# Electronic Supplementary Material (ESI) for CrystEngComm # 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_l _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H92 In12 N12 Ni O3 S20' _chemical_formula_weight 2818.94 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' In In -0.7276 1.3100 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.9686(10) _cell_length_b 18.8743(9) _cell_length_c 26.1162(14) _cell_angle_alpha 90.00 _cell_angle_beta 107.4360(10) _cell_angle_gamma 90.00 _cell_volume 8920.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 37861 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour purple _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5776 _exptl_absorpt_coefficient_mu 3.757 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3014 _exptl_absorpt_correction_T_max 0.5512 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43775 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15654 _reflns_number_gt 12921 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One protonated 1,2-diaminocyclohexane and three water molecules contribution to the scattering factors has been taken into account with PLATON/SQUEEZE. ; _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^)+(0.0550P)^2^+57.6728P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15654 _refine_ls_number_parameters 659 _refine_ls_number_restraints 459 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1387 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.13038(4) -0.05253(4) 0.34145(3) 0.03657(18) Uani 1 1 d U . . In2 In 0.07046(4) 0.11399(4) 0.25594(3) 0.03709(18) Uani 1 1 d U . . In3 In 0.22495(4) -0.01926(3) 0.22841(3) 0.03278(17) Uani 1 1 d U . . In4 In 0.27553(4) 0.09909(3) 0.36329(3) 0.03278(17) Uani 1 1 d U . . In5 In 0.01696(4) 0.28639(4) 0.16746(3) 0.03972(19) Uani 1 1 d U . . In6 In 0.15900(4) 0.15813(4) 0.13630(3) 0.03394(17) Uani 1 1 d U . . In7 In 0.20829(4) 0.27966(4) 0.27149(3) 0.03514(17) Uani 1 1 d U . . In8 In 0.30604(4) 0.03200(4) 0.12060(3) 0.03218(17) Uani 1 1 d U . . In9 In 0.36684(4) 0.15173(3) 0.24588(3) 0.03048(16) Uani 1 1 d U . . In10 In 0.40537(4) 0.25776(3) 0.37352(3) 0.03193(17) Uani 1 1 d U . . In11 In 0.43715(3) 0.07288(3) 0.00282(3) 0.02778(15) Uani 1 1 d U . . In12 In 0.48810(3) -0.05932(3) 0.10925(3) 0.02768(15) Uani 1 1 d U . . Ni1 Ni 0.25971(7) -0.19126(7) -0.06876(6) 0.0416(3) Uani 1 1 d U . . S1 S 0.08896(14) -0.14659(14) 0.38985(11) 0.0423(6) Uani 1 1 d U . . S2 S 0.02486(15) 0.02363(16) 0.30294(14) 0.0564(8) Uani 1 1 d U . . S3 S 0.18376(16) -0.11074(14) 0.27763(11) 0.0440(6) Uani 1 1 d U . . S4 S 0.23036(16) 0.00833(15) 0.41011(11) 0.0457(7) Uani 1 1 d U . . S5 S -0.03165(14) 0.19156(16) 0.21289(12) 0.0478(7) Uani 1 1 d U . . S6 S 0.11772(13) 0.06008(13) 0.18578(11) 0.0366(6) Uani 1 1 d U . . S7 S 0.17097(14) 0.18174(13) 0.32230(10) 0.0369(6) Uani 1 1 d U . . S8 S 0.27405(15) -0.07384(13) 0.16280(11) 0.0392(6) Uani 1 1 d U . . S9 S 0.32585(13) 0.04972(12) 0.29214(10) 0.0333(5) Uani 1 1 d U . . S10 S 0.38133(14) 0.15750(13) 0.42430(10) 0.0387(6) Uani 1 1 d U . . S11 S 0.06454(16) 0.24310(15) 0.09627(11) 0.0470(7) Uani 1 1 d U . . S12 S 0.10193(16) 0.35617(15) 0.23912(13) 0.0569(8) Uani 1 1 d U . . S13 S 0.19605(14) 0.09429(15) 0.06899(10) 0.0410(6) Uani 1 1 d U . . S14 S 0.25910(13) 0.22975(13) 0.20090(10) 0.0349(5) Uani 1 1 d U . . S15 S 0.30658(14) 0.34348(13) 0.33563(10) 0.0378(6) Uani 1 1 d U . . S16 S 0.36684(12) -0.01373(12) 0.05426(9) 0.0277(5) Uani 1 1 d U . . S17 S 0.41044(14) 0.10237(14) 0.17575(10) 0.0367(6) Uani 1 1 d U . . S18 S 0.46404(14) 0.21791(14) 0.30767(11) 0.0414(6) Uani 1 1 d U . . S19 S 0.43971(12) -0.02555(12) -0.06438(9) 0.0267(5) Uani 1 1 d U . . S20 S 0.49183(12) 0.16334(11) -0.05745(9) 0.0255(5) Uani 1 1 d U . . N1 N 0.3219(4) 0.1196(4) -0.0356(3) 0.0344(19) Uani 1 1 d U . . H1 H 0.2866 0.0986 -0.0600 0.041 Uiso 1 1 calc R . . N2 N 0.4314(4) 0.1672(4) 0.0565(3) 0.0317(18) Uani 1 1 d U . . H2 H 0.4689 0.1839 0.0817 0.038 Uiso 1 1 calc R . . N3 N 0.4527(4) -0.1179(4) 0.1755(3) 0.0357(19) Uani 1 1 d U . . H3 H 0.4249 -0.1555 0.1700 0.043 Uiso 1 1 calc R . . N4 N 0.5584(5) -0.0128(5) 0.1873(3) 0.045(2) Uani 1 1 d U . . H4 H 0.5825 0.0269 0.1900 0.054 Uiso 1 1 calc R . . N5 N 0.3102(5) -0.1866(5) 0.0160(3) 0.045(2) Uani 1 1 d U . . H5 H 0.3299 -0.1494 0.0345 0.054 Uiso 1 1 calc R . . N6 N 0.2681(5) -0.3017(5) -0.0530(3) 0.046(2) Uani 1 1 d U . . H6 H 0.2466 -0.3352 -0.0750 0.055 Uiso 1 1 calc R . . N7 N 0.3600(4) -0.1906(5) -0.0897(3) 0.039(2) Uani 1 1 d U . . H7 H 0.4042 -0.1956 -0.0676 0.047 Uiso 1 1 calc R . . N8 N 0.2140(5) -0.2081(5) -0.1519(3) 0.048(2) Uani 1 1 d U . . H8 H 0.1671 -0.2076 -0.1693 0.057 Uiso 1 1 calc R . . N9 N 0.2511(4) -0.0796(5) -0.0753(4) 0.049(2) Uani 1 1 d U . . H9 H 0.2875 -0.0504 -0.0726 0.059 Uiso 1 1 calc R . . N10 N 0.1518(5) -0.1777(5) -0.0591(4) 0.056(3) Uani 1 1 d U . . H10 H 0.1199 -0.2116 -0.0611 0.068 Uiso 1 1 calc R . . C1 C 0.3160(6) 0.1895(7) -0.0133(5) 0.058(3) Uani 1 1 d U . . H1A H 0.3435 0.2208 -0.0310 0.069 Uiso 1 1 calc R . . C2 C 0.2390(6) 0.2197(6) -0.0301(5) 0.054(3) Uani 1 1 d U . . H2A H 0.2054 0.1861 -0.0206 0.065 Uiso 1 1 calc R . . H2B H 0.2224 0.2257 -0.0692 0.065 Uiso 1 1 calc R . . C3 C 0.2348(9) 0.2912(9) -0.0033(7) 0.095(5) Uani 1 1 d U . . H3A H 0.2547 0.3278 -0.0217 0.114 Uiso 1 1 calc R . . H3B H 0.1827 0.3025 -0.0085 0.114 Uiso 1 1 calc R . . C4 C 0.2732(9) 0.2948(9) 0.0526(7) 0.092(5) Uani 1 1 d U . . H4A H 0.2450 0.2680 0.0719 0.110 Uiso 1 1 calc R . . H4B H 0.2743 0.3443 0.0640 0.110 Uiso 1 1 calc R . . C5 C 0.3506(6) 0.2674(6) 0.0690(5) 0.051(3) Uani 1 1 d U . . H5A H 0.3681 0.2621 0.1081 0.061 Uiso 1 1 calc R . . H5B H 0.3828 0.3015 0.0586 0.061 Uiso 1 1 calc R . . C6 C 0.3553(7) 0.1962(7) 0.0428(6) 0.064(4) Uani 1 1 d U . . H6A H 0.3293 0.1633 0.0605 0.077 Uiso 1 1 calc R . . C7 C 0.4835(6) -0.0833(6) 0.2288(4) 0.042(3) Uani 1 1 d U . . H7A H 0.4530 -0.0409 0.2291 0.050 Uiso 1 1 calc R . . C8 C 0.4787(6) -0.1306(6) 0.2746(4) 0.048(3) Uani 1 1 d U . . H8A H 0.4268 -0.1407 0.2712 0.057 Uiso 1 1 calc R . . H8B H 0.5037 -0.1757 0.2732 0.057 Uiso 1 1 calc R . . C9 C 0.5146(9) -0.0944(8) 0.3274(5) 0.080(4) Uani 1 1 d U . . H9A H 0.4866 -0.0516 0.3301 0.096 Uiso 1 1 calc R . . H9B H 0.5137 -0.1261 0.3569 0.096 Uiso 1 1 calc R . . C10 C 0.5931(9) -0.0745(8) 0.3327(5) 0.079(4) Uani 1 1 d U . . H10A H 0.6217 -0.1171 0.3307 0.095 Uiso 1 1 calc R . . H10B H 0.6157 -0.0518 0.3675 0.095 Uiso 1 1 calc R . . C11 C 0.5944(9) -0.0241(7) 0.2879(4) 0.074(4) Uani 1 1 d U . . H11A H 0.6455 -0.0116 0.2907 0.089 Uiso 1 1 calc R . . H11B H 0.5679 0.0195 0.2910 0.089 Uiso 1 1 calc R . . C12 C 0.5582(6) -0.0587(6) 0.2341(4) 0.049(3) Uani 1 1 d U . . H12 H 0.5879 -0.1012 0.2323 0.058 Uiso 1 1 calc R . . C13 C 0.3054(9) -0.2577(7) 0.0373(5) 0.076(4) Uani 1 1 d U . . H13 H 0.2528 -0.2629 0.0354 0.091 Uiso 1 1 calc R . . C14 C 0.3478(7) -0.2665(7) 0.0976(5) 0.059(3) Uani 1 1 d U . . H14A H 0.3992 -0.2517 0.1038 0.070 Uiso 1 1 calc R . . H14B H 0.3258 -0.2353 0.1186 0.070 Uiso 1 1 calc R . . C15 C 0.3467(11) -0.3409(8) 0.1167(6) 0.094(5) Uani 1 1 d U . . H15A H 0.3832 -0.3453 0.1521 0.113 Uiso 1 1 calc R . . H15B H 0.2980 -0.3504 0.1209 0.113 Uiso 1 1 calc R . . C16 C 0.3616(13) -0.3930(9) 0.0828(6) 0.120(5) Uani 1 1 d U . . H16A H 0.3546 -0.4399 0.0966 0.145 Uiso 1 1 calc R . . H16B H 0.4134 -0.3891 0.0836 0.145 Uiso 1 1 calc R . . C17 C 0.3114(11) -0.3870(8) 0.0232(6) 0.099(5) Uani 1 1 d U . . H17A H 0.3272 -0.4216 0.0009 0.118 Uiso 1 1 calc R . . H17B H 0.2599 -0.3973 0.0211 0.118 Uiso 1 1 calc R . . C18 C 0.3172(10) -0.3110(6) 0.0022(5) 0.079(4) Uani 1 1 d U . . H18 H 0.3685 -0.3052 0.0009 0.095 Uiso 1 1 calc R . . C19 C 0.3417(6) -0.1804(7) -0.1468(5) 0.059(3) Uani 1 1 d U . . H19 H 0.3292 -0.1296 -0.1533 0.071 Uiso 1 1 calc R . . C20 C 0.4021(5) -0.1946(6) -0.1713(4) 0.046(3) Uani 1 1 d U . . H20A H 0.4203 -0.2429 -0.1620 0.055 Uiso 1 1 calc R . . H20B H 0.4431 -0.1621 -0.1553 0.055 Uiso 1 1 calc R . . C21 C 0.3795(7) -0.1864(7) -0.2319(5) 0.059(3) Uani 1 1 d U . . H21A H 0.3714 -0.1361 -0.2410 0.071 Uiso 1 1 calc R . . H21B H 0.4199 -0.2030 -0.2450 0.071 Uiso 1 1 calc R . . C22 C 0.3128(8) -0.2257(8) -0.2589(5) 0.074(4) Uani 1 1 d U . . H22A H 0.3234 -0.2766 -0.2551 0.089 Uiso 1 1 calc R . . H22B H 0.2978 -0.2143 -0.2973 0.089 Uiso 1 1 calc R . . C23 C 0.2489(6) -0.2085(7) -0.2360(5) 0.055(3) Uani 1 1 d U . . H23A H 0.2339 -0.1589 -0.2437 0.066 Uiso 1 1 calc R . . H23B H 0.2063 -0.2386 -0.2532 0.066 Uiso 1 1 calc R . . C24 C 0.2729(6) -0.2207(7) -0.1755(5) 0.054(3) Uani 1 1 d U . . H24 H 0.2856 -0.2716 -0.1700 0.065 Uiso 1 1 calc R . . C25 C 0.1731(7) -0.0600(6) -0.0851(6) 0.068(4) Uani 1 1 d U . . H25 H 0.1462 -0.0722 -0.1228 0.081 Uiso 1 1 calc R . . C26 C 0.1618(7) 0.0168(8) -0.0775(7) 0.087(5) Uani 1 1 d U . . H26A H 0.1806 0.0444 -0.1024 0.105 Uiso 1 1 calc R . . H26B H 0.1896 0.0306 -0.0408 0.105 Uiso 1 1 calc R . . C27 C 0.0789(10) 0.0335(12) -0.0875(10) 0.137(7) Uani 1 1 d U . . H27A H 0.0731 0.0838 -0.0805 0.164 Uiso 1 1 calc R . . H27B H 0.0520 0.0242 -0.1253 0.164 Uiso 1 1 calc R . . C28 C 0.0465(10) -0.0103(11) -0.0524(10) 0.133(7) Uani 1 1 d U . . H28A H 0.0677 0.0049 -0.0151 0.160 Uiso 1 1 calc R . . H28B H -0.0069 -0.0021 -0.0626 0.160 Uiso 1 1 calc R . . C29 C 0.0601(7) -0.0860(8) -0.0562(7) 0.087(5) Uani 1 1 d U . . H29A H 0.0302 -0.1032 -0.0914 0.104 Uiso 1 1 calc R . . H29B H 0.0439 -0.1111 -0.0289 0.104 Uiso 1 1 calc R . . C30 C 0.1402(7) -0.1036(7) -0.0488(6) 0.073(4) Uani 1 1 d U . . H30 H 0.1685 -0.0931 -0.0111 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.0371(4) 0.0312(4) 0.0436(4) 0.0013(3) 0.0154(3) -0.0061(3) In2 0.0294(4) 0.0339(4) 0.0484(5) 0.0008(3) 0.0124(3) 0.0019(3) In3 0.0346(4) 0.0281(3) 0.0386(4) -0.0021(3) 0.0155(3) -0.0003(3) In4 0.0348(4) 0.0288(3) 0.0351(4) -0.0012(3) 0.0110(3) -0.0056(3) In5 0.0337(4) 0.0355(4) 0.0456(5) -0.0053(3) 0.0053(3) 0.0082(3) In6 0.0319(4) 0.0332(4) 0.0362(4) -0.0023(3) 0.0093(3) 0.0049(3) In7 0.0341(4) 0.0297(4) 0.0373(4) -0.0040(3) 0.0041(3) 0.0014(3) In8 0.0331(4) 0.0322(4) 0.0340(4) -0.0034(3) 0.0144(3) 0.0011(3) In9 0.0309(3) 0.0310(4) 0.0301(4) -0.0047(3) 0.0100(3) -0.0031(3) In10 0.0332(4) 0.0295(3) 0.0331(4) -0.0051(3) 0.0101(3) -0.0056(3) In11 0.0271(3) 0.0285(3) 0.0268(4) -0.0015(3) 0.0067(3) 0.0037(3) In12 0.0307(3) 0.0294(3) 0.0234(3) 0.0013(3) 0.0087(3) 0.0024(3) Ni1 0.0325(7) 0.0425(8) 0.0483(9) -0.0065(6) 0.0099(6) -0.0058(6) S1 0.0344(13) 0.0433(15) 0.0447(16) 0.0060(12) 0.0051(11) -0.0129(12) S2 0.0363(15) 0.0495(17) 0.087(2) 0.0169(16) 0.0240(15) 0.0011(14) S3 0.0559(17) 0.0316(13) 0.0486(17) -0.0001(12) 0.0220(13) -0.0015(13) S4 0.0529(16) 0.0451(15) 0.0394(16) 0.0041(12) 0.0142(13) -0.0196(13) S5 0.0301(13) 0.0507(16) 0.0595(19) 0.0008(14) 0.0088(12) 0.0086(13) S6 0.0338(13) 0.0309(13) 0.0450(15) -0.0011(11) 0.0117(11) 0.0044(11) S7 0.0364(13) 0.0330(13) 0.0422(15) -0.0021(11) 0.0133(11) -0.0009(11) S8 0.0456(15) 0.0297(13) 0.0503(16) -0.0053(11) 0.0265(13) -0.0013(12) S9 0.0343(13) 0.0307(12) 0.0369(14) -0.0025(10) 0.0137(11) -0.0023(11) S10 0.0442(14) 0.0330(13) 0.0360(14) -0.0009(11) 0.0076(11) -0.0085(12) S11 0.0466(15) 0.0467(16) 0.0444(16) 0.0029(13) 0.0084(13) 0.0177(13) S12 0.0481(17) 0.0382(15) 0.067(2) -0.0128(14) -0.0087(14) 0.0123(14) S13 0.0388(14) 0.0511(16) 0.0326(14) -0.0029(12) 0.0097(11) 0.0081(13) S14 0.0357(13) 0.0318(13) 0.0345(14) -0.0013(10) 0.0064(11) 0.0003(11) S15 0.0397(14) 0.0307(12) 0.0367(14) -0.0066(11) 0.0021(11) -0.0008(11) S16 0.0267(11) 0.0289(12) 0.0286(12) -0.0017(9) 0.0098(9) 0.0037(10) S17 0.0376(13) 0.0401(14) 0.0351(14) -0.0061(11) 0.0152(11) -0.0031(12) S18 0.0385(14) 0.0463(15) 0.0428(16) -0.0170(12) 0.0172(12) -0.0138(12) S19 0.0275(11) 0.0274(11) 0.0243(12) -0.0002(9) 0.0066(9) -0.0005(10) S20 0.0265(11) 0.0250(11) 0.0248(12) 0.0028(9) 0.0072(9) 0.0040(9) N1 0.021(4) 0.041(5) 0.032(5) -0.002(4) -0.007(3) 0.004(4) N2 0.029(4) 0.037(4) 0.026(4) -0.001(3) 0.002(3) 0.002(4) N3 0.040(5) 0.037(5) 0.028(4) 0.002(4) 0.008(4) -0.007(4) N4 0.056(5) 0.046(5) 0.025(5) 0.008(4) 0.000(4) -0.019(4) N5 0.047(5) 0.043(5) 0.042(5) -0.016(4) 0.007(4) -0.022(4) N6 0.066(6) 0.041(5) 0.025(5) -0.006(4) 0.006(4) -0.013(5) N7 0.032(4) 0.062(6) 0.021(4) -0.003(4) 0.005(3) -0.003(4) N8 0.028(4) 0.066(6) 0.042(5) -0.013(5) 0.000(4) -0.003(4) N9 0.025(4) 0.037(5) 0.081(7) -0.003(5) 0.008(4) -0.007(4) N10 0.041(5) 0.049(6) 0.080(7) -0.008(5) 0.022(5) -0.013(5) C1 0.039(6) 0.066(8) 0.064(8) -0.030(6) 0.009(6) 0.021(6) C2 0.041(6) 0.058(7) 0.068(8) 0.023(6) 0.024(6) 0.020(6) C3 0.094(11) 0.091(11) 0.101(13) -0.009(9) 0.029(10) 0.059(10) C4 0.101(12) 0.078(10) 0.100(13) 0.001(9) 0.038(10) 0.034(9) C5 0.062(7) 0.043(6) 0.050(7) -0.010(5) 0.021(6) 0.012(6) C6 0.046(7) 0.048(7) 0.091(10) -0.011(7) 0.008(7) 0.014(6) C7 0.059(7) 0.049(6) 0.022(5) 0.004(4) 0.019(5) -0.006(5) C8 0.058(7) 0.053(7) 0.033(6) 0.011(5) 0.015(5) -0.006(6) C9 0.124(13) 0.080(10) 0.044(8) 0.013(7) 0.039(8) 0.007(9) C10 0.118(12) 0.081(10) 0.020(6) 0.000(6) -0.006(7) -0.009(9) C11 0.123(12) 0.068(8) 0.025(6) -0.001(6) 0.013(7) -0.045(8) C12 0.062(7) 0.049(6) 0.030(6) 0.003(5) 0.005(5) -0.013(6) C13 0.110(11) 0.050(8) 0.055(8) 0.005(6) 0.006(8) -0.016(8) C14 0.067(8) 0.058(7) 0.056(8) -0.004(6) 0.027(6) -0.013(6) C15 0.149(13) 0.077(9) 0.043(8) -0.005(7) 0.007(8) -0.018(9) C16 0.194(13) 0.088(9) 0.059(8) 0.008(7) 0.007(9) 0.016(10) C17 0.179(14) 0.062(8) 0.047(8) -0.006(7) 0.021(9) -0.006(9) C18 0.139(13) 0.037(7) 0.059(9) -0.003(6) 0.027(9) 0.006(8) C19 0.041(6) 0.065(8) 0.068(9) 0.001(6) 0.012(6) -0.004(6) C20 0.027(5) 0.059(7) 0.052(7) 0.006(5) 0.010(5) 0.001(5) C21 0.054(7) 0.077(9) 0.052(8) 0.005(6) 0.024(6) -0.011(7) C22 0.084(10) 0.092(10) 0.048(8) -0.009(7) 0.022(7) -0.010(8) C23 0.049(7) 0.055(7) 0.051(7) -0.008(6) -0.002(6) -0.015(6) C24 0.048(7) 0.063(8) 0.047(7) -0.009(6) 0.007(5) -0.005(6) C25 0.069(8) 0.045(7) 0.094(11) 0.003(7) 0.030(8) -0.003(7) C26 0.055(8) 0.066(9) 0.133(14) -0.023(9) 0.017(8) -0.005(7) C27 0.084(11) 0.117(14) 0.205(18) -0.026(13) 0.037(11) 0.025(11) C28 0.079(11) 0.125(14) 0.202(18) -0.030(13) 0.054(11) 0.026(11) C29 0.045(7) 0.088(11) 0.126(13) -0.051(10) 0.023(8) -0.015(8) C30 0.059(8) 0.068(9) 0.098(11) -0.010(8) 0.035(8) 0.004(7) _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 In1 S2 2.424(3) . ? In1 S1 2.442(3) . ? In1 S3 2.454(3) . ? In1 S4 2.469(3) . ? In2 S2 2.408(3) . ? In2 S5 2.420(3) . ? In2 S6 2.486(3) . ? In2 S7 2.509(3) . ? In3 S8 2.413(2) . ? In3 S3 2.418(3) . ? In3 S9 2.494(2) . ? In3 S6 2.502(2) . ? In4 S4 2.407(3) . ? In4 S10 2.422(3) . ? In4 S7 2.498(3) . ? In4 S9 2.509(2) . ? In5 S11 2.438(3) . ? In5 S12 2.455(3) . ? In5 S1 2.465(3) 2 ? In5 S5 2.473(3) . ? In6 S11 2.399(3) . ? In6 S13 2.403(3) . ? In6 S6 2.513(3) . ? In6 S14 2.522(3) . ? In7 S12 2.418(3) . ? In7 S15 2.421(2) . ? In7 S7 2.498(3) . ? In7 S14 2.506(3) . ? In8 S13 2.422(3) . ? In8 S8 2.444(3) . ? In8 S17 2.460(3) . ? In8 S16 2.505(2) . ? In9 S18 2.404(3) . ? In9 S17 2.411(2) . ? In9 S14 2.507(3) . ? In9 S9 2.517(2) . ? In10 S18 2.431(3) . ? In10 S10 2.431(3) . ? In10 S15 2.449(3) . ? In10 S20 2.527(2) 4_566 ? In11 N2 2.290(8) . ? In11 N1 2.290(7) . ? In11 S19 2.566(2) . ? In11 S19 2.567(2) 3_655 ? In11 S16 2.707(2) . ? In11 S20 2.729(2) . ? In12 N4 2.253(8) . ? In12 N3 2.316(8) . ? In12 S16 2.473(2) . ? In12 S20 2.478(2) 3_655 ? In12 S19 2.603(2) 3_655 ? Ni1 N8 2.106(9) . ? Ni1 N9 2.116(9) . ? Ni1 N6 2.121(9) . ? Ni1 N7 2.130(8) . ? Ni1 N5 2.135(8) . ? Ni1 N10 2.151(9) . ? S1 In5 2.465(3) 2_545 ? S19 In11 2.567(2) 3_655 ? S19 In12 2.603(2) 3_655 ? S20 In12 2.478(2) 3_655 ? S20 In10 2.527(2) 4_565 ? N1 C1 1.459(13) . ? N1 H1 0.8700 . ? N2 C6 1.483(13) . ? N2 H2 0.8700 . ? N3 C7 1.489(12) . ? N3 H3 0.8700 . ? N4 C12 1.500(13) . ? N4 H4 0.8700 . ? N5 C13 1.465(15) . ? N5 H5 0.8700 . ? N6 C18 1.474(16) . ? N6 H6 0.8700 . ? N7 C19 1.440(14) . ? N7 H7 0.8700 . ? N8 C24 1.449(14) . ? N8 H8 0.8700 . ? N9 C25 1.471(15) . ? N9 H9 0.8700 . ? N10 C30 1.454(16) . ? N10 H10 0.8700 . ? C1 C6 1.438(17) . ? C1 C2 1.506(14) . ? C1 H1A 0.9900 . ? C2 C3 1.534(18) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 C4 1.42(2) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.493(18) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 C6 1.521(15) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 H6A 0.9900 . ? C7 C12 1.457(15) . ? C7 C8 1.518(13) . ? C7 H7A 0.9900 . ? C8 C9 1.507(17) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.50(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C11 1.513(17) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.513(15) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 H12 0.9900 . ? C13 C18 1.423(18) . ? C13 C14 1.548(17) . ? C13 H13 0.9900 . ? C14 C15 1.492(18) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.41(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.57(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 C18 1.551(18) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18 0.9900 . ? C19 C20 1.493(15) . ? C19 C24 1.502(15) . ? C19 H19 0.9900 . ? C20 C21 1.518(15) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.454(17) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 C23 1.540(17) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.525(16) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 H24 0.9900 . ? C25 C26 1.487(18) . ? C25 C30 1.526(18) . ? C25 H25 0.9900 . ? C26 C27 1.55(2) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.50(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.46(2) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.510(17) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 In1 S1 106.99(10) . . ? S2 In1 S3 116.18(11) . . ? S1 In1 S3 106.76(10) . . ? S2 In1 S4 112.61(11) . . ? S1 In1 S4 104.98(9) . . ? S3 In1 S4 108.55(10) . . ? S2 In2 S5 107.79(10) . . ? S2 In2 S6 110.47(10) . . ? S5 In2 S6 108.69(10) . . ? S2 In2 S7 108.88(11) . . ? S5 In2 S7 110.45(9) . . ? S6 In2 S7 110.52(8) . . ? S8 In3 S3 109.13(9) . . ? S8 In3 S9 108.33(9) . . ? S3 In3 S9 108.88(9) . . ? S8 In3 S6 112.01(9) . . ? S3 In3 S6 108.35(9) . . ? S9 In3 S6 110.09(8) . . ? S4 In4 S10 109.92(9) . . ? S4 In4 S7 107.72(10) . . ? S10 In4 S7 113.12(9) . . ? S4 In4 S9 112.60(9) . . ? S10 In4 S9 103.43(9) . . ? S7 In4 S9 110.12(9) . . ? S11 In5 S12 116.91(11) . . ? S11 In5 S1 97.44(9) . 2 ? S12 In5 S1 114.65(9) . 2 ? S11 In5 S5 113.56(10) . . ? S12 In5 S5 106.05(11) . . ? S1 In5 S5 108.03(9) 2 . ? S11 In6 S13 111.13(10) . . ? S11 In6 S6 114.16(9) . . ? S13 In6 S6 102.21(9) . . ? S11 In6 S14 104.33(9) . . ? S13 In6 S14 115.57(9) . . ? S6 In6 S14 109.81(9) . . ? S12 In7 S15 109.49(9) . . ? S12 In7 S7 106.74(11) . . ? S15 In7 S7 106.42(9) . . ? S12 In7 S14 115.58(10) . . ? S15 In7 S14 108.04(9) . . ? S7 In7 S14 110.20(8) . . ? S13 In8 S8 111.02(9) . . ? S13 In8 S17 118.15(9) . . ? S8 In8 S17 116.26(9) . . ? S13 In8 S16 106.30(8) . . ? S8 In8 S16 104.97(8) . . ? S17 In8 S16 97.72(8) . . ? S18 In9 S17 110.00(9) . . ? S18 In9 S14 111.27(9) . . ? S17 In9 S14 106.74(9) . . ? S18 In9 S9 111.12(9) . . ? S17 In9 S9 107.14(8) . . ? S14 In9 S9 110.40(8) . . ? S18 In10 S10 110.22(10) . . ? S18 In10 S15 112.06(10) . . ? S10 In10 S15 119.26(9) . . ? S18 In10 S20 110.50(8) . 4_566 ? S10 In10 S20 104.91(8) . 4_566 ? S15 In10 S20 98.82(8) . 4_566 ? N2 In11 N1 75.8(3) . . ? N2 In11 S19 175.01(19) . . ? N1 In11 S19 101.0(2) . . ? N2 In11 S19 95.08(19) . 3_655 ? N1 In11 S19 168.0(2) . 3_655 ? S19 In11 S19 88.64(7) . 3_655 ? N2 In11 S16 92.6(2) . . ? N1 In11 S16 84.4(2) . . ? S19 In11 S16 90.88(7) . . ? S19 In11 S16 88.29(7) 3_655 . ? N2 In11 S20 87.9(2) . . ? N1 In11 S20 89.1(2) . . ? S19 In11 S20 88.29(7) . . ? S19 In11 S20 98.47(7) 3_655 . ? S16 In11 S20 173.16(7) . . ? N4 In12 N3 74.7(3) . . ? N4 In12 S16 125.8(2) . . ? N3 In12 S16 99.9(2) . . ? N4 In12 S20 131.1(2) . 3_655 ? N3 In12 S20 99.0(2) . 3_655 ? S16 In12 S20 103.12(7) . 3_655 ? N4 In12 S19 85.4(2) . 3_655 ? N3 In12 S19 160.0(2) . 3_655 ? S16 In12 S19 92.73(7) . 3_655 ? S20 In12 S19 93.10(7) 3_655 3_655 ? N8 Ni1 N9 94.0(4) . . ? N8 Ni1 N6 92.0(3) . . ? N9 Ni1 N6 173.4(4) . . ? N8 Ni1 N7 82.0(3) . . ? N9 Ni1 N7 91.5(3) . . ? N6 Ni1 N7 92.0(3) . . ? N8 Ni1 N5 173.4(4) . . ? N9 Ni1 N5 92.4(4) . . ? N6 Ni1 N5 81.7(3) . . ? N7 Ni1 N5 96.2(3) . . ? N8 Ni1 N10 91.5(4) . . ? N9 Ni1 N10 80.7(3) . . ? N6 Ni1 N10 96.5(4) . . ? N7 Ni1 N10 169.5(4) . . ? N5 Ni1 N10 91.2(4) . . ? In1 S1 In5 112.88(11) . 2_545 ? In2 S2 In1 104.68(10) . . ? In3 S3 In1 107.83(10) . . ? In4 S4 In1 105.97(10) . . ? In2 S5 In5 107.41(10) . . ? In2 S6 In3 109.97(10) . . ? In2 S6 In6 108.33(9) . . ? In3 S6 In6 109.42(9) . . ? In7 S7 In4 112.00(10) . . ? In7 S7 In2 106.73(10) . . ? In4 S7 In2 108.61(9) . . ? In3 S8 In8 99.91(9) . . ? In3 S9 In4 107.58(9) . . ? In3 S9 In9 111.39(10) . . ? In4 S9 In9 108.20(9) . . ? In4 S10 In10 104.44(10) . . ? In6 S11 In5 106.90(11) . . ? In7 S12 In5 103.56(11) . . ? In6 S13 In8 103.20(10) . . ? In7 S14 In9 108.38(9) . . ? In7 S14 In6 108.37(9) . . ? In9 S14 In6 110.07(9) . . ? In7 S15 In10 106.75(9) . . ? In12 S16 In8 105.02(9) . . ? In12 S16 In11 89.28(7) . . ? In8 S16 In11 122.18(9) . . ? In9 S17 In8 104.72(9) . . ? In9 S18 In10 102.36(9) . . ? In11 S19 In11 91.36(7) . 3_655 ? In11 S19 In12 89.01(7) . 3_655 ? In11 S19 In12 89.62(7) 3_655 3_655 ? In12 S20 In10 104.51(8) 3_655 4_565 ? In12 S20 In11 88.07(7) 3_655 . ? In10 S20 In11 120.18(8) 4_565 . ? C1 N1 In11 110.5(6) . . ? C1 N1 H1 124.7 . . ? In11 N1 H1 124.7 . . ? C6 N2 In11 111.2(6) . . ? C6 N2 H2 124.4 . . ? In11 N2 H2 124.4 . . ? C7 N3 In12 111.6(6) . . ? C7 N3 H3 124.2 . . ? In12 N3 H3 124.2 . . ? C12 N4 In12 111.5(6) . . ? C12 N4 H4 124.2 . . ? In12 N4 H4 124.2 . . ? C13 N5 Ni1 107.2(7) . . ? C13 N5 H5 126.4 . . ? Ni1 N5 H5 126.4 . . ? C18 N6 Ni1 107.2(7) . . ? C18 N6 H6 126.4 . . ? Ni1 N6 H6 126.4 . . ? C19 N7 Ni1 108.1(6) . . ? C19 N7 H7 125.9 . . ? Ni1 N7 H7 125.9 . . ? C24 N8 Ni1 109.4(6) . . ? C24 N8 H8 125.3 . . ? Ni1 N8 H8 125.3 . . ? C25 N9 Ni1 108.4(7) . . ? C25 N9 H9 125.8 . . ? Ni1 N9 H9 125.8 . . ? C30 N10 Ni1 109.8(7) . . ? C30 N10 H10 125.1 . . ? Ni1 N10 H10 125.1 . . ? C6 C1 N1 114.1(10) . . ? C6 C1 C2 115.1(10) . . ? N1 C1 C2 114.2(10) . . ? C6 C1 H1A 103.8 . . ? N1 C1 H1A 103.8 . . ? C2 C1 H1A 103.8 . . ? C1 C2 C3 112.2(11) . . ? C1 C2 H2A 109.2 . . ? C3 C2 H2A 109.2 . . ? C1 C2 H2B 109.2 . . ? C3 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C4 C3 C2 115.4(13) . . ? C4 C3 H3A 108.4 . . ? C2 C3 H3A 108.4 . . ? C4 C3 H3B 108.4 . . ? C2 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? C3 C4 C5 115.8(13) . . ? C3 C4 H4A 108.3 . . ? C5 C4 H4A 108.3 . . ? C3 C4 H4B 108.3 . . ? C5 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? C4 C5 C6 111.2(11) . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C1 C6 N2 112.5(10) . . ? C1 C6 C5 117.0(10) . . ? N2 C6 C5 113.7(10) . . ? C1 C6 H6A 103.9 . . ? N2 C6 H6A 103.9 . . ? C5 C6 H6A 103.9 . . ? C12 C7 N3 109.1(8) . . ? C12 C7 C8 113.5(9) . . ? N3 C7 C8 112.3(9) . . ? C12 C7 H7A 107.2 . . ? N3 C7 H7A 107.2 . . ? C8 C7 H7A 107.2 . . ? C9 C8 C7 109.7(10) . . ? C9 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? C9 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C8 111.1(11) . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C9 C10 C11 109.3(12) . . ? C9 C10 H10A 109.8 . . ? C11 C10 H10A 109.8 . . ? C9 C10 H10B 109.8 . . ? C11 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? C10 C11 C12 109.8(10) . . ? C10 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? C10 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C7 C12 N4 110.2(9) . . ? C7 C12 C11 112.6(10) . . ? N4 C12 C11 113.3(9) . . ? C7 C12 H12 106.8 . . ? N4 C12 H12 106.8 . . ? C11 C12 H12 106.8 . . ? C18 C13 N5 111.4(12) . . ? C18 C13 C14 116.4(12) . . ? N5 C13 C14 114.3(10) . . ? C18 C13 H13 104.4 . . ? N5 C13 H13 104.4 . . ? C14 C13 H13 104.4 . . ? C15 C14 C13 112.7(11) . . ? C15 C14 H14A 109.1 . . ? C13 C14 H14A 109.1 . . ? C15 C14 H14B 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C16 C15 C14 115.0(14) . . ? C16 C15 H15A 108.5 . . ? C14 C15 H15A 108.5 . . ? C16 C15 H15B 108.5 . . ? C14 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? C15 C16 C17 113.5(16) . . ? C15 C16 H16A 108.9 . . ? C17 C16 H16A 108.9 . . ? C15 C16 H16B 108.9 . . ? C17 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C18 C17 C16 109.3(13) . . ? C18 C17 H17A 109.8 . . ? C16 C17 H17A 109.8 . . ? C18 C17 H17B 109.8 . . ? C16 C17 H17B 109.8 . . ? H17A C17 H17B 108.3 . . ? C13 C18 N6 111.7(12) . . ? C13 C18 C17 112.7(12) . . ? N6 C18 C17 111.3(11) . . ? C13 C18 H18 106.9 . . ? N6 C18 H18 106.9 . . ? C17 C18 H18 106.9 . . ? N7 C19 C20 116.3(9) . . ? N7 C19 C24 110.6(10) . . ? C20 C19 C24 111.1(10) . . ? N7 C19 H19 106.1 . . ? C20 C19 H19 106.1 . . ? C24 C19 H19 106.1 . . ? C19 C20 C21 114.5(9) . . ? C19 C20 H20A 108.6 . . ? C21 C20 H20A 108.6 . . ? C19 C20 H20B 108.6 . . ? C21 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C22 C21 C20 112.8(10) . . ? C22 C21 H21A 109.0 . . ? C20 C21 H21A 109.0 . . ? C22 C21 H21B 109.0 . . ? C20 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C21 C22 C23 112.0(11) . . ? C21 C22 H22A 109.2 . . ? C23 C22 H22A 109.2 . . ? C21 C22 H22B 109.2 . . ? C23 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C24 C23 C22 110.2(10) . . ? C24 C23 H23A 109.6 . . ? C22 C23 H23A 109.6 . . ? C24 C23 H23B 109.6 . . ? C22 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? N8 C24 C19 111.8(10) . . ? N8 C24 C23 112.8(9) . . ? C19 C24 C23 112.7(10) . . ? N8 C24 H24 106.4 . . ? C19 C24 H24 106.4 . . ? C23 C24 H24 106.4 . . ? N9 C25 C26 113.6(11) . . ? N9 C25 C30 109.4(11) . . ? C26 C25 C30 109.9(12) . . ? N9 C25 H25 107.9 . . ? C26 C25 H25 107.9 . . ? C30 C25 H25 107.9 . . ? C25 C26 C27 110.9(13) . . ? C25 C26 H26A 109.5 . . ? C27 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C26 111.5(18) . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27B 109.3 . . ? C26 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? C29 C28 C27 112.8(17) . . ? C29 C28 H28A 109.0 . . ? C27 C28 H28A 109.0 . . ? C29 C28 H28B 109.0 . . ? C27 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C28 C29 C30 113.4(13) . . ? C28 C29 H29A 108.9 . . ? C30 C29 H29A 108.9 . . ? C28 C29 H29B 108.9 . . ? C30 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? N10 C30 C29 113.0(11) . . ? N10 C30 C25 106.9(11) . . ? C29 C30 C25 112.7(13) . . ? N10 C30 H30 108.0 . . ? C29 C30 H30 108.0 . . ? C25 C30 H30 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 In1 S1 In5 56.78(15) . . . 2_545 ? S3 In1 S1 In5 -68.23(13) . . . 2_545 ? S4 In1 S1 In5 176.65(11) . . . 2_545 ? S5 In2 S2 In1 178.06(11) . . . . ? S6 In2 S2 In1 59.44(15) . . . . ? S7 In2 S2 In1 -62.10(14) . . . . ? S1 In1 S2 In2 -179.76(11) . . . . ? S3 In1 S2 In2 -60.68(15) . . . . ? S4 In1 S2 In2 65.39(15) . . . . ? S8 In3 S3 In1 -178.00(10) . . . . ? S9 In3 S3 In1 63.93(13) . . . . ? S6 In3 S3 In1 -55.79(13) . . . . ? S2 In1 S3 In3 60.48(14) . . . . ? S1 In1 S3 In3 179.69(10) . . . . ? S4 In1 S3 In3 -67.61(13) . . . . ? S10 In4 S4 In1 -175.27(10) . . . . ? S7 In4 S4 In1 61.07(13) . . . . ? S9 In4 S4 In1 -60.54(13) . . . . ? S2 In1 S4 In4 -65.84(14) . . . . ? S1 In1 S4 In4 178.11(11) . . . . ? S3 In1 S4 In4 64.24(13) . . . . ? S2 In2 S5 In5 178.07(12) . . . . ? S6 In2 S5 In5 -62.18(13) . . . . ? S7 In2 S5 In5 59.23(13) . . . . ? S11 In5 S5 In2 63.10(14) . . . . ? S12 In5 S5 In2 -66.64(13) . . . . ? S1 In5 S5 In2 169.99(10) 2 . . . ? S2 In2 S6 In3 -62.85(13) . . . . ? S5 In2 S6 In3 179.08(10) . . . . ? S7 In2 S6 In3 57.72(12) . . . . ? S2 In2 S6 In6 177.61(10) . . . . ? S5 In2 S6 In6 59.54(12) . . . . ? S7 In2 S6 In6 -61.83(11) . . . . ? S8 In3 S6 In2 179.95(9) . . . . ? S3 In3 S6 In2 59.52(12) . . . . ? S9 In3 S6 In2 -59.44(12) . . . . ? S8 In3 S6 In6 -61.18(12) . . . . ? S3 In3 S6 In6 178.39(10) . . . . ? S9 In3 S6 In6 59.43(12) . . . . ? S11 In6 S6 In2 -57.26(13) . . . . ? S13 In6 S6 In2 -177.34(9) . . . . ? S14 In6 S6 In2 59.48(11) . . . . ? S11 In6 S6 In3 -177.15(10) . . . . ? S13 In6 S6 In3 62.77(11) . . . . ? S14 In6 S6 In3 -60.41(11) . . . . ? S12 In7 S7 In4 -177.23(10) . . . . ? S15 In7 S7 In4 -60.37(12) . . . . ? S14 In7 S7 In4 56.53(12) . . . . ? S12 In7 S7 In2 64.02(12) . . . . ? S15 In7 S7 In2 -179.12(9) . . . . ? S14 In7 S7 In2 -62.21(11) . . . . ? S4 In4 S7 In7 -179.79(10) . . . . ? S10 In4 S7 In7 58.52(13) . . . . ? S9 In4 S7 In7 -56.64(12) . . . . ? S4 In4 S7 In2 -62.16(12) . . . . ? S10 In4 S7 In2 176.15(9) . . . . ? S9 In4 S7 In2 60.98(11) . . . . ? S2 In2 S7 In7 -175.82(10) . . . . ? S5 In2 S7 In7 -57.64(12) . . . . ? S6 In2 S7 In7 62.67(11) . . . . ? S2 In2 S7 In4 63.25(12) . . . . ? S5 In2 S7 In4 -178.57(10) . . . . ? S6 In2 S7 In4 -58.26(12) . . . . ? S3 In3 S8 In8 178.59(10) . . . . ? S9 In3 S8 In8 -63.00(11) . . . . ? S6 In3 S8 In8 58.61(12) . . . . ? S13 In8 S8 In3 -69.28(12) . . . . ? S17 In8 S8 In3 69.59(12) . . . . ? S16 In8 S8 In3 176.26(8) . . . . ? S8 In3 S9 In4 -176.30(9) . . . . ? S3 In3 S9 In4 -57.74(12) . . . . ? S6 In3 S9 In4 60.90(11) . . . . ? S8 In3 S9 In9 65.28(11) . . . . ? S3 In3 S9 In9 -176.15(9) . . . . ? S6 In3 S9 In9 -57.51(11) . . . . ? S4 In4 S9 In3 57.92(12) . . . . ? S10 In4 S9 In3 176.53(9) . . . . ? S7 In4 S9 In3 -62.32(11) . . . . ? S4 In4 S9 In9 178.37(9) . . . . ? S10 In4 S9 In9 -63.02(11) . . . . ? S7 In4 S9 In9 58.13(11) . . . . ? S18 In9 S9 In3 179.96(9) . . . . ? S17 In9 S9 In3 -59.86(11) . . . . ? S14 In9 S9 In3 56.01(11) . . . . ? S18 In9 S9 In4 61.92(12) . . . . ? S17 In9 S9 In4 -177.89(9) . . . . ? S14 In9 S9 In4 -62.03(11) . . . . ? S4 In4 S10 In10 -171.23(10) . . . . ? S7 In4 S10 In10 -50.79(12) . . . . ? S9 In4 S10 In10 68.32(11) . . . . ? S18 In10 S10 In4 -75.48(12) . . . . ? S15 In10 S10 In4 56.21(13) . . . . ? S20 In10 S10 In4 165.55(9) 4_566 . . . ? S13 In6 S11 In5 169.37(10) . . . . ? S6 In6 S11 In5 54.42(14) . . . . ? S14 In6 S11 In5 -65.45(13) . . . . ? S12 In5 S11 In6 66.58(14) . . . . ? S1 In5 S11 In6 -170.87(11) 2 . . . ? S5 In5 S11 In6 -57.45(14) . . . . ? S15 In7 S12 In5 173.04(11) . . . . ? S7 In7 S12 In5 -72.15(14) . . . . ? S14 In7 S12 In5 50.79(16) . . . . ? S11 In5 S12 In7 -54.75(16) . . . . ? S1 In5 S12 In7 -167.87(11) 2 . . . ? S5 In5 S12 In7 73.02(14) . . . . ? S11 In6 S13 In8 168.93(10) . . . . ? S6 In6 S13 In8 -68.89(11) . . . . ? S14 In6 S13 In8 50.31(13) . . . . ? S8 In8 S13 In6 79.32(12) . . . . ? S17 In8 S13 In6 -58.69(13) . . . . ? S16 In8 S13 In6 -167.06(9) . . . . ? S12 In7 S14 In9 -179.13(10) . . . . ? S15 In7 S14 In9 57.85(11) . . . . ? S7 In7 S14 In9 -58.04(11) . . . . ? S12 In7 S14 In6 -59.70(13) . . . . ? S15 In7 S14 In6 177.28(9) . . . . ? S7 In7 S14 In6 61.39(11) . . . . ? S18 In9 S14 In7 -61.88(12) . . . . ? S17 In9 S14 In7 178.10(9) . . . . ? S9 In9 S14 In7 61.98(11) . . . . ? S18 In9 S14 In6 179.76(9) . . . . ? S17 In9 S14 In6 59.74(11) . . . . ? S9 In9 S14 In6 -56.38(12) . . . . ? S11 In6 S14 In7 63.48(12) . . . . ? S13 In6 S14 In7 -174.20(9) . . . . ? S6 In6 S14 In7 -59.27(11) . . . . ? S11 In6 S14 In9 -178.16(10) . . . . ? S13 In6 S14 In9 -55.84(13) . . . . ? S6 In6 S14 In9 59.09(11) . . . . ? S12 In7 S15 In10 173.46(11) . . . . ? S7 In7 S15 In10 58.45(12) . . . . ? S14 In7 S15 In10 -59.89(12) . . . . ? S18 In10 S15 In7 68.11(12) . . . . ? S10 In10 S15 In7 -62.77(13) . . . . ? S20 In10 S15 In7 -175.44(9) 4_566 . . . ? N4 In12 S16 In8 -35.0(3) . . . . ? N3 In12 S16 In8 43.2(2) . . . . ? S20 In12 S16 In8 144.93(8) 3_655 . . . ? S19 In12 S16 In8 -121.24(8) 3_655 . . . ? N4 In12 S16 In11 88.3(3) . . . . ? N3 In12 S16 In11 166.4(2) . . . . ? S20 In12 S16 In11 -91.83(7) 3_655 . . . ? S19 In12 S16 In11 2.00(7) 3_655 . . . ? S13 In8 S16 In12 171.02(9) . . . . ? S8 In8 S16 In12 -71.26(10) . . . . ? S17 In8 S16 In12 48.63(10) . . . . ? S13 In8 S16 In11 72.19(12) . . . . ? S8 In8 S16 In11 -170.09(10) . . . . ? S17 In8 S16 In11 -50.20(12) . . . . ? N2 In11 S16 In12 -97.03(19) . . . . ? N1 In11 S16 In12 -172.5(2) . . . . ? S19 In11 S16 In12 86.59(7) . . . . ? S19 In11 S16 In12 -2.02(7) 3_655 . . . ? S20 In11 S16 In12 169.6(6) . . . . ? N2 In11 S16 In8 10.3(2) . . . . ? N1 In11 S16 In8 -65.1(2) . . . . ? S19 In11 S16 In8 -166.05(10) . . . . ? S19 In11 S16 In8 105.33(11) 3_655 . . . ? S20 In11 S16 In8 -83.1(6) . . . . ? S18 In9 S17 In8 176.87(10) . . . . ? S14 In9 S17 In8 -62.30(11) . . . . ? S9 In9 S17 In8 55.97(11) . . . . ? S13 In8 S17 In9 68.03(12) . . . . ? S8 In8 S17 In9 -67.83(12) . . . . ? S16 In8 S17 In9 -178.78(9) . . . . ? S17 In9 S18 In10 -178.67(9) . . . . ? S14 In9 S18 In10 63.26(12) . . . . ? S9 In9 S18 In10 -60.20(12) . . . . ? S10 In10 S18 In9 67.98(12) . . . . ? S15 In10 S18 In9 -67.36(12) . . . . ? S20 In10 S18 In9 -176.53(8) 4_566 . . . ? N2 In11 S19 In11 138(2) . . . 3_655 ? N1 In11 S19 In11 -172.7(2) . . . 3_655 ? S19 In11 S19 In11 0.0 3_655 . . 3_655 ? S16 In11 S19 In11 -88.27(7) . . . 3_655 ? S20 In11 S19 In11 98.51(7) . . . 3_655 ? N2 In11 S19 In12 49(2) . . . 3_655 ? N1 In11 S19 In12 97.7(2) . . . 3_655 ? S19 In11 S19 In12 -89.60(7) 3_655 . . 3_655 ? S16 In11 S19 In12 -177.87(7) . . . 3_655 ? S20 In11 S19 In12 8.91(7) . . . 3_655 ? N2 In11 S20 In12 173.82(19) . . . 3_655 ? N1 In11 S20 In12 -110.4(2) . . . 3_655 ? S19 In11 S20 In12 -9.37(7) . . . 3_655 ? S19 In11 S20 In12 79.00(7) 3_655 . . 3_655 ? S16 In11 S20 In12 -92.5(6) . . . 3_655 ? N2 In11 S20 In10 -80.5(2) . . . 4_565 ? N1 In11 S20 In10 -4.7(2) . . . 4_565 ? S19 In11 S20 In10 96.31(10) . . . 4_565 ? S19 In11 S20 In10 -175.32(9) 3_655 . . 4_565 ? S16 In11 S20 In10 13.2(6) . . . 4_565 ? N2 In11 N1 C1 13.0(7) . . . . ? S19 In11 N1 C1 -163.1(7) . . . . ? S19 In11 N1 C1 54.3(14) 3_655 . . . ? S16 In11 N1 C1 107.1(7) . . . . ? S20 In11 N1 C1 -75.0(7) . . . . ? N1 In11 N2 C6 9.9(7) . . . . ? S19 In11 N2 C6 60(3) . . . . ? S19 In11 N2 C6 -162.2(7) 3_655 . . . ? S16 In11 N2 C6 -73.7(7) . . . . ? S20 In11 N2 C6 99.5(7) . . . . ? N4 In12 N3 C7 11.2(6) . . . . ? S16 In12 N3 C7 -113.3(6) . . . . ? S20 In12 N3 C7 141.5(6) 3_655 . . . ? S19 In12 N3 C7 15.2(11) 3_655 . . . ? N3 In12 N4 C12 16.6(7) . . . . ? S16 In12 N4 C12 107.9(7) . . . . ? S20 In12 N4 C12 -72.0(8) 3_655 . . . ? S19 In12 N4 C12 -162.1(7) 3_655 . . . ? N8 Ni1 N5 C13 -30(3) . . . . ? N9 Ni1 N5 C13 164.1(9) . . . . ? N6 Ni1 N5 C13 -13.0(9) . . . . ? N7 Ni1 N5 C13 -104.1(9) . . . . ? N10 Ni1 N5 C13 83.3(9) . . . . ? N8 Ni1 N6 C18 165.5(9) . . . . ? N9 Ni1 N6 C18 -39(3) . . . . ? N7 Ni1 N6 C18 83.4(9) . . . . ? N5 Ni1 N6 C18 -12.6(9) . . . . ? N10 Ni1 N6 C18 -102.8(9) . . . . ? N8 Ni1 N7 C19 16.8(7) . . . . ? N9 Ni1 N7 C19 -77.0(8) . . . . ? N6 Ni1 N7 C19 108.6(8) . . . . ? N5 Ni1 N7 C19 -169.6(7) . . . . ? N10 Ni1 N7 C19 -35(2) . . . . ? N9 Ni1 N8 C24 99.6(8) . . . . ? N6 Ni1 N8 C24 -83.1(8) . . . . ? N7 Ni1 N8 C24 8.6(8) . . . . ? N5 Ni1 N8 C24 -66(3) . . . . ? N10 Ni1 N8 C24 -179.7(8) . . . . ? N8 Ni1 N9 C25 75.0(9) . . . . ? N6 Ni1 N9 C25 -81(3) . . . . ? N7 Ni1 N9 C25 157.0(8) . . . . ? N5 Ni1 N9 C25 -106.7(8) . . . . ? N10 Ni1 N9 C25 -15.9(8) . . . . ? N8 Ni1 N10 C30 -107.9(9) . . . . ? N9 Ni1 N10 C30 -14.1(9) . . . . ? N6 Ni1 N10 C30 159.9(9) . . . . ? N7 Ni1 N10 C30 -57(2) . . . . ? N5 Ni1 N10 C30 78.1(9) . . . . ? In11 N1 C1 C6 -36.1(13) . . . . ? In11 N1 C1 C2 -171.4(8) . . . . ? C6 C1 C2 C3 42.0(17) . . . . ? N1 C1 C2 C3 176.9(11) . . . . ? C1 C2 C3 C4 -44.5(19) . . . . ? C2 C3 C4 C5 48(2) . . . . ? C3 C4 C5 C6 -46(2) . . . . ? N1 C1 C6 N2 46.6(15) . . . . ? C2 C1 C6 N2 -178.5(10) . . . . ? N1 C1 C6 C5 -179.1(10) . . . . ? C2 C1 C6 C5 -44.1(17) . . . . ? In11 N2 C6 C1 -32.5(13) . . . . ? In11 N2 C6 C5 -168.4(9) . . . . ? C4 C5 C6 C1 44.6(17) . . . . ? C4 C5 C6 N2 178.4(12) . . . . ? In12 N3 C7 C12 -38.0(10) . . . . ? In12 N3 C7 C8 -164.7(7) . . . . ? C12 C7 C8 C9 52.5(14) . . . . ? N3 C7 C8 C9 176.8(10) . . . . ? C7 C8 C9 C10 -56.2(15) . . . . ? C8 C9 C10 C11 60.4(16) . . . . ? C9 C10 C11 C12 -58.4(17) . . . . ? N3 C7 C12 N4 53.7(12) . . . . ? C8 C7 C12 N4 179.7(9) . . . . ? N3 C7 C12 C11 -178.8(9) . . . . ? C8 C7 C12 C11 -52.8(14) . . . . ? In12 N4 C12 C7 -43.6(11) . . . . ? In12 N4 C12 C11 -170.7(9) . . . . ? C10 C11 C12 C7 55.2(16) . . . . ? C10 C11 C12 N4 -178.9(12) . . . . ? Ni1 N5 C13 C18 38.5(15) . . . . ? Ni1 N5 C13 C14 172.9(10) . . . . ? C18 C13 C14 C15 -43.3(19) . . . . ? N5 C13 C14 C15 -175.4(13) . . . . ? C13 C14 C15 C16 45(2) . . . . ? C14 C15 C16 C17 -53(2) . . . . ? C15 C16 C17 C18 54(2) . . . . ? N5 C13 C18 N6 -52.9(17) . . . . ? C14 C13 C18 N6 173.7(11) . . . . ? N5 C13 C18 C17 -179.1(13) . . . . ? C14 C13 C18 C17 47(2) . . . . ? Ni1 N6 C18 C13 38.2(14) . . . . ? Ni1 N6 C18 C17 165.3(11) . . . . ? C16 C17 C18 C13 -51(2) . . . . ? C16 C17 C18 N6 -177.3(14) . . . . ? Ni1 N7 C19 C20 -166.6(9) . . . . ? Ni1 N7 C19 C24 -38.8(11) . . . . ? N7 C19 C20 C21 177.3(10) . . . . ? C24 C19 C20 C21 49.7(15) . . . . ? C19 C20 C21 C22 -50.9(16) . . . . ? C20 C21 C22 C23 52.5(16) . . . . ? C21 C22 C23 C24 -54.8(15) . . . . ? Ni1 N8 C24 C19 -32.3(12) . . . . ? Ni1 N8 C24 C23 -160.4(8) . . . . ? N7 C19 C24 N8 48.7(14) . . . . ? C20 C19 C24 N8 179.4(10) . . . . ? N7 C19 C24 C23 176.9(10) . . . . ? C20 C19 C24 C23 -52.4(14) . . . . ? C22 C23 C24 N8 -177.6(10) . . . . ? C22 C23 C24 C19 54.8(14) . . . . ? Ni1 N9 C25 C26 166.0(11) . . . . ? Ni1 N9 C25 C30 42.8(12) . . . . ? N9 C25 C26 C27 -179.0(15) . . . . ? C30 C25 C26 C27 -56(2) . . . . ? C25 C26 C27 C28 56(2) . . . . ? C26 C27 C28 C29 -53(2) . . . . ? C27 C28 C29 C30 51(2) . . . . ? Ni1 N10 C30 C29 164.6(11) . . . . ? Ni1 N10 C30 C25 40.0(13) . . . . ? C28 C29 C30 N10 -172.9(16) . . . . ? C28 C29 C30 C25 -52(2) . . . . ? N9 C25 C30 N10 -55.7(14) . . . . ? C26 C25 C30 N10 178.8(12) . . . . ? N9 C25 C30 C29 179.5(11) . . . . ? C26 C25 C30 C29 54.1(17) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.399 _refine_diff_density_min -1.175 _refine_diff_density_rms 0.168 # SQUEEZE RESULTS (APPEND TO CIF) 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 1 0.914 0.000 0.500 1158.3 63.2 2 0.951 0.500 1.000 1158.3 67.0 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 923788' ####################################################################### # # 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_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H192 In8 N24 Ni4 O12 S16' _chemical_formula_weight 3252.86 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' In In -0.7276 1.3100 '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 monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.042(4) _cell_length_b 9.8206(8) _cell_length_c 24.305(2) _cell_angle_alpha 90.00 _cell_angle_beta 127.353(2) _cell_angle_gamma 90.00 _cell_volume 6079.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 13796 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description Chip _exptl_crystal_colour pink _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.777 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 2.422 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4441 _exptl_absorpt_correction_T_max 0.7937 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16980 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6838 _reflns_number_gt 6071 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+38.9307P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6838 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1344 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 Ni1 Ni 0.59710(3) 0.80816(8) 0.45951(4) 0.02566(18) Uani 1 1 d . . . In1 In 0.689909(14) 0.29289(4) 0.43140(2) 0.02544(12) Uani 1 1 d . . . In2 In 0.565525(14) 0.35954(4) 0.30676(2) 0.02496(12) Uani 1 1 d . . . S1 S 0.73425(5) 0.07009(15) 0.47678(7) 0.0285(3) Uani 1 1 d . . . S2 S 0.64172(6) 0.34408(19) 0.30753(8) 0.0356(4) Uani 1 1 d . . . S3 S 0.61432(6) 0.33983(17) 0.43415(7) 0.0302(3) Uani 1 1 d . . . S4 S 0.5000 0.1729(2) 0.2500 0.0292(4) Uani 1 2 d S . . S5 S 0.5000 0.5467(2) 0.2500 0.0270(4) Uani 1 2 d S . . N1 N 0.5504(2) 0.6281(5) 0.4245(3) 0.0325(11) Uani 1 1 d . . . N2 N 0.5338(2) 0.8828(5) 0.4584(3) 0.0323(11) Uani 1 1 d . . . N3 N 0.63852(19) 0.9952(5) 0.4979(2) 0.0302(11) Uani 1 1 d . . . N4 N 0.6425(2) 0.7627(6) 0.5678(3) 0.0336(11) Uani 1 1 d . . . N5 N 0.6552(2) 0.7206(5) 0.4532(3) 0.0321(11) Uani 1 1 d . . . N6 N 0.56369(19) 0.8646(5) 0.3551(3) 0.0302(11) Uani 1 1 d . . . C1 C 0.5068(3) 0.6497(8) 0.4283(6) 0.068(3) Uani 1 1 d . . . C2 C 0.4643(3) 0.5395(7) 0.3927(4) 0.0426(16) Uani 1 1 d . . . C3 C 0.4210(4) 0.5671(10) 0.3996(7) 0.085(4) Uani 1 1 d . . . C4 C 0.4046(4) 0.7039(12) 0.3939(7) 0.093(4) Uani 1 1 d . . . C5 C 0.4476(3) 0.8102(8) 0.4300(4) 0.0435(17) Uani 1 1 d . . . C6 C 0.4902(4) 0.7860(9) 0.4213(6) 0.072(3) Uani 1 1 d . . . C7 C 0.6637(3) 1.0040(8) 0.5723(4) 0.0501(19) Uani 1 1 d . . . C8 C 0.7051(3) 1.1149(8) 0.6087(4) 0.0462(18) Uani 1 1 d . . . C9 C 0.7321(4) 1.1205(12) 0.6862(4) 0.074(3) Uani 1 1 d . . . C10 C 0.7529(4) 0.9891(12) 0.7181(4) 0.082(3) Uani 1 1 d . . . C11 C 0.7103(3) 0.8698(9) 0.6835(3) 0.055(2) Uani 1 1 d . . . C12 C 0.6847(3) 0.8697(8) 0.6044(4) 0.051(2) Uani 1 1 d . . . C13 C 0.6397(2) 0.7379(6) 0.3818(3) 0.0297(12) Uani 1 1 d . . . C14 C 0.6868(2) 0.7340(7) 0.3812(3) 0.0336(14) Uani 1 1 d . . . C15 C 0.6699(3) 0.7620(8) 0.3075(4) 0.0443(17) Uani 1 1 d . . . C16 C 0.6389(3) 0.8953(8) 0.2785(3) 0.0422(16) Uani 1 1 d . . . C17 C 0.5907(3) 0.8912(7) 0.2773(3) 0.0369(14) Uani 1 1 d . . . C18 C 0.6086(2) 0.8695(6) 0.3518(3) 0.0281(12) Uani 1 1 d . . . O1 O 0.3000(2) 0.4996(6) 0.4135(3) 0.0583(15) Uani 1 1 d . . . O2 O 0.4150(3) 0.1988(7) 0.3643(3) 0.0661(17) Uani 1 1 d . . . O3 O 0.5129(2) 0.1637(6) 0.3917(3) 0.0489(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0241(4) 0.0253(4) 0.0282(4) 0.0005(3) 0.0161(3) 0.0014(3) In1 0.01614(19) 0.0270(2) 0.0254(2) -0.00045(15) 0.00854(16) 0.00154(14) In2 0.01648(19) 0.0257(2) 0.0242(2) 0.00131(15) 0.00793(16) 0.00098(14) S1 0.0205(6) 0.0237(7) 0.0308(7) -0.0029(6) 0.0101(5) 0.0002(5) S2 0.0223(7) 0.0527(10) 0.0283(7) 0.0040(7) 0.0135(6) 0.0027(7) S3 0.0209(7) 0.0384(8) 0.0258(7) 0.0018(6) 0.0112(6) 0.0061(6) S4 0.0241(10) 0.0222(9) 0.0318(10) 0.000 0.0121(8) 0.000 S5 0.0200(9) 0.0210(9) 0.0267(9) 0.000 0.0073(8) 0.000 N1 0.032(3) 0.027(3) 0.046(3) -0.005(2) 0.028(2) -0.001(2) N2 0.028(3) 0.030(3) 0.043(3) -0.008(2) 0.024(2) -0.004(2) N3 0.030(3) 0.028(3) 0.031(3) -0.002(2) 0.018(2) -0.004(2) N4 0.034(3) 0.033(3) 0.027(3) 0.004(2) 0.015(2) 0.004(2) N5 0.032(3) 0.037(3) 0.030(3) 0.007(2) 0.020(2) 0.011(2) N6 0.024(2) 0.035(3) 0.031(3) 0.004(2) 0.017(2) 0.005(2) C1 0.053(5) 0.032(4) 0.143(9) -0.015(5) 0.071(6) -0.008(3) C2 0.036(4) 0.032(3) 0.059(4) -0.001(3) 0.029(3) -0.006(3) C3 0.051(5) 0.047(5) 0.172(11) 0.005(6) 0.075(7) -0.006(4) C4 0.066(6) 0.085(8) 0.154(11) -0.048(8) 0.081(8) -0.026(6) C5 0.032(3) 0.052(4) 0.054(4) -0.011(3) 0.029(3) -0.001(3) C6 0.055(5) 0.049(5) 0.133(9) -0.045(5) 0.068(6) -0.020(4) C7 0.061(5) 0.045(4) 0.034(4) -0.006(3) 0.023(3) -0.015(4) C8 0.051(4) 0.049(4) 0.042(4) -0.021(3) 0.030(3) -0.019(3) C9 0.081(7) 0.089(7) 0.036(4) -0.021(5) 0.028(5) -0.027(6) C10 0.058(6) 0.092(8) 0.039(4) -0.023(5) 0.000(4) 0.000(5) C11 0.055(5) 0.066(5) 0.022(3) -0.005(3) 0.012(3) -0.003(4) C12 0.058(5) 0.048(4) 0.030(4) -0.003(3) 0.018(3) -0.008(4) C13 0.029(3) 0.032(3) 0.028(3) 0.002(2) 0.017(2) 0.006(2) C14 0.033(3) 0.039(3) 0.036(3) 0.005(3) 0.025(3) 0.009(3) C15 0.059(5) 0.044(4) 0.043(4) 0.009(3) 0.038(4) 0.014(3) C16 0.046(4) 0.051(4) 0.037(3) 0.011(3) 0.028(3) 0.009(3) C17 0.036(3) 0.045(4) 0.026(3) 0.007(3) 0.017(3) 0.004(3) C18 0.025(3) 0.035(3) 0.022(3) 0.005(2) 0.013(2) 0.005(2) O1 0.074(4) 0.050(3) 0.060(3) -0.001(3) 0.045(3) 0.014(3) O2 0.070(4) 0.074(4) 0.078(4) -0.006(3) 0.057(4) -0.005(3) O3 0.043(3) 0.054(3) 0.055(3) 0.014(3) 0.033(3) 0.003(2) _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 N3 2.122(5) . ? Ni1 N1 2.133(5) . ? Ni1 N5 2.139(5) . ? Ni1 N2 2.141(5) . ? Ni1 N4 2.143(5) . ? Ni1 N6 2.144(5) . ? In1 S2 2.4617(16) . ? In1 S1 2.4730(14) 7_656 ? In1 S1 2.4741(15) . ? In1 S3 2.5059(16) . ? In1 In2 3.2923(6) . ? In1 In1 3.3282(8) 7_656 ? In2 S2 2.4349(16) . ? In2 S4 2.4814(16) . ? In2 S5 2.4852(15) . ? In2 S3 2.4889(15) . ? In2 In2 3.3447(8) 2_655 ? S1 In1 2.4730(14) 7_656 ? S4 In2 2.4813(16) 2_655 ? S5 In2 2.4852(15) 2_655 ? N1 C1 1.470(9) . ? N2 C6 1.464(9) . ? N3 C7 1.471(8) . ? N4 C12 1.505(9) . ? N5 C13 1.497(7) . ? N6 C18 1.489(8) . ? C1 C6 1.411(11) . ? C1 C2 1.529(10) . ? C2 C3 1.520(12) . ? C3 C4 1.418(14) . ? C4 C5 1.513(12) . ? C5 C6 1.520(10) . ? C7 C12 1.471(11) . ? C7 C8 1.519(10) . ? C8 C9 1.523(10) . ? C9 C10 1.443(15) . ? C10 C11 1.598(14) . ? C11 C12 1.566(10) . ? C13 C14 1.517(8) . ? C13 C18 1.522(8) . ? C14 C15 1.550(9) . ? C15 C16 1.532(10) . ? C16 C17 1.526(10) . ? C17 C18 1.547(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ni1 N1 173.6(2) . . ? N3 Ni1 N5 92.3(2) . . ? N1 Ni1 N5 94.0(2) . . ? N3 Ni1 N2 92.53(19) . . ? N1 Ni1 N2 81.3(2) . . ? N5 Ni1 N2 174.7(2) . . ? N3 Ni1 N4 82.1(2) . . ? N1 Ni1 N4 96.1(2) . . ? N5 Ni1 N4 91.9(2) . . ? N2 Ni1 N4 91.1(2) . . ? N3 Ni1 N6 91.51(19) . . ? N1 Ni1 N6 91.0(2) . . ? N5 Ni1 N6 81.38(19) . . ? N2 Ni1 N6 96.2(2) . . ? N4 Ni1 N6 170.6(2) . . ? S2 In1 S1 122.43(6) . 7_656 ? S2 In1 S1 119.36(6) . . ? S1 In1 S1 95.44(5) 7_656 . ? S2 In1 S3 95.50(5) . . ? S1 In1 S3 108.20(5) 7_656 . ? S1 In1 S3 116.98(5) . . ? S2 In1 In2 47.41(4) . . ? S1 In1 In2 134.46(4) 7_656 . ? S1 In1 In2 129.29(4) . . ? S3 In1 In2 48.54(3) . . ? S2 In1 In1 139.72(4) . 7_656 ? S1 In1 In1 47.73(3) 7_656 7_656 ? S1 In1 In1 47.71(3) . 7_656 ? S3 In1 In1 124.70(4) . 7_656 ? In2 In1 In1 172.35(2) . 7_656 ? S2 In2 S4 117.68(5) . . ? S2 In2 S5 123.77(5) . . ? S4 In2 S5 95.33(5) . . ? S2 In2 S3 96.63(5) . . ? S4 In2 S3 108.37(4) . . ? S5 In2 S3 115.44(4) . . ? S2 In2 In1 48.10(4) . . ? S4 In2 In1 120.55(4) . . ? S5 In2 In1 143.24(3) . . ? S3 In2 In1 48.99(4) . . ? S2 In2 In2 139.25(4) . 2_655 ? S4 In2 In2 47.63(3) . 2_655 ? S5 In2 In2 47.71(3) . 2_655 ? S3 In2 In2 123.57(4) . 2_655 ? In1 In2 In2 166.434(15) . 2_655 ? In1 S1 In1 84.56(5) 7_656 . ? In2 S2 In1 84.50(5) . . ? In2 S3 In1 82.47(5) . . ? In2 S4 In2 84.75(7) . 2_655 ? In2 S5 In2 84.58(6) 2_655 . ? C1 N1 Ni1 108.6(4) . . ? C6 N2 Ni1 109.2(4) . . ? C7 N3 Ni1 108.7(4) . . ? C12 N4 Ni1 106.1(4) . . ? C13 N5 Ni1 110.3(3) . . ? C18 N6 Ni1 105.5(3) . . ? C6 C1 N1 115.6(7) . . ? C6 C1 C2 117.5(7) . . ? N1 C1 C2 114.5(6) . . ? C3 C2 C1 111.7(7) . . ? C4 C3 C2 117.8(8) . . ? C3 C4 C5 116.4(9) . . ? C4 C5 C6 112.9(7) . . ? C1 C6 N2 113.1(7) . . ? C1 C6 C5 115.9(8) . . ? N2 C6 C5 114.5(6) . . ? C12 C7 N3 109.4(6) . . ? C12 C7 C8 112.2(7) . . ? N3 C7 C8 113.1(6) . . ? C7 C8 C9 112.7(7) . . ? C10 C9 C8 111.3(8) . . ? C9 C10 C11 113.8(7) . . ? C12 C11 C10 106.9(7) . . ? C7 C12 N4 110.7(6) . . ? C7 C12 C11 112.3(7) . . ? N4 C12 C11 109.8(6) . . ? N5 C13 C14 112.0(5) . . ? N5 C13 C18 108.2(5) . . ? C14 C13 C18 112.5(5) . . ? C13 C14 C15 110.7(5) . . ? C16 C15 C14 111.0(5) . . ? C17 C16 C15 110.5(6) . . ? C16 C17 C18 109.3(5) . . ? N6 C18 C13 108.7(5) . . ? N6 C18 C17 112.6(5) . . ? C13 C18 C17 110.3(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 In1 In2 S2 96.81(8) 7_656 . . . ? S1 In1 In2 S2 -96.22(8) . . . . ? S3 In1 In2 S2 170.37(8) . . . . ? In1 In1 In2 S2 -160.09(18) 7_656 . . . ? S2 In1 In2 S4 101.25(6) . . . . ? S1 In1 In2 S4 -161.95(6) 7_656 . . . ? S1 In1 In2 S4 5.03(6) . . . . ? S3 In1 In2 S4 -88.38(5) . . . . ? In1 In1 In2 S4 -58.84(17) 7_656 . . . ? S2 In1 In2 S5 -92.67(7) . . . . ? S1 In1 In2 S5 4.14(7) 7_656 . . . ? S1 In1 In2 S5 171.11(5) . . . . ? S3 In1 In2 S5 77.70(6) . . . . ? In1 In1 In2 S5 107.24(16) 7_656 . . . ? S2 In1 In2 S3 -170.37(8) . . . . ? S1 In1 In2 S3 -73.56(8) 7_656 . . . ? S1 In1 In2 S3 93.41(7) . . . . ? In1 In1 In2 S3 29.54(17) 7_656 . . . ? S2 In1 In2 In2 128.33(10) . . . 2_655 ? S1 In1 In2 In2 -134.86(9) 7_656 . . 2_655 ? S1 In1 In2 In2 32.11(11) . . . 2_655 ? S3 In1 In2 In2 -61.30(10) . . . 2_655 ? In1 In1 In2 In2 -31.8(2) 7_656 . . 2_655 ? S2 In1 S1 In1 132.20(5) . . . 7_656 ? S1 In1 S1 In1 0.0 7_656 . . 7_656 ? S3 In1 S1 In1 -113.61(5) . . . 7_656 ? In2 In1 S1 In1 -170.70(3) . . . 7_656 ? S4 In2 S2 In1 -107.49(5) . . . . ? S5 In2 S2 In1 134.02(4) . . . . ? S3 In2 S2 In1 7.30(6) . . . . ? In2 In2 S2 In1 -163.63(2) 2_655 . . . ? S1 In1 S2 In2 -122.89(5) 7_656 . . . ? S1 In1 S2 In2 118.01(6) . . . . ? S3 In1 S2 In2 -7.23(6) . . . . ? In1 In1 S2 In2 175.98(4) 7_656 . . . ? S2 In2 S3 In1 -7.20(6) . . . . ? S4 In2 S3 In1 114.89(5) . . . . ? S5 In2 S3 In1 -139.65(4) . . . . ? In2 In2 S3 In1 165.705(16) 2_655 . . . ? S2 In1 S3 In2 7.11(6) . . . . ? S1 In1 S3 In2 133.89(5) 7_656 . . . ? S1 In1 S3 In2 -119.89(5) . . . . ? In1 In1 S3 In2 -175.42(3) 7_656 . . . ? S2 In2 S4 In2 -132.79(5) . . . 2_655 ? S5 In2 S4 In2 0.0 . . . 2_655 ? S3 In2 S4 In2 119.05(4) . . . 2_655 ? In1 In2 S4 In2 171.69(3) . . . 2_655 ? S2 In2 S5 In2 128.58(6) . . . 2_655 ? S4 In2 S5 In2 0.0 . . . 2_655 ? S3 In2 S5 In2 -113.27(5) . . . 2_655 ? In1 In2 S5 In2 -167.99(4) . . . 2_655 ? N3 Ni1 N1 C1 9(2) . . . . ? N5 Ni1 N1 C1 175.1(6) . . . . ? N2 Ni1 N1 C1 -7.3(6) . . . . ? N4 Ni1 N1 C1 82.8(6) . . . . ? N6 Ni1 N1 C1 -103.4(6) . . . . ? N3 Ni1 N2 C6 169.5(6) . . . . ? N1 Ni1 N2 C6 -12.3(6) . . . . ? N5 Ni1 N2 C6 15(2) . . . . ? N4 Ni1 N2 C6 -108.4(6) . . . . ? N6 Ni1 N2 C6 77.7(6) . . . . ? N1 Ni1 N3 C7 61(2) . . . . ? N5 Ni1 N3 C7 -105.2(5) . . . . ? N2 Ni1 N3 C7 77.1(5) . . . . ? N4 Ni1 N3 C7 -13.6(5) . . . . ? N6 Ni1 N3 C7 173.4(5) . . . . ? N3 Ni1 N4 C12 -13.8(5) . . . . ? N1 Ni1 N4 C12 172.5(5) . . . . ? N5 Ni1 N4 C12 78.3(5) . . . . ? N2 Ni1 N4 C12 -106.2(5) . . . . ? N6 Ni1 N4 C12 34.1(15) . . . . ? N3 Ni1 N5 C13 -94.7(4) . . . . ? N1 Ni1 N5 C13 86.8(4) . . . . ? N2 Ni1 N5 C13 60(2) . . . . ? N4 Ni1 N5 C13 -176.9(4) . . . . ? N6 Ni1 N5 C13 -3.5(4) . . . . ? N3 Ni1 N6 C18 66.9(4) . . . . ? N1 Ni1 N6 C18 -119.0(4) . . . . ? N5 Ni1 N6 C18 -25.2(4) . . . . ? N2 Ni1 N6 C18 159.6(4) . . . . ? N4 Ni1 N6 C18 19.6(14) . . . . ? Ni1 N1 C1 C6 28.0(11) . . . . ? Ni1 N1 C1 C2 169.5(6) . . . . ? C6 C1 C2 C3 -40.2(13) . . . . ? N1 C1 C2 C3 179.1(8) . . . . ? C1 C2 C3 C4 39.0(14) . . . . ? C2 C3 C4 C5 -41.8(17) . . . . ? C3 C4 C5 C6 41.6(15) . . . . ? N1 C1 C6 N2 -40.9(13) . . . . ? C2 C1 C6 N2 178.8(8) . . . . ? N1 C1 C6 C5 -176.1(8) . . . . ? C2 C1 C6 C5 43.7(14) . . . . ? Ni1 N2 C6 C1 31.5(10) . . . . ? Ni1 N2 C6 C5 167.3(7) . . . . ? C4 C5 C6 C1 -42.6(13) . . . . ? C4 C5 C6 N2 -177.1(9) . . . . ? Ni1 N3 C7 C12 39.7(7) . . . . ? Ni1 N3 C7 C8 165.5(5) . . . . ? C12 C7 C8 C9 -54.0(10) . . . . ? N3 C7 C8 C9 -178.3(7) . . . . ? C7 C8 C9 C10 53.3(11) . . . . ? C8 C9 C10 C11 -55.1(12) . . . . ? C9 C10 C11 C12 54.8(11) . . . . ? N3 C7 C12 N4 -54.5(9) . . . . ? C8 C7 C12 N4 179.1(6) . . . . ? N3 C7 C12 C11 -177.7(6) . . . . ? C8 C7 C12 C11 56.0(9) . . . . ? Ni1 N4 C12 C7 40.1(7) . . . . ? Ni1 N4 C12 C11 164.8(5) . . . . ? C10 C11 C12 C7 -54.1(10) . . . . ? C10 C11 C12 N4 -177.8(7) . . . . ? Ni1 N5 C13 C14 155.9(4) . . . . ? Ni1 N5 C13 C18 31.3(6) . . . . ? N5 C13 C14 C15 -176.1(5) . . . . ? C18 C13 C14 C15 -54.0(7) . . . . ? C13 C14 C15 C16 54.0(8) . . . . ? C14 C15 C16 C17 -57.6(8) . . . . ? C15 C16 C17 C18 59.5(7) . . . . ? Ni1 N6 C18 C13 50.2(5) . . . . ? Ni1 N6 C18 C17 172.8(4) . . . . ? N5 C13 C18 N6 -55.1(6) . . . . ? C14 C13 C18 N6 -179.4(5) . . . . ? N5 C13 C18 C17 -179.1(5) . . . . ? C14 C13 C18 C17 56.6(7) . . . . ? C16 C17 C18 N6 179.8(5) . . . . ? C16 C17 C18 C13 -58.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.221 _refine_diff_density_min -0.948 _refine_diff_density_rms 0.146 _database_code_depnum_ccdc_archive 'CCDC 923789' ####################################################################### # # 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_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H222 Co8 In16 N30 O5 S37' _chemical_formula_weight 5299.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'F d d d ' _symmetry_space_group_name_Hall '-F 2uv 2vw ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 24.8713(15) _cell_length_b 28.3131(16) _cell_length_c 52.118(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 36701(4) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 20608 _exptl_absorpt_coefficient_mu 3.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3671 _exptl_absorpt_correction_T_max 0.6340 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72053 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 19.94 _reflns_number_total 4052 _reflns_number_gt 3154 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two protonated 1,2-diaminocyclohexane, one 1,2-diaminocyclohexane and five water molecules contribution to the scattering factors has been taken into account with PLATON/SQUEEZE. ; _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^)+(0.0001P)^2^+5000.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4052 _refine_ls_number_parameters 315 _refine_ls_number_restraints 155 _refine_ls_R_factor_all 0.1322 _refine_ls_R_factor_gt 0.1170 _refine_ls_wR_factor_ref 0.1963 _refine_ls_wR_factor_gt 0.1907 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.242 _refine_ls_shift/su_max 0.115 _refine_ls_shift/su_mean 0.007 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 0.07090(12) 0.07674(11) 0.09933(5) 0.0655(9) Uani 1 1 d . . . Co2 Co 0.1032(2) 0.3474(2) -0.01678(11) 0.1429(19) Uani 1 1 d U . . In1 In -0.03936(8) 0.26663(7) 0.04634(4) 0.0887(7) Uani 1 1 d . . . In2 In 0.07099(7) 0.17218(7) 0.04566(3) 0.0770(6) Uani 1 1 d . . . In3 In 0.07133(8) 0.27233(7) 0.09952(4) 0.0835(7) Uani 1 1 d . . . In4 In -0.04238(7) 0.17352(7) 0.09996(3) 0.0812(6) Uani 1 1 d . . . S2 S 0.0127(3) 0.2176(3) 0.01767(13) 0.092(2) Uani 1 1 d . A . S3 S -0.1011(3) 0.2209(3) 0.07266(14) 0.091(2) Uani 1 1 d . A . S4 S 0.0152(3) 0.3208(3) 0.07184(15) 0.097(2) Uani 1 1 d . A . S5 S 0.1250 0.1250 0.01714(17) 0.084(3) Uani 1 2 d S . . S6 S 0.0138(2) 0.1213(2) 0.07307(11) 0.0720(17) Uani 1 1 d . A . S7 S 0.1297(3) 0.2222(2) 0.07235(11) 0.0721(17) Uani 1 1 d . . . S8 S -0.1025(4) 0.1250 0.1250 0.092(3) Uani 1 2 d S . . S9 S 0.0143(2) 0.2232(2) 0.12787(12) 0.0720(17) Uani 1 1 d . . . S10 S 0.1250 0.3255(4) 0.1250 0.092(3) Uani 1 2 d S . . S11 S 0.1250 0.1250 0.1250 0.064(3) Uani 1 4 d S . . S1 S -0.0912(6) 0.3212(5) 0.0247(3) 0.055(3) Uiso 0.40 1 d P A 1 S12 S -0.1250 0.3750 0.0562(4) 0.055(3) Uiso 0.40 2 d SP . 1 S1' S -0.0963(4) 0.3111(3) 0.01377(19) 0.051(2) Uiso 0.60 1 d P . 2 S12' S -0.1345(7) 0.3680(7) 0.0387(3) 0.051(2) Uiso 0.30 1 d P . 2 N1 N 0.1207(19) 0.3369(17) 0.0261(8) 0.227(11) Uani 1 1 d U . . N2 N 0.1285(19) 0.4180(13) -0.0067(9) 0.224(11) Uani 1 1 d U . . N3 N 0.0881(13) 0.3635(13) -0.0570(6) 0.171(10) Uani 1 1 d U . . N4 N 0.0205(14) 0.3648(15) -0.0134(6) 0.188(10) Uani 1 1 d U . . N5 N 0.0889(18) 0.2735(14) -0.0279(8) 0.202(11) Uani 1 1 d U . . N6 N 0.1870(14) 0.3283(15) -0.0240(8) 0.190(11) Uani 1 1 d U . . C1 C 0.129(3) 0.386(2) 0.0360(10) 0.246(11) Uani 1 1 d DU . . H1 H 0.0903 0.3929 0.0386 0.295 Uiso 1 1 calc R . . C2 C 0.144(3) 0.385(2) 0.0639(10) 0.258(13) Uani 1 1 d DU . . H2A H 0.1711 0.3616 0.0665 0.309 Uiso 1 1 calc R . . H2B H 0.1123 0.3759 0.0738 0.309 Uiso 1 1 calc R . . C3 C 0.164(3) 0.432(2) 0.0741(8) 0.272(14) Uiso 1 1 d DU . . H3A H 0.1335 0.4511 0.0791 0.327 Uiso 1 1 calc RD . . H3B H 0.1856 0.4259 0.0892 0.327 Uiso 1 1 calc R . . C4 C 0.1964(19) 0.457(2) 0.0544(11) 0.278(14) Uiso 1 1 d DU . . H4A H 0.2255 0.4375 0.0479 0.333 Uiso 1 1 calc RD . . H4B H 0.2110 0.4863 0.0611 0.333 Uiso 1 1 calc R . . C5 C 0.154(2) 0.4655(16) 0.0344(8) 0.267(11) Uani 1 1 d DU . . H5A H 0.1227 0.4797 0.0423 0.321 Uiso 1 1 calc RD . . H5B H 0.1677 0.4874 0.0216 0.321 Uiso 1 1 calc R . . C6 C 0.138(2) 0.420(2) 0.0214(10) 0.258(10) Uani 1 1 d DU . . H6 H 0.1755 0.4106 0.0193 0.310 Uiso 1 1 calc RD . . C7 C 0.0321(18) 0.3737(19) -0.0611(9) 0.185(9) Uani 1 1 d U . . H7 H 0.0171 0.3418 -0.0628 0.222 Uiso 1 1 calc R . . C8 C 0.0144(18) 0.3953(18) -0.0848(9) 0.188(10) Uani 1 1 d U . . H8A H 0.0286 0.3768 -0.0989 0.226 Uiso 1 1 calc R . . H8B H 0.0305 0.4264 -0.0859 0.226 Uiso 1 1 calc R . . C9 C -0.043(2) 0.4003(18) -0.0886(9) 0.193(12) Uiso 1 1 d DU . . H9A H -0.0585 0.3697 -0.0930 0.232 Uiso 1 1 calc R . . H9B H -0.0497 0.4213 -0.1030 0.232 Uiso 1 1 calc R . . C10 C -0.072(2) 0.4191(19) -0.0657(9) 0.213(12) Uiso 1 1 d DU . . H10A H -0.0647 0.4528 -0.0644 0.256 Uiso 1 1 calc R . . H10B H -0.1100 0.4149 -0.0679 0.256 Uiso 1 1 calc R . . C11 C -0.0548(18) 0.3962(18) -0.0418(9) 0.217(10) Uani 1 1 d U . . H11A H -0.0715 0.3653 -0.0409 0.261 Uiso 1 1 calc R . . H11B H -0.0681 0.4147 -0.0274 0.261 Uiso 1 1 calc R . . C12 C 0.0049(18) 0.3903(19) -0.0389(9) 0.198(9) Uani 1 1 d U . . H12 H 0.0184 0.4226 -0.0367 0.237 Uiso 1 1 calc R . . C13 C 0.183(2) 0.284(2) -0.0371(11) 0.199(11) Uani 1 1 d DU . . H13 H 0.1746 0.2930 -0.0549 0.239 Uiso 1 1 calc R . . C14 C 0.237(2) 0.259(2) -0.0389(12) 0.27(2) Uiso 1 1 d DU . . H14A H 0.2486 0.2497 -0.0219 0.326 Uiso 1 1 calc R . . H14B H 0.2636 0.2797 -0.0463 0.326 Uiso 1 1 calc R . . C15 C 0.229(3) 0.212(2) -0.0571(13) 0.287(16) Uiso 1 1 d DU . . H15A H 0.2250 0.2224 -0.0747 0.344 Uiso 1 1 calc R . . H15B H 0.2616 0.1933 -0.0561 0.344 Uiso 1 1 calc R . . C16 C 0.182(3) 0.179(2) -0.0509(12) 0.288(15) Uani 1 1 d DU . . H16A H 0.1914 0.1594 -0.0365 0.346 Uiso 1 1 calc R . . H16B H 0.1755 0.1587 -0.0655 0.346 Uiso 1 1 calc R . . C17 C 0.127(3) 0.206(2) -0.0443(11) 0.260(15) Uiso 1 1 d DU . . H17A H 0.1087 0.2146 -0.0601 0.312 Uiso 1 1 calc R . . H17B H 0.1032 0.1846 -0.0350 0.312 Uiso 1 1 calc R . . C18 C 0.136(2) 0.249(2) -0.0286(11) 0.207(11) Uiso 1 1 d DU . . H18 H 0.1436 0.2390 -0.0111 0.248 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.065(2) 0.076(2) 0.0550(18) -0.0005(16) -0.0029(15) -0.0015(16) Co2 0.115(4) 0.166(5) 0.148(4) 0.037(4) 0.015(3) -0.014(3) In1 0.0831(14) 0.0934(15) 0.0894(14) 0.0112(11) -0.0050(11) 0.0140(11) In2 0.0762(12) 0.0863(13) 0.0686(12) 0.0038(10) -0.0014(9) 0.0113(10) In3 0.0837(13) 0.0897(14) 0.0771(13) 0.0018(10) 0.0014(10) -0.0001(11) In4 0.0735(12) 0.0919(14) 0.0782(13) 0.0070(10) -0.0011(10) 0.0013(10) S2 0.083(5) 0.118(6) 0.075(4) 0.015(4) -0.005(4) 0.021(4) S3 0.078(4) 0.104(5) 0.090(5) 0.019(4) -0.008(4) 0.002(4) S4 0.093(5) 0.088(5) 0.108(6) 0.010(4) -0.012(4) -0.005(4) S5 0.083(6) 0.103(7) 0.066(6) 0.000 0.000 0.029(6) S6 0.071(4) 0.079(4) 0.066(4) 0.001(3) -0.009(3) 0.002(3) S7 0.073(4) 0.083(4) 0.060(4) 0.000(3) 0.002(3) -0.001(3) S8 0.064(6) 0.099(7) 0.112(8) 0.019(6) 0.000 0.000 S9 0.071(4) 0.076(4) 0.069(4) -0.001(3) 0.004(3) 0.002(3) S10 0.097(7) 0.087(7) 0.094(7) 0.000 -0.010(6) 0.000 S11 0.068(7) 0.065(7) 0.058(7) 0.000 0.000 0.000 N1 0.27(2) 0.23(2) 0.176(17) 0.12(2) 0.05(2) 0.03(2) N2 0.28(2) 0.173(17) 0.22(2) 0.092(19) 0.08(2) 0.02(2) N3 0.136(17) 0.21(2) 0.167(19) 0.065(18) 0.028(17) 0.048(19) N4 0.163(19) 0.25(2) 0.149(19) 0.053(18) 0.048(17) 0.06(2) N5 0.21(2) 0.187(16) 0.21(2) 0.006(17) 0.012(18) -0.013(18) N6 0.16(2) 0.19(2) 0.22(2) 0.03(2) 0.04(2) 0.01(2) C1 0.285(19) 0.240(19) 0.213(17) 0.106(18) 0.056(17) 0.035(19) C2 0.28(2) 0.26(2) 0.236(18) 0.060(17) 0.023(17) 0.014(17) C5 0.299(19) 0.242(18) 0.261(18) 0.163(15) 0.162(16) 0.150(16) C6 0.297(19) 0.239(17) 0.239(18) 0.135(17) 0.091(18) 0.083(17) C7 0.158(15) 0.232(18) 0.166(16) 0.058(15) 0.040(15) 0.052(16) C8 0.173(17) 0.219(18) 0.173(16) 0.039(15) 0.011(15) 0.028(16) C11 0.203(15) 0.245(18) 0.203(16) 0.126(15) 0.122(15) 0.139(15) C12 0.181(15) 0.244(18) 0.168(16) 0.072(15) 0.069(15) 0.082(16) C13 0.181(17) 0.202(19) 0.213(19) 0.024(16) 0.026(16) 0.008(17) C16 0.290(19) 0.284(19) 0.291(19) 0.124(14) 0.127(14) 0.126(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 S9 2.322(7) 8_544 ? Co1 S7 2.325(7) 14_445 ? Co1 S11 2.338(3) . ? Co1 S6 2.341(7) . ? Co2 N4 2.12(3) . ? Co2 N2 2.16(4) . ? Co2 N3 2.18(3) . ? Co2 N5 2.20(4) . ? Co2 N6 2.19(4) . ? Co2 N1 2.29(4) . ? In1 S1 2.306(15) . ? In1 S2 2.416(7) . ? In1 S3 2.432(7) . ? In1 S4 2.441(8) . ? In1 S1' 2.543(10) . ? In2 S5 2.408(6) . ? In2 S2 2.426(7) . ? In2 S7 2.463(6) . ? In2 S6 2.477(7) . ? In3 S10 2.411(7) . ? In3 S4 2.432(8) . ? In3 S9 2.476(6) . ? In3 S7 2.475(6) . ? In4 S8 2.413(6) . ? In4 S3 2.441(7) . ? In4 S9 2.466(7) . ? In4 S6 2.470(7) . ? S5 In2 2.408(6) 14_445 ? S7 Co1 2.325(7) 14_445 ? S8 In4 2.413(6) 8_544 ? S9 Co1 2.322(7) 8_544 ? S10 In3 2.411(7) 11_454 ? S11 Co1 2.338(3) 11_454 ? S11 Co1 2.338(3) 8_544 ? S11 Co1 2.338(3) 14_445 ? S1 S12 2.39(2) . ? S12 S1 2.39(2) 2_455 ? S1' S12' 2.28(2) . ? S1' S12' 2.44(2) 2_455 ? S12' S12' 0.62(3) 2_455 ? S12' S1' 2.44(2) 2_455 ? N1 C1 1.49(7) . ? N2 C6 1.48(6) . ? N3 C7 1.44(5) . ? N4 C12 1.56(5) . ? N5 C18 1.35(6) . ? N6 C13 1.42(6) . ? C1 C6 1.26(6) . ? C1 C2 1.50(2) . ? C2 C3 1.50(2) . ? C3 C4 1.49(2) . ? C4 C5 1.51(2) . ? C5 C6 1.51(2) . ? C7 C12 1.42(5) . ? C7 C8 1.45(5) . ? C8 C9 1.46(5) . ? C9 C10 1.48(2) . ? C10 C11 1.47(5) . ? C11 C12 1.50(6) . ? C13 C14 1.51(2) . ? C13 C18 1.61(6) . ? C14 C15 1.65(8) . ? C15 C16 1.53(2) . ? C16 C17 1.60(7) . ? C17 C18 1.49(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 S9 Co1 S7 105.5(3) 8_544 14_445 ? S9 Co1 S11 114.33(19) 8_544 . ? S7 Co1 S11 112.93(19) 14_445 . ? S9 Co1 S6 105.0(2) 8_544 . ? S7 Co1 S6 106.7(2) 14_445 . ? S11 Co1 S6 111.6(2) . . ? N4 Co2 N2 92.8(17) . . ? N4 Co2 N3 82.1(12) . . ? N2 Co2 N3 95.2(16) . . ? N4 Co2 N5 94.9(17) . . ? N2 Co2 N5 172.3(17) . . ? N3 Co2 N5 85.3(15) . . ? N4 Co2 N6 174.7(15) . . ? N2 Co2 N6 89.6(17) . . ? N3 Co2 N6 92.9(14) . . ? N5 Co2 N6 82.7(17) . . ? N4 Co2 N1 97.7(15) . . ? N2 Co2 N1 80.0(17) . . ? N3 Co2 N1 175.2(17) . . ? N5 Co2 N1 99.4(17) . . ? N6 Co2 N1 87.4(16) . . ? S1 In1 S2 112.5(4) . . ? S1 In1 S3 106.2(4) . . ? S2 In1 S3 112.4(3) . . ? S1 In1 S4 98.9(4) . . ? S2 In1 S4 113.6(3) . . ? S3 In1 S4 112.2(3) . . ? S1 In1 S1' 14.4(4) . . ? S2 In1 S1' 99.8(3) . . ? S3 In1 S1' 106.7(3) . . ? S4 In1 S1' 111.2(3) . . ? S5 In2 S2 104.8(2) . . ? S5 In2 S7 109.68(18) . . ? S2 In2 S7 112.9(3) . . ? S5 In2 S6 110.72(18) . . ? S2 In2 S6 108.2(2) . . ? S7 In2 S6 110.4(2) . . ? S10 In3 S4 107.0(3) . . ? S10 In3 S9 109.86(18) . . ? S4 In3 S9 110.0(2) . . ? S10 In3 S7 110.43(19) . . ? S4 In3 S7 108.7(2) . . ? S9 In3 S7 110.8(2) . . ? S8 In4 S3 104.9(2) . . ? S8 In4 S9 111.07(18) . . ? S3 In4 S9 111.9(2) . . ? S8 In4 S6 108.46(19) . . ? S3 In4 S6 109.7(2) . . ? S9 In4 S6 110.6(2) . . ? In1 S2 In2 104.7(3) . . ? In1 S3 In4 104.1(3) . . ? In3 S4 In1 106.7(3) . . ? In2 S5 In2 103.8(3) 14_445 . ? Co1 S6 In4 109.5(2) . . ? Co1 S6 In2 107.6(2) . . ? In4 S6 In2 107.7(2) . . ? Co1 S7 In2 108.2(3) 14_445 . ? Co1 S7 In3 107.8(2) 14_445 . ? In2 S7 In3 107.8(2) . . ? In4 S8 In4 103.5(4) 8_544 . ? Co1 S9 In4 107.5(3) 8_544 . ? Co1 S9 In3 107.4(2) 8_544 . ? In4 S9 In3 107.2(2) . . ? In3 S10 In3 102.7(4) 11_454 . ? Co1 S11 Co1 108.48(15) 11_454 . ? Co1 S11 Co1 110.21(14) 11_454 8_544 ? Co1 S11 Co1 109.73(15) . 8_544 ? Co1 S11 Co1 109.73(15) 11_454 14_445 ? Co1 S11 Co1 110.21(14) . 14_445 ? Co1 S11 Co1 108.48(15) 8_544 14_445 ? In1 S1 S12 106.8(7) . . ? S1 S12 S1 93.4(10) . 2_455 ? S12' S1' S12' 14.5(8) . 2_455 ? S12' S1' In1 101.7(6) . . ? S12' S1' In1 99.3(6) 2_455 . ? S12' S12' S1' 98(3) 2_455 . ? S12' S12' S1' 68(3) 2_455 2_455 ? S1' S12' S1' 111.2(8) . 2_455 ? C1 N1 Co2 104(3) . . ? C6 N2 Co2 109(3) . . ? C7 N3 Co2 111(3) . . ? C12 N4 Co2 106(2) . . ? C18 N5 Co2 110(4) . . ? C13 N6 Co2 104(3) . . ? C6 C1 N1 122(5) . . ? C6 C1 C2 123(6) . . ? N1 C1 C2 111(5) . . ? C1 C2 C3 115(5) . . ? C4 C3 C2 111(5) . . ? C3 C4 C5 99.9(18) . . ? C6 C5 C4 111(2) . . ? C1 C6 N2 123(6) . . ? C1 C6 C5 116(5) . . ? N2 C6 C5 121(5) . . ? C12 C7 C8 114(4) . . ? C12 C7 N3 114(4) . . ? C8 C7 N3 120(4) . . ? C7 C8 C9 117(4) . . ? C8 C9 C10 113(4) . . ? C11 C10 C9 113(4) . . ? C10 C11 C12 114(4) . . ? C7 C12 C11 115(5) . . ? C7 C12 N4 115(4) . . ? C11 C12 N4 112(3) . . ? N6 C13 C14 113(5) . . ? N6 C13 C18 117(4) . . ? C14 C13 C18 112(5) . . ? C13 C14 C15 108(5) . . ? C16 C15 C14 117(6) . . ? C15 C16 C17 115(5) . . ? C18 C17 C16 112(6) . . ? N5 C18 C17 108(5) . . ? N5 C18 C13 109(5) . . ? C17 C18 C13 118(5) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 19.94 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 4.639 _refine_diff_density_min -1.734 _refine_diff_density_rms 0.184 # SQUEEZE RESULTS (APPEND TO CIF) 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 1 0.384 -0.003 0.001 8775.7 802.1 _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 923790' ####################################################################### # # 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_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C168 H408 Co17 In32 N56 O6 S68' _chemical_formula_weight 10165.64 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' In In -0.7276 1.3100 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.9417(10) _cell_length_b 26.2387(10) _cell_length_c 27.3488(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.4540(10) _cell_angle_gamma 90.00 _cell_volume 16239.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 60758 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.969 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9026 _exptl_absorpt_coefficient_mu 3.543 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2602 _exptl_absorpt_correction_T_max 0.7183 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86962 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 36866 _reflns_number_gt 25976 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+170.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 36866 _refine_ls_number_parameters 1335 _refine_ls_number_restraints 429 _refine_ls_R_factor_all 0.1141 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.2020 _refine_ls_wR_factor_gt 0.1798 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.035 _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 In1 In 0.55881(4) 0.37871(3) 0.79937(3) 0.0483(2) Uani 1 1 d . . . In2 In 0.41848(3) 0.31086(3) 0.82498(3) 0.03845(17) Uani 1 1 d . . . In3 In 0.42231(3) 0.37844(3) 0.69499(3) 0.03892(17) Uani 1 1 d . . . In4 In 0.42645(3) 0.46160(3) 0.81685(3) 0.03989(17) Uani 1 1 d . . . In5 In 0.27580(3) 0.24915(3) 0.84703(3) 0.03662(17) Uani 1 1 d . . . In6 In 0.28289(3) 0.38310(3) 0.59701(2) 0.03267(15) Uani 1 1 d . . . In7 In 0.29299(3) 0.54071(3) 0.83782(3) 0.03985(17) Uani 1 1 d . . . In8 In 0.13288(3) 0.18107(3) 0.87109(3) 0.03747(17) Uani 1 1 d . . . In9 In 0.13623(3) 0.24778(3) 0.74247(2) 0.03355(16) Uani 1 1 d . . . In10 In 0.13298(3) 0.33007(3) 0.86320(3) 0.03600(16) Uani 1 1 d . . . In11 In 0.13396(3) 0.31631(3) 0.61992(2) 0.03206(15) Uani 1 1 d . . . In12 In 0.14320(3) 0.47517(3) 0.86264(3) 0.03718(17) Uani 1 1 d . . . In13 In 0.14091(3) 0.38640(3) 0.49648(2) 0.03186(15) Uani 1 1 d . . . In14 In 0.14692(3) 0.46809(3) 0.61616(2) 0.03064(15) Uani 1 1 d . . . In15 In 0.15278(3) 0.54399(3) 0.73380(3) 0.03478(16) Uani 1 1 d . . . In16 In 0.16016(4) 0.61985(3) 0.85743(3) 0.04247(19) Uani 1 1 d . . . S1 S 0.66796(15) 0.37083(16) 0.81929(18) 0.0772(12) Uani 1 1 d . . . S2 S 0.52557(13) 0.30420(13) 0.83980(12) 0.0521(7) Uani 1 1 d . . . S3 S 0.53042(13) 0.37342(13) 0.70797(12) 0.0514(7) Uani 1 1 d . . . S4 S 0.53371(13) 0.46246(12) 0.82760(13) 0.0523(7) Uani 1 1 d . . . S5 S 0.38189(13) 0.23895(12) 0.86623(12) 0.0491(7) Uani 1 1 d . . . S6 S 0.37954(12) 0.30658(10) 0.73456(10) 0.0388(6) Uani 1 1 d . . . S7 S 0.38349(12) 0.39112(11) 0.85961(10) 0.0391(6) Uani 1 1 d . . . S8 S 0.39018(13) 0.37554(13) 0.60566(10) 0.0473(7) Uani 1 1 d . . . S9 S 0.38812(11) 0.46023(10) 0.72688(10) 0.0380(6) Uani 1 1 d . . . S10 S 0.40001(13) 0.54016(12) 0.85413(12) 0.0501(7) Uani 1 1 d . . . S11 S 0.24017(13) 0.17862(11) 0.89130(10) 0.0424(6) Uani 1 1 d . . . S12 S 0.24503(12) 0.24402(9) 0.75605(9) 0.0348(5) Uani 1 1 d . . . S13 S 0.24321(12) 0.32925(10) 0.88220(9) 0.0383(6) Uani 1 1 d . . . S14 S 0.24385(11) 0.31017(9) 0.63904(8) 0.0334(5) Uani 1 1 d . . . S15 S 0.24760(10) 0.39223(9) 0.75525(8) 0.0289(5) Uani 1 1 d . . . S16 S 0.25344(12) 0.46735(10) 0.87817(9) 0.0390(6) Uani 1 1 d . . . S17 S 0.24889(12) 0.37774(11) 0.50874(9) 0.0378(6) Uani 1 1 d . . . S18 S 0.25631(11) 0.46550(9) 0.63261(9) 0.0328(5) Uani 1 1 d . . . S19 S 0.26238(12) 0.53939(9) 0.74622(10) 0.0373(6) Uani 1 1 d . . . S20 S 0.26765(14) 0.62010(11) 0.87370(13) 0.0532(8) Uani 1 1 d . . . S22 S 0.10061(12) 0.17256(10) 0.78110(9) 0.0374(6) Uani 1 1 d . . . S23 S 0.09234(13) 0.25839(11) 0.90302(10) 0.0429(6) Uani 1 1 d . . . S24 S 0.09326(13) 0.24186(10) 0.65554(9) 0.0397(6) Uani 1 1 d . . . S25 S 0.09914(12) 0.32888(9) 0.77283(9) 0.0344(5) Uani 1 1 d . . . S26 S 0.09944(14) 0.40506(11) 0.90173(11) 0.0469(7) Uani 1 1 d . . . S27 S 0.10095(12) 0.31036(10) 0.53122(9) 0.0376(6) Uani 1 1 d . . . S28 S 0.10302(11) 0.39629(9) 0.65668(8) 0.0318(5) Uani 1 1 d . . . S29 S 0.11138(12) 0.46968(10) 0.77137(9) 0.0366(5) Uani 1 1 d . . . S30 S 0.11036(14) 0.55333(11) 0.89644(11) 0.0487(7) Uani 1 1 d . . . S31 S 0.09567(13) 0.39418(10) 0.40890(9) 0.0415(6) Uani 1 1 d . . . S32 S 0.11046(12) 0.46828(9) 0.52778(8) 0.0339(5) Uani 1 1 d . . . S33 S 0.11050(13) 0.54700(10) 0.64623(9) 0.0399(6) Uani 1 1 d . . . S34 S 0.12441(13) 0.62445(10) 0.76719(10) 0.0402(6) Uani 1 1 d . . . S35 S 0.1305(2) 0.70135(14) 0.89106(15) 0.0760(12) Uani 1 1 d . . . Co1 Co 0.27794(6) 0.31739(5) 0.72298(5) 0.0299(3) Uani 1 1 d . . . Co2 Co 0.28091(6) 0.39482(5) 0.83954(5) 0.0326(3) Uani 1 1 d . . . Co3 Co 0.28584(6) 0.45997(5) 0.71747(5) 0.0297(3) Uani 1 1 d . . . Co4 Co 0.14568(6) 0.39592(5) 0.73961(4) 0.0286(3) Uani 1 1 d . . . Co5 Co 0.0000 0.5000 0.5000 0.0353(4) Uani 1 2 d S . . Co6 Co -0.01058(7) 0.14875(6) 0.75718(5) 0.0418(3) Uani 1 1 d . . . Co7 Co 0.64297(10) 0.94257(8) 0.10503(8) 0.0703(5) Uani 1 1 d . . . Co8 Co 0.36867(13) 0.70542(10) 0.75718(10) 0.0967(8) Uani 1 1 d . . . Co9 Co 0.5805(3) 0.4980(3) 0.9823(3) 0.268(3) Uiso 1 1 d . . . N1 N 0.0253(5) 0.5233(4) 0.4342(3) 0.051(2) Uani 1 1 d U . . N2 N 0.0265(4) 0.5713(3) 0.5247(4) 0.046(2) Uani 1 1 d U . . N3 N -0.0349(6) 0.1857(6) 0.8196(5) 0.081(3) Uani 1 1 d U . . N4 N -0.0330(5) 0.2196(4) 0.7232(5) 0.072(3) Uani 1 1 d U . . N5 N 0.0140(5) 0.1070(4) 0.6972(4) 0.061(3) Uani 1 1 d U . . N6 N 0.0107(5) 0.0804(4) 0.7958(5) 0.066(3) Uani 1 1 d U . . N7 N 0.7284(6) 0.9575(5) 0.0860(5) 0.078(3) Uani 1 1 d U . . N8 N 0.6158(7) 0.9987(5) 0.0466(6) 0.093(4) Uani 1 1 d U . . N9 N 0.6234(5) 0.8803(4) 0.0534(4) 0.063(3) Uani 1 1 d . . . N10 N 0.5512(6) 0.9280(5) 0.1127(5) 0.085(4) Uani 1 1 d . . . N11 N 0.6796(6) 0.8959(5) 0.1683(5) 0.081(4) Uani 1 1 d . . . N12 N 0.6547(7) 0.9999(5) 0.1640(5) 0.082(4) Uani 1 1 d . . . N13 N 0.4071(11) 0.6312(9) 0.7572(9) 0.157(7) Uani 1 1 d U . . N14 N 0.4638(11) 0.7289(10) 0.7706(11) 0.193(8) Uani 1 1 d U . . N15 N 0.3591(9) 0.7204(7) 0.6784(6) 0.123(6) Uani 1 1 d U . . N16 N 0.2793(8) 0.6782(7) 0.7363(6) 0.112(5) Uani 1 1 d U . . N17 N 0.3409(12) 0.7833(8) 0.7708(8) 0.161(7) Uani 1 1 d U . . N18 N 0.3629(10) 0.7079(8) 0.8393(7) 0.131(6) Uani 1 1 d U . . N19 N 0.498(2) 0.407(2) 1.034(2) 0.39(3) Uiso 1 1 d . . . N20 N 0.4793(12) 0.4571(10) 0.9665(10) 0.182(10) Uiso 1 1 d . . . N21 N 0.5234(15) 0.3930(13) 0.9696(13) 0.243(14) Uiso 1 1 d . . . N22 N 0.646(3) 0.467(2) 0.932(2) 0.42(3) Uiso 1 1 d . . . N23 N 0.1976(8) 0.1834(7) 0.5619(7) 0.125(6) Uani 1 1 d . . . N24 N 0.2180(5) 0.2540(4) 0.4885(4) 0.058(3) Uani 1 1 d . . . N25 N 0.0868(9) 0.1781(7) 0.5006(6) 0.125(6) Uani 1 1 d . . . N26 N 0.0930(12) 0.1231(9) 0.5918(9) 0.158(8) Uani 1 1 d . . . C1 C 0.0497(9) 0.5987(6) 0.4857(7) 0.090(4) Uani 1 1 d U . . C2 C 0.0649(8) 0.6540(6) 0.4956(7) 0.086(4) Uani 1 1 d U . . C3 C 0.0887(11) 0.6796(7) 0.4522(9) 0.119(5) Uani 1 1 d U . . C4 C 0.0821(11) 0.6583(8) 0.4070(8) 0.122(6) Uani 1 1 d U . . C5 C 0.0652(9) 0.6009(6) 0.3963(6) 0.089(4) Uani 1 1 d U . . C6 C 0.0427(9) 0.5775(6) 0.4411(6) 0.092(4) Uani 1 1 d U . . C7 C -0.0505(12) 0.2404(9) 0.8030(9) 0.135(5) Uani 1 1 d U . . C8 C -0.0788(13) 0.2688(10) 0.8442(10) 0.158(7) Uani 1 1 d U . . C9 C -0.0937(16) 0.3215(12) 0.8242(13) 0.186(8) Uani 1 1 d U . . C10 C -0.1148(16) 0.3311(11) 0.7766(13) 0.181(8) Uani 1 1 d U . . C11 C -0.0816(13) 0.3028(8) 0.7425(11) 0.151(7) Uani 1 1 d U . . C12 C -0.0584(12) 0.2522(8) 0.7549(10) 0.130(5) Uani 1 1 d U . . C13 C 0.0209(8) 0.0514(6) 0.7147(6) 0.077(4) Uani 1 1 d U . . C14 C 0.0555(9) 0.0179(7) 0.6823(8) 0.101(5) Uani 1 1 d U . . C15 C 0.0620(11) -0.0344(8) 0.7002(10) 0.126(6) Uani 1 1 d U . . C16 C 0.0870(13) -0.0375(8) 0.7533(11) 0.138(6) Uani 1 1 d U . . C17 C 0.0498(10) -0.0066(7) 0.7885(8) 0.112(5) Uani 1 1 d U . . C18 C 0.0409(9) 0.0494(7) 0.7681(7) 0.089(4) Uani 1 1 d U . . C19 C 0.7238(10) 1.0048(8) 0.0544(9) 0.113(5) Uani 1 1 d U . . C20 C 0.7779(10) 1.0218(8) 0.0377(9) 0.119(6) Uani 1 1 d U . . C21 C 0.7681(12) 1.0737(10) 0.0065(11) 0.150(7) Uani 1 1 d U . . C22 C 0.7108(13) 1.0781(12) -0.0227(12) 0.168(7) Uani 1 1 d U . . C23 C 0.6597(11) 1.0623(10) -0.0048(10) 0.142(6) Uani 1 1 d U . . C24 C 0.6675(10) 1.0086(9) 0.0215(9) 0.122(5) Uani 1 1 d U . . C25 C 0.5588(7) 0.8727(6) 0.0398(6) 0.070(4) Uani 1 1 d . . . C26 C 0.5407(7) 0.8249(6) 0.0129(6) 0.076(4) Uani 1 1 d . . . C27 C 0.4711(8) 0.8183(9) 0.0031(8) 0.111(7) Uani 1 1 d . . . C28 C 0.4486(9) 0.8194(8) 0.0541(10) 0.116(8) Uani 1 1 d . . . C29 C 0.4663(8) 0.8704(8) 0.0832(10) 0.117(8) Uani 1 1 d . . . C30 C 0.5351(7) 0.8775(7) 0.0910(7) 0.081(5) Uani 1 1 d . . . C31 C 0.6900(10) 0.9264(7) 0.2140(6) 0.105(7) Uani 1 1 d . . . C32 C 0.7401(10) 0.9017(7) 0.2538(7) 0.106(7) Uani 1 1 d . . . C33 C 0.7480(14) 0.9370(10) 0.3011(9) 0.158(11) Uani 1 1 d . . . C34 C 0.7564(15) 0.9905(12) 0.2894(12) 0.183(14) Uani 1 1 d . . . C35 C 0.7060(12) 1.0141(8) 0.2485(8) 0.119(8) Uani 1 1 d . . . C36 C 0.6983(11) 0.9803(7) 0.2024(7) 0.112(7) Uani 1 1 d . . . C37 C 0.4723(18) 0.6405(15) 0.7795(14) 0.192(8) Uiso 1 1 d U . . C38 C 0.513(2) 0.5953(18) 0.7616(17) 0.247(14) Uiso 1 1 d U . . C39 C 0.575(2) 0.6085(17) 0.8145(17) 0.240(12) Uiso 1 1 d U . . C40 C 0.5978(17) 0.6553(15) 0.7854(16) 0.240(9) Uani 1 1 d U . . C41 C 0.5595(17) 0.6731(14) 0.7441(16) 0.237(8) Uani 1 1 d U . . C42 C 0.4948(15) 0.6861(13) 0.7546(14) 0.201(7) Uani 1 1 d U . . C43 C 0.3040(11) 0.7143(9) 0.6569(8) 0.123(5) Uani 1 1 d U . . C44 C 0.2880(11) 0.7166(10) 0.5987(8) 0.130(6) Uani 1 1 d U . . C45 C 0.2237(13) 0.7129(12) 0.5773(9) 0.151(7) Uani 1 1 d U . . C46 C 0.1945(13) 0.6684(12) 0.6021(10) 0.165(7) Uani 1 1 d U . . C47 C 0.2059(12) 0.6730(11) 0.6590(10) 0.150(7) Uani 1 1 d U . . C48 C 0.2680(11) 0.6741(10) 0.6794(8) 0.129(5) Uani 1 1 d U . . C49 C 0.3216(15) 0.7919(13) 0.8180(12) 0.166(6) Uani 1 1 d U . . C50 C 0.2939(15) 0.8403(14) 0.8281(13) 0.177(8) Uiso 1 1 d U . . C51 C 0.2668(17) 0.8395(14) 0.8683(15) 0.213(8) Uani 1 1 d U . . C52 C 0.2896(17) 0.8093(14) 0.9113(14) 0.201(8) Uani 1 1 d U . . C53 C 0.3224(15) 0.7573(12) 0.9032(12) 0.171(7) Uani 1 1 d U . . C54 C 0.3262(15) 0.7544(14) 0.8458(13) 0.169(7) Uiso 1 1 d U . . C55 C 0.2534(13) 0.1843(10) 0.5437(10) 0.145(10) Uani 1 1 d . . . C56 C 0.3051(14) 0.1699(15) 0.5876(14) 0.208(18) Uani 1 1 d . . . C57 C 0.3606(19) 0.1710(16) 0.568(2) 0.27(3) Uani 1 1 d . . . C58 C 0.3775(12) 0.2264(15) 0.5484(14) 0.207(16) Uani 1 1 d . . . C59 C 0.3261(8) 0.2406(8) 0.5066(8) 0.097(6) Uani 1 1 d . . . C60 C 0.2664(10) 0.2342(9) 0.5265(7) 0.107(7) Uani 1 1 d . . . C61 C 0.0300(14) 0.1806(10) 0.5277(9) 0.136(9) Uani 1 1 d . . . C62 C -0.0301(12) 0.1905(12) 0.4923(9) 0.138(9) Uani 1 1 d . . . C63 C -0.0430(15) 0.1391(14) 0.4576(9) 0.175(13) Uani 1 1 d . . . C64 C -0.0389(14) 0.0890(12) 0.4875(10) 0.151(11) Uani 1 1 d . . . C65 C 0.0219(16) 0.0833(12) 0.5208(10) 0.164(12) Uani 1 1 d . . . C66 C 0.0288(14) 0.1304(9) 0.5587(9) 0.134(9) Uani 1 1 d . . . O1 O 0.5067(11) 0.2242(10) 0.1278(8) 0.237(13) Uani 1 1 d . . . O2 O 0.5376(6) 0.4986(5) 0.7086(5) 0.109(4) Uani 1 1 d . . . O3 O 0.5599(9) 0.4176(8) 0.6011(6) 0.164(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.0321(4) 0.0564(5) 0.0543(5) -0.0001(4) 0.0010(3) 0.0028(4) In2 0.0327(4) 0.0419(4) 0.0394(4) 0.0053(3) 0.0018(3) 0.0040(3) In3 0.0314(4) 0.0484(4) 0.0370(4) 0.0030(3) 0.0060(3) 0.0018(3) In4 0.0338(4) 0.0431(4) 0.0408(4) -0.0033(3) 0.0002(3) 0.0003(3) In5 0.0399(4) 0.0378(4) 0.0317(3) 0.0080(3) 0.0045(3) -0.0004(3) In6 0.0347(4) 0.0380(4) 0.0254(3) 0.0005(3) 0.0053(3) 0.0016(3) In7 0.0406(4) 0.0360(4) 0.0415(4) -0.0083(3) 0.0025(3) -0.0006(3) In8 0.0451(4) 0.0379(4) 0.0293(3) 0.0074(3) 0.0057(3) -0.0069(3) In9 0.0420(4) 0.0328(3) 0.0257(3) 0.0033(3) 0.0052(3) -0.0065(3) In10 0.0449(4) 0.0358(4) 0.0284(3) 0.0022(3) 0.0095(3) -0.0022(3) In11 0.0396(4) 0.0321(3) 0.0239(3) 0.0014(3) 0.0036(3) -0.0015(3) In12 0.0446(4) 0.0353(4) 0.0321(4) -0.0030(3) 0.0077(3) 0.0035(3) In13 0.0399(4) 0.0328(3) 0.0223(3) -0.0006(3) 0.0033(3) 0.0057(3) In14 0.0367(4) 0.0309(3) 0.0237(3) -0.0004(3) 0.0031(3) 0.0038(3) In15 0.0421(4) 0.0313(3) 0.0300(3) -0.0044(3) 0.0029(3) 0.0063(3) In16 0.0493(5) 0.0376(4) 0.0396(4) -0.0107(3) 0.0043(3) 0.0066(3) S1 0.0344(17) 0.080(3) 0.113(3) -0.015(2) -0.0019(19) 0.0022(17) S2 0.0342(15) 0.0613(19) 0.0594(18) 0.0123(15) 0.0040(13) 0.0084(13) S3 0.0317(14) 0.073(2) 0.0500(16) 0.0017(15) 0.0084(12) 0.0040(14) S4 0.0352(15) 0.0554(17) 0.0630(19) -0.0055(15) -0.0019(13) -0.0033(13) S5 0.0397(15) 0.0518(16) 0.0543(17) 0.0198(14) 0.0032(13) 0.0066(13) S6 0.0332(13) 0.0440(14) 0.0384(13) 0.0030(12) 0.0033(10) 0.0033(11) S7 0.0351(14) 0.0450(14) 0.0358(13) -0.0016(11) 0.0021(10) 0.0013(11) S8 0.0364(15) 0.072(2) 0.0350(13) 0.0044(14) 0.0110(11) 0.0048(13) S9 0.0323(13) 0.0431(14) 0.0383(13) 0.0020(11) 0.0048(10) -0.0002(11) S10 0.0410(16) 0.0462(16) 0.0597(18) -0.0137(14) -0.0013(13) -0.0046(12) S11 0.0488(16) 0.0425(14) 0.0359(13) 0.0140(12) 0.0073(11) -0.0005(12) S12 0.0433(14) 0.0313(12) 0.0297(12) 0.0049(10) 0.0060(10) -0.0005(10) S13 0.0442(15) 0.0404(13) 0.0294(12) 0.0043(11) 0.0035(10) 0.0003(11) S14 0.0387(13) 0.0357(12) 0.0252(11) -0.0005(10) 0.0038(9) -0.0007(10) S15 0.0311(12) 0.0303(11) 0.0244(10) -0.0012(9) 0.0026(9) -0.0009(9) S16 0.0438(15) 0.0396(13) 0.0328(12) -0.0052(11) 0.0041(11) 0.0022(11) S17 0.0403(14) 0.0488(15) 0.0249(11) -0.0005(11) 0.0068(10) 0.0027(11) S18 0.0358(13) 0.0348(12) 0.0280(11) 0.0012(10) 0.0054(10) 0.0005(10) S19 0.0432(15) 0.0296(12) 0.0385(13) -0.0040(11) 0.0049(11) 0.0012(10) S20 0.0491(17) 0.0437(15) 0.0644(19) -0.0231(15) 0.0023(14) -0.0009(13) S22 0.0456(15) 0.0362(13) 0.0295(12) 0.0041(10) 0.0040(10) -0.0111(11) S23 0.0526(17) 0.0410(14) 0.0385(14) 0.0063(12) 0.0175(12) -0.0055(12) S24 0.0515(16) 0.0393(13) 0.0267(11) 0.0023(11) 0.0015(11) -0.0131(12) S25 0.0397(14) 0.0354(12) 0.0284(11) 0.0010(10) 0.0064(10) -0.0067(10) S26 0.0605(19) 0.0420(14) 0.0434(15) -0.0012(13) 0.0242(13) 0.0018(13) S27 0.0490(16) 0.0369(13) 0.0252(11) 0.0005(10) 0.0012(10) -0.0044(11) S28 0.0369(13) 0.0335(12) 0.0241(11) 0.0018(9) 0.0022(9) 0.0006(10) S29 0.0431(14) 0.0337(12) 0.0322(12) -0.0014(10) 0.0043(10) 0.0056(11) S30 0.0577(19) 0.0447(15) 0.0465(16) -0.0055(13) 0.0164(14) 0.0089(13) S31 0.0587(17) 0.0419(14) 0.0218(11) -0.0063(10) -0.0001(11) 0.0182(12) S32 0.0467(15) 0.0325(12) 0.0216(10) -0.0004(9) 0.0028(10) 0.0086(10) S33 0.0546(17) 0.0334(13) 0.0294(12) -0.0028(10) 0.0006(11) 0.0125(11) S34 0.0469(16) 0.0351(13) 0.0375(13) -0.0066(11) 0.0039(11) 0.0091(11) S35 0.100(3) 0.056(2) 0.068(2) -0.0265(18) 0.003(2) 0.029(2) Co1 0.0330(7) 0.0310(6) 0.0256(6) 0.0019(5) 0.0045(5) -0.0005(5) Co2 0.0345(7) 0.0345(7) 0.0277(6) -0.0009(6) 0.0020(5) -0.0003(5) Co3 0.0316(7) 0.0306(6) 0.0264(6) 0.0000(5) 0.0032(5) 0.0007(5) Co4 0.0334(7) 0.0287(6) 0.0235(6) -0.0002(5) 0.0038(5) 0.0002(5) Co5 0.0455(12) 0.0304(9) 0.0299(9) 0.0038(8) 0.0061(8) 0.0008(8) Co6 0.0514(9) 0.0378(7) 0.0362(7) 0.0034(6) 0.0070(6) -0.0046(7) Co7 0.0775(14) 0.0644(12) 0.0730(13) -0.0060(10) 0.0244(11) 0.0103(10) Co8 0.104(2) 0.0909(17) 0.0977(18) 0.0280(15) 0.0231(15) -0.0212(15) N1 0.061(6) 0.054(5) 0.038(5) 0.011(4) 0.008(4) -0.003(5) N2 0.050(6) 0.033(4) 0.054(5) 0.001(4) 0.008(4) 0.005(4) N3 0.079(8) 0.104(9) 0.064(7) -0.030(7) 0.018(6) -0.004(7) N4 0.065(7) 0.047(6) 0.103(9) 0.021(6) 0.009(6) 0.000(5) N5 0.057(6) 0.068(6) 0.056(6) -0.008(5) 0.005(5) 0.001(5) N6 0.061(7) 0.057(6) 0.079(7) 0.025(6) 0.003(6) -0.009(5) N7 0.072(8) 0.073(8) 0.092(9) 0.010(7) 0.022(7) 0.003(6) N8 0.099(9) 0.079(8) 0.107(10) 0.018(8) 0.035(8) 0.013(8) N9 0.045(6) 0.074(8) 0.071(7) -0.013(6) 0.015(5) 0.002(5) N10 0.074(9) 0.083(9) 0.104(11) -0.011(8) 0.033(8) 0.014(7) N11 0.095(10) 0.082(9) 0.071(8) -0.012(7) 0.026(7) 0.016(8) N12 0.117(12) 0.068(8) 0.060(7) -0.010(7) 0.013(7) 0.019(8) N13 0.154(14) 0.142(13) 0.177(15) 0.003(13) 0.029(13) -0.004(11) N14 0.156(16) 0.182(16) 0.254(19) 0.128(15) 0.068(14) 0.009(12) N15 0.133(12) 0.147(13) 0.086(9) 0.015(10) 0.006(9) -0.072(11) N16 0.113(11) 0.126(12) 0.097(9) 0.031(10) 0.013(8) -0.023(10) N17 0.253(18) 0.110(12) 0.136(13) 0.001(11) 0.081(13) -0.042(13) N18 0.164(14) 0.130(11) 0.106(11) 0.018(10) 0.039(10) -0.008(11) N23 0.109(14) 0.138(15) 0.132(15) 0.061(13) 0.028(12) 0.022(12) N24 0.060(7) 0.055(6) 0.057(6) 0.008(5) 0.001(5) 0.013(5) N25 0.174(19) 0.113(13) 0.098(12) 0.010(11) 0.055(12) -0.004(13) N26 0.18(2) 0.144(19) 0.149(19) 0.015(16) 0.032(17) 0.017(17) C1 0.138(10) 0.059(7) 0.080(7) -0.001(6) 0.038(8) -0.030(7) C2 0.113(11) 0.048(7) 0.096(9) 0.010(7) 0.016(8) -0.022(7) C3 0.168(13) 0.078(9) 0.115(11) 0.014(8) 0.031(11) -0.044(10) C4 0.183(13) 0.084(9) 0.101(10) 0.019(9) 0.035(11) -0.066(10) C5 0.132(11) 0.077(8) 0.061(7) 0.025(7) 0.025(8) -0.034(8) C6 0.142(10) 0.072(7) 0.067(7) 0.010(6) 0.028(8) -0.045(8) C7 0.165(12) 0.113(10) 0.120(10) -0.042(9) 0.001(10) 0.063(10) C8 0.188(15) 0.134(12) 0.143(12) -0.065(11) 0.001(12) 0.069(12) C9 0.232(17) 0.141(13) 0.176(15) -0.049(14) 0.004(15) 0.084(13) C10 0.233(17) 0.117(12) 0.187(16) -0.032(13) 0.016(15) 0.073(12) C11 0.193(15) 0.079(10) 0.180(14) -0.007(10) 0.022(13) 0.057(11) C12 0.164(12) 0.082(9) 0.141(10) -0.005(9) 0.013(11) 0.047(9) C13 0.101(9) 0.056(7) 0.075(7) 0.002(6) 0.017(7) 0.015(7) C14 0.110(11) 0.074(8) 0.117(10) -0.015(8) 0.017(9) 0.017(8) C15 0.146(13) 0.081(9) 0.146(12) -0.007(11) 0.006(12) 0.038(10) C16 0.172(15) 0.084(10) 0.156(13) 0.010(11) 0.018(12) 0.029(10) C17 0.141(13) 0.065(8) 0.131(11) 0.034(8) 0.027(10) 0.008(9) C18 0.110(10) 0.073(8) 0.088(8) 0.017(7) 0.022(8) -0.004(7) C19 0.099(9) 0.100(9) 0.139(11) 0.042(9) 0.014(8) -0.010(8) C20 0.097(10) 0.107(11) 0.156(13) 0.048(10) 0.027(10) -0.013(9) C21 0.121(12) 0.134(13) 0.193(15) 0.080(12) 0.017(12) -0.014(12) C22 0.130(13) 0.175(14) 0.197(16) 0.099(12) 0.021(12) -0.004(12) C23 0.115(12) 0.148(13) 0.163(14) 0.089(11) 0.023(11) 0.003(11) C24 0.100(9) 0.125(10) 0.138(11) 0.061(9) 0.015(8) -0.005(9) C25 0.061(9) 0.072(9) 0.077(10) 0.009(8) 0.014(7) 0.000(7) C26 0.068(10) 0.076(10) 0.079(10) -0.001(9) 0.001(8) 0.003(8) C27 0.056(11) 0.150(19) 0.119(16) 0.027(14) -0.010(10) 0.000(11) C28 0.073(13) 0.105(15) 0.18(2) -0.009(16) 0.055(14) -0.005(11) C29 0.067(12) 0.107(15) 0.19(2) 0.001(16) 0.047(14) 0.017(11) C30 0.062(10) 0.090(12) 0.101(12) -0.012(10) 0.041(9) 0.007(8) C31 0.17(2) 0.069(11) 0.064(10) -0.012(9) -0.021(11) 0.034(12) C32 0.142(19) 0.081(12) 0.083(12) -0.001(10) -0.015(12) 0.004(12) C33 0.22(3) 0.116(19) 0.106(18) 0.003(16) -0.051(18) -0.02(2) C34 0.21(3) 0.13(2) 0.18(3) -0.01(2) -0.07(2) -0.03(2) C35 0.18(2) 0.091(14) 0.084(13) -0.039(12) 0.006(14) 0.001(14) C36 0.19(2) 0.059(10) 0.081(12) -0.014(10) 0.008(14) 0.017(12) C40 0.223(14) 0.239(15) 0.297(16) 0.186(13) 0.160(13) 0.119(13) C41 0.210(15) 0.217(16) 0.309(17) 0.166(14) 0.118(14) 0.068(13) C42 0.181(12) 0.184(13) 0.269(14) 0.166(12) 0.125(11) 0.055(10) C43 0.125(11) 0.141(11) 0.096(9) 0.034(10) 0.002(9) -0.049(10) C44 0.141(13) 0.153(14) 0.092(9) -0.004(11) 0.005(10) -0.044(12) C45 0.145(14) 0.184(15) 0.114(12) 0.020(12) -0.006(11) -0.038(13) C46 0.156(14) 0.209(16) 0.118(12) 0.026(13) -0.012(11) -0.063(13) C47 0.134(12) 0.190(15) 0.119(11) 0.014(13) -0.002(11) -0.065(12) C48 0.122(11) 0.155(12) 0.104(9) 0.029(10) 0.003(9) -0.053(10) C49 0.208(12) 0.149(11) 0.153(11) 0.015(10) 0.062(10) 0.007(10) C51 0.235(15) 0.209(14) 0.219(15) 0.086(12) 0.104(13) 0.116(13) C52 0.235(17) 0.186(16) 0.196(16) 0.044(14) 0.080(15) 0.075(14) C53 0.198(15) 0.160(14) 0.165(13) 0.020(11) 0.060(12) 0.035(12) C55 0.15(2) 0.13(2) 0.16(2) 0.087(18) 0.043(19) 0.037(17) C56 0.11(2) 0.27(4) 0.23(4) 0.13(3) 0.00(2) 0.09(3) C57 0.19(4) 0.20(4) 0.39(7) 0.19(4) 0.01(4) 0.02(3) C58 0.085(18) 0.26(4) 0.26(4) 0.10(3) -0.02(2) 0.01(2) C59 0.057(10) 0.110(14) 0.123(16) 0.012(12) 0.008(10) 0.020(10) C60 0.119(17) 0.118(16) 0.080(12) 0.027(12) 0.002(11) 0.024(13) C61 0.20(3) 0.13(2) 0.101(16) -0.001(15) 0.076(19) -0.015(19) C62 0.12(2) 0.20(3) 0.094(16) -0.009(18) 0.034(15) -0.021(19) C63 0.23(4) 0.21(3) 0.091(16) -0.05(2) 0.06(2) -0.08(3) C64 0.18(3) 0.17(3) 0.109(18) 0.002(19) 0.043(18) -0.07(2) C65 0.21(3) 0.17(3) 0.104(18) -0.017(19) 0.01(2) -0.04(2) C66 0.20(3) 0.113(17) 0.089(15) -0.006(14) 0.021(16) -0.062(18) O1 0.24(3) 0.27(3) 0.173(19) 0.088(19) -0.059(17) -0.10(2) O2 0.093(9) 0.116(10) 0.123(11) 0.030(9) 0.035(8) -0.025(8) O3 0.198(18) 0.208(18) 0.095(10) 0.007(12) 0.051(11) -0.077(15) _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 In1 S4 2.430(3) . ? In1 S2 2.430(3) . ? In1 S3 2.481(3) . ? In1 S1 2.482(4) . ? In2 S5 2.419(3) . ? In2 S2 2.430(3) . ? In2 S6 2.490(3) . ? In2 S7 2.495(3) . ? In3 S8 2.434(3) . ? In3 S3 2.451(3) . ? In3 S6 2.457(3) . ? In3 S9 2.491(3) . ? In4 S10 2.421(3) . ? In4 S4 2.430(3) . ? In4 S9 2.473(3) . ? In4 S7 2.478(3) . ? In5 S5 2.419(3) . ? In5 S11 2.425(3) . ? In5 S12 2.476(3) . ? In5 S13 2.478(3) . ? In6 S17 2.416(2) . ? In6 S8 2.442(3) . ? In6 S14 2.475(3) . ? In6 S18 2.488(3) . ? In7 S20 2.414(3) . ? In7 S10 2.422(3) . ? In7 S16 2.465(3) . ? In7 S19 2.488(3) . ? In8 S11 2.433(3) . ? In8 S31 2.447(3) 4_566 ? In8 S23 2.452(3) . ? In8 S22 2.461(3) . ? In9 S24 2.424(3) . ? In9 S22 2.442(2) . ? In9 S12 2.464(3) . ? In9 S25 2.485(3) . ? In10 S26 2.417(3) . ? In10 S23 2.434(3) . ? In10 S25 2.466(2) . ? In10 S13 2.497(3) . ? In11 S27 2.425(2) . ? In11 S24 2.436(3) . ? In11 S28 2.481(3) . ? In11 S14 2.494(3) . ? In12 S30 2.420(3) . ? In12 S26 2.426(3) . ? In12 S29 2.487(3) . ? In12 S16 2.503(3) . ? In13 S27 2.452(3) . ? In13 S17 2.455(3) . ? In13 S32 2.456(2) . ? In13 S31 2.457(2) . ? In14 S32 2.424(2) . ? In14 S33 2.427(3) . ? In14 S18 2.477(3) . ? In14 S28 2.481(2) . ? In15 S34 2.431(3) . ? In15 S33 2.433(3) . ? In15 S29 2.466(3) . ? In15 S19 2.484(3) . ? In16 S30 2.427(3) . ? In16 S20 2.433(3) . ? In16 S35 2.467(3) . ? In16 S34 2.473(3) . ? S6 Co1 2.318(3) . ? S7 Co2 2.329(3) . ? S9 Co3 2.318(3) . ? S12 Co1 2.306(3) . ? S13 Co2 2.324(3) . ? S14 Co1 2.308(3) . ? S15 Co3 2.301(3) . ? S15 Co1 2.307(3) . ? S15 Co2 2.307(3) . ? S15 Co4 2.309(3) . ? S16 Co2 2.314(3) . ? S18 Co3 2.313(3) . ? S19 Co3 2.321(3) . ? S22 Co6 2.603(3) . ? S25 Co4 2.319(3) . ? S28 Co4 2.318(3) . ? S29 Co4 2.312(3) . ? S31 In8 2.447(3) 4_565 ? S32 Co5 2.657(3) . ? S34 Co6 2.664(3) 2_556 ? Co5 N2 2.048(9) 3_566 ? Co5 N2 2.048(9) . ? Co5 N1 2.072(9) . ? Co5 N1 2.072(9) 3_566 ? Co5 S32 2.657(3) 3_566 ? Co6 N6 2.098(11) . ? Co6 N4 2.104(11) . ? Co6 N3 2.117(12) . ? Co6 N5 2.123(11) . ? Co6 S34 2.664(3) 2_546 ? Co7 N7 2.143(13) . ? Co7 N9 2.158(11) . ? Co7 N11 2.173(14) . ? Co7 N10 2.183(14) . ? Co7 N8 2.187(14) . ? Co7 N12 2.189(12) . ? Co8 N13 2.14(2) . ? Co8 N16 2.157(17) . ? Co8 N15 2.165(16) . ? Co8 N17 2.19(2) . ? Co8 N14 2.24(3) . ? Co8 N18 2.273(18) . ? Co9 N22 2.35(6) . ? Co9 N20 2.42(3) 3_667 ? N1 C6 1.481(18) . ? N2 C1 1.456(18) . ? N3 C7 1.53(3) . ? N4 C12 1.41(2) . ? N5 C13 1.535(18) . ? N6 C18 1.37(2) . ? N7 C19 1.51(2) . ? N8 C24 1.49(2) . ? N9 C25 1.481(18) . ? N10 C30 1.47(2) . ? N11 C31 1.47(2) . ? N12 C36 1.42(2) . ? N13 C37 1.54(4) . ? N14 C42 1.44(4) . ? N15 C43 1.31(3) . ? N16 C48 1.54(3) . ? N17 C49 1.45(3) . ? N18 C54 1.51(4) . ? N20 Co9 2.42(3) 3_667 ? N23 C55 1.45(3) . ? N24 C60 1.49(2) . ? N25 C61 1.60(3) . ? N26 C66 1.61(3) . ? C1 C6 1.33(2) . ? C1 C2 1.50(2) . ? C2 C3 1.54(2) . ? C3 C4 1.34(3) . ? C4 C5 1.57(2) . ? C5 C6 1.534(19) . ? C7 C12 1.33(3) . ? C7 C8 1.58(3) . ? C8 C9 1.50(4) . ? C9 C10 1.33(4) . ? C10 C11 1.49(4) . ? C11 C12 1.45(3) . ? C13 C18 1.46(2) . ? C13 C14 1.56(2) . ? C14 C15 1.46(3) . ? C15 C16 1.47(3) . ? C16 C17 1.61(3) . ? C17 C18 1.57(2) . ? C19 C24 1.45(3) . ? C19 C20 1.46(3) . ? C20 C21 1.60(3) . ? C21 C22 1.43(3) . ? C22 C23 1.41(3) . ? C23 C24 1.58(3) . ? C25 C26 1.48(2) . ? C25 C30 1.59(2) . ? C26 C27 1.58(2) . ? C27 C28 1.57(3) . ? C28 C29 1.58(3) . ? C29 C30 1.57(2) . ? C31 C36 1.47(3) . ? C31 C32 1.59(2) . ? C32 C33 1.58(3) . ? C33 C34 1.46(3) . ? C34 C35 1.60(3) . ? C35 C36 1.53(2) . ? C37 C42 1.51(4) . ? C37 C38 1.63(5) . ? C38 C39 1.89(6) . ? C39 C40 1.60(5) . ? C40 C41 1.39(5) . ? C41 C42 1.60(4) . ? C43 C48 1.53(3) . ? C43 C44 1.58(3) . ? C44 C45 1.50(3) . ? C45 C46 1.56(3) . ? C46 C47 1.54(3) . ? C47 C48 1.44(3) . ? C49 C54 1.24(4) . ? C49 C50 1.47(4) . ? C50 C51 1.35(4) . ? C51 C52 1.44(4) . ? C52 C53 1.59(4) . ? C53 C54 1.59(4) . ? C55 C60 1.44(3) . ? C55 C56 1.59(4) . ? C56 C57 1.46(5) . ? C57 C58 1.62(4) . ? C58 C59 1.55(3) . ? C59 C60 1.56(3) . ? C61 C66 1.57(3) . ? C61 C62 1.57(4) . ? C62 C63 1.65(4) . ? C63 C64 1.54(4) . ? C64 C65 1.54(4) . ? C65 C66 1.60(3) . ? 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 S4 In1 S2 118.34(12) . . ? S4 In1 S3 109.51(12) . . ? S2 In1 S3 111.31(12) . . ? S4 In1 S1 106.79(12) . . ? S2 In1 S1 102.35(13) . . ? S3 In1 S1 107.75(13) . . ? S5 In2 S2 106.56(11) . . ? S5 In2 S6 109.43(10) . . ? S2 In2 S6 110.52(10) . . ? S5 In2 S7 108.86(10) . . ? S2 In2 S7 112.15(11) . . ? S6 In2 S7 109.25(9) . . ? S8 In3 S3 106.03(10) . . ? S8 In3 S6 109.94(10) . . ? S3 In3 S6 111.28(10) . . ? S8 In3 S9 108.50(10) . . ? S3 In3 S9 111.40(11) . . ? S6 In3 S9 109.59(9) . . ? S10 In4 S4 105.07(11) . . ? S10 In4 S9 111.02(10) . . ? S4 In4 S9 107.94(10) . . ? S10 In4 S7 106.87(10) . . ? S4 In4 S7 115.04(11) . . ? S9 In4 S7 110.77(9) . . ? S5 In5 S11 102.52(10) . . ? S5 In5 S12 108.83(10) . . ? S11 In5 S12 113.35(9) . . ? S5 In5 S13 111.50(11) . . ? S11 In5 S13 107.79(10) . . ? S12 In5 S13 112.45(9) . . ? S17 In6 S8 104.30(9) . . ? S17 In6 S14 109.69(9) . . ? S8 In6 S14 109.16(10) . . ? S17 In6 S18 112.45(9) . . ? S8 In6 S18 109.92(10) . . ? S14 In6 S18 111.08(8) . . ? S20 In7 S10 103.58(11) . . ? S20 In7 S16 111.16(11) . . ? S10 In7 S16 110.45(11) . . ? S20 In7 S19 111.98(11) . . ? S10 In7 S19 107.17(10) . . ? S16 In7 S19 112.09(9) . . ? S11 In8 S31 107.03(10) . 4_566 ? S11 In8 S23 111.70(10) . . ? S31 In8 S23 109.76(10) 4_566 . ? S11 In8 S22 110.59(10) . . ? S31 In8 S22 106.32(9) 4_566 . ? S23 In8 S22 111.22(10) . . ? S24 In9 S22 105.16(9) . . ? S24 In9 S12 112.57(9) . . ? S22 In9 S12 107.76(9) . . ? S24 In9 S25 106.03(9) . . ? S22 In9 S25 112.97(9) . . ? S12 In9 S25 112.21(9) . . ? S26 In10 S23 105.14(10) . . ? S26 In10 S25 112.14(10) . . ? S23 In10 S25 110.98(9) . . ? S26 In10 S13 107.48(10) . . ? S23 In10 S13 110.45(10) . . ? S25 In10 S13 110.48(9) . . ? S27 In11 S24 105.73(9) . . ? S27 In11 S28 113.38(9) . . ? S24 In11 S28 111.24(9) . . ? S27 In11 S14 110.14(9) . . ? S24 In11 S14 107.76(9) . . ? S28 In11 S14 108.44(8) . . ? S30 In12 S26 107.27(10) . . ? S30 In12 S29 111.96(10) . . ? S26 In12 S29 108.89(10) . . ? S30 In12 S16 111.96(10) . . ? S26 In12 S16 110.04(10) . . ? S29 In12 S16 106.70(9) . . ? S27 In13 S17 107.75(9) . . ? S27 In13 S32 115.53(9) . . ? S17 In13 S32 111.82(9) . . ? S27 In13 S31 108.68(10) . . ? S17 In13 S31 113.32(9) . . ? S32 In13 S31 99.69(8) . . ? S32 In14 S33 104.74(8) . . ? S32 In14 S18 110.76(9) . . ? S33 In14 S18 110.91(9) . . ? S32 In14 S28 110.35(9) . . ? S33 In14 S28 107.99(9) . . ? S18 In14 S28 111.82(8) . . ? S34 In15 S33 104.69(9) . . ? S34 In15 S29 112.64(9) . . ? S33 In15 S29 108.50(10) . . ? S34 In15 S19 108.56(9) . . ? S33 In15 S19 111.54(10) . . ? S29 In15 S19 110.80(9) . . ? S30 In16 S20 117.24(12) . . ? S30 In16 S35 106.31(13) . . ? S20 In16 S35 105.24(13) . . ? S30 In16 S34 111.77(11) . . ? S20 In16 S34 110.03(11) . . ? S35 In16 S34 105.26(11) . . ? In2 S2 In1 104.51(11) . . ? In3 S3 In1 103.58(11) . . ? In4 S4 In1 103.97(12) . . ? In2 S5 In5 103.09(11) . . ? Co1 S6 In3 108.14(11) . . ? Co1 S6 In2 108.60(11) . . ? In3 S6 In2 107.38(11) . . ? Co2 S7 In4 108.82(11) . . ? Co2 S7 In2 108.75(11) . . ? In4 S7 In2 105.85(10) . . ? In3 S8 In6 103.24(10) . . ? Co3 S9 In4 107.36(11) . . ? Co3 S9 In3 109.25(11) . . ? In4 S9 In3 106.25(10) . . ? In4 S10 In7 104.13(11) . . ? In5 S11 In8 106.12(10) . . ? Co1 S12 In9 107.22(10) . . ? Co1 S12 In5 106.92(10) . . ? In9 S12 In5 105.29(9) . . ? Co2 S13 In5 105.79(11) . . ? Co2 S13 In10 109.69(11) . . ? In5 S13 In10 106.64(10) . . ? Co1 S14 In6 108.01(10) . . ? Co1 S14 In11 111.64(10) . . ? In6 S14 In11 106.45(9) . . ? Co3 S15 Co1 108.95(10) . . ? Co3 S15 Co2 109.74(10) . . ? Co1 S15 Co2 109.63(10) . . ? Co3 S15 Co4 109.49(10) . . ? Co1 S15 Co4 108.96(10) . . ? Co2 S15 Co4 110.06(10) . . ? Co2 S16 In7 106.86(11) . . ? Co2 S16 In12 109.47(11) . . ? In7 S16 In12 107.22(10) . . ? In6 S17 In13 106.50(9) . . ? Co3 S18 In14 107.76(10) . . ? Co3 S18 In6 106.73(10) . . ? In14 S18 In6 105.01(9) . . ? Co3 S19 In15 106.44(11) . . ? Co3 S19 In7 108.10(11) . . ? In15 S19 In7 104.42(10) . . ? In7 S20 In16 103.17(11) . . ? In9 S22 In8 107.00(10) . . ? In9 S22 Co6 117.97(11) . . ? In8 S22 Co6 113.24(10) . . ? In10 S23 In8 106.52(10) . . ? In9 S24 In11 102.70(10) . . ? Co4 S25 In10 107.08(10) . . ? Co4 S25 In9 108.28(10) . . ? In10 S25 In9 106.09(10) . . ? In10 S26 In12 103.93(10) . . ? In11 S27 In13 105.07(10) . . ? Co4 S28 In11 106.86(10) . . ? Co4 S28 In14 107.63(10) . . ? In11 S28 In14 107.29(9) . . ? Co4 S29 In15 109.09(11) . . ? Co4 S29 In12 111.33(11) . . ? In15 S29 In12 107.63(10) . . ? In12 S30 In16 104.06(11) . . ? In8 S31 In13 102.95(10) 4_565 . ? In14 S32 In13 105.93(9) . . ? In14 S32 Co5 116.26(9) . . ? In13 S32 Co5 119.13(10) . . ? In14 S33 In15 101.66(9) . . ? In15 S34 In16 105.50(10) . . ? In15 S34 Co6 115.20(11) . 2_556 ? In16 S34 Co6 114.34(11) . 2_556 ? S12 Co1 S15 114.96(10) . . ? S12 Co1 S14 104.02(10) . . ? S15 Co1 S14 112.09(10) . . ? S12 Co1 S6 103.35(11) . . ? S15 Co1 S6 114.32(10) . . ? S14 Co1 S6 107.13(10) . . ? S15 Co2 S16 114.21(10) . . ? S15 Co2 S13 112.98(10) . . ? S16 Co2 S13 103.18(11) . . ? S15 Co2 S7 112.96(10) . . ? S16 Co2 S7 105.49(11) . . ? S13 Co2 S7 107.21(11) . . ? S15 Co3 S18 115.38(10) . . ? S15 Co3 S9 113.96(10) . . ? S18 Co3 S9 103.62(10) . . ? S15 Co3 S19 114.50(10) . . ? S18 Co3 S19 103.74(10) . . ? S9 Co3 S19 104.27(11) . . ? S15 Co4 S29 111.25(10) . . ? S15 Co4 S28 115.69(10) . . ? S29 Co4 S28 104.42(10) . . ? S15 Co4 S25 114.39(10) . . ? S29 Co4 S25 106.30(10) . . ? S28 Co4 S25 103.83(10) . . ? N2 Co5 N2 180.000(1) 3_566 . ? N2 Co5 N1 95.4(4) 3_566 . ? N2 Co5 N1 84.6(4) . . ? N2 Co5 N1 84.6(4) 3_566 3_566 ? N2 Co5 N1 95.4(4) . 3_566 ? N1 Co5 N1 180.000(2) . 3_566 ? N2 Co5 S32 88.5(3) 3_566 3_566 ? N2 Co5 S32 91.5(3) . 3_566 ? N1 Co5 S32 92.8(3) . 3_566 ? N1 Co5 S32 87.2(3) 3_566 3_566 ? N2 Co5 S32 91.5(3) 3_566 . ? N2 Co5 S32 88.5(3) . . ? N1 Co5 S32 87.2(3) . . ? N1 Co5 S32 92.8(3) 3_566 . ? S32 Co5 S32 180.0 3_566 . ? N6 Co6 N4 176.0(5) . . ? N6 Co6 N3 93.2(6) . . ? N4 Co6 N3 82.8(6) . . ? N6 Co6 N5 83.0(5) . . ? N4 Co6 N5 101.0(5) . . ? N3 Co6 N5 176.2(5) . . ? N6 Co6 S22 86.7(3) . . ? N4 Co6 S22 93.3(3) . . ? N3 Co6 S22 93.7(4) . . ? N5 Co6 S22 86.8(3) . . ? N6 Co6 S34 93.3(3) . 2_546 ? N4 Co6 S34 86.7(3) . 2_546 ? N3 Co6 S34 86.2(4) . 2_546 ? N5 Co6 S34 93.3(3) . 2_546 ? S22 Co6 S34 179.92(13) . 2_546 ? N7 Co7 N9 94.6(5) . . ? N7 Co7 N11 92.7(5) . . ? N9 Co7 N11 96.1(5) . . ? N7 Co7 N10 171.6(6) . . ? N9 Co7 N10 80.2(5) . . ? N11 Co7 N10 94.4(6) . . ? N7 Co7 N8 82.1(5) . . ? N9 Co7 N8 91.6(5) . . ? N11 Co7 N8 171.0(6) . . ? N10 Co7 N8 91.4(6) . . ? N7 Co7 N12 92.7(5) . . ? N9 Co7 N12 171.6(5) . . ? N11 Co7 N12 79.3(5) . . ? N10 Co7 N12 93.1(5) . . ? N8 Co7 N12 93.6(5) . . ? N13 Co8 N16 94.1(8) . . ? N13 Co8 N15 98.0(9) . . ? N16 Co8 N15 82.0(6) . . ? N13 Co8 N17 168.9(10) . . ? N16 Co8 N17 93.7(9) . . ? N15 Co8 N17 90.9(8) . . ? N13 Co8 N14 81.9(10) . . ? N16 Co8 N14 173.0(10) . . ? N15 Co8 N14 92.9(8) . . ? N17 Co8 N14 91.1(10) . . ? N13 Co8 N18 96.7(8) . . ? N16 Co8 N18 93.7(7) . . ? N15 Co8 N18 164.9(8) . . ? N17 Co8 N18 74.9(8) . . ? N14 Co8 N18 92.5(9) . . ? N22 Co9 N20 170.7(17) . 3_667 ? C6 N1 Co5 106.2(8) . . ? C1 N2 Co5 109.6(8) . . ? C7 N3 Co6 105.7(12) . . ? C12 N4 Co6 111.1(12) . . ? C13 N5 Co6 106.1(8) . . ? C18 N6 Co6 108.9(10) . . ? C19 N7 Co7 108.0(11) . . ? C24 N8 Co7 107.5(12) . . ? C25 N9 Co7 111.0(9) . . ? C30 N10 Co7 107.5(9) . . ? C31 N11 Co7 111.0(10) . . ? C36 N12 Co7 106.4(10) . . ? C37 N13 Co8 103.3(19) . . ? C42 N14 Co8 105(2) . . ? C43 N15 Co8 110.9(14) . . ? C48 N16 Co8 106.6(12) . . ? C49 N17 Co8 115.8(18) . . ? C54 N18 Co8 105.3(18) . . ? C6 C1 N2 117.5(13) . . ? C6 C1 C2 123.9(15) . . ? N2 C1 C2 116.5(14) . . ? C1 C2 C3 112.5(15) . . ? C4 C3 C2 121.9(16) . . ? C3 C4 C5 123.8(16) . . ? C6 C5 C4 109.9(15) . . ? C1 C6 N1 120.7(13) . . ? C1 C6 C5 124.1(15) . . ? N1 C6 C5 113.6(14) . . ? C12 C7 N3 119.8(18) . . ? C12 C7 C8 126(2) . . ? N3 C7 C8 110(2) . . ? C9 C8 C7 106(2) . . ? C10 C9 C8 124(3) . . ? C9 C10 C11 112(3) . . ? C12 C11 C10 121(3) . . ? C7 C12 N4 117.6(19) . . ? C7 C12 C11 115(2) . . ? N4 C12 C11 126(2) . . ? C18 C13 N5 110.2(13) . . ? C18 C13 C14 116.4(15) . . ? N5 C13 C14 113.3(13) . . ? C15 C14 C13 112.0(18) . . ? C14 C15 C16 113(2) . . ? C15 C16 C17 114(2) . . ? C18 C17 C16 108.1(17) . . ? N6 C18 C13 115.3(16) . . ? N6 C18 C17 113.9(15) . . ? C13 C18 C17 112.9(16) . . ? C24 C19 C20 120(2) . . ? C24 C19 N7 112.6(17) . . ? C20 C19 N7 116.7(18) . . ? C19 C20 C21 112.0(19) . . ? C22 C21 C20 114(2) . . ? C23 C22 C21 122(3) . . ? C22 C23 C24 113(2) . . ? C19 C24 N8 113.5(19) . . ? C19 C24 C23 111.5(19) . . ? N8 C24 C23 109.1(18) . . ? C26 C25 N9 115.3(13) . . ? C26 C25 C30 113.4(13) . . ? N9 C25 C30 103.9(12) . . ? C25 C26 C27 111.8(15) . . ? C28 C27 C26 108.5(16) . . ? C27 C28 C29 111.7(18) . . ? C30 C29 C28 109.8(15) . . ? N10 C30 C29 110.0(14) . . ? N10 C30 C25 109.1(13) . . ? C29 C30 C25 110.6(16) . . ? N11 C31 C36 110.5(15) . . ? N11 C31 C32 111.1(14) . . ? C36 C31 C32 115.8(18) . . ? C33 C32 C31 107.2(17) . . ? C34 C33 C32 113(2) . . ? C33 C34 C35 115(2) . . ? C36 C35 C34 109(2) . . ? N12 C36 C31 113.9(18) . . ? N12 C36 C35 111.8(16) . . ? C31 C36 C35 112.5(17) . . ? C42 C37 N13 109(3) . . ? C42 C37 C38 101(3) . . ? N13 C37 C38 109(3) . . ? C37 C38 C39 92(3) . . ? C40 C39 C38 91(3) . . ? C41 C40 C39 117(4) . . ? C40 C41 C42 114(3) . . ? N14 C42 C37 105(3) . . ? N14 C42 C41 138(3) . . ? C37 C42 C41 108(3) . . ? N15 C43 C48 116.5(19) . . ? N15 C43 C44 120(2) . . ? C48 C43 C44 112.3(19) . . ? C45 C44 C43 116(2) . . ? C44 C45 C46 110(2) . . ? C47 C46 C45 112(2) . . ? C48 C47 C46 113(2) . . ? C47 C48 C43 115(2) . . ? C47 C48 N16 113(2) . . ? C43 C48 N16 110.2(18) . . ? C54 C49 N17 115(3) . . ? C54 C49 C50 125(3) . . ? N17 C49 C50 120(3) . . ? C51 C50 C49 114(3) . . ? C50 C51 C52 121(3) . . ? C51 C52 C53 118(3) . . ? C54 C53 C52 106(3) . . ? C49 C54 N18 124(3) . . ? C49 C54 C53 124(3) . . ? N18 C54 C53 106(3) . . ? C60 C55 N23 112(2) . . ? C60 C55 C56 107(3) . . ? N23 C55 C56 109(2) . . ? C57 C56 C55 108(3) . . ? C56 C57 C58 114(4) . . ? C59 C58 C57 106(3) . . ? C58 C59 C60 109(2) . . ? C55 C60 N24 112(2) . . ? C55 C60 C59 116.9(19) . . ? N24 C60 C59 108.5(15) . . ? C66 C61 C62 112(2) . . ? C66 C61 N25 108(2) . . ? C62 C61 N25 114.8(18) . . ? C61 C62 C63 106(2) . . ? C64 C63 C62 114(2) . . ? C65 C64 C63 111(2) . . ? C64 C65 C66 107(3) . . ? C61 C66 C65 107.9(19) . . ? C61 C66 N26 108(2) . . ? C65 C66 N26 105(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S5 In2 S2 In1 -178.45(12) . . . . ? S6 In2 S2 In1 62.75(15) . . . . ? S7 In2 S2 In1 -59.42(15) . . . . ? S4 In1 S2 In2 60.70(16) . . . . ? S3 In1 S2 In2 -67.44(14) . . . . ? S1 In1 S2 In2 177.70(14) . . . . ? S8 In3 S3 In1 178.70(12) . . . . ? S6 In3 S3 In1 -61.78(14) . . . . ? S9 In3 S3 In1 60.84(14) . . . . ? S4 In1 S3 In3 -66.31(15) . . . . ? S2 In1 S3 In3 66.43(15) . . . . ? S1 In1 S3 In3 177.89(13) . . . . ? S10 In4 S4 In1 173.05(12) . . . . ? S9 In4 S4 In1 -68.42(14) . . . . ? S7 In4 S4 In1 55.82(15) . . . . ? S2 In1 S4 In4 -57.87(16) . . . . ? S3 In1 S4 In4 71.11(14) . . . . ? S1 In1 S4 In4 -172.48(15) . . . . ? S2 In2 S5 In5 -178.73(12) . . . . ? S6 In2 S5 In5 -59.22(14) . . . . ? S7 In2 S5 In5 60.12(14) . . . . ? S11 In5 S5 In2 -177.91(11) . . . . ? S12 In5 S5 In2 61.78(14) . . . . ? S13 In5 S5 In2 -62.84(14) . . . . ? S8 In3 S6 Co1 -65.43(13) . . . . ? S3 In3 S6 Co1 177.41(11) . . . . ? S9 In3 S6 Co1 53.75(13) . . . . ? S8 In3 S6 In2 177.56(10) . . . . ? S3 In3 S6 In2 60.39(13) . . . . ? S9 In3 S6 In2 -63.26(12) . . . . ? S5 In2 S6 Co1 65.88(14) . . . . ? S2 In2 S6 Co1 -177.08(11) . . . . ? S7 In2 S6 Co1 -53.22(13) . . . . ? S5 In2 S6 In3 -177.41(10) . . . . ? S2 In2 S6 In3 -60.37(13) . . . . ? S7 In2 S6 In3 63.49(12) . . . . ? S10 In4 S7 Co2 67.73(13) . . . . ? S4 In4 S7 Co2 -176.07(11) . . . . ? S9 In4 S7 Co2 -53.32(13) . . . . ? S10 In4 S7 In2 -175.55(10) . . . . ? S4 In4 S7 In2 -59.34(13) . . . . ? S9 In4 S7 In2 63.40(12) . . . . ? S5 In2 S7 Co2 -65.17(13) . . . . ? S2 In2 S7 Co2 177.17(11) . . . . ? S6 In2 S7 Co2 54.28(13) . . . . ? S5 In2 S7 In4 178.05(10) . . . . ? S2 In2 S7 In4 60.39(13) . . . . ? S6 In2 S7 In4 -62.50(12) . . . . ? S3 In3 S8 In6 -178.51(12) . . . . ? S6 In3 S8 In6 61.10(14) . . . . ? S9 In3 S8 In6 -58.74(14) . . . . ? S17 In6 S8 In3 -178.30(11) . . . . ? S14 In6 S8 In3 -61.12(13) . . . . ? S18 In6 S8 In3 60.94(13) . . . . ? S10 In4 S9 Co3 -64.97(14) . . . . ? S4 In4 S9 Co3 -179.63(11) . . . . ? S7 In4 S9 Co3 53.59(13) . . . . ? S10 In4 S9 In3 178.22(10) . . . . ? S4 In4 S9 In3 63.56(13) . . . . ? S7 In4 S9 In3 -63.21(12) . . . . ? S8 In3 S9 Co3 66.97(13) . . . . ? S3 In3 S9 Co3 -176.68(11) . . . . ? S6 In3 S9 Co3 -53.09(13) . . . . ? S8 In3 S9 In4 -177.50(10) . . . . ? S3 In3 S9 In4 -61.14(13) . . . . ? S6 In3 S9 In4 62.44(12) . . . . ? S4 In4 S10 In7 176.29(12) . . . . ? S9 In4 S10 In7 59.85(14) . . . . ? S7 In4 S10 In7 -61.05(14) . . . . ? S20 In7 S10 In4 -178.82(12) . . . . ? S16 In7 S10 In4 62.07(14) . . . . ? S19 In7 S10 In4 -60.29(14) . . . . ? S5 In5 S11 In8 -176.63(11) . . . . ? S12 In5 S11 In8 -59.50(13) . . . . ? S13 In5 S11 In8 65.62(12) . . . . ? S31 In8 S11 In5 174.86(10) 4_566 . . . ? S23 In8 S11 In5 -64.98(13) . . . . ? S22 In8 S11 In5 59.46(13) . . . . ? S24 In9 S12 Co1 67.46(12) . . . . ? S22 In9 S12 Co1 -177.05(10) . . . . ? S25 In9 S12 Co1 -52.06(12) . . . . ? S24 In9 S12 In5 -178.92(9) . . . . ? S22 In9 S12 In5 -63.43(11) . . . . ? S25 In9 S12 In5 61.55(11) . . . . ? S5 In5 S12 Co1 -70.72(13) . . . . ? S11 In5 S12 Co1 175.91(10) . . . . ? S13 In5 S12 Co1 53.33(13) . . . . ? S5 In5 S12 In9 175.45(10) . . . . ? S11 In5 S12 In9 62.08(12) . . . . ? S13 In5 S12 In9 -60.50(12) . . . . ? S5 In5 S13 Co2 66.78(13) . . . . ? S11 In5 S13 Co2 178.56(10) . . . . ? S12 In5 S13 Co2 -55.78(13) . . . . ? S5 In5 S13 In10 -176.49(9) . . . . ? S11 In5 S13 In10 -64.70(12) . . . . ? S12 In5 S13 In10 60.95(12) . . . . ? S26 In10 S13 Co2 -69.56(13) . . . . ? S23 In10 S13 Co2 176.25(10) . . . . ? S25 In10 S13 Co2 53.08(13) . . . . ? S26 In10 S13 In5 176.32(9) . . . . ? S23 In10 S13 In5 62.13(12) . . . . ? S25 In10 S13 In5 -61.04(11) . . . . ? S17 In6 S14 Co1 179.90(10) . . . . ? S8 In6 S14 Co1 66.20(13) . . . . ? S18 In6 S14 Co1 -55.16(13) . . . . ? S17 In6 S14 In11 -60.08(11) . . . . ? S8 In6 S14 In11 -173.79(9) . . . . ? S18 In6 S14 In11 64.85(11) . . . . ? S27 In11 S14 Co1 178.75(10) . . . . ? S24 In11 S14 Co1 -66.37(12) . . . . ? S28 In11 S14 Co1 54.16(12) . . . . ? S27 In11 S14 In6 61.11(11) . . . . ? S24 In11 S14 In6 175.99(9) . . . . ? S28 In11 S14 In6 -63.49(10) . . . . ? S20 In7 S16 Co2 179.69(11) . . . . ? S10 In7 S16 Co2 -65.91(13) . . . . ? S19 In7 S16 Co2 53.52(13) . . . . ? S20 In7 S16 In12 62.40(13) . . . . ? S10 In7 S16 In12 176.79(10) . . . . ? S19 In7 S16 In12 -63.77(12) . . . . ? S30 In12 S16 Co2 -175.73(11) . . . . ? S26 In12 S16 Co2 65.07(13) . . . . ? S29 In12 S16 Co2 -52.91(13) . . . . ? S30 In12 S16 In7 -60.15(13) . . . . ? S26 In12 S16 In7 -179.35(9) . . . . ? S29 In12 S16 In7 62.66(11) . . . . ? S8 In6 S17 In13 -179.13(11) . . . . ? S14 In6 S17 In13 64.07(12) . . . . ? S18 In6 S17 In13 -60.07(13) . . . . ? S27 In13 S17 In6 -67.70(12) . . . . ? S32 In13 S17 In6 60.29(12) . . . . ? S31 In13 S17 In6 172.02(10) . . . . ? S32 In14 S18 Co3 -176.26(9) . . . . ? S33 In14 S18 Co3 67.88(12) . . . . ? S28 In14 S18 Co3 -52.72(12) . . . . ? S32 In14 S18 In6 -62.75(11) . . . . ? S33 In14 S18 In6 -178.61(8) . . . . ? S28 In14 S18 In6 60.78(11) . . . . ? S17 In6 S18 Co3 175.43(10) . . . . ? S8 In6 S18 Co3 -68.85(12) . . . . ? S14 In6 S18 Co3 52.06(12) . . . . ? S17 In6 S18 In14 61.21(11) . . . . ? S8 In6 S18 In14 176.92(9) . . . . ? S14 In6 S18 In14 -62.16(11) . . . . ? S34 In15 S19 Co3 176.95(10) . . . . ? S33 In15 S19 Co3 -68.22(12) . . . . ? S29 In15 S19 Co3 52.77(13) . . . . ? S34 In15 S19 In7 62.72(11) . . . . ? S33 In15 S19 In7 177.56(9) . . . . ? S29 In15 S19 In7 -61.46(11) . . . . ? S20 In7 S19 Co3 -177.63(11) . . . . ? S10 In7 S19 Co3 69.43(13) . . . . ? S16 In7 S19 Co3 -51.91(14) . . . . ? S20 In7 S19 In15 -64.58(13) . . . . ? S10 In7 S19 In15 -177.52(10) . . . . ? S16 In7 S19 In15 61.14(11) . . . . ? S10 In7 S20 In16 -179.70(12) . . . . ? S16 In7 S20 In16 -61.08(15) . . . . ? S19 In7 S20 In16 65.15(15) . . . . ? S30 In16 S20 In7 63.67(16) . . . . ? S35 In16 S20 In7 -178.45(14) . . . . ? S34 In16 S20 In7 -65.51(14) . . . . ? S24 In9 S22 In8 -173.49(11) . . . . ? S12 In9 S22 In8 66.23(12) . . . . ? S25 In9 S22 In8 -58.30(13) . . . . ? S24 In9 S22 Co6 -44.48(14) . . . . ? S12 In9 S22 Co6 -164.77(11) . . . . ? S25 In9 S22 Co6 70.71(13) . . . . ? S11 In8 S22 In9 -64.81(13) . . . . ? S31 In8 S22 In9 179.35(11) 4_566 . . . ? S23 In8 S22 In9 59.91(13) . . . . ? S11 In8 S22 Co6 163.52(10) . . . . ? S31 In8 S22 Co6 47.68(14) 4_566 . . . ? S23 In8 S22 Co6 -71.76(13) . . . . ? S26 In10 S23 In8 -174.64(11) . . . . ? S25 In10 S23 In8 63.89(13) . . . . ? S13 In10 S23 In8 -58.98(13) . . . . ? S11 In8 S23 In10 61.10(13) . . . . ? S31 In8 S23 In10 179.64(10) 4_566 . . . ? S22 In8 S23 In10 -62.99(13) . . . . ? S22 In9 S24 In11 -178.01(10) . . . . ? S12 In9 S24 In11 -60.96(13) . . . . ? S25 In9 S24 In11 62.08(12) . . . . ? S27 In11 S24 In9 175.01(10) . . . . ? S28 In11 S24 In9 -61.50(13) . . . . ? S14 In11 S24 In9 57.25(12) . . . . ? S26 In10 S25 Co4 66.20(13) . . . . ? S23 In10 S25 Co4 -176.54(11) . . . . ? S13 In10 S25 Co4 -53.68(13) . . . . ? S26 In10 S25 In9 -178.33(10) . . . . ? S23 In10 S25 In9 -61.07(12) . . . . ? S13 In10 S25 In9 61.79(11) . . . . ? S24 In9 S25 Co4 -71.93(12) . . . . ? S22 In9 S25 Co4 173.40(10) . . . . ? S12 In9 S25 Co4 51.34(12) . . . . ? S24 In9 S25 In10 173.41(9) . . . . ? S22 In9 S25 In10 58.75(12) . . . . ? S12 In9 S25 In10 -63.31(11) . . . . ? S23 In10 S26 In12 178.44(11) . . . . ? S25 In10 S26 In12 -60.86(14) . . . . ? S13 In10 S26 In12 60.75(13) . . . . ? S30 In12 S26 In10 178.31(11) . . . . ? S29 In12 S26 In10 56.96(14) . . . . ? S16 In12 S26 In10 -59.66(14) . . . . ? S24 In11 S27 In13 178.99(10) . . . . ? S28 In11 S27 In13 56.85(13) . . . . ? S14 In11 S27 In13 -64.86(12) . . . . ? S17 In13 S27 In11 67.48(12) . . . . ? S32 In13 S27 In11 -58.35(13) . . . . ? S31 In13 S27 In11 -169.36(9) . . . . ? S27 In11 S28 Co4 -175.61(10) . . . . ? S24 In11 S28 Co4 65.37(12) . . . . ? S14 In11 S28 Co4 -52.96(12) . . . . ? S27 In11 S28 In14 -60.41(12) . . . . ? S24 In11 S28 In14 -179.42(9) . . . . ? S14 In11 S28 In14 62.24(11) . . . . ? S32 In14 S28 Co4 175.92(9) . . . . ? S33 In14 S28 Co4 -70.14(12) . . . . ? S18 In14 S28 Co4 52.15(12) . . . . ? S32 In14 S28 In11 61.24(11) . . . . ? S33 In14 S28 In11 175.18(9) . . . . ? S18 In14 S28 In11 -62.53(11) . . . . ? S34 In15 S29 Co4 -176.97(10) . . . . ? S33 In15 S29 Co4 67.62(13) . . . . ? S19 In15 S29 Co4 -55.15(13) . . . . ? S34 In15 S29 In12 -56.05(13) . . . . ? S33 In15 S29 In12 -171.46(9) . . . . ? S19 In15 S29 In12 65.77(11) . . . . ? S30 In12 S29 Co4 178.24(12) . . . . ? S26 In12 S29 Co4 -63.31(14) . . . . ? S16 In12 S29 Co4 55.43(13) . . . . ? S30 In12 S29 In15 58.74(13) . . . . ? S26 In12 S29 In15 177.18(10) . . . . ? S16 In12 S29 In15 -64.08(11) . . . . ? S26 In12 S30 In16 177.61(11) . . . . ? S29 In12 S30 In16 -62.98(14) . . . . ? S16 In12 S30 In16 56.79(14) . . . . ? S20 In16 S30 In12 -61.70(15) . . . . ? S35 In16 S30 In12 -179.01(13) . . . . ? S34 In16 S30 In12 66.65(14) . . . . ? S27 In13 S31 In8 -65.28(13) . . . 4_565 ? S17 In13 S31 In8 54.48(14) . . . 4_565 ? S32 In13 S31 In8 173.44(11) . . . 4_565 ? S33 In14 S32 In13 -176.47(10) . . . . ? S18 In14 S32 In13 63.90(12) . . . . ? S28 In14 S32 In13 -60.48(12) . . . . ? S33 In14 S32 Co5 -41.61(13) . . . . ? S18 In14 S32 Co5 -161.25(9) . . . . ? S28 In14 S32 Co5 74.38(12) . . . . ? S27 In13 S32 In14 61.31(13) . . . . ? S17 In13 S32 In14 -62.41(12) . . . . ? S31 In13 S32 In14 177.52(11) . . . . ? S27 In13 S32 Co5 -71.98(12) . . . . ? S17 In13 S32 Co5 164.30(9) . . . . ? S31 In13 S32 Co5 44.23(13) . . . . ? S32 In14 S33 In15 -177.88(10) . . . . ? S18 In14 S33 In15 -58.35(12) . . . . ? S28 In14 S33 In15 64.50(12) . . . . ? S34 In15 S33 In14 176.40(10) . . . . ? S29 In15 S33 In14 -63.12(12) . . . . ? S19 In15 S33 In14 59.20(12) . . . . ? S33 In15 S34 In16 175.78(11) . . . . ? S29 In15 S34 In16 58.09(13) . . . . ? S19 In15 S34 In16 -64.99(13) . . . . ? S33 In15 S34 Co6 48.68(14) . . . 2_556 ? S29 In15 S34 Co6 -69.00(13) . . . 2_556 ? S19 In15 S34 Co6 167.92(11) . . . 2_556 ? S30 In16 S34 In15 -64.58(13) . . . . ? S20 In16 S34 In15 67.51(13) . . . . ? S35 In16 S34 In15 -179.57(14) . . . . ? S30 In16 S34 Co6 63.04(13) . . . 2_556 ? S20 In16 S34 Co6 -164.88(11) . . . 2_556 ? S35 In16 S34 Co6 -51.95(17) . . . 2_556 ? In9 S12 Co1 S15 57.66(13) . . . . ? In5 S12 Co1 S15 -54.85(14) . . . . ? In9 S12 Co1 S14 -65.28(12) . . . . ? In5 S12 Co1 S14 -177.79(10) . . . . ? In9 S12 Co1 S6 -177.08(10) . . . . ? In5 S12 Co1 S6 70.41(12) . . . . ? Co3 S15 Co1 S12 179.64(10) . . . . ? Co2 S15 Co1 S12 59.54(14) . . . . ? Co4 S15 Co1 S12 -60.97(13) . . . . ? Co3 S15 Co1 S14 -61.85(13) . . . . ? Co2 S15 Co1 S14 178.04(10) . . . . ? Co4 S15 Co1 S14 57.54(13) . . . . ? Co3 S15 Co1 S6 60.31(13) . . . . ? Co2 S15 Co1 S6 -59.79(14) . . . . ? Co4 S15 Co1 S6 179.70(10) . . . . ? In6 S14 Co1 S12 -175.31(10) . . . . ? In11 S14 Co1 S12 67.99(13) . . . . ? In6 S14 Co1 S15 59.90(13) . . . . ? In11 S14 Co1 S15 -56.80(13) . . . . ? In6 S14 Co1 S6 -66.27(13) . . . . ? In11 S14 Co1 S6 177.03(10) . . . . ? In3 S6 Co1 S12 175.29(10) . . . . ? In2 S6 Co1 S12 -68.49(13) . . . . ? In3 S6 Co1 S15 -59.04(13) . . . . ? In2 S6 Co1 S15 57.19(14) . . . . ? In3 S6 Co1 S14 65.80(13) . . . . ? In2 S6 Co1 S14 -177.98(10) . . . . ? Co3 S15 Co2 S16 60.99(14) . . . . ? Co1 S15 Co2 S16 -179.39(11) . . . . ? Co4 S15 Co2 S16 -59.57(14) . . . . ? Co3 S15 Co2 S13 178.50(11) . . . . ? Co1 S15 Co2 S13 -61.87(14) . . . . ? Co4 S15 Co2 S13 57.95(14) . . . . ? Co3 S15 Co2 S7 -59.58(14) . . . . ? Co1 S15 Co2 S7 60.04(14) . . . . ? Co4 S15 Co2 S7 179.87(10) . . . . ? In7 S16 Co2 S15 -58.40(14) . . . . ? In12 S16 Co2 S15 57.40(14) . . . . ? In7 S16 Co2 S13 178.59(10) . . . . ? In12 S16 Co2 S13 -65.61(13) . . . . ? In7 S16 Co2 S7 66.25(13) . . . . ? In12 S16 Co2 S7 -177.95(10) . . . . ? In5 S13 Co2 S15 59.65(13) . . . . ? In10 S13 Co2 S15 -55.01(14) . . . . ? In5 S13 Co2 S16 -176.52(10) . . . . ? In10 S13 Co2 S16 68.82(13) . . . . ? In5 S13 Co2 S7 -65.44(13) . . . . ? In10 S13 Co2 S7 179.90(10) . . . . ? In4 S7 Co2 S15 56.32(14) . . . . ? In2 S7 Co2 S15 -58.54(14) . . . . ? In4 S7 Co2 S16 -69.10(13) . . . . ? In2 S7 Co2 S16 176.04(10) . . . . ? In4 S7 Co2 S13 -178.58(10) . . . . ? In2 S7 Co2 S13 66.56(13) . . . . ? Co1 S15 Co3 S18 61.14(14) . . . . ? Co2 S15 Co3 S18 -178.82(10) . . . . ? Co4 S15 Co3 S18 -57.92(13) . . . . ? Co1 S15 Co3 S9 -58.60(13) . . . . ? Co2 S15 Co3 S9 61.44(14) . . . . ? Co4 S15 Co3 S9 -177.66(10) . . . . ? Co1 S15 Co3 S19 -178.53(10) . . . . ? Co2 S15 Co3 S19 -58.48(14) . . . . ? Co4 S15 Co3 S19 62.41(13) . . . . ? In14 S18 Co3 S15 56.28(13) . . . . ? In6 S18 Co3 S15 -56.07(13) . . . . ? In14 S18 Co3 S9 -178.46(10) . . . . ? In6 S18 Co3 S9 69.20(12) . . . . ? In14 S18 Co3 S19 -69.77(12) . . . . ? In6 S18 Co3 S19 177.88(10) . . . . ? In4 S9 Co3 S15 -58.39(13) . . . . ? In3 S9 Co3 S15 56.43(13) . . . . ? In4 S9 Co3 S18 175.44(10) . . . . ? In3 S9 Co3 S18 -69.74(12) . . . . ? In4 S9 Co3 S19 67.15(12) . . . . ? In3 S9 Co3 S19 -178.03(10) . . . . ? In15 S19 Co3 S15 -57.39(13) . . . . ? In7 S19 Co3 S15 54.30(14) . . . . ? In15 S19 Co3 S18 69.22(12) . . . . ? In7 S19 Co3 S18 -179.09(10) . . . . ? In15 S19 Co3 S9 177.42(10) . . . . ? In7 S19 Co3 S9 -70.89(13) . . . . ? Co3 S15 Co4 S29 -61.41(13) . . . . ? Co1 S15 Co4 S29 179.53(10) . . . . ? Co2 S15 Co4 S29 59.29(13) . . . . ? Co3 S15 Co4 S28 57.51(13) . . . . ? Co1 S15 Co4 S28 -61.55(13) . . . . ? Co2 S15 Co4 S28 178.21(10) . . . . ? Co3 S15 Co4 S25 178.13(10) . . . . ? Co1 S15 Co4 S25 59.07(13) . . . . ? Co2 S15 Co4 S25 -61.17(13) . . . . ? In15 S29 Co4 S15 58.83(13) . . . . ? In12 S29 Co4 S15 -59.80(14) . . . . ? In15 S29 Co4 S28 -66.64(13) . . . . ? In12 S29 Co4 S28 174.73(10) . . . . ? In15 S29 Co4 S25 -176.05(10) . . . . ? In12 S29 Co4 S25 65.32(13) . . . . ? In11 S28 Co4 S15 59.74(13) . . . . ? In14 S28 Co4 S15 -55.23(13) . . . . ? In11 S28 Co4 S29 -177.65(10) . . . . ? In14 S28 Co4 S29 67.38(12) . . . . ? In11 S28 Co4 S25 -66.44(12) . . . . ? In14 S28 Co4 S25 178.59(10) . . . . ? In10 S25 Co4 S15 58.96(13) . . . . ? In9 S25 Co4 S15 -55.04(13) . . . . ? In10 S25 Co4 S29 -64.22(13) . . . . ? In9 S25 Co4 S29 -178.22(10) . . . . ? In10 S25 Co4 S28 -174.05(10) . . . . ? In9 S25 Co4 S28 71.95(12) . . . . ? In14 S32 Co5 N2 -113.0(3) . . . 3_566 ? In13 S32 Co5 N2 15.7(3) . . . 3_566 ? In14 S32 Co5 N2 67.0(3) . . . . ? In13 S32 Co5 N2 -164.3(3) . . . . ? In14 S32 Co5 N1 151.7(3) . . . . ? In13 S32 Co5 N1 -79.6(3) . . . . ? In14 S32 Co5 N1 -28.3(3) . . . 3_566 ? In13 S32 Co5 N1 100.4(3) . . . 3_566 ? In14 S32 Co5 S32 -54(100) . . . 3_566 ? In13 S32 Co5 S32 74(100) . . . 3_566 ? In9 S22 Co6 N6 170.5(4) . . . . ? In8 S22 Co6 N6 -63.5(4) . . . . ? In9 S22 Co6 N4 -13.5(4) . . . . ? In8 S22 Co6 N4 112.5(4) . . . . ? In9 S22 Co6 N3 -96.5(4) . . . . ? In8 S22 Co6 N3 29.5(4) . . . . ? In9 S22 Co6 N5 87.3(3) . . . . ? In8 S22 Co6 N5 -146.6(3) . . . . ? In9 S22 Co6 S34 -98(100) . . . 2_546 ? In8 S22 Co6 S34 28(94) . . . 2_546 ? N2 Co5 N1 C6 175.6(10) 3_566 . . . ? N2 Co5 N1 C6 -4.4(10) . . . . ? N1 Co5 N1 C6 99(100) 3_566 . . . ? S32 Co5 N1 C6 86.8(10) 3_566 . . . ? S32 Co5 N1 C6 -93.2(10) . . . . ? N2 Co5 N2 C1 0(100) 3_566 . . . ? N1 Co5 N2 C1 -1.8(11) . . . . ? N1 Co5 N2 C1 178.2(11) 3_566 . . . ? S32 Co5 N2 C1 -94.5(10) 3_566 . . . ? S32 Co5 N2 C1 85.5(10) . . . . ? N6 Co6 N3 C7 177.1(13) . . . . ? N4 Co6 N3 C7 -2.6(13) . . . . ? N5 Co6 N3 C7 -172(7) . . . . ? S22 Co6 N3 C7 90.3(13) . . . . ? S34 Co6 N3 C7 -89.7(13) 2_546 . . . ? N6 Co6 N4 C12 -11(7) . . . . ? N3 Co6 N4 C12 -6.9(14) . . . . ? N5 Co6 N4 C12 172.4(14) . . . . ? S22 Co6 N4 C12 -100.2(14) . . . . ? S34 Co6 N4 C12 79.7(14) 2_546 . . . ? N6 Co6 N5 C13 10.1(9) . . . . ? N4 Co6 N5 C13 -170.2(9) . . . . ? N3 Co6 N5 C13 -1(7) . . . . ? S22 Co6 N5 C13 97.1(9) . . . . ? S34 Co6 N5 C13 -82.9(9) 2_546 . . . ? N4 Co6 N6 C18 -164(6) . . . . ? N3 Co6 N6 C18 -167.3(11) . . . . ? N5 Co6 N6 C18 13.4(11) . . . . ? S22 Co6 N6 C18 -73.8(11) . . . . ? S34 Co6 N6 C18 106.3(11) 2_546 . . . ? N9 Co7 N7 C19 104.4(13) . . . . ? N11 Co7 N7 C19 -159.3(13) . . . . ? N10 Co7 N7 C19 53(4) . . . . ? N8 Co7 N7 C19 13.4(12) . . . . ? N12 Co7 N7 C19 -79.8(13) . . . . ? N7 Co7 N8 C24 9.3(14) . . . . ? N9 Co7 N8 C24 -85.1(14) . . . . ? N11 Co7 N8 C24 64(4) . . . . ? N10 Co7 N8 C24 -165.4(14) . . . . ? N12 Co7 N8 C24 101.5(14) . . . . ? N7 Co7 N9 C25 -156.2(9) . . . . ? N11 Co7 N9 C25 110.6(9) . . . . ? N10 Co7 N9 C25 17.1(9) . . . . ? N8 Co7 N9 C25 -74.0(10) . . . . ? N12 Co7 N9 C25 54(4) . . . . ? N7 Co7 N10 C30 68(4) . . . . ? N9 Co7 N10 C30 15.8(11) . . . . ? N11 Co7 N10 C30 -79.7(11) . . . . ? N8 Co7 N10 C30 107.1(12) . . . . ? N12 Co7 N10 C30 -159.2(11) . . . . ? N7 Co7 N11 C31 93.9(13) . . . . ? N9 Co7 N11 C31 -171.2(13) . . . . ? N10 Co7 N11 C31 -90.6(13) . . . . ? N8 Co7 N11 C31 40(4) . . . . ? N12 Co7 N11 C31 1.6(13) . . . . ? N7 Co7 N12 C36 -69.9(14) . . . . ? N9 Co7 N12 C36 80(4) . . . . ? N11 Co7 N12 C36 22.3(13) . . . . ? N10 Co7 N12 C36 116.2(14) . . . . ? N8 Co7 N12 C36 -152.2(14) . . . . ? N16 Co8 N13 C37 -171.4(19) . . . . ? N15 Co8 N13 C37 106.1(19) . . . . ? N17 Co8 N13 C37 -37(5) . . . . ? N14 Co8 N13 C37 14.3(19) . . . . ? N18 Co8 N13 C37 -77.3(19) . . . . ? N13 Co8 N14 C42 19.7(18) . . . . ? N16 Co8 N14 C42 -36(7) . . . . ? N15 Co8 N14 C42 -78.0(19) . . . . ? N17 Co8 N14 C42 -169.0(18) . . . . ? N18 Co8 N14 C42 116.1(19) . . . . ? N13 Co8 N15 C43 102.9(19) . . . . ? N16 Co8 N15 C43 9.9(18) . . . . ? N17 Co8 N15 C43 -83.7(19) . . . . ? N14 Co8 N15 C43 -174.8(19) . . . . ? N18 Co8 N15 C43 -64(3) . . . . ? N13 Co8 N16 C48 -85.0(15) . . . . ? N15 Co8 N16 C48 12.5(15) . . . . ? N17 Co8 N16 C48 102.9(15) . . . . ? N14 Co8 N16 C48 -30(7) . . . . ? N18 Co8 N16 C48 177.9(15) . . . . ? N13 Co8 N17 C49 -55(5) . . . . ? N16 Co8 N17 C49 80(2) . . . . ? N15 Co8 N17 C49 162(2) . . . . ? N14 Co8 N17 C49 -105(2) . . . . ? N18 Co8 N17 C49 -13(2) . . . . ? N13 Co8 N18 C54 -170.1(18) . . . . ? N16 Co8 N18 C54 -75.4(18) . . . . ? N15 Co8 N18 C54 -3(4) . . . . ? N17 Co8 N18 C54 17.4(18) . . . . ? N14 Co8 N18 C54 107.8(18) . . . . ? Co5 N2 C1 C6 9(2) . . . . ? Co5 N2 C1 C2 173.3(13) . . . . ? C6 C1 C2 C3 -17(3) . . . . ? N2 C1 C2 C3 -179.7(17) . . . . ? C1 C2 C3 C4 16(3) . . . . ? C2 C3 C4 C5 -16(4) . . . . ? C3 C4 C5 C6 14(3) . . . . ? N2 C1 C6 N1 -14(3) . . . . ? C2 C1 C6 N1 -177.4(17) . . . . ? N2 C1 C6 C5 -179.2(17) . . . . ? C2 C1 C6 C5 18(4) . . . . ? Co5 N1 C6 C1 12(2) . . . . ? Co5 N1 C6 C5 177.9(13) . . . . ? C4 C5 C6 C1 -15(3) . . . . ? C4 C5 C6 N1 179.6(17) . . . . ? Co6 N3 C7 C12 13(3) . . . . ? Co6 N3 C7 C8 171.1(16) . . . . ? C12 C7 C8 C9 -23(4) . . . . ? N3 C7 C8 C9 -179(2) . . . . ? C7 C8 C9 C10 38(5) . . . . ? C8 C9 C10 C11 -45(6) . . . . ? C9 C10 C11 C12 35(5) . . . . ? N3 C7 C12 N4 -21(4) . . . . ? C8 C7 C12 N4 -175(2) . . . . ? N3 C7 C12 C11 171(2) . . . . ? C8 C7 C12 C11 17(5) . . . . ? Co6 N4 C12 C7 17(3) . . . . ? Co6 N4 C12 C11 -177(2) . . . . ? C10 C11 C12 C7 -22(4) . . . . ? C10 C11 C12 N4 172(3) . . . . ? Co6 N5 C13 C18 -31.3(16) . . . . ? Co6 N5 C13 C14 -163.7(12) . . . . ? C18 C13 C14 C15 50(2) . . . . ? N5 C13 C14 C15 179.2(17) . . . . ? C13 C14 C15 C16 -52(3) . . . . ? C14 C15 C16 C17 57(3) . . . . ? C15 C16 C17 C18 -52(3) . . . . ? Co6 N6 C18 C13 -37.1(17) . . . . ? Co6 N6 C18 C17 -169.9(13) . . . . ? N5 C13 C18 N6 48(2) . . . . ? C14 C13 C18 N6 178.3(15) . . . . ? N5 C13 C18 C17 -179.2(15) . . . . ? C14 C13 C18 C17 -48(2) . . . . ? C16 C17 C18 N6 -178.6(18) . . . . ? C16 C17 C18 C13 48(2) . . . . ? Co7 N7 C19 C24 -36(2) . . . . ? Co7 N7 C19 C20 179.5(17) . . . . ? C24 C19 C20 C21 41(3) . . . . ? N7 C19 C20 C21 -177(2) . . . . ? C19 C20 C21 C22 -34(4) . . . . ? C20 C21 C22 C23 40(5) . . . . ? C21 C22 C23 C24 -45(4) . . . . ? C20 C19 C24 N8 -169.6(19) . . . . ? N7 C19 C24 N8 47(3) . . . . ? C20 C19 C24 C23 -46(3) . . . . ? N7 C19 C24 C23 170.8(19) . . . . ? Co7 N8 C24 C19 -32(2) . . . . ? Co7 N8 C24 C23 -157.5(16) . . . . ? C22 C23 C24 C19 44(4) . . . . ? C22 C23 C24 N8 171(2) . . . . ? Co7 N9 C25 C26 -168.1(11) . . . . ? Co7 N9 C25 C30 -43.4(13) . . . . ? N9 C25 C26 C27 176.2(13) . . . . ? C30 C25 C26 C27 56.6(18) . . . . ? C25 C26 C27 C28 -58(2) . . . . ? C26 C27 C28 C29 58(2) . . . . ? C27 C28 C29 C30 -57(2) . . . . ? Co7 N10 C30 C29 -165.9(13) . . . . ? Co7 N10 C30 C25 -44.4(15) . . . . ? C28 C29 C30 N10 173.1(17) . . . . ? C28 C29 C30 C25 53(2) . . . . ? C26 C25 C30 N10 -175.3(13) . . . . ? N9 C25 C30 N10 58.9(16) . . . . ? C26 C25 C30 C29 -54.2(19) . . . . ? N9 C25 C30 C29 179.9(14) . . . . ? Co7 N11 C31 C36 -25(2) . . . . ? Co7 N11 C31 C32 -155.0(14) . . . . ? N11 C31 C32 C33 179.9(19) . . . . ? C36 C31 C32 C33 53(3) . . . . ? C31 C32 C33 C34 -51(3) . . . . ? C32 C33 C34 C35 55(4) . . . . ? C33 C34 C35 C36 -53(4) . . . . ? Co7 N12 C36 C31 -45(2) . . . . ? Co7 N12 C36 C35 -173.7(15) . . . . ? N11 C31 C36 N12 48(2) . . . . ? C32 C31 C36 N12 175.7(17) . . . . ? N11 C31 C36 C35 176.9(19) . . . . ? C32 C31 C36 C35 -56(3) . . . . ? C34 C35 C36 N12 -179(2) . . . . ? C34 C35 C36 C31 52(3) . . . . ? Co8 N13 C37 C42 -47(3) . . . . ? Co8 N13 C37 C38 -156(2) . . . . ? C42 C37 C38 C39 86(3) . . . . ? N13 C37 C38 C39 -160(3) . . . . ? C37 C38 C39 C40 -81(3) . . . . ? C38 C39 C40 C41 14(4) . . . . ? C39 C40 C41 C42 52(5) . . . . ? Co8 N14 C42 C37 -50(3) . . . . ? Co8 N14 C42 C41 169(4) . . . . ? N13 C37 C42 N14 68(4) . . . . ? C38 C37 C42 N14 -177(3) . . . . ? N13 C37 C42 C41 -138(3) . . . . ? C38 C37 C42 C41 -23(4) . . . . ? C40 C41 C42 N14 89(5) . . . . ? C40 C41 C42 C37 -51(5) . . . . ? Co8 N15 C43 C48 -32(3) . . . . ? Co8 N15 C43 C44 -172.5(17) . . . . ? N15 C43 C44 C45 -176(2) . . . . ? C48 C43 C44 C45 42(3) . . . . ? C43 C44 C45 C46 -47(3) . . . . ? C44 C45 C46 C47 53(4) . . . . ? C45 C46 C47 C48 -58(4) . . . . ? C46 C47 C48 C43 53(4) . . . . ? C46 C47 C48 N16 -179(2) . . . . ? N15 C43 C48 C47 172(3) . . . . ? C44 C43 C48 C47 -44(3) . . . . ? N15 C43 C48 N16 44(3) . . . . ? C44 C43 C48 N16 -173(2) . . . . ? Co8 N16 C48 C47 -160.5(18) . . . . ? Co8 N16 C48 C43 -31(2) . . . . ? Co8 N17 C49 C54 3(4) . . . . ? Co8 N17 C49 C50 -171(2) . . . . ? C54 C49 C50 C51 -7(6) . . . . ? N17 C49 C50 C51 166(3) . . . . ? C49 C50 C51 C52 34(6) . . . . ? C50 C51 C52 C53 -32(6) . . . . ? C51 C52 C53 C54 5(5) . . . . ? N17 C49 C54 N18 16(5) . . . . ? C50 C49 C54 N18 -170(3) . . . . ? N17 C49 C54 C53 165(3) . . . . ? C50 C49 C54 C53 -21(6) . . . . ? Co8 N18 C54 C49 -25(4) . . . . ? Co8 N18 C54 C53 -179.3(19) . . . . ? C52 C53 C54 C49 20(5) . . . . ? C52 C53 C54 N18 174(3) . . . . ? C60 C55 C56 C57 -59(4) . . . . ? N23 C55 C56 C57 180(3) . . . . ? C55 C56 C57 C58 62(5) . . . . ? C56 C57 C58 C59 -60(5) . . . . ? C57 C58 C59 C60 51(4) . . . . ? N23 C55 C60 N24 -55(3) . . . . ? C56 C55 C60 N24 -174(2) . . . . ? N23 C55 C60 C59 179.0(19) . . . . ? C56 C55 C60 C59 59(3) . . . . ? C58 C59 C60 C55 -59(3) . . . . ? C58 C59 C60 N24 173(2) . . . . ? C66 C61 C62 C63 -56(2) . . . . ? N25 C61 C62 C63 68(3) . . . . ? C61 C62 C63 C64 51(3) . . . . ? C62 C63 C64 C65 -57(3) . . . . ? C63 C64 C65 C66 61(3) . . . . ? C62 C61 C66 C65 65(3) . . . . ? N25 C61 C66 C65 -62(3) . . . . ? C62 C61 C66 N26 177.9(19) . . . . ? N25 C61 C66 N26 51(2) . . . . ? C64 C65 C66 C61 -64(3) . . . . ? C64 C65 C66 N26 -179(2) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 4.248 _refine_diff_density_min -2.944 _refine_diff_density_rms 0.292 ########End _database_code_depnum_ccdc_archive 'CCDC 923791'