ? C17 H17 0.9500 . ? C18 N8 1.360(8) . ? C18 H18 0.9500 . ? C12 H12 0.9500 . ? C7 H7 0.9500 . ? C14 N8 1.355(8) . ? C3 C4 1.362(12) . ? C3 C2 1.373(13) . ? C3 H3 0.9500 . ? C16 H16 0.9500 . ? C4 N5 1.352(9) . ? C4 H4 0.9500 . ? C2 H2 0.9500 . ? C25 C26 1.385(9) . ? C25 C24 1.404(8) . ? C25 H25 0.9500 . ? C24 N2 1.344(7) . ? C24 C23 1.483(9) . ? C28 N3 1.329(7) . ? C28 C37 1.462(8) . ? C26 C27 1.389(8) . ? C26 H26 0.9500 . ? C23 N1 1.370(8) . ? C23 C22 1.379(8) . ? C27 C37 1.367(8) . ? C27 H27 0.9500 . ? C35 N4 1.347(8) . ? C35 C34 1.376(9) . ? C35 H35 0.9500 . ? C19 N1 1.352(8) . ? C19 C20 1.356(9) . ? C19 H19 0.9500 . ? C30 C29 1.355(9) . ? C30 N3 1.384(7) . ? C30 C31 1.471(8) . ? C33 C34 1.371(9) . ? C33 C32 1.386(9) . ? C33 H33 0.9500 . ? C31 N4 1.362(7) . ? C31 C32 1.368(9) . ? C29 H29 0.9500 . ? C32 H32 0.9500 . ? C22 C21 1.376(9) . ? C22 H22 0.9500 . ? C34 H34 0.9500 . ? C20 C21 1.377(9) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? N2 C37 1.345(8) . ? N1 O8 1.336(6) . ? N8 O13 1.338(7) . ? O15 Cl5 1.435(5) . ? O17 Cl5 1.441(5) . ? O12 Cl2 1.425(5) . ? O16 Cl5 1.441(4) . ? O23 Cl5 1.423(5) . ? O20 Cl2 1.419(5) . ? N9 C36 1.140(8) . ? C36 C38 1.447(10) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? O7 H7A 0.8500 . ? O7 H7B 0.8500 . ? Cl2 O19 1.438(5) . ? Cl2 O18A 1.446(9) . ? Cl2 O18 1.453(5) . ? Cl2 O19A 1.457(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 O8 Cu1 N2 89.6(2) . . ? O8 Cu1 O7 89.30(18) . . ? N2 Cu1 O7 165.4(2) . . ? O8 Cu1 N3 168.00(19) . . ? N2 Cu1 N3 82.7(2) . . ? O7 Cu1 N3 95.86(19) . . ? O8 Cu1 O21 86.20(18) . . ? N2 Cu1 O21 101.08(19) . . ? O7 Cu1 O21 93.40(17) . . ? N3 Cu1 O21 104.24(18) . . ? O4 Cl3 O5 110.7(3) . . ? O4 Cl3 O6 109.3(3) . . ? O5 Cl3 O6 109.6(3) . . ? O4 Cl3 O21 109.6(3) . . ? O5 Cl3 O21 109.0(3) . . ? O6 Cl3 O21 108.5(3) . . ? C29 S5 C28 89.7(3) . . ? O13 Cu2 N7 88.0(2) . . ? O13 Cu2 N9 88.0(2) . . ? N7 Cu2 N9 170.1(2) . . ? O13 Cu2 N6 166.3(2) . . ? N7 Cu2 N6 81.8(2) . . ? N9 Cu2 N6 100.6(2) . . ? O13 Cu2 O24 98.6(2) . . ? N7 Cu2 O24 96.4(2) . . ? N9 Cu2 O24 93.1(2) . . ? N6 Cu2 O24 91.65(19) . . ? C7 S7 C8 89.1(3) . . ? O25 Cl4 O14 112.5(3) . . ? O25 Cl4 O24 107.7(3) . . ? O14 Cl4 O24 108.6(3) . . ? O25 Cl4 O26 110.1(4) . . ? O14 Cl4 O26 109.9(4) . . ? O24 Cl4 O26 107.8(4) . . ? O2 Cl6 O22 110.0(3) . . ? O2 Cl6 O1 110.3(3) . . ? O22 Cl6 O1 109.1(3) . . ? O2 Cl6 O3 110.3(3) . . ? O22 Cl6 O3 109.2(3) . . ? O1 Cl6 O3 107.8(3) . . ? O9 Cl1 O11 109.2(3) . . ? O9 Cl1 O27 110.6(3) . . ? O11 Cl1 O27 109.3(3) . . ? O9 Cl1 O10 109.7(3) . . ? O11 Cl1 O10 108.9(3) . . ? O27 Cl1 O10 109.1(3) . . ? N7 C13 C12 120.7(6) . . ? N7 C13 C14 118.9(6) . . ? C12 C13 C14 120.3(6) . . ? N6 C8 C9 119.6(5) . . ? N6 C8 S7 114.7(5) . . ? C9 C8 S7 125.7(5) . . ? C10 C11 C12 120.0(6) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? N7 C9 C10 123.2(6) . . ? N7 C9 C8 112.6(6) . . ? C10 C9 C8 124.2(6) . . ? C7 C6 N6 114.0(6) . . ? C7 C6 C5 125.4(6) . . ? N6 C6 C5 120.6(5) . . ? C16 C15 C14 121.1(7) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C11 C10 C9 118.0(6) . . ? C11 C10 H10 121.0 . . ? C9 C10 H10 121.0 . . ? N5 C5 C1 119.2(7) . . ? N5 C5 C6 116.7(6) . . ? C1 C5 C6 124.1(7) . . ? C5 C1 C2 118.8(8) . . ? C5 C1 H1 120.6 . . ? C2 C1 H1 120.6 . . ? C18 C17 C16 119.8(7) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 N8 121.4(7) . . ? C17 C18 H18 119.3 . . ? N8 C18 H18 119.3 . . ? C11 C12 C13 118.9(6) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C6 C7 S7 111.6(5) . . ? C6 C7 H7 124.2 . . ? S7 C7 H7 124.2 . . ? N8 C14 C15 118.1(6) . . ? N8 C14 C13 121.3(6) . . ? C15 C14 C13 120.6(6) . . ? C4 C3 C2 118.5(8) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C17 C16 C15 118.3(7) . . ? C17 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? N5 C4 C3 120.8(9) . . ? N5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C3 C2 C1 120.8(8) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C26 C25 C24 119.9(6) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? N2 C24 C25 120.0(6) . . ? N2 C24 C23 120.0(5) . . ? C25 C24 C23 119.9(6) . . ? N3 C28 C37 118.9(6) . . ? N3 C28 S5 114.5(4) . . ? C37 C28 S5 126.6(5) . . ? C25 C26 C27 119.1(6) . . ? C25 C26 H26 120.5 . . ? C27 C26 H26 120.5 . . ? N1 C23 C22 118.1(6) . . ? N1 C23 C24 121.1(6) . . ? C22 C23 C24 120.8(6) . . ? C37 C27 C26 118.1(6) . . ? C37 C27 H27 121.0 . . ? C26 C27 H27 121.0 . . ? N4 C35 C34 120.4(7) . . ? N4 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? N1 C19 C20 121.1(6) . . ? N1 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C29 C30 N3 114.8(5) . . ? C29 C30 C31 124.9(6) . . ? N3 C30 C31 120.4(6) . . ? C34 C33 C32 120.1(7) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? N4 C31 C32 119.7(6) . . ? N4 C31 C30 115.7(6) . . ? C32 C31 C30 124.6(6) . . ? C30 C29 S5 110.9(5) . . ? C30 C29 H29 124.6 . . ? S5 C29 H29 124.6 . . ? C31 C32 C33 119.5(6) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C21 C22 C23 121.1(6) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C33 C34 C35 119.1(6) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C19 C20 C21 119.6(7) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 119.0(6) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C28 N3 C30 110.2(5) . . ? C28 N3 Cu1 109.2(4) . . ? C30 N3 Cu1 138.1(4) . . ? C13 N7 C9 119.2(6) . . ? C13 N7 Cu2 126.1(4) . . ? C9 N7 Cu2 113.5(4) . . ? C24 N2 C37 119.3(5) . . ? C24 N2 Cu1 126.3(4) . . ? C37 N2 Cu1 113.6(4) . . ? O8 N1 C19 115.2(5) . . ? O8 N1 C23 123.8(5) . . ? C19 N1 C23 120.9(6) . . ? C35 N4 C31 121.2(6) . . ? C8 N6 C6 110.6(5) . . ? C8 N6 Cu2 109.2(4) . . ? C6 N6 Cu2 137.9(4) . . ? O13 N8 C14 122.4(5) . . ? O13 N8 C18 116.2(5) . . ? C14 N8 C18 121.3(6) . . ? C5 N5 C4 121.9(7) . . ? N8 O13 Cu2 119.4(4) . . ? N1 O8 Cu1 120.7(3) . . ? Cl3 O21 Cu1 125.9(3) . . ? Cl4 O24 Cu2 129.1(3) . . ? C36 N9 Cu2 170.1(6) . . ? N9 C36 C38 178.0(8) . . ? N2 C37 C27 123.6(6) . . ? N2 C37 C28 112.8(5) . . ? C27 C37 C28 123.5(6) . . ? Cu1 O7 H7A 109.6 . . ? Cu1 O7 H7B 112.9 . . ? H7A O7 H7B 133.5 . . ? O23 Cl5 O15 110.5(3) . . ? O23 Cl5 O17 108.8(3) . . ? O15 Cl5 O17 110.3(3) . . ? O23 Cl5 O16 109.4(3) . . ? O15 Cl5 O16 110.5(3) . . ? O17 Cl5 O16 107.2(3) . . ? O20 Cl2 O12 110.7(3) . . ? O20 Cl2 O19 113.7(4) . . ? O12 Cl2 O19 109.9(4) . . ? O20 Cl2 O18A 111.8(12) . . ? O12 Cl2 O18A 136.0(12) . . ? O19 Cl2 O18A 61.5(13) . . ? O20 Cl2 O18 107.9(4) . . ? O12 Cl2 O18 106.1(3) . . ? O19 Cl2 O18 108.2(5) . . ? O18A Cl2 O18 49.5(13) . . ? O20 Cl2 O19A 82.4(15) . . ? O12 Cl2 O19A 102.0(13) . . ? O19 Cl2 O19A 39.4(13) . . ? O18A Cl2 O19A 94.4(18) . . ? O18 Cl2 O19A 143.9(14) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.592 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.124 data_mo_mml6_ni_0m _database_code_depnum_ccdc_archive 'CCDC 918505' #TrackingRef 'Ni2L2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C109 H78 Cl8 N29 Ni4 O51 S8' _chemical_formula_weight 3384.92 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7357(5) _cell_length_b 13.4575(6) _cell_length_c 23.2619(11) _cell_angle_alpha 82.9930(10) _cell_angle_beta 78.8390(10) _cell_angle_gamma 82.3710(10) _cell_volume 3252.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9659 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 33.05 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1719 _exptl_absorpt_coefficient_mu 0.968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8299 _exptl_absorpt_correction_T_max 0.9532 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 57654 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0950 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 30.53 _reflns_number_total 19730 _reflns_number_gt 11017 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0809P)^2^+0.8773P] 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 19730 _refine_ls_number_parameters 983 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.1322 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1773 _refine_ls_wR_factor_gt 0.1483 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.037 _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 Ni1 Ni 0.85312(4) 0.35475(3) 0.26082(2) 0.02048(11) Uani 1 1 d . . . Ni2 Ni 0.47380(4) 0.25339(3) 0.25020(2) 0.02239(11) Uani 1 1 d . . . S1 S 0.51252(11) 0.27405(8) 0.43316(5) 0.0339(2) Uani 1 1 d . . . S2 S 0.59055(11) 0.62359(7) 0.21605(5) 0.0369(3) Uani 1 1 d . . . S3 S 0.66983(12) 0.32600(8) 0.06817(5) 0.0407(3) Uani 1 1 d . . . S4 S 0.86950(11) 0.02579(6) 0.28024(5) 0.0397(3) Uani 1 1 d . . . Cl1 Cl 0.59976(10) 0.31543(7) 0.57731(4) 0.0347(2) Uani 1 1 d . . . Cl2 Cl 0.95117(13) 0.79171(8) 0.19786(6) 0.0521(3) Uani 1 1 d . . . Cl3 Cl 0.82609(15) 0.85952(9) 0.47079(7) 0.0625(4) Uani 1 1 d . . . Cl4 Cl 0.37484(13) 0.29520(13) 0.97992(6) 0.0629(4) Uani 1 1 d . . . N1 N 0.4803(3) 0.0901(2) 0.17860(16) 0.0329(8) Uani 1 1 d . . . N2 N 0.5208(3) 0.1180(2) 0.29618(15) 0.0279(7) Uani 1 1 d . . . N3 N 0.5309(3) 0.3025(2) 0.32121(13) 0.0229(6) Uani 1 1 d . . . N4 N 0.6854(3) 0.45142(19) 0.25564(13) 0.0223(6) Uani 1 1 d . . . N5 N 0.8911(3) 0.4190(2) 0.17572(14) 0.0253(7) Uani 1 1 d . . . N6 N 1.0789(3) 0.2479(2) 0.19917(16) 0.0313(7) Uani 1 1 d . . . N7 N 0.2417(3) 0.3360(3) 0.32321(17) 0.0411(9) Uani 1 1 d . . . N8 N 0.3982(3) 0.3825(2) 0.20744(15) 0.0280(7) Uani 1 1 d . . . N9 N 0.6232(3) 0.2777(2) 0.17883(13) 0.0240(6) Uani 1 1 d . . . N10 N 0.8082(3) 0.21236(19) 0.25138(14) 0.0231(6) Uani 1 1 d . . . N11 N 0.8407(3) 0.2904(2) 0.34563(13) 0.0227(6) Uani 1 1 d . . . N12 N 0.8631(3) 0.5052(2) 0.33803(14) 0.0248(7) Uani 1 1 d . . . N13 N 0.7480(5) 0.1782(4) 0.9335(2) 0.0718(15) Uani 1 1 d . . . N14 N 0.2432(6) 0.8306(5) 0.2809(3) 0.0788(16) Uani 1 1 d . . . O1 O 0.4059(3) 0.16984(18) 0.19899(13) 0.0332(6) Uani 1 1 d . . . O2 O 0.2936(3) 0.2522(2) 0.29871(13) 0.0367(7) Uani 1 1 d . . . O3 O 1.0427(2) 0.30064(19) 0.24554(12) 0.0303(6) Uani 1 1 d . . . O4 O 0.9259(2) 0.46650(17) 0.28937(11) 0.0269(6) Uani 1 1 d . . . O5 O 0.5033(4) 0.2929(2) 0.62763(14) 0.0557(9) Uani 1 1 d . . . O6 O 0.6936(4) 0.3653(3) 0.59392(18) 0.0712(12) Uani 1 1 d . . . O7 O 0.5429(3) 0.3818(2) 0.53356(15) 0.0517(9) Uani 1 1 d . . . O8 O 0.6549(4) 0.2245(2) 0.55233(16) 0.0602(10) Uani 1 1 d . . . O9 O 0.8583(5) 0.8140(3) 0.2493(2) 0.0849(14) Uani 1 1 d . A . O11 O 1.0269(4) 0.8699(3) 0.1820(3) 0.106(2) Uani 1 1 d . A . O12 O 0.8767(7) 0.7998(5) 0.1521(3) 0.157(3) Uani 1 1 d . A . O13 O 0.9056(7) 0.7662(3) 0.4781(3) 0.160(3) Uani 1 1 d . . . O14 O 0.8425(5) 0.8899(3) 0.4087(2) 0.0930(16) Uani 1 1 d . . . O15 O 0.8579(7) 0.9354(3) 0.5003(3) 0.136(3) Uani 1 1 d . . . O16 O 0.7017(6) 0.8394(5) 0.4872(3) 0.149(3) Uani 1 1 d . . . O17 O 0.2675(4) 0.2518(3) 0.96988(18) 0.0771(12) Uani 1 1 d . B . O18 O 0.4304(5) 0.3411(4) 0.9273(3) 0.126(2) Uani 1 1 d . B . O19 O 0.4605(6) 0.2112(7) 0.9958(3) 0.189(4) Uani 1 1 d . B . O21 O 0.7469(6) 0.0925(4) 0.9570(3) 0.117(2) Uani 1 1 d . . . O22 O 0.7934(5) 0.2449(4) 0.9507(2) 0.0866(14) Uani 1 1 d . . . O23 O 0.2927(6) 0.7516(5) 0.2649(2) 0.152(3) Uani 1 1 d . . . O24 O 0.2714(6) 0.9105(6) 0.2553(3) 0.135(2) Uani 1 1 d . . . C1 C 0.4972(5) 0.0837(3) 0.1197(2) 0.0444(11) Uani 1 1 d . . . H1 H 0.4615 0.1374 0.0953 0.053 Uiso 1 1 calc R . . C2 C 0.5649(6) 0.0011(4) 0.0949(2) 0.0590(14) Uani 1 1 d . . . H2 H 0.5755 -0.0033 0.0537 0.071 Uiso 1 1 calc R . . C3 C 0.6168(6) -0.0751(4) 0.1308(3) 0.0605(15) Uani 1 1 d . . . H3 H 0.6642 -0.1330 0.1144 0.073 Uiso 1 1 calc R . . C4 C 0.6009(5) -0.0685(3) 0.1903(2) 0.0474(12) Uani 1 1 d . . . H4 H 0.6368 -0.1220 0.2148 0.057 Uiso 1 1 calc R . . C5 C 0.5324(4) 0.0163(3) 0.2151(2) 0.0362(10) Uani 1 1 d . . . C6 C 0.5211(4) 0.0262(3) 0.27900(19) 0.0336(9) Uani 1 1 d . . . C7 C 0.5208(5) -0.0596(3) 0.3197(2) 0.0448(12) Uani 1 1 d . . . H7 H 0.5207 -0.1242 0.3072 0.054 Uiso 1 1 calc R . . C8 C 0.5206(5) -0.0495(3) 0.3775(2) 0.0537(14) Uani 1 1 d . . . H8 H 0.5209 -0.1074 0.4054 0.064 Uiso 1 1 calc R . . C9 C 0.5201(5) 0.0457(3) 0.3957(2) 0.0436(11) Uani 1 1 d . . . H9 H 0.5205 0.0540 0.4356 0.052 Uiso 1 1 calc R . . C10 C 0.5191(4) 0.1271(3) 0.35367(18) 0.0309(9) Uani 1 1 d . . . C11 C 0.5213(4) 0.2315(3) 0.36590(17) 0.0274(8) Uani 1 1 d . . . C12 C 0.5244(4) 0.3939(3) 0.39967(18) 0.0304(8) Uani 1 1 d . . . H12 H 0.5235 0.4515 0.4197 0.036 Uiso 1 1 calc R . . C13 C 0.5355(3) 0.3949(3) 0.34018(17) 0.0244(8) Uani 1 1 d . . . C14 C 0.5721(4) 0.4748(2) 0.29359(17) 0.0239(7) Uani 1 1 d . . . C15 C 0.5096(4) 0.5665(3) 0.27900(18) 0.0305(8) Uani 1 1 d . . . H15 H 0.4316 0.5948 0.3009 0.037 Uiso 1 1 calc R . . C16 C 0.7071(4) 0.5228(2) 0.21239(17) 0.0255(8) Uani 1 1 d . . . C17 C 0.8208(4) 0.5084(3) 0.16637(17) 0.0280(8) Uani 1 1 d . . . C18 C 0.8557(5) 0.5761(3) 0.11773(19) 0.0399(10) Uani 1 1 d . . . H18 H 0.8062 0.6393 0.1122 0.048 Uiso 1 1 calc R . . C19 C 0.9638(5) 0.5497(4) 0.0777(2) 0.0475(12) Uani 1 1 d . . . H19 H 0.9905 0.5954 0.0445 0.057 Uiso 1 1 calc R . . C20 C 1.0337(4) 0.4564(4) 0.0858(2) 0.0422(11) Uani 1 1 d . . . H20 H 1.1066 0.4368 0.0576 0.051 Uiso 1 1 calc R . . C21 C 0.9960(4) 0.3920(3) 0.13570(17) 0.0306(8) Uani 1 1 d . . . C22 C 1.0619(4) 0.2891(3) 0.14434(19) 0.0327(9) Uani 1 1 d . . . C23 C 1.1050(4) 0.2322(3) 0.0972(2) 0.0438(11) Uani 1 1 d . . . H23 H 1.0973 0.2609 0.0585 0.053 Uiso 1 1 calc R . . C24 C 1.1597(5) 0.1326(4) 0.1064(3) 0.0545(14) Uani 1 1 d . . . H24 H 1.1866 0.0926 0.0743 0.065 Uiso 1 1 calc R . . C25 C 1.1739(4) 0.0935(4) 0.1625(3) 0.0500(13) Uani 1 1 d . . . H25 H 1.2109 0.0260 0.1696 0.060 Uiso 1 1 calc R . . C26 C 1.1343(4) 0.1525(3) 0.2082(2) 0.0392(10) Uani 1 1 d . . . H26 H 1.1461 0.1259 0.2468 0.047 Uiso 1 1 calc R . . C27 C 0.1960(4) 0.3274(5) 0.3818(2) 0.0558(14) Uani 1 1 d . . . H27 H 0.2025 0.2632 0.4038 0.067 Uiso 1 1 calc R . . C28 C 0.1403(5) 0.4105(6) 0.4099(3) 0.0680(18) Uani 1 1 d . . . H28 H 0.1080 0.4035 0.4510 0.082 Uiso 1 1 calc R . . C29 C 0.1313(5) 0.5030(5) 0.3788(3) 0.0676(18) Uani 1 1 d . . . H29 H 0.0936 0.5610 0.3980 0.081 Uiso 1 1 calc R . . C30 C 0.1774(4) 0.5111(4) 0.3197(3) 0.0515(13) Uani 1 1 d . . . H30 H 0.1704 0.5753 0.2978 0.062 Uiso 1 1 calc R . . C31 C 0.2349(4) 0.4266(3) 0.2904(2) 0.0401(10) Uani 1 1 d . . . C32 C 0.2879(4) 0.4370(3) 0.22707(19) 0.0323(9) Uani 1 1 d . . . C33 C 0.2285(5) 0.5083(3) 0.1895(2) 0.0446(12) Uani 1 1 d . . . H33 H 0.1482 0.5441 0.2036 0.054 Uiso 1 1 calc R . . C34 C 0.2874(5) 0.5263(3) 0.1320(2) 0.0485(13) Uani 1 1 d . . . H34 H 0.2485 0.5758 0.1063 0.058 Uiso 1 1 calc R . . C35 C 0.4039(5) 0.4723(3) 0.1114(2) 0.0403(11) Uani 1 1 d . . . H35 H 0.4465 0.4843 0.0718 0.048 Uiso 1 1 calc R . . C36 C 0.4557(4) 0.4000(2) 0.15080(18) 0.0287(8) Uani 1 1 d . . . C37 C 0.5780(4) 0.3366(3) 0.13616(17) 0.0278(8) Uani 1 1 d . . . C38 C 0.7763(4) 0.2391(3) 0.09897(19) 0.0363(9) Uani 1 1 d . . . H38 H 0.8517 0.2062 0.0775 0.044 Uiso 1 1 calc R . . C39 C 0.7383(4) 0.2238(2) 0.15807(17) 0.0261(8) Uani 1 1 d . . . C40 C 0.7988(4) 0.1626(3) 0.20419(17) 0.0277(8) Uani 1 1 d . . . C41 C 0.8338(4) 0.0614(3) 0.2114(2) 0.0365(10) Uani 1 1 d . . . H41 H 0.8378 0.0167 0.1823 0.044 Uiso 1 1 calc R . . C42 C 0.8411(4) 0.1493(2) 0.29533(18) 0.0281(8) Uani 1 1 d . . . C43 C 0.8543(4) 0.1886(3) 0.34966(18) 0.0288(8) Uani 1 1 d . . . C44 C 0.8746(4) 0.1291(3) 0.40032(19) 0.0360(10) Uani 1 1 d . . . H44 H 0.8830 0.0577 0.4019 0.043 Uiso 1 1 calc R . . C45 C 0.8825(4) 0.1766(3) 0.44901(19) 0.0379(10) Uani 1 1 d . . . H45 H 0.8955 0.1378 0.4847 0.045 Uiso 1 1 calc R . . C46 C 0.8714(4) 0.2801(3) 0.44547(18) 0.0332(9) Uani 1 1 d . . . H46 H 0.8788 0.3131 0.4783 0.040 Uiso 1 1 calc R . . C47 C 0.8491(4) 0.3361(2) 0.39304(17) 0.0261(8) Uani 1 1 d . . . C48 C 0.8283(3) 0.4468(3) 0.38997(17) 0.0256(8) Uani 1 1 d . . . C49 C 0.7727(4) 0.4968(3) 0.43961(19) 0.0346(9) Uani 1 1 d . . . H49 H 0.7470 0.4583 0.4761 0.041 Uiso 1 1 calc R . . C50 C 0.7544(4) 0.6005(3) 0.4368(2) 0.0416(11) Uani 1 1 d . . . H50 H 0.7182 0.6331 0.4712 0.050 Uiso 1 1 calc R . . C51 C 0.7889(5) 0.6564(3) 0.3839(2) 0.0428(11) Uani 1 1 d . . . H51 H 0.7762 0.7279 0.3812 0.051 Uiso 1 1 calc R . . C52 C 0.8425(4) 0.6071(3) 0.3349(2) 0.0377(10) Uani 1 1 d . . . H52 H 0.8653 0.6454 0.2981 0.045 Uiso 1 1 calc R . . C53 C 0.6916(6) 0.2015(5) 0.8796(3) 0.0660(15) Uani 1 1 d . . . H53A H 0.6716 0.1391 0.8675 0.099 Uiso 1 1 calc R . . H53B H 0.7526 0.2331 0.8481 0.099 Uiso 1 1 calc R . . H53C H 0.6131 0.2478 0.8876 0.099 Uiso 1 1 calc R . . C54 C 0.1408(7) 0.8353(5) 0.3326(3) 0.0777(19) Uani 1 1 d . . . H54A H 0.0602 0.8250 0.3217 0.117 Uiso 1 1 calc R . . H54B H 0.1324 0.9015 0.3474 0.117 Uiso 1 1 calc R . . H54C H 0.1615 0.7827 0.3634 0.117 Uiso 1 1 calc R . . C1S C 0.9392(16) 0.9592(13) 0.0378(7) 0.081(4) Uani 0.50 1 d PU . . N1S N 1.0000 1.0000 0.0000 0.107(3) Uani 1 2 d SU . . O10 O 1.0134(8) 0.6973(4) 0.2008(4) 0.084(4) Uani 0.80(2) 1 d P A 1 O10' O 1.0547(18) 0.730(2) 0.2354(14) 0.067(11) Uani 0.20(2) 1 d P A 2 O20 O 0.3511(9) 0.3264(11) 1.0352(5) 0.118(7) Uani 0.601(18) 1 d P B 1 O20' O 0.3010(12) 0.4010(10) 0.9964(7) 0.082(5) Uani 0.399(18) 1 d P B 2 O1S O 0.9556(11) 0.9078(7) 0.0079(5) 0.094(3) Uani 0.50 1 d PU . . O2S O 0.9415(9) 1.0339(7) 0.0579(4) 0.080(2) Uani 0.50 1 d PU . . O1W O 0.1789(8) 0.0784(6) 0.3540(4) 0.079(3) Uani 0.50 1 d PDU . . H1W H 0.2194 0.0622 0.3824 0.095 Uiso 0.50 1 d PRD . . H2W H 0.2066 0.1311 0.3346 0.095 Uiso 0.50 1 d PRD . . 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 Ni1 0.0181(2) 0.01936(18) 0.0235(3) -0.00005(16) -0.00414(19) -0.00189(16) Ni2 0.0201(3) 0.0236(2) 0.0247(3) -0.00005(17) -0.0077(2) -0.00331(17) S1 0.0377(6) 0.0418(5) 0.0233(5) -0.0001(4) -0.0049(4) -0.0121(4) S2 0.0446(7) 0.0233(4) 0.0390(6) 0.0015(4) -0.0093(5) 0.0076(4) S3 0.0468(7) 0.0506(6) 0.0236(5) -0.0015(4) -0.0050(5) -0.0051(5) S4 0.0457(7) 0.0202(4) 0.0586(7) -0.0062(4) -0.0263(6) 0.0044(4) Cl1 0.0426(6) 0.0307(4) 0.0313(5) -0.0035(4) -0.0048(5) -0.0084(4) Cl2 0.0632(9) 0.0371(5) 0.0528(8) -0.0049(5) 0.0003(7) -0.0088(5) Cl3 0.0802(10) 0.0435(6) 0.0742(10) 0.0196(6) -0.0406(8) -0.0287(6) Cl4 0.0356(7) 0.1035(11) 0.0460(8) -0.0155(8) 0.0015(6) -0.0007(7) N1 0.033(2) 0.0323(15) 0.038(2) -0.0055(14) -0.0123(16) -0.0103(14) N2 0.0239(17) 0.0274(14) 0.0336(19) 0.0017(13) -0.0069(15) -0.0096(12) N3 0.0180(16) 0.0273(13) 0.0240(16) -0.0024(12) -0.0037(13) -0.0043(11) N4 0.0215(16) 0.0214(12) 0.0243(16) -0.0021(11) -0.0057(13) -0.0016(11) N5 0.0229(17) 0.0272(13) 0.0251(17) -0.0030(12) -0.0002(14) -0.0060(12) N6 0.0145(16) 0.0403(16) 0.039(2) -0.0125(15) -0.0016(15) -0.0012(13) N7 0.0206(19) 0.063(2) 0.043(2) -0.0144(19) -0.0071(17) -0.0068(16) N8 0.0238(17) 0.0259(13) 0.036(2) -0.0071(13) -0.0103(15) 0.0004(12) N9 0.0243(17) 0.0240(13) 0.0251(17) -0.0029(12) -0.0077(14) -0.0024(12) N10 0.0182(16) 0.0198(12) 0.0323(18) -0.0018(12) -0.0084(14) -0.0004(11) N11 0.0182(16) 0.0245(13) 0.0262(17) -0.0005(12) -0.0058(13) -0.0049(11) N12 0.0242(17) 0.0251(13) 0.0258(17) -0.0038(12) -0.0053(14) -0.0026(12) N13 0.066(4) 0.062(3) 0.070(4) -0.004(3) 0.005(3) 0.028(3) N14 0.065(4) 0.102(4) 0.065(4) 0.017(3) -0.031(3) 0.012(3) O1 0.0327(16) 0.0290(12) 0.0426(17) -0.0049(12) -0.0176(14) -0.0028(11) O2 0.0216(15) 0.0480(16) 0.0402(18) -0.0038(13) -0.0031(13) -0.0066(12) O3 0.0193(14) 0.0388(13) 0.0334(16) -0.0119(12) -0.0045(12) 0.0017(11) O4 0.0244(14) 0.0286(12) 0.0278(15) -0.0062(10) 0.0002(12) -0.0076(10) O5 0.079(3) 0.0482(18) 0.0341(19) -0.0038(14) 0.0118(18) -0.0194(17) O6 0.075(3) 0.076(2) 0.077(3) 0.005(2) -0.036(2) -0.039(2) O7 0.062(2) 0.0496(17) 0.045(2) 0.0024(15) -0.0157(18) -0.0079(16) O8 0.067(3) 0.0436(17) 0.062(2) -0.0140(16) 0.008(2) 0.0010(16) O9 0.094(3) 0.055(2) 0.081(3) 0.010(2) 0.019(3) 0.011(2) O11 0.073(3) 0.0385(19) 0.184(6) -0.015(3) 0.038(3) -0.0067(19) O12 0.160(7) 0.171(6) 0.166(7) -0.073(5) -0.085(5) 0.024(5) O13 0.232(7) 0.050(2) 0.254(8) 0.013(3) -0.202(7) -0.008(3) O14 0.139(5) 0.056(2) 0.077(3) 0.010(2) 0.000(3) -0.027(3) O15 0.225(7) 0.055(2) 0.171(6) 0.009(3) -0.141(5) -0.039(3) O16 0.123(5) 0.169(6) 0.160(6) -0.038(5) 0.024(5) -0.090(5) O17 0.083(3) 0.089(3) 0.066(3) -0.001(2) -0.028(2) -0.020(2) O18 0.080(4) 0.109(4) 0.155(6) 0.036(4) 0.032(4) -0.007(3) O19 0.101(5) 0.305(10) 0.122(6) 0.096(6) -0.032(4) 0.032(6) O21 0.118(5) 0.080(3) 0.123(5) 0.026(3) 0.003(4) 0.029(3) O22 0.101(4) 0.090(3) 0.067(3) -0.024(3) -0.017(3) 0.017(3) O23 0.162(6) 0.183(6) 0.069(4) -0.001(4) -0.019(4) 0.123(5) O24 0.116(5) 0.192(7) 0.115(5) 0.037(5) -0.047(4) -0.090(5) C1 0.053(3) 0.043(2) 0.045(3) -0.007(2) -0.019(2) -0.014(2) C2 0.079(4) 0.053(3) 0.053(3) -0.023(2) -0.021(3) -0.008(3) C3 0.069(4) 0.046(3) 0.075(4) -0.032(3) -0.022(3) 0.003(2) C4 0.062(3) 0.0299(19) 0.057(3) -0.0118(19) -0.024(3) -0.004(2) C5 0.041(3) 0.0253(16) 0.048(3) -0.0020(16) -0.019(2) -0.0106(16) C6 0.039(2) 0.0252(16) 0.040(2) 0.0028(16) -0.017(2) -0.0084(16) C7 0.055(3) 0.0266(18) 0.059(3) 0.0060(19) -0.025(3) -0.0141(18) C8 0.080(4) 0.033(2) 0.054(3) 0.012(2) -0.025(3) -0.023(2) C9 0.059(3) 0.041(2) 0.036(3) 0.0080(18) -0.018(2) -0.016(2) C10 0.033(2) 0.0310(17) 0.031(2) 0.0040(15) -0.0102(18) -0.0115(16) C11 0.022(2) 0.0348(17) 0.027(2) 0.0018(15) -0.0073(16) -0.0102(15) C12 0.026(2) 0.0339(18) 0.033(2) -0.0071(16) -0.0050(18) -0.0048(15) C13 0.0151(18) 0.0295(16) 0.029(2) -0.0049(15) -0.0046(16) -0.0015(13) C14 0.0216(19) 0.0252(15) 0.027(2) -0.0066(14) -0.0072(16) -0.0028(13) C15 0.031(2) 0.0293(17) 0.030(2) -0.0080(15) -0.0055(18) 0.0045(15) C16 0.025(2) 0.0222(14) 0.029(2) -0.0007(14) -0.0069(17) -0.0003(13) C17 0.031(2) 0.0282(16) 0.024(2) 0.0015(14) -0.0059(17) -0.0044(15) C18 0.048(3) 0.039(2) 0.033(2) 0.0101(18) -0.010(2) -0.0124(19) C19 0.055(3) 0.058(3) 0.027(2) 0.012(2) -0.003(2) -0.022(2) C20 0.034(3) 0.061(3) 0.031(2) -0.006(2) 0.003(2) -0.016(2) C21 0.025(2) 0.045(2) 0.022(2) -0.0061(16) -0.0003(17) -0.0115(17) C22 0.020(2) 0.044(2) 0.033(2) -0.0116(18) 0.0019(18) -0.0061(16) C23 0.029(2) 0.059(3) 0.041(3) -0.019(2) 0.005(2) -0.001(2) C24 0.035(3) 0.066(3) 0.066(4) -0.039(3) -0.003(3) 0.005(2) C25 0.032(3) 0.050(2) 0.073(4) -0.030(3) -0.014(3) 0.008(2) C26 0.024(2) 0.041(2) 0.054(3) -0.015(2) -0.013(2) 0.0062(17) C27 0.020(2) 0.105(4) 0.045(3) -0.015(3) -0.004(2) -0.017(3) C28 0.029(3) 0.124(5) 0.060(4) -0.045(4) 0.002(3) -0.018(3) C29 0.029(3) 0.097(4) 0.088(5) -0.061(4) -0.003(3) -0.010(3) C30 0.026(2) 0.066(3) 0.070(4) -0.036(3) -0.009(2) -0.005(2) C31 0.017(2) 0.055(2) 0.053(3) -0.021(2) -0.011(2) 0.0005(18) C32 0.026(2) 0.0292(17) 0.046(3) -0.0125(17) -0.016(2) 0.0026(15) C33 0.039(3) 0.0304(19) 0.071(4) -0.012(2) -0.029(3) 0.0084(18) C34 0.052(3) 0.0315(19) 0.070(4) 0.000(2) -0.039(3) 0.0031(19) C35 0.050(3) 0.0330(19) 0.041(3) 0.0080(18) -0.023(2) -0.0062(19) C36 0.032(2) 0.0248(16) 0.033(2) -0.0024(15) -0.0143(18) -0.0038(15) C37 0.032(2) 0.0282(16) 0.027(2) -0.0032(15) -0.0103(17) -0.0080(15) C38 0.029(2) 0.044(2) 0.035(2) -0.0143(18) -0.0004(19) -0.0017(18) C39 0.026(2) 0.0256(15) 0.028(2) -0.0082(14) -0.0040(17) -0.0032(14) C40 0.023(2) 0.0279(16) 0.033(2) -0.0087(15) -0.0050(17) -0.0013(14) C41 0.033(2) 0.0294(17) 0.052(3) -0.0132(18) -0.020(2) 0.0049(16) C42 0.023(2) 0.0207(14) 0.041(2) -0.0036(15) -0.0073(18) -0.0012(13) C43 0.025(2) 0.0256(16) 0.038(2) 0.0013(15) -0.0119(18) -0.0054(14) C44 0.042(3) 0.0230(16) 0.043(3) 0.0083(16) -0.016(2) -0.0038(16) C45 0.043(3) 0.0356(19) 0.035(2) 0.0098(17) -0.014(2) -0.0066(18) C46 0.034(2) 0.0373(19) 0.031(2) -0.0005(16) -0.0128(19) -0.0063(17) C47 0.0203(19) 0.0274(16) 0.030(2) 0.0015(15) -0.0050(16) -0.0047(14) C48 0.0169(18) 0.0301(16) 0.030(2) -0.0012(15) -0.0046(16) -0.0041(14) C49 0.030(2) 0.041(2) 0.034(2) -0.0070(17) -0.0026(19) -0.0094(17) C50 0.034(3) 0.045(2) 0.047(3) -0.022(2) -0.004(2) -0.0007(19) C51 0.049(3) 0.0291(18) 0.050(3) -0.0098(19) -0.010(2) 0.0029(18) C52 0.046(3) 0.0269(17) 0.040(3) -0.0019(17) -0.012(2) 0.0004(17) C53 0.053(4) 0.084(4) 0.057(4) -0.015(3) 0.002(3) -0.001(3) C54 0.083(5) 0.071(4) 0.067(4) -0.006(3) -0.003(4) 0.021(3) C1S 0.082(8) 0.087(8) 0.077(8) -0.017(7) -0.012(7) -0.011(7) N1S 0.108(7) 0.097(6) 0.138(8) -0.036(6) -0.080(6) 0.021(5) O10 0.074(5) 0.037(2) 0.123(7) -0.003(3) 0.006(5) 0.016(3) O10' 0.045(11) 0.050(13) 0.11(2) 0.031(13) -0.045(12) 0.010(8) O20 0.059(6) 0.193(14) 0.121(10) -0.118(10) 0.019(6) -0.048(7) O20' 0.063(8) 0.094(9) 0.093(11) -0.054(8) -0.014(7) 0.024(6) O1S 0.115(7) 0.080(5) 0.102(6) -0.007(5) -0.041(6) -0.034(5) O2S 0.092(6) 0.089(5) 0.059(5) -0.017(4) -0.015(4) -0.001(5) O1W 0.087(7) 0.068(5) 0.088(7) -0.017(4) -0.015(5) -0.024(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 Ni1 O4 2.017(2) . ? Ni1 N11 2.043(3) . ? Ni1 O3 2.046(3) . ? Ni1 N5 2.049(3) . ? Ni1 N10 2.084(3) . ? Ni1 N4 2.091(3) . ? Ni2 O1 2.024(3) . ? Ni2 O2 2.043(3) . ? Ni2 N8 2.045(3) . ? Ni2 N2 2.051(3) . ? Ni2 N3 2.075(3) . ? Ni2 N9 2.101(3) . ? S1 C11 1.712(4) . ? S1 C12 1.713(4) . ? S2 C15 1.703(4) . ? S2 C16 1.717(4) . ? S3 C37 1.706(4) . ? S3 C38 1.717(4) . ? S4 C41 1.716(4) . ? S4 C42 1.717(3) . ? Cl1 O6 1.417(4) . ? Cl1 O8 1.427(3) . ? Cl1 O5 1.436(3) . ? Cl1 O7 1.442(3) . ? Cl2 O10 1.355(5) . ? Cl2 O11 1.386(4) . ? Cl2 O9 1.435(4) . ? Cl2 O12 1.436(6) . ? Cl2 O10' 1.625(18) . ? Cl3 O16 1.370(6) . ? Cl3 O15 1.409(4) . ? Cl3 O13 1.433(5) . ? Cl3 O14 1.436(5) . ? Cl4 O18 1.365(5) . ? Cl4 O20 1.367(8) . ? Cl4 O19 1.419(7) . ? Cl4 O17 1.429(4) . ? Cl4 O20' 1.587(11) . ? N1 O1 1.329(4) . ? N1 C1 1.358(6) . ? N1 C5 1.361(5) . ? N2 C6 1.343(4) . ? N2 C10 1.354(5) . ? N3 C11 1.322(4) . ? N3 C13 1.380(4) . ? N4 C16 1.313(4) . ? N4 C14 1.381(5) . ? N5 C17 1.350(4) . ? N5 C21 1.354(5) . ? N6 O3 1.330(4) . ? N6 C26 1.351(5) . ? N6 C22 1.363(5) . ? N7 O2 1.332(4) . ? N7 C27 1.354(6) . ? N7 C31 1.358(6) . ? N8 C32 1.338(5) . ? N8 C36 1.349(5) . ? N9 C37 1.319(5) . ? N9 C39 1.379(5) . ? N10 C42 1.318(5) . ? N10 C40 1.380(5) . ? N11 C47 1.350(5) . ? N11 C43 1.352(4) . ? N12 O4 1.328(4) . ? N12 C52 1.355(4) . ? N12 C48 1.374(5) . ? N13 O21 1.215(6) . ? N13 O22 1.218(7) . ? N13 C53 1.477(8) . ? N14 O23 1.192(7) . ? N14 O24 1.209(7) . ? N14 C54 1.465(8) . ? C1 C2 1.370(7) . ? C1 H1 0.9500 . ? C2 C3 1.371(7) . ? C2 H2 0.9500 . ? C3 C4 1.375(7) . ? C3 H3 0.9500 . ? C4 C5 1.396(6) . ? C4 H4 0.9500 . ? C5 C6 1.488(6) . ? C6 C7 1.401(5) . ? C7 C8 1.369(7) . ? C7 H7 0.9500 . ? C8 C9 1.396(6) . ? C8 H8 0.9500 . ? C9 C10 1.377(5) . ? C9 H9 0.9500 . ? C10 C11 1.470(5) . ? C12 C13 1.364(5) . ? C12 H12 0.9500 . ? C13 C14 1.465(5) . ? C14 C15 1.362(5) . ? C15 H15 0.9500 . ? C16 C17 1.468(5) . ? C17 C18 1.388(5) . ? C18 C19 1.376(7) . ? C18 H18 0.9500 . ? C19 C20 1.387(7) . ? C19 H19 0.9500 . ? C20 C21 1.388(6) . ? C20 H20 0.9500 . ? C21 C22 1.479(6) . ? C22 C23 1.384(6) . ? C23 C24 1.399(7) . ? C23 H23 0.9500 . ? C24 C25 1.376(7) . ? C24 H24 0.9500 . ? C25 C26 1.373(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.372(8) . ? C27 H27 0.9500 . ? C28 C29 1.364(9) . ? C28 H28 0.9500 . ? C29 C30 1.365(8) . ? C29 H29 0.9500 . ? C30 C31 1.405(6) . ? C30 H30 0.9500 . ? C31 C32 1.470(6) . ? C32 C33 1.392(6) . ? C33 C34 1.372(7) . ? C33 H33 0.9500 . ? C34 C35 1.391(7) . ? C34 H34 0.9500 . ? C35 C36 1.390(5) . ? C35 H35 0.9500 . ? C36 C37 1.472(5) . ? C38 C39 1.355(6) . ? C38 H38 0.9500 . ? C39 C40 1.471(5) . ? C40 C41 1.362(5) . ? C41 H41 0.9500 . ? C42 C43 1.466(5) . ? C43 C44 1.378(5) . ? C44 C45 1.388(6) . ? C44 H44 0.9500 . ? C45 C46 1.375(5) . ? C45 H45 0.9500 . ? C46 C47 1.398(5) . ? C46 H46 0.9500 . ? C47 C48 1.473(5) . ? C48 C49 1.398(6) . ? C49 C50 1.380(5) . ? C49 H49 0.9500 . ? C50 C51 1.374(6) . ? C50 H50 0.9500 . ? C51 C52 1.379(6) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C1S O1S 1.014(17) . ? C1S N1S 1.120(16) . ? C1S O2S 1.164(18) . ? N1S C1S 1.120(16) 2_775 ? N1S O1S 1.367(9) 2_775 ? N1S O1S 1.367(9) . ? N1S O2S 1.470(9) . ? N1S O2S 1.470(9) 2_775 ? O1W H1W 0.8500 . ? O1W H2W 0.8502 . ? 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 O4 Ni1 N11 84.99(11) . . ? O4 Ni1 O3 80.62(10) . . ? N11 Ni1 O3 88.83(11) . . ? O4 Ni1 N5 90.88(11) . . ? N11 Ni1 N5 172.34(12) . . ? O3 Ni1 N5 84.12(12) . . ? O4 Ni1 N10 161.68(11) . . ? N11 Ni1 N10 79.66(11) . . ? O3 Ni1 N10 89.06(11) . . ? N5 Ni1 N10 103.16(12) . . ? O4 Ni1 N4 88.92(10) . . ? N11 Ni1 N4 107.70(12) . . ? O3 Ni1 N4 159.66(11) . . ? N5 Ni1 N4 78.61(12) . . ? N10 Ni1 N4 105.20(11) . . ? O1 Ni2 O2 82.93(12) . . ? O1 Ni2 N8 90.17(11) . . ? O2 Ni2 N8 84.35(12) . . ? O1 Ni2 N2 85.05(11) . . ? O2 Ni2 N2 87.49(12) . . ? N8 Ni2 N2 170.99(13) . . ? O1 Ni2 N3 162.71(11) . . ? O2 Ni2 N3 88.66(12) . . ? N8 Ni2 N3 104.05(11) . . ? N2 Ni2 N3 79.50(12) . . ? O1 Ni2 N9 87.12(12) . . ? O2 Ni2 N9 160.62(12) . . ? N8 Ni2 N9 79.08(12) . . ? N2 Ni2 N9 108.23(12) . . ? N3 Ni2 N9 104.98(11) . . ? C11 S1 C12 89.81(18) . . ? C15 S2 C16 90.15(18) . . ? C37 S3 C38 89.7(2) . . ? C41 S4 C42 89.78(18) . . ? O6 Cl1 O8 111.3(3) . . ? O6 Cl1 O5 110.0(2) . . ? O8 Cl1 O5 109.4(2) . . ? O6 Cl1 O7 107.9(2) . . ? O8 Cl1 O7 108.5(2) . . ? O5 Cl1 O7 109.7(2) . . ? O10 Cl2 O11 116.3(4) . . ? O10 Cl2 O9 114.7(3) . . ? O11 Cl2 O9 108.9(3) . . ? O10 Cl2 O12 107.5(6) . . ? O11 Cl2 O12 104.4(4) . . ? O9 Cl2 O12 103.8(4) . . ? O10 Cl2 O10' 44.1(10) . . ? O11 Cl2 O10' 90.5(9) . . ? O9 Cl2 O10' 93.9(11) . . ? O12 Cl2 O10' 151.4(14) . . ? O16 Cl3 O15 114.2(4) . . ? O16 Cl3 O13 107.4(4) . . ? O15 Cl3 O13 112.5(3) . . ? O16 Cl3 O14 105.4(4) . . ? O15 Cl3 O14 110.0(3) . . ? O13 Cl3 O14 106.8(4) . . ? O18 Cl4 O20 130.4(7) . . ? O18 Cl4 O19 107.8(4) . . ? O20 Cl4 O19 92.7(8) . . ? O18 Cl4 O17 107.6(4) . . ? O20 Cl4 O17 110.2(4) . . ? O19 Cl4 O17 104.3(4) . . ? O18 Cl4 O20' 89.1(6) . . ? O20 Cl4 O20' 55.6(6) . . ? O19 Cl4 O20' 146.7(7) . . ? O17 Cl4 O20' 97.1(5) . . ? O1 N1 C1 116.6(3) . . ? O1 N1 C5 121.7(3) . . ? C1 N1 C5 121.6(4) . . ? C6 N2 C10 119.2(3) . . ? C6 N2 Ni2 126.3(3) . . ? C10 N2 Ni2 112.3(2) . . ? C11 N3 C13 110.9(3) . . ? C11 N3 Ni2 109.5(2) . . ? C13 N3 Ni2 135.5(2) . . ? C16 N4 C14 111.8(3) . . ? C16 N4 Ni1 109.9(2) . . ? C14 N4 Ni1 135.6(2) . . ? C17 N5 C21 119.7(3) . . ? C17 N5 Ni1 113.4(2) . . ? C21 N5 Ni1 124.8(3) . . ? O3 N6 C26 117.7(4) . . ? O3 N6 C22 121.1(3) . . ? C26 N6 C22 121.2(4) . . ? O2 N7 C27 117.5(4) . . ? O2 N7 C31 121.1(4) . . ? C27 N7 C31 121.4(4) . . ? C32 N8 C36 119.3(3) . . ? C32 N8 Ni2 125.6(3) . . ? C36 N8 Ni2 113.9(2) . . ? C37 N9 C39 111.6(3) . . ? C37 N9 Ni2 109.5(3) . . ? C39 N9 Ni2 134.3(2) . . ? C42 N10 C40 111.8(3) . . ? C42 N10 Ni1 108.4(2) . . ? C40 N10 Ni1 134.7(2) . . ? C47 N11 C43 118.6(3) . . ? C47 N11 Ni1 126.7(2) . . ? C43 N11 Ni1 112.9(2) . . ? O4 N12 C52 116.0(3) . . ? O4 N12 C48 122.6(3) . . ? C52 N12 C48 121.3(3) . . ? O21 N13 O22 124.9(6) . . ? O21 N13 C53 116.8(6) . . ? O22 N13 C53 118.3(5) . . ? O23 N14 O24 122.8(8) . . ? O23 N14 C54 120.9(7) . . ? O24 N14 C54 116.3(7) . . ? N1 O1 Ni2 118.4(2) . . ? N7 O2 Ni2 116.9(2) . . ? N6 O3 Ni1 114.7(2) . . ? N12 O4 Ni1 118.1(2) . . ? N1 C1 C2 121.2(5) . . ? N1 C1 H1 119.4 . . ? C2 C1 H1 119.4 . . ? C1 C2 C3 118.5(5) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C2 C3 C4 120.5(5) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 120.5(4) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? N1 C5 C4 117.7(4) . . ? N1 C5 C6 121.7(4) . . ? C4 C5 C6 120.6(4) . . ? N2 C6 C7 120.8(4) . . ? N2 C6 C5 118.7(3) . . ? C7 C6 C5 120.4(3) . . ? C8 C7 C6 119.4(4) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 120.1(4) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 117.7(4) . . ? C10 C9 H9 121.2 . . ? C8 C9 H9 121.2 . . ? N2 C10 C9 122.8(4) . . ? N2 C10 C11 113.3(3) . . ? C9 C10 C11 123.8(4) . . ? N3 C11 C10 118.5(3) . . ? N3 C11 S1 114.3(3) . . ? C10 C11 S1 127.2(3) . . ? C13 C12 S1 110.4(3) . . ? C13 C12 H12 124.8 . . ? S1 C12 H12 124.8 . . ? C12 C13 N3 114.5(3) . . ? C12 C13 C14 129.2(3) . . ? N3 C13 C14 115.4(3) . . ? C15 C14 N4 113.9(3) . . ? C15 C14 C13 130.9(4) . . ? N4 C14 C13 115.1(3) . . ? C14 C15 S2 110.6(3) . . ? C14 C15 H15 124.7 . . ? S2 C15 H15 124.7 . . ? N4 C16 C17 119.1(3) . . ? N4 C16 S2 113.5(3) . . ? C17 C16 S2 127.4(3) . . ? N5 C17 C18 121.8(4) . . ? N5 C17 C16 112.4(3) . . ? C18 C17 C16 125.8(4) . . ? C19 C18 C17 118.5(4) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? C18 C19 C20 120.0(4) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C21 119.2(4) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? N5 C21 C20 120.7(4) . . ? N5 C21 C22 117.9(3) . . ? C20 C21 C22 121.3(4) . . ? N6 C22 C23 118.9(4) . . ? N6 C22 C21 120.4(3) . . ? C23 C22 C21 120.7(4) . . ? C22 C23 C24 120.3(5) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 119.0(4) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C26 C25 C24 119.6(4) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? N6 C26 C25 121.0(5) . . ? N6 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? N7 C27 C28 120.7(6) . . ? N7 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C29 C28 C27 120.0(6) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 118.9(5) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C29 C30 C31 121.6(6) . . ? C29 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? N7 C31 C30 117.4(5) . . ? N7 C31 C32 121.6(4) . . ? C30 C31 C32 121.0(5) . . ? N8 C32 C33 121.2(4) . . ? N8 C32 C31 118.8(4) . . ? C33 C32 C31 119.8(4) . . ? C34 C33 C32 119.3(4) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 120.1(4) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 117.5(4) . . ? C36 C35 H35 121.2 . . ? C34 C35 H35 121.2 . . ? N8 C36 C35 122.4(4) . . ? N8 C36 C37 113.1(3) . . ? C35 C36 C37 124.4(4) . . ? N9 C37 C36 118.7(4) . . ? N9 C37 S3 114.0(3) . . ? C36 C37 S3 127.3(3) . . ? C39 C38 S3 110.8(3) . . ? C39 C38 H38 124.6 . . ? S3 C38 H38 124.6 . . ? C38 C39 N9 113.9(3) . . ? C38 C39 C40 131.8(4) . . ? N9 C39 C40 114.3(3) . . ? C41 C40 N10 113.9(3) . . ? C41 C40 C39 130.1(3) . . ? N10 C40 C39 115.5(3) . . ? C40 C41 S4 110.6(3) . . ? C40 C41 H41 124.7 . . ? S4 C41 H41 124.7 . . ? N10 C42 C43 119.6(3) . . ? N10 C42 S4 113.8(3) . . ? C43 C42 S4 126.7(3) . . ? N11 C43 C44 123.0(4) . . ? N11 C43 C42 112.7(3) . . ? C44 C43 C42 124.2(3) . . ? C43 C44 C45 118.0(3) . . ? C43 C44 H44 121.0 . . ? C45 C44 H44 121.0 . . ? C46 C45 C44 119.9(4) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 119.3(4) . . ? C45 C46 H46 120.4 . . ? C47 C46 H46 120.4 . . ? N11 C47 C46 121.2(3) . . ? N11 C47 C48 119.0(3) . . ? C46 C47 C48 119.8(3) . . ? N12 C48 C49 117.4(3) . . ? N12 C48 C47 121.1(3) . . ? C49 C48 C47 121.5(3) . . ? C50 C49 C48 121.5(4) . . ? C50 C49 H49 119.3 . . ? C48 C49 H49 119.3 . . ? C51 C50 C49 119.5(4) . . ? C51 C50 H50 120.3 . . ? C49 C50 H50 120.3 . . ? C50 C51 C52 119.0(4) . . ? C50 C51 H51 120.5 . . ? C52 C51 H51 120.5 . . ? N12 C52 C51 121.4(4) . . ? N12 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? N13 C53 H53A 109.5 . . ? N13 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N13 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N14 C54 H54A 109.5 . . ? N14 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N14 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O1S C1S N1S 79.5(14) . . ? O1S C1S O2S 160(2) . . ? N1S C1S O2S 80.1(13) . . ? C1S N1S C1S 180.0(14) 2_775 . ? C1S N1S O1S 46.8(9) 2_775 2_775 ? C1S N1S O1S 133.2(9) . 2_775 ? C1S N1S O1S 133.1(9) 2_775 . ? C1S N1S O1S 46.9(9) . . ? O1S N1S O1S 179.998(2) 2_775 . ? C1S N1S O2S 128.8(9) 2_775 . ? C1S N1S O2S 51.2(9) . . ? O1S N1S O2S 81.9(6) 2_775 . ? O1S N1S O2S 98.1(6) . . ? C1S N1S O2S 51.2(9) 2_775 2_775 ? C1S N1S O2S 128.8(9) . 2_775 ? O1S N1S O2S 98.1(6) 2_775 2_775 ? O1S N1S O2S 81.9(6) . 2_775 ? O2S N1S O2S 179.997(2) . 2_775 ? C1S O1S N1S 53.7(11) . . ? C1S O2S N1S 48.6(9) . . ? H1W O1W H2W 107.9 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.180 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.103