Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Teresa Rodriguez-Blas' _publ_contact_author_address ; Departamento de Quimica Fundamental Universidade da Coruna Facultad de Ciencias. Campus da Zap A Coruna 15071 SPAIN ; _publ_contact_author_email MAYTER@UDC.ES _publ_section_title ; Designing Dinuclear Transition Metal Complexes: A New Example of the Versatility of N,N' Bis(2-aminobenzyl) -4-13-diaza-18-crown-6 ; loop_ _publ_author_name 'Teresa Rodriguez-Blas' 'Fernando Avecilla' 'Juan-Modesto Clemente-Juan' 'A.de Blas' ; D.Esteban-Gomez ; 'Carlos Platas-Iglesias' 'Jose Antonio Real' 'Lea Vaiana' #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 238131' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H44 Co2 N5 O5, 3(Cl O4)' _chemical_formula_sum 'C28 H44 Cl3 Co2 N5 O17' _chemical_formula_weight 946.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.839(2) _cell_length_b 17.753(3) _cell_length_c 18.532(3) _cell_angle_alpha 84.699(4) _cell_angle_beta 71.771(3) _cell_angle_gamma 82.569(4) _cell_volume 3972.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 1.113 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6771 _exptl_absorpt_correction_T_max 0.9065 _exptl_absorpt_process_details 'Sadabs (Scheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24618 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.1022 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.10 _reflns_number_total 17022 _reflns_number_gt 5471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0829P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17022 _refine_ls_number_parameters 1116 _refine_ls_number_restraints 383 _refine_ls_R_factor_all 0.1831 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1907 _refine_ls_wR_factor_gt 0.1360 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.894 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1S N 0.5124(7) 0.7208(5) 0.1225(5) 0.054(3) Uani 1 1 d . . . C1S C 1.0550(9) 0.1782(6) 0.0797(6) 0.052(3) Uani 1 1 d . . . Cl1 Cl 0.3300(3) 0.1682(2) 0.12826(19) 0.0682(10) Uani 1 1 d DU . . O1W O 0.2907(5) 0.7367(3) 0.2364(3) 0.0436(19) Uani 1 1 d . . . H1W H 0.2957 0.6891 0.2294 0.052 Uiso 1 1 d R . . Co1 Co 0.41293(11) 0.79912(7) 0.20361(7) 0.0374(4) Uani 1 1 d . . . O1 O 0.3816(6) 0.8626(4) 0.0985(4) 0.054(2) Uani 1 1 d . . . N1 N 0.5175(7) 0.8883(4) 0.1797(5) 0.045(2) Uani 1 1 d . . . C1 C 0.5886(8) 0.8493(6) 0.2905(6) 0.048(3) Uani 1 1 d . . . O2W O 0.7906(5) 0.2372(3) 0.2360(3) 0.0415(19) Uani 1 1 d . . . H2W H 0.7957 0.1900 0.2287 0.050 Uiso 1 1 d R . . N2S N 1.0122(7) 0.2202(5) 0.1227(5) 0.050(3) Uani 1 1 d . . . Cl2 Cl 0.8302(3) 0.6676(2) 0.12894(19) 0.0673(10) Uani 1 1 d DU . . C2S C 1.1105(9) 0.1215(6) 0.0230(6) 0.078(4) Uani 1 1 d . . . H2S1 H 1.1879 0.1144 0.0176 0.117 Uiso 1 1 calc R . . H2S2 H 1.1000 0.1390 -0.0251 0.117 Uiso 1 1 calc R . . H2S3 H 1.0797 0.0741 0.0395 0.117 Uiso 1 1 calc R . . Co2 Co 0.13472(11) 0.77084(8) 0.26742(8) 0.0453(4) Uani 1 1 d . . . O2 O 0.1415(7) 0.8355(4) 0.1664(4) 0.069(2) Uani 1 1 d . . . N2 N -0.0341(7) 0.8250(5) 0.2966(5) 0.056(3) Uani 1 1 d . . . C2 C 0.6196(10) 0.8979(7) 0.3329(8) 0.071(4) Uani 1 1 d . . . H2 H 0.6612 0.9370 0.3077 0.085 Uiso 1 1 calc R . . Co3 Co 0.91290(11) 0.29909(7) 0.20376(7) 0.0367(4) Uani 1 1 d . . . Cl3 Cl 0.2971(3) 0.55717(18) 0.11799(18) 0.0575(9) Uani 1 1 d DU . . C3S C 0.5541(9) 0.6772(6) 0.0784(7) 0.056(3) Uani 1 1 d . . . O3 O 0.2973(5) 0.8914(3) 0.2747(3) 0.0412(18) Uani 1 1 d . . . N3 N 0.5005(6) 0.7417(4) 0.2783(4) 0.048(2) Uani 1 1 d . . . H3A H 0.4588 0.7071 0.3083 0.057 Uiso 1 1 calc R . . H3B H 0.5628 0.7162 0.2497 0.057 Uiso 1 1 calc R . . C3 C 0.5916(12) 0.8902(8) 0.4077(10) 0.102(6) Uani 1 1 d . . . H3 H 0.6141 0.9234 0.4345 0.122 Uiso 1 1 calc R . . Co4 Co 0.63491(11) 0.27075(8) 0.26735(8) 0.0459(4) Uani 1 1 d . . . Cl4 Cl 0.7979(3) 0.05734(19) 0.11850(18) 0.0584(9) Uani 1 1 d DU . . N4 N 0.0763(7) 0.6668(5) 0.2682(6) 0.095(4) Uani 1 1 d . . . H4A H 0.0726 0.6612 0.2213 0.114 Uiso 1 1 calc R . . H4B H 0.1264 0.6298 0.2772 0.114 Uiso 1 1 calc R . . C4S C 0.6106(9) 0.6209(6) 0.0221(6) 0.087(5) Uani 1 1 d . . . H4S1 H 0.6514 0.5814 0.0444 0.131 Uiso 1 1 calc R . . H4S2 H 0.6603 0.6451 -0.0211 0.131 Uiso 1 1 calc R . . H4S3 H 0.5572 0.5992 0.0062 0.131 Uiso 1 1 calc R . . O4 O 0.1161(5) 0.8162(4) 0.3702(3) 0.0432(19) Uani 1 1 d . . . C4 C 0.5291(11) 0.8329(8) 0.4467(7) 0.087(5) Uani 1 1 d . . . H4 H 0.5074 0.8285 0.4996 0.105 Uiso 1 1 calc R . . O5 O 0.8786(5) 0.3626(4) 0.0995(4) 0.050(2) Uani 1 1 d . . . N5 N 1.0170(7) 0.3893(4) 0.1794(4) 0.039(2) Uani 1 1 d . . . Cl5 Cl 0.3158(4) 0.5779(2) 0.4007(2) 0.0865(12) Uani 1 1 d DU . . C5 C 0.4985(9) 0.7813(7) 0.4056(7) 0.069(4) Uani 1 1 d . . . H5 H 0.4577 0.7420 0.4313 0.083 Uiso 1 1 calc R . . O6 O 0.6423(6) 0.3345(4) 0.1653(4) 0.067(2) Uani 1 1 d . . . N6 N 0.4677(7) 0.3256(5) 0.2939(5) 0.056(3) Uani 1 1 d . . . Cl6 Cl 0.8148(4) 0.0771(2) 0.4008(2) 0.0856(12) Uani 1 1 d DU . . C6 C 0.5296(8) 0.7890(6) 0.3259(6) 0.044(3) Uani 1 1 d . . . O7 O 0.7959(5) 0.3916(3) 0.2749(4) 0.0445(19) Uani 1 1 d . . . N7 N 1.0001(6) 0.2422(4) 0.2803(4) 0.042(2) Uani 1 1 d . . . H7NA H 0.9572 0.2091 0.3118 0.051 Uiso 1 1 calc R . . H7NB H 1.0615 0.2152 0.2525 0.051 Uiso 1 1 calc R . . C7 C 0.6182(8) 0.8658(5) 0.2059(6) 0.049(3) Uani 1 1 d . . . H7A H 0.6594 0.8209 0.1804 0.058 Uiso 1 1 calc R . . H7B H 0.6655 0.9066 0.1915 0.058 Uiso 1 1 calc R . . O8 O 0.6179(5) 0.3159(4) 0.3707(4) 0.049(2) Uani 1 1 d . . . N8 N 0.5792(7) 0.1660(5) 0.2670(6) 0.101(5) Uani 1 1 d . . . H8NA H 0.5731 0.1623 0.2204 0.121 Uiso 1 1 calc R . . H8NB H 0.6328 0.1299 0.2723 0.121 Uiso 1 1 calc R . . C8 C 0.5522(9) 0.9000(5) 0.0944(5) 0.054(3) Uani 1 1 d . . . H8A H 0.5972 0.9420 0.0795 0.064 Uiso 1 1 calc R . . H8B H 0.5977 0.8547 0.0725 0.064 Uiso 1 1 calc R . . O9 O 0.2494(7) 0.1781(5) 0.2002(5) 0.105(3) Uani 1 1 d . A . C9 C 0.4588(9) 0.9160(6) 0.0616(6) 0.057(3) Uani 1 1 d . . . H9A H 0.4244 0.9677 0.0708 0.068 Uiso 1 1 calc R . . H9B H 0.4850 0.9101 0.0072 0.068 Uiso 1 1 calc R . . O10 O 0.3087(9) 0.2246(6) 0.0759(6) 0.142(4) Uani 1 1 d . A . C10 C 0.3003(11) 0.8672(6) 0.0608(6) 0.090(5) Uani 1 1 d . . . H10A H 0.3359 0.8578 0.0074 0.108 Uiso 1 1 calc R . . H10B H 0.2620 0.9182 0.0637 0.108 Uiso 1 1 calc R . . O11 O 0.3186(9) 0.0984(5) 0.1000(5) 0.126(4) Uani 1 1 d . A . C11 C 0.2192(10) 0.8116(6) 0.0945(6) 0.079(4) Uani 1 1 d . . . H11A H 0.1790 0.8058 0.0593 0.095 Uiso 1 1 calc R . . H11B H 0.2579 0.7625 0.1027 0.095 Uiso 1 1 calc R . . O12A O 0.4354(17) 0.1939(16) 0.1213(19) 0.144(12) Uani 0.44(4) 1 d PDU A 1 O12B O 0.4324(15) 0.1470(15) 0.1445(16) 0.095(8) Uani 0.56(4) 1 d PDU A 2 C12 C 0.0380(10) 0.8776(7) 0.1630(7) 0.083(4) Uani 1 1 d . . . H12A H -0.0007 0.8479 0.1403 0.100 Uiso 1 1 calc R . . H12B H 0.0513 0.9251 0.1329 0.100 Uiso 1 1 calc R . . O13A O 0.9377(11) 0.672(3) 0.1299(16) 0.118(12) Uani 0.68(6) 1 d PDU B 1 O13B O 0.921(3) 0.630(2) 0.148(3) 0.121(13) Uani 0.32(6) 1 d PDU B 2 C13 C -0.0279(9) 0.8926(7) 0.2432(7) 0.079(4) Uani 1 1 d . . . H13A H 0.0041 0.9311 0.2608 0.095 Uiso 1 1 calc R . . H13B H -0.1022 0.9130 0.2444 0.095 Uiso 1 1 calc R . . O14 O 0.8188(9) 0.6001(6) 0.0985(6) 0.131(4) Uani 1 1 d . B . C14 C -0.0707(8) 0.8449(6) 0.3770(6) 0.055(3) Uani 1 1 d . . . H14A H -0.0953 0.8006 0.4096 0.066 Uiso 1 1 calc R . . H14B H -0.1324 0.8843 0.3852 0.066 Uiso 1 1 calc R . . O15 O 0.7489(7) 0.6781(5) 0.2009(4) 0.099(3) Uani 1 1 d . B . C15 C 0.0218(9) 0.8726(6) 0.3971(6) 0.066(4) Uani 1 1 d . . . H15A H 0.0376 0.9222 0.3724 0.080 Uiso 1 1 calc R . . H15B H 0.0029 0.8762 0.4517 0.080 Uiso 1 1 calc R . . O16 O 0.8122(10) 0.7239(6) 0.0775(6) 0.166(6) Uani 1 1 d . B . C16 C 0.2127(8) 0.8259(5) 0.3931(5) 0.044(3) Uani 1 1 d . . . H16A H 0.2658 0.7814 0.3803 0.053 Uiso 1 1 calc R . . H16B H 0.1903 0.8292 0.4479 0.053 Uiso 1 1 calc R . . O17A O 0.3096(15) 0.5795(9) 0.1844(8) 0.143(7) Uani 0.680(13) 1 d PDU C 1 O18A O 0.1860(9) 0.5625(10) 0.1223(9) 0.127(6) Uani 0.680(13) 1 d PDU C 1 O19A O 0.3533(13) 0.6011(13) 0.0557(10) 0.169(8) Uani 0.680(13) 1 d PDU C 1 O20A O 0.3474(15) 0.4850(7) 0.1079(8) 0.142(6) Uani 0.680(13) 1 d PDU C 1 O17B O 0.219(3) 0.5336(19) 0.1833(15) 0.154(12) Uani 0.320(13) 1 d PDU C 2 O18B O 0.382(3) 0.547(2) 0.150(2) 0.176(13) Uani 0.320(13) 1 d PDU C 2 O19B O 0.280(3) 0.6310(8) 0.0958(17) 0.109(11) Uani 0.320(13) 1 d PDU C 2 O20B O 0.272(3) 0.5136(13) 0.0694(16) 0.144(11) Uani 0.320(13) 1 d PDU C 2 C17 C 0.2664(8) 0.8942(5) 0.3566(5) 0.046(3) Uani 1 1 d . . . H17A H 0.2162 0.9395 0.3727 0.055 Uiso 1 1 calc R . . H17B H 0.3315 0.8965 0.3719 0.055 Uiso 1 1 calc R . . C18 C 0.3342(9) 0.9620(5) 0.2341(5) 0.052(3) Uani 1 1 d . . . H18A H 0.2979 1.0046 0.2650 0.062 Uiso 1 1 calc R . . H18B H 0.3145 0.9688 0.1873 0.062 Uiso 1 1 calc R . . C19 C 0.4572(8) 0.9597(5) 0.2161(6) 0.049(3) Uani 1 1 d . . . H19A H 0.4823 1.0032 0.1823 0.058 Uiso 1 1 calc R . . H19B H 0.4748 0.9638 0.2628 0.058 Uiso 1 1 calc R . . C20 C -0.1118(10) 0.7767(7) 0.2822(7) 0.074(4) Uani 1 1 d . . . H20A H -0.1841 0.8053 0.2923 0.089 Uiso 1 1 calc R . . H20B H -0.0866 0.7653 0.2289 0.089 Uiso 1 1 calc R . . O21A O 0.6853(10) 0.0800(15) 0.1328(10) 0.138(8) Uani 0.553(18) 1 d PDU D 1 O22A O 0.834(2) 0.0772(9) 0.1787(11) 0.119(7) Uani 0.553(18) 1 d PDU D 1 O23A O 0.8545(17) 0.0963(16) 0.0515(10) 0.150(9) Uani 0.553(18) 1 d PDU D 1 O24A O 0.8228(15) -0.0203(6) 0.1144(13) 0.124(7) Uani 0.553(18) 1 d PDU D 1 O21B O 0.715(2) 0.0326(15) 0.0962(17) 0.140(10) Uani 0.447(18) 1 d PDU D 2 O22B O 0.755(3) 0.0421(18) 0.1968(8) 0.166(12) Uani 0.447(18) 1 d PDU D 2 O23B O 0.809(2) 0.1318(8) 0.1004(18) 0.146(11) Uani 0.447(18) 1 d PDU D 2 O24B O 0.8898(18) 0.0092(16) 0.0922(17) 0.169(11) Uani 0.447(18) 1 d PDU D 2 C21 C -0.1220(9) 0.7043(7) 0.3292(7) 0.056(3) Uani 1 1 d . . . C22 C -0.2183(8) 0.6814(7) 0.3797(6) 0.073(4) Uani 1 1 d . . . H22 H -0.2833 0.7135 0.3856 0.087 Uiso 1 1 calc R . . C23 C -0.2225(11) 0.6136(7) 0.4215(6) 0.076(4) Uani 1 1 d . . . H23 H -0.2895 0.6012 0.4551 0.091 Uiso 1 1 calc R . . C24 C -0.1299(11) 0.5640(6) 0.4147(6) 0.072(4) Uani 1 1 d . . . H24 H -0.1328 0.5176 0.4427 0.087 Uiso 1 1 calc R . . O25 O 0.3453(11) 0.5302(6) 0.4583(7) 0.190(6) Uani 1 1 d . E . C25 C -0.0325(9) 0.5844(7) 0.3652(7) 0.071(4) Uani 1 1 d . . . H25 H 0.0323 0.5521 0.3599 0.085 Uiso 1 1 calc R . . O26A O 0.248(2) 0.6379(15) 0.4384(16) 0.189(11) Uani 0.523(19) 1 d PDU E 1 O28A O 0.2601(15) 0.5254(10) 0.3796(11) 0.130(8) Uani 0.523(19) 1 d PDU E 1 O26B O 0.339(2) 0.6496(9) 0.4088(12) 0.116(9) Uani 0.477(19) 1 d PDU E 2 O28B O 0.2126(16) 0.600(2) 0.3857(17) 0.219(13) Uani 0.477(19) 1 d PDU E 2 C26 C -0.0303(9) 0.6543(7) 0.3226(6) 0.061(4) Uani 1 1 d . . . C27 C 1.0897(8) 0.3517(6) 0.2885(7) 0.054(3) Uani 1 1 d . . . O27 O 0.4077(13) 0.5770(7) 0.3348(6) 0.225(7) Uani 1 1 d . E . C28 C 1.1207(9) 0.3981(6) 0.3337(7) 0.066(4) Uani 1 1 d . . . H28 H 1.1635 0.4373 0.3108 0.079 Uiso 1 1 calc R . . C29 C 1.0878(11) 0.3860(7) 0.4129(7) 0.086(5) Uani 1 1 d . . . H29 H 1.1077 0.4178 0.4423 0.104 Uiso 1 1 calc R . . O29A O 0.821(3) 0.1474(10) 0.4187(15) 0.112(12) Uani 0.41(3) 1 d PDU F 1 O29B O 0.752(2) 0.1420(11) 0.4187(18) 0.255(16) Uani 0.59(3) 1 d PDU F 2 C30 C 1.0259(12) 0.3270(8) 0.4478(8) 0.096(5) Uani 1 1 d . . . H30 H 1.0032 0.3200 0.5005 0.116 Uiso 1 1 calc R . . O30 O 0.9099(11) 0.0818(9) 0.3464(9) 0.260(9) Uani 1 1 d . F . C31 C 0.9975(9) 0.2783(7) 0.4040(6) 0.065(4) Uani 1 1 d . . . H31 H 0.9571 0.2379 0.4267 0.078 Uiso 1 1 calc R . . O31 O 0.7559(15) 0.0394(11) 0.3773(9) 0.301(11) Uani 1 1 d . F . C32 C 1.0311(8) 0.2918(6) 0.3255(6) 0.048(3) Uani 1 1 d . . . O32 O 0.8357(13) 0.0319(7) 0.4628(6) 0.225(8) Uani 1 1 d . F . C33 C 1.1166(8) 0.3672(6) 0.2038(6) 0.051(3) Uani 1 1 d . . . H33A H 1.1643 0.4077 0.1881 0.061 Uiso 1 1 calc R . . H33B H 1.1566 0.3220 0.1785 0.061 Uiso 1 1 calc R . . C34 C 1.0552(9) 0.3993(6) 0.0939(6) 0.057(3) Uani 1 1 d . . . H34A H 1.1006 0.4411 0.0785 0.069 Uiso 1 1 calc R . . H34B H 1.0999 0.3535 0.0729 0.069 Uiso 1 1 calc R . . C35 C 0.9595(10) 0.4151(6) 0.0633(6) 0.064(4) Uani 1 1 d . . . H35A H 0.9262 0.4670 0.0727 0.077 Uiso 1 1 calc R . . H35B H 0.9846 0.4097 0.0087 0.077 Uiso 1 1 calc R . . C36 C 0.7981(8) 0.3653(7) 0.0589(5) 0.075(4) Uani 1 1 d . . . H36A H 0.7616 0.4166 0.0584 0.090 Uiso 1 1 calc R . . H36B H 0.8360 0.3531 0.0066 0.090 Uiso 1 1 calc R . . C37 C 0.7165(9) 0.3135(7) 0.0923(5) 0.086(5) Uani 1 1 d . . . H37A H 0.7537 0.2632 0.0979 0.104 Uiso 1 1 calc R . . H37B H 0.6739 0.3108 0.0578 0.104 Uiso 1 1 calc R . . C38 C 0.5421(11) 0.3784(7) 0.1610(7) 0.089(5) Uani 1 1 d . . . H38A H 0.5019 0.3496 0.1386 0.107 Uiso 1 1 calc R . . H38B H 0.5582 0.4251 0.1302 0.107 Uiso 1 1 calc R . . C39 C 0.4752(10) 0.3957(6) 0.2415(7) 0.077(4) Uani 1 1 d . . . H39A H 0.5089 0.4331 0.2593 0.092 Uiso 1 1 calc R . . H39B H 0.4015 0.4175 0.2423 0.092 Uiso 1 1 calc R . . C40 C 0.4313(9) 0.3459(6) 0.3755(7) 0.069(4) Uani 1 1 d . . . H40A H 0.4049 0.3019 0.4081 0.082 Uiso 1 1 calc R . . H40B H 0.3709 0.3862 0.3837 0.082 Uiso 1 1 calc R . . C41 C 0.5256(8) 0.3717(6) 0.3966(6) 0.058(3) Uani 1 1 d . . . H41A H 0.5429 0.4212 0.3721 0.070 Uiso 1 1 calc R . . H41B H 0.5061 0.3752 0.4512 0.070 Uiso 1 1 calc R . . C42 C 0.7130(8) 0.3259(6) 0.3943(5) 0.053(3) Uani 1 1 d . . . H42A H 0.7658 0.2810 0.3828 0.064 Uiso 1 1 calc R . . H42B H 0.6894 0.3304 0.4489 0.064 Uiso 1 1 calc R . . C43 C 0.7685(8) 0.3940(5) 0.3566(5) 0.047(3) Uani 1 1 d . . . H43A H 0.7200 0.4398 0.3735 0.057 Uiso 1 1 calc R . . H43B H 0.8351 0.3951 0.3705 0.057 Uiso 1 1 calc R . . C44 C 0.8309(7) 0.4620(5) 0.2339(5) 0.045(3) Uani 1 1 d . . . H44A H 0.7940 0.5049 0.2643 0.054 Uiso 1 1 calc R . . H44B H 0.8117 0.4680 0.1869 0.054 Uiso 1 1 calc R . . C45 C 0.9565(8) 0.4600(5) 0.2162(5) 0.047(3) Uani 1 1 d . . . H45A H 0.9817 0.5037 0.1829 0.057 Uiso 1 1 calc R . . H45B H 0.9735 0.4635 0.2632 0.057 Uiso 1 1 calc R . . C46 C 0.3895(9) 0.2748(7) 0.2815(7) 0.072(4) Uani 1 1 d . . . H46A H 0.4117 0.2644 0.2280 0.086 Uiso 1 1 calc R . . H46B H 0.3159 0.3017 0.2943 0.086 Uiso 1 1 calc R . . C47 C 0.3861(9) 0.1997(6) 0.3285(6) 0.053(3) Uani 1 1 d . . . C48 C 0.2851(11) 0.1832(7) 0.3778(7) 0.078(4) Uani 1 1 d . . . H48 H 0.2240 0.2186 0.3813 0.094 Uiso 1 1 calc R . . C49 C 0.2717(10) 0.1167(9) 0.4217(8) 0.086(5) Uani 1 1 d . . . H49 H 0.2025 0.1062 0.4536 0.103 Uiso 1 1 calc R . . C50 C 0.3637(12) 0.0658(7) 0.4174(7) 0.083(5) Uani 1 1 d . . . H50 H 0.3566 0.0205 0.4472 0.099 Uiso 1 1 calc R . . C51 C 0.4664(11) 0.0806(6) 0.3694(7) 0.077(4) Uani 1 1 d . . . H51 H 0.5283 0.0468 0.3689 0.092 Uiso 1 1 calc R . . C52 C 0.4762(8) 0.1461(6) 0.3223(7) 0.058(3) 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 N1S 0.059(7) 0.050(7) 0.051(7) -0.013(5) -0.008(5) -0.010(5) C1S 0.042(7) 0.054(8) 0.056(8) -0.017(6) -0.004(6) -0.001(6) Cl1 0.068(3) 0.073(3) 0.054(2) -0.011(2) -0.013(2) 0.020(2) O1W 0.043(5) 0.033(4) 0.056(5) -0.007(3) -0.014(4) -0.008(3) Co1 0.0361(9) 0.0372(9) 0.0371(9) -0.0043(7) -0.0069(7) -0.0073(7) O1 0.063(6) 0.065(6) 0.038(5) 0.000(4) -0.022(4) -0.008(4) N1 0.043(6) 0.032(6) 0.050(6) -0.005(5) 0.000(5) -0.004(4) C1 0.041(7) 0.060(8) 0.046(7) -0.014(6) -0.017(6) 0.006(6) O2W 0.035(4) 0.035(4) 0.050(4) -0.008(3) -0.002(4) -0.009(3) N2S 0.046(6) 0.051(7) 0.050(6) -0.014(5) -0.007(5) -0.001(5) Cl2 0.071(3) 0.068(3) 0.056(2) -0.0110(19) -0.017(2) 0.016(2) C2S 0.073(9) 0.080(10) 0.081(9) -0.030(7) -0.019(7) -0.003(7) Co2 0.0401(10) 0.0506(10) 0.0431(10) -0.0074(8) -0.0079(8) -0.0061(8) O2 0.062(6) 0.103(7) 0.036(5) 0.006(4) -0.011(4) -0.006(5) N2 0.052(7) 0.054(7) 0.063(7) 0.014(5) -0.024(5) -0.005(5) C2 0.076(10) 0.055(9) 0.090(11) -0.021(8) -0.040(9) 0.012(7) Co3 0.0364(9) 0.0366(9) 0.0349(9) -0.0023(7) -0.0064(7) -0.0073(7) Cl3 0.065(2) 0.052(2) 0.057(2) -0.0080(16) -0.0179(18) -0.0076(16) C3S 0.055(8) 0.054(9) 0.064(9) -0.003(7) -0.017(7) -0.026(6) O3 0.047(5) 0.043(5) 0.031(4) -0.007(3) -0.007(4) -0.004(4) N3 0.047(6) 0.048(6) 0.052(6) -0.002(5) -0.018(5) -0.015(5) C3 0.106(13) 0.082(11) 0.144(15) -0.032(11) -0.071(12) -0.004(9) Co4 0.0406(10) 0.0507(10) 0.0453(10) -0.0070(8) -0.0102(8) -0.0053(8) Cl4 0.063(2) 0.058(2) 0.055(2) -0.0074(16) -0.0160(18) -0.0117(17) N4 0.063(8) 0.065(8) 0.135(10) -0.045(7) 0.015(7) -0.017(6) C4S 0.090(10) 0.073(9) 0.086(10) -0.057(8) 0.010(8) -0.018(8) O4 0.040(5) 0.050(5) 0.037(4) -0.006(3) -0.006(4) -0.008(4) C4 0.103(12) 0.113(12) 0.049(8) -0.035(8) -0.040(8) 0.043(9) O5 0.045(5) 0.056(5) 0.047(5) 0.006(4) -0.012(4) -0.013(4) N5 0.039(6) 0.036(6) 0.042(6) -0.002(4) -0.012(5) -0.007(4) Cl5 0.132(4) 0.056(3) 0.066(3) 0.000(2) -0.016(2) -0.023(2) C5 0.061(9) 0.073(9) 0.061(9) 0.018(7) -0.014(7) 0.006(7) O6 0.057(6) 0.091(7) 0.059(6) 0.009(5) -0.029(5) -0.010(5) N6 0.048(6) 0.064(7) 0.056(6) -0.010(5) -0.013(5) -0.006(5) Cl6 0.124(4) 0.056(2) 0.070(3) -0.006(2) -0.009(2) -0.034(2) C6 0.029(6) 0.055(7) 0.039(7) 0.012(5) -0.006(5) 0.002(5) O7 0.048(5) 0.039(5) 0.041(5) -0.007(4) -0.004(4) -0.003(4) N7 0.038(5) 0.038(5) 0.046(5) 0.008(4) -0.008(4) -0.003(4) C7 0.030(7) 0.039(7) 0.072(9) -0.005(6) -0.009(6) -0.006(5) O8 0.034(5) 0.057(5) 0.050(5) -0.016(4) -0.004(4) 0.003(4) N8 0.057(7) 0.083(8) 0.136(10) -0.063(7) 0.036(7) -0.030(6) C8 0.067(9) 0.043(7) 0.039(7) -0.001(5) 0.006(7) -0.020(6) O9 0.088(8) 0.149(10) 0.065(7) -0.032(6) -0.009(6) 0.017(6) C9 0.063(8) 0.055(8) 0.044(8) 0.013(6) -0.004(7) -0.018(6) O10 0.155(11) 0.111(9) 0.119(9) 0.053(7) -0.014(8) 0.026(7) C10 0.121(12) 0.071(8) 0.055(8) 0.010(6) 0.004(8) -0.017(7) O11 0.173(11) 0.079(7) 0.105(8) -0.026(6) -0.020(7) 0.018(7) C11 0.128(12) 0.071(8) 0.054(8) 0.002(6) -0.051(8) -0.015(7) O12A 0.060(12) 0.27(3) 0.096(19) -0.06(2) -0.003(12) -0.018(17) O12B 0.071(10) 0.102(18) 0.114(17) -0.023(12) -0.039(11) 0.022(9) C12 0.074(10) 0.106(12) 0.076(10) 0.032(8) -0.042(8) -0.013(8) O13A 0.052(7) 0.19(3) 0.107(16) -0.046(16) -0.024(9) 0.023(10) O13B 0.087(18) 0.057(18) 0.19(3) 0.058(19) -0.033(17) 0.032(13) C13 0.051(8) 0.093(11) 0.087(10) -0.006(8) -0.016(7) 0.002(7) O14 0.148(10) 0.109(9) 0.136(9) -0.054(7) -0.035(8) -0.003(7) C14 0.043(7) 0.069(9) 0.052(7) -0.012(6) -0.011(6) -0.003(6) O15 0.078(7) 0.138(9) 0.060(6) -0.024(6) 0.000(5) 0.021(6) C15 0.055(9) 0.052(8) 0.084(10) -0.030(7) -0.010(7) 0.011(6) O16 0.175(12) 0.111(9) 0.153(11) 0.069(8) 0.000(9) 0.020(8) C16 0.053(8) 0.045(7) 0.033(7) -0.003(5) -0.012(6) -0.006(6) O17A 0.186(15) 0.128(12) 0.137(10) -0.101(9) -0.091(10) 0.067(11) O18A 0.061(6) 0.191(15) 0.125(13) 0.048(10) -0.032(7) -0.022(7) O19A 0.093(12) 0.255(17) 0.173(13) 0.135(15) -0.071(11) -0.093(13) O20A 0.204(15) 0.091(8) 0.134(11) -0.077(7) -0.072(11) 0.081(9) O17B 0.20(2) 0.13(2) 0.106(15) -0.019(15) 0.034(17) -0.09(2) O18B 0.153(18) 0.20(3) 0.20(3) 0.05(2) -0.123(18) 0.02(2) O19B 0.21(3) 0.039(8) 0.13(2) 0.006(10) -0.12(2) -0.017(13) O20B 0.27(3) 0.057(12) 0.127(16) -0.076(13) -0.085(18) 0.039(16) C17 0.047(7) 0.052(8) 0.040(7) -0.011(6) -0.014(6) -0.003(6) C18 0.066(9) 0.043(8) 0.046(7) -0.005(6) -0.015(6) -0.004(6) C19 0.051(8) 0.034(7) 0.062(8) -0.003(6) -0.018(6) -0.008(6) C20 0.053(9) 0.103(12) 0.074(10) 0.004(8) -0.032(8) -0.009(8) O21A 0.064(7) 0.24(2) 0.091(11) -0.080(12) -0.005(7) 0.049(10) O22A 0.23(2) 0.068(10) 0.111(11) 0.006(8) -0.116(14) -0.034(11) O23A 0.107(14) 0.24(2) 0.109(11) 0.107(15) -0.053(11) -0.077(16) O24A 0.095(11) 0.068(7) 0.199(17) -0.054(9) -0.010(12) -0.029(7) O21B 0.134(15) 0.134(18) 0.19(2) 0.055(15) -0.091(16) -0.105(14) O22B 0.23(3) 0.17(2) 0.055(8) 0.003(11) -0.017(10) 0.068(18) O23B 0.16(2) 0.066(8) 0.22(3) 0.012(12) -0.06(2) -0.072(11) O24B 0.088(12) 0.159(18) 0.21(2) -0.08(2) 0.020(14) 0.033(13) C21 0.031(6) 0.073(8) 0.068(8) -0.017(7) -0.024(6) 0.008(5) C22 0.020(6) 0.106(11) 0.083(10) -0.003(8) -0.003(6) -0.012(6) C23 0.078(10) 0.093(11) 0.048(8) -0.010(7) 0.006(7) -0.035(8) C24 0.103(11) 0.056(8) 0.064(8) -0.026(6) -0.029(8) -0.004(7) O25 0.201(13) 0.133(10) 0.193(13) 0.055(9) -0.040(10) 0.039(9) C25 0.041(7) 0.076(10) 0.101(10) -0.044(8) -0.015(7) -0.007(6) O26A 0.22(2) 0.159(17) 0.20(2) -0.137(16) -0.081(18) 0.061(15) O28A 0.122(14) 0.106(13) 0.159(17) -0.073(11) -0.009(12) -0.035(10) O26B 0.19(2) 0.063(10) 0.120(16) 0.040(10) -0.064(14) -0.070(13) O28B 0.130(16) 0.35(4) 0.22(2) -0.02(3) -0.093(17) -0.069(17) C26 0.054(8) 0.070(8) 0.063(8) -0.014(6) -0.006(6) -0.042(6) C27 0.033(7) 0.050(8) 0.087(10) -0.016(7) -0.030(7) 0.005(6) O27 0.306(18) 0.195(13) 0.098(7) -0.021(8) 0.059(9) -0.049(12) C28 0.056(8) 0.069(9) 0.089(10) -0.020(8) -0.047(8) 0.003(7) C29 0.115(12) 0.093(11) 0.078(9) -0.048(8) -0.077(9) 0.045(9) O29A 0.24(3) 0.049(11) 0.081(16) 0.001(11) -0.084(19) -0.038(16) O29B 0.37(3) 0.089(15) 0.22(3) -0.026(15) -0.01(3) 0.087(17) C30 0.115(14) 0.112(13) 0.072(10) -0.014(9) -0.055(10) 0.025(10) O30 0.158(12) 0.227(16) 0.34(2) 0.031(14) 0.031(13) -0.115(11) C31 0.053(8) 0.090(10) 0.055(8) -0.010(7) -0.026(7) 0.011(7) O31 0.34(2) 0.38(2) 0.245(17) -0.124(16) -0.066(15) -0.226(19) C32 0.036(7) 0.057(8) 0.056(8) -0.021(6) -0.023(6) 0.008(6) O32 0.37(2) 0.186(13) 0.103(9) 0.078(9) -0.046(11) -0.089(12) C33 0.044(8) 0.052(8) 0.054(8) -0.003(6) -0.010(6) -0.011(6) C34 0.051(8) 0.054(8) 0.055(8) 0.009(6) 0.001(7) -0.016(6) C35 0.080(10) 0.064(9) 0.032(7) 0.003(6) 0.002(7) -0.005(7) C36 0.048(6) 0.149(11) 0.042(7) -0.001(7) -0.032(6) -0.020(7) C37 0.070(8) 0.166(13) 0.025(6) -0.014(7) -0.004(6) -0.045(8) C38 0.073(11) 0.110(13) 0.076(11) 0.032(9) -0.024(9) -0.001(9) C39 0.078(10) 0.057(8) 0.092(10) 0.027(7) -0.034(8) 0.003(7) C40 0.040(8) 0.068(9) 0.086(10) -0.011(7) -0.006(7) 0.010(6) C41 0.046(8) 0.066(9) 0.053(7) -0.012(6) 0.000(6) -0.003(6) C42 0.043(7) 0.079(9) 0.040(7) -0.004(6) -0.014(6) -0.013(6) C43 0.054(8) 0.048(8) 0.038(7) -0.009(6) -0.008(6) -0.010(6) C44 0.042(7) 0.029(6) 0.053(7) 0.006(5) -0.003(6) 0.003(5) C45 0.051(8) 0.035(7) 0.049(7) -0.006(5) -0.005(6) -0.002(6) C46 0.047(8) 0.093(11) 0.081(10) 0.010(8) -0.032(8) -0.011(7) C47 0.046(7) 0.077(9) 0.041(6) 0.001(6) -0.012(5) -0.028(6) C48 0.069(10) 0.087(11) 0.075(10) -0.008(8) -0.014(8) -0.009(8) C49 0.045(8) 0.124(14) 0.083(11) -0.031(10) 0.002(8) -0.022(8) C50 0.102(11) 0.096(11) 0.063(9) -0.004(7) -0.019(8) -0.068(9) C51 0.095(11) 0.040(7) 0.104(11) -0.017(7) -0.038(9) -0.009(7) C52 0.029(6) 0.057(7) 0.082(8) -0.043(6) -0.005(5) 0.010(5) _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 N1S C3S 1.137(11) . ? N1S Co1 2.132(8) . ? C1S N2S 1.106(10) . ? C1S C2S 1.472(12) . ? Cl1 O10 1.391(9) . ? Cl1 O9 1.418(8) . ? Cl1 O11 1.429(9) . ? Cl1 O12B 1.436(13) . ? Cl1 O12A 1.448(15) . ? O1W Co2 1.933(6) . ? O1W Co1 1.946(6) . ? O1W H1W 0.8583 . ? Co1 N1 2.133(7) . ? Co1 N3 2.153(8) . ? Co1 O3 2.274(6) . ? Co1 O1 2.279(7) . ? O1 C10 1.417(14) . ? O1 C9 1.432(11) . ? N1 C19 1.497(10) . ? N1 C8 1.504(11) . ? N1 C7 1.515(11) . ? C1 C6 1.385(13) . ? C1 C2 1.389(14) . ? C1 C7 1.502(13) . ? O2W Co4 1.928(6) . ? O2W Co3 1.941(6) . ? O2W H2W 0.8528 . ? N2S Co3 2.138(8) . ? Cl2 O16 1.365(10) . ? Cl2 O13B 1.396(19) . ? Cl2 O13A 1.398(14) . ? Cl2 O14 1.414(8) . ? Cl2 O15 1.423(7) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? Co2 O4 2.069(6) . ? Co2 N4 2.079(8) . ? Co2 O2 2.087(7) . ? Co2 N2 2.177(9) . ? O2 C11 1.454(11) . ? O2 C12 1.455(12) . ? N2 C13 1.477(13) . ? N2 C14 1.476(11) . ? N2 C20 1.494(13) . ? C2 C3 1.319(16) . ? C2 H2 0.9300 . ? Co3 N5 2.144(7) . ? Co3 N7 2.173(7) . ? Co3 O5 2.280(7) . ? Co3 O7 2.284(6) . ? Cl3 O19B 1.348(13) . ? Cl3 O20A 1.359(9) . ? Cl3 O18B 1.374(14) . ? Cl3 O17B 1.377(14) . ? Cl3 O20B 1.376(13) . ? Cl3 O19A 1.384(10) . ? Cl3 O17A 1.389(9) . ? Cl3 O18A 1.396(10) . ? C3S C4S 1.464(13) . ? O3 C17 1.447(9) . ? O3 C18 1.455(10) . ? N3 C6 1.432(11) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? C3 C4 1.383(17) . ? C3 H3 0.9300 . ? Co4 N8 2.078(8) . ? Co4 O8 2.082(6) . ? Co4 O6 2.095(7) . ? Co4 N6 2.165(9) . ? Cl4 O23B 1.347(12) . ? Cl4 O24B 1.348(12) . ? Cl4 O24A 1.377(11) . ? Cl4 O21B 1.387(12) . ? Cl4 O22B 1.396(12) . ? Cl4 O21A 1.397(11) . ? Cl4 O23A 1.399(11) . ? Cl4 O22A 1.423(10) . ? N4 C26 1.453(12) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? C4S H4S1 0.9600 . ? C4S H4S2 0.9600 . ? C4S H4S3 0.9600 . ? O4 C15 1.455(10) . ? O4 C16 1.465(10) . ? C4 C5 1.408(15) . ? C4 H4 0.9300 . ? O5 C36 1.451(10) . ? O5 C35 1.448(11) . ? N5 C33 1.481(11) . ? N5 C45 1.489(10) . ? N5 C34 1.504(11) . ? Cl5 O26B 1.377(12) . ? Cl5 O26A 1.377(13) . ? Cl5 O28A 1.394(12) . ? Cl5 O27 1.408(11) . ? Cl5 O25 1.415(11) . ? Cl5 O28B 1.437(15) . ? C5 C6 1.401(13) . ? C5 H5 0.9300 . ? O6 C38 1.436(12) . ? O6 C37 1.440(10) . ? N6 C40 1.500(12) . ? N6 C39 1.501(12) . ? N6 C46 1.514(12) . ? Cl6 O31 1.265(11) . ? Cl6 O30 1.325(12) . ? Cl6 O29B 1.323(13) . ? Cl6 O29A 1.338(14) . ? Cl6 O32 1.415(11) . ? O7 C43 1.446(9) . ? O7 C44 1.450(9) . ? N7 C32 1.439(11) . ? N7 H7NA 0.9000 . ? N7 H7NB 0.9000 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? O8 C41 1.430(10) . ? O8 C42 1.455(11) . ? N8 C52 1.460(12) . ? N8 H8NA 0.9000 . ? N8 H8NB 0.9000 . ? C8 C9 1.490(14) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.483(14) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.492(14) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.501(13) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.475(11) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.505(13) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.480(14) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C26 1.360(15) . ? C21 C22 1.381(13) . ? C22 C23 1.366(15) . ? C22 H22 0.9300 . ? C23 C24 1.365(15) . ? C23 H23 0.9300 . ? C24 C25 1.369(14) . ? C24 H24 0.9300 . ? C25 C26 1.407(15) . ? C25 H25 0.9300 . ? C27 C32 1.385(13) . ? C27 C28 1.399(13) . ? C27 C33 1.504(14) . ? C28 C29 1.398(14) . ? C28 H28 0.9300 . ? C29 C30 1.383(17) . ? C29 H29 0.9300 . ? C30 C31 1.391(15) . ? C30 H30 0.9300 . ? C31 C32 1.389(13) . ? C31 H31 0.9300 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.493(14) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.437(13) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.506(14) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.517(13) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.487(11) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.538(12) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.523(14) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.382(14) . ? C47 C52 1.382(14) . ? C48 C49 1.368(16) . ? C48 H48 0.9300 . ? C49 C50 1.377(17) . ? C49 H49 0.9300 . ? C50 C51 1.383(15) . ? C50 H50 0.9300 . ? C51 C52 1.382(15) . ? C51 H51 0.9300 . ? 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 C3S N1S Co1 172.0(9) . . ? N2S C1S C2S 179.0(13) . . ? O10 Cl1 O9 109.8(6) . . ? O10 Cl1 O11 105.1(7) . . ? O9 Cl1 O11 108.9(6) . . ? O10 Cl1 O12B 127.2(13) . . ? O9 Cl1 O12B 105.2(12) . . ? O11 Cl1 O12B 99.3(12) . . ? O10 Cl1 O12A 92.3(13) . . ? O9 Cl1 O12A 114.8(14) . . ? O11 Cl1 O12A 123.5(14) . . ? Co2 O1W Co1 127.7(3) . . ? Co2 O1W H1W 105.7 . . ? Co1 O1W H1W 125.1 . . ? O1W Co1 N1S 93.1(3) . . ? O1W Co1 N1 166.4(3) . . ? N1S Co1 N1 99.7(3) . . ? O1W Co1 N3 95.7(3) . . ? N1S Co1 N3 85.1(3) . . ? N1 Co1 N3 89.9(3) . . ? O1W Co1 O3 87.1(2) . . ? N1S Co1 O3 170.9(3) . . ? N1 Co1 O3 79.5(3) . . ? N3 Co1 O3 103.9(3) . . ? O1W Co1 O1 100.8(3) . . ? N1S Co1 O1 82.8(3) . . ? N1 Co1 O1 76.6(3) . . ? N3 Co1 O1 160.0(3) . . ? O3 Co1 O1 88.3(2) . . ? C10 O1 C9 108.9(8) . . ? C10 O1 Co1 136.8(6) . . ? C9 O1 Co1 114.2(6) . . ? C19 N1 C8 110.6(8) . . ? C19 N1 C7 109.0(7) . . ? C8 N1 C7 109.7(8) . . ? C19 N1 Co1 111.5(6) . . ? C8 N1 Co1 104.2(6) . . ? C7 N1 Co1 111.7(6) . . ? C6 C1 C2 120.6(11) . . ? C6 C1 C7 121.6(9) . . ? C2 C1 C7 117.8(11) . . ? Co4 O2W Co3 128.1(3) . . ? Co4 O2W H2W 105.6 . . ? Co3 O2W H2W 124.8 . . ? C1S N2S Co3 173.6(9) . . ? O16 Cl2 O13B 137(2) . . ? O16 Cl2 O13A 105(2) . . ? O16 Cl2 O14 104.0(8) . . ? O13B Cl2 O14 89(2) . . ? O13A Cl2 O14 112.9(16) . . ? O16 Cl2 O15 110.0(6) . . ? O13B Cl2 O15 103(2) . . ? O13A Cl2 O15 113.7(9) . . ? O14 Cl2 O15 110.3(6) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? O1W Co2 O4 100.8(3) . . ? O1W Co2 N4 98.2(3) . . ? O4 Co2 N4 118.8(3) . . ? O1W Co2 O2 94.2(3) . . ? O4 Co2 O2 124.3(3) . . ? N4 Co2 O2 111.4(4) . . ? O1W Co2 N2 172.0(3) . . ? O4 Co2 N2 77.9(3) . . ? N4 Co2 N2 89.3(3) . . ? O2 Co2 N2 80.3(3) . . ? C11 O2 C12 116.5(9) . . ? C11 O2 Co2 120.7(7) . . ? C12 O2 Co2 115.6(6) . . ? C13 N2 C14 112.6(9) . . ? C13 N2 C20 107.3(10) . . ? C14 N2 C20 110.7(8) . . ? C13 N2 Co2 104.0(6) . . ? C14 N2 Co2 109.4(7) . . ? C20 N2 Co2 112.7(7) . . ? C3 C2 C1 121.8(14) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? O2W Co3 N2S 92.8(3) . . ? O2W Co3 N5 165.9(3) . . ? N2S Co3 N5 100.2(3) . . ? O2W Co3 N7 96.0(3) . . ? N2S Co3 N7 85.8(3) . . ? N5 Co3 N7 90.2(3) . . ? O2W Co3 O5 99.7(3) . . ? N2S Co3 O5 83.5(3) . . ? N5 Co3 O5 76.8(3) . . ? N7 Co3 O5 161.4(3) . . ? O2W Co3 O7 86.7(2) . . ? N2S Co3 O7 170.8(3) . . ? N5 Co3 O7 79.5(3) . . ? N7 Co3 O7 103.4(3) . . ? O5 Co3 O7 87.5(2) . . ? O19B Cl3 O20A 153.7(17) . . ? O19B Cl3 O18B 110(2) . . ? O20A Cl3 O18B 70.8(18) . . ? O19B Cl3 O17B 115(2) . . ? O20A Cl3 O17B 91.1(17) . . ? O18B Cl3 O17B 95(2) . . ? O19B Cl3 O20B 108.3(17) . . ? O20A Cl3 O20B 61.3(12) . . ? O18B Cl3 O20B 131(2) . . ? O17B Cl3 O20B 97(2) . . ? O19B Cl3 O19A 47.8(14) . . ? O20A Cl3 O19A 106.2(12) . . ? O18B Cl3 O19A 94.2(17) . . ? O17B Cl3 O19A 162.4(19) . . ? O20B Cl3 O19A 89.1(16) . . ? O19B Cl3 O17A 89.3(13) . . ? O20A Cl3 O17A 106.7(9) . . ? O18B Cl3 O17A 46.0(19) . . ? O17B Cl3 O17A 66.1(15) . . ? O20B Cl3 O17A 159.7(16) . . ? O19A Cl3 O17A 110.6(13) . . ? O19B Cl3 O18A 79.4(16) . . ? O20A Cl3 O18A 112.5(11) . . ? O18B Cl3 O18A 152.9(19) . . ? O17B Cl3 O18A 59.0(19) . . ? O20B Cl3 O18A 64.2(14) . . ? O19A Cl3 O18A 109.7(9) . . ? O17A Cl3 O18A 111.0(10) . . ? N1S C3S C4S 178.5(13) . . ? C17 O3 C18 113.5(7) . . ? C17 O3 Co1 126.2(6) . . ? C18 O3 Co1 104.0(5) . . ? C6 N3 Co1 116.1(6) . . ? C6 N3 H3A 108.3 . . ? Co1 N3 H3A 108.3 . . ? C6 N3 H3B 108.3 . . ? Co1 N3 H3B 108.3 . . ? H3A N3 H3B 107.4 . . ? C2 C3 C4 120.3(13) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? O2W Co4 N8 97.4(3) . . ? O2W Co4 O8 100.2(3) . . ? N8 Co4 O8 119.4(3) . . ? O2W Co4 O6 93.6(3) . . ? N8 Co4 O6 110.7(4) . . ? O8 Co4 O6 125.2(3) . . ? O2W Co4 N6 170.9(3) . . ? N8 Co4 N6 90.6(3) . . ? O8 Co4 N6 79.4(3) . . ? O6 Co4 N6 79.4(3) . . ? O23B Cl4 O24B 116.0(17) . . ? O23B Cl4 O24A 158.4(15) . . ? O23B Cl4 O21B 112.7(16) . . ? O24B Cl4 O21B 107.6(17) . . ? O24A Cl4 O21B 74.7(12) . . ? O23B Cl4 O22B 112.2(17) . . ? O24B Cl4 O22B 108.2(18) . . ? O24A Cl4 O22B 85.6(14) . . ? O21B Cl4 O22B 98.6(18) . . ? O23B Cl4 O21A 84.3(15) . . ? O24B Cl4 O21A 153.0(15) . . ? O24A Cl4 O21A 112.6(12) . . ? O21B Cl4 O21A 45.7(12) . . ? O22B Cl4 O21A 77.1(15) . . ? O23B Cl4 O23A 47.8(13) . . ? O24B Cl4 O23A 77.9(14) . . ? O24A Cl4 O23A 111.8(14) . . ? O21B Cl4 O23A 100.6(13) . . ? O22B Cl4 O23A 156.9(18) . . ? O21A Cl4 O23A 107.9(14) . . ? O23B Cl4 O22A 78.9(13) . . ? O24B Cl4 O22A 91.8(16) . . ? O24A Cl4 O22A 105.8(12) . . ? O21B Cl4 O22A 148.0(14) . . ? O22B Cl4 O22A 50.3(15) . . ? O21A Cl4 O22A 110.4(12) . . ? O23A Cl4 O22A 108.3(12) . . ? C26 N4 Co2 117.3(6) . . ? C26 N4 H4A 108.0 . . ? Co2 N4 H4A 108.0 . . ? C26 N4 H4B 108.0 . . ? Co2 N4 H4B 108.0 . . ? H4A N4 H4B 107.2 . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? C15 O4 C16 115.1(7) . . ? C15 O4 Co2 116.5(6) . . ? C16 O4 Co2 120.6(5) . . ? C3 C4 C5 119.4(12) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C36 O5 C35 110.5(8) . . ? C36 O5 Co3 137.8(6) . . ? C35 O5 Co3 111.7(6) . . ? C33 N5 C45 109.5(7) . . ? C33 N5 C34 107.1(8) . . ? C45 N5 C34 112.6(8) . . ? C33 N5 Co3 111.5(6) . . ? C45 N5 Co3 111.3(6) . . ? C34 N5 Co3 104.6(5) . . ? O26B Cl5 O26A 49.8(13) . . ? O26B Cl5 O28A 155.1(14) . . ? O26A Cl5 O28A 114.3(15) . . ? O26B Cl5 O27 85.8(12) . . ? O26A Cl5 O27 130.5(17) . . ? O28A Cl5 O27 97.6(9) . . ? O26B Cl5 O25 106.2(12) . . ? O26A Cl5 O25 104.7(13) . . ? O28A Cl5 O25 96.2(11) . . ? O27 Cl5 O25 108.5(9) . . ? O26B Cl5 O28B 97.2(17) . . ? O26A Cl5 O28B 61.7(15) . . ? O28A Cl5 O28B 58.8(15) . . ? O27 Cl5 O28B 113.5(14) . . ? O25 Cl5 O28B 133.0(14) . . ? C6 C5 C4 120.0(11) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C38 O6 C37 113.6(9) . . ? C38 O6 Co4 116.5(7) . . ? C37 O6 Co4 123.9(7) . . ? C40 N6 C39 111.1(9) . . ? C40 N6 C46 109.8(8) . . ? C39 N6 C46 111.0(10) . . ? C40 N6 Co4 108.0(7) . . ? C39 N6 Co4 104.8(6) . . ? C46 N6 Co4 112.0(7) . . ? O31 Cl6 O30 108.2(10) . . ? O31 Cl6 O29B 103.2(17) . . ? O30 Cl6 O29B 116.2(14) . . ? O31 Cl6 O29A 141.5(17) . . ? O30 Cl6 O29A 88.4(15) . . ? O31 Cl6 O32 104.9(11) . . ? O30 Cl6 O32 108.2(11) . . ? O29B Cl6 O32 115.3(16) . . ? O29A Cl6 O32 102.2(14) . . ? C1 C6 C5 117.7(10) . . ? C1 C6 N3 117.1(9) . . ? C5 C6 N3 125.1(10) . . ? C43 O7 C44 113.7(7) . . ? C43 O7 Co3 124.9(6) . . ? C44 O7 Co3 104.1(5) . . ? C32 N7 Co3 115.2(6) . . ? C32 N7 H7NA 108.5 . . ? Co3 N7 H7NA 108.5 . . ? C32 N7 H7NB 108.5 . . ? Co3 N7 H7NB 108.5 . . ? H7NA N7 H7NB 107.5 . . ? C1 C7 N1 112.3(8) . . ? C1 C7 H7A 109.1 . . ? N1 C7 H7A 109.1 . . ? C1 C7 H7B 109.1 . . ? N1 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? C41 O8 C42 114.5(8) . . ? C41 O8 Co4 115.6(6) . . ? C42 O8 Co4 121.9(6) . . ? C52 N8 Co4 120.6(6) . . ? C52 N8 H8NA 107.2 . . ? Co4 N8 H8NA 107.2 . . ? C52 N8 H8NB 107.2 . . ? Co4 N8 H8NB 107.2 . . ? H8NA N8 H8NB 106.8 . . ? C9 C8 N1 114.3(9) . . ? C9 C8 H8A 108.7 . . ? N1 C8 H8A 108.7 . . ? C9 C8 H8B 108.7 . . ? N1 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? O1 C9 C8 106.8(8) . . ? O1 C9 H9A 110.4 . . ? C8 C9 H9A 110.4 . . ? O1 C9 H9B 110.4 . . ? C8 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? O1 C10 C11 111.9(9) . . ? O1 C10 H10A 109.2 . . ? C11 C10 H10A 109.2 . . ? O1 C10 H10B 109.2 . . ? C11 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? O2 C11 C10 111.7(9) . . ? O2 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? O2 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? O2 C12 C13 106.1(9) . . ? O2 C12 H12A 110.5 . . ? C13 C12 H12A 110.5 . . ? O2 C12 H12B 110.5 . . ? C13 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? N2 C13 C12 114.4(10) . . ? N2 C13 H13A 108.7 . . ? C12 C13 H13A 108.7 . . ? N2 C13 H13B 108.7 . . ? C12 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? N2 C14 C15 110.5(9) . . ? N2 C14 H14A 109.6 . . ? C15 C14 H14A 109.6 . . ? N2 C14 H14B 109.6 . . ? C15 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? O4 C15 C14 105.5(8) . . ? O4 C15 H15A 110.6 . . ? C14 C15 H15A 110.6 . . ? O4 C15 H15B 110.6 . . ? C14 C15 H15B 110.6 . . ? H15A C15 H15B 108.8 . . ? O4 C16 C17 113.2(8) . . ? O4 C16 H16A 108.9 . . ? C17 C16 H16A 108.9 . . ? O4 C16 H16B 108.9 . . ? C17 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? O3 C17 C16 109.7(7) . . ? O3 C17 H17A 109.7 . . ? C16 C17 H17A 109.7 . . ? O3 C17 H17B 109.7 . . ? C16 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? O3 C18 C19 109.9(8) . . ? O3 C18 H18A 109.7 . . ? C19 C18 H18A 109.7 . . ? O3 C18 H18B 109.7 . . ? C19 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? N1 C19 C18 112.5(8) . . ? N1 C19 H19A 109.1 . . ? C18 C19 H19A 109.1 . . ? N1 C19 H19B 109.1 . . ? C18 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C21 C20 N2 113.5(10) . . ? C21 C20 H20A 108.9 . . ? N2 C20 H20A 108.9 . . ? C21 C20 H20B 108.9 . . ? N2 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C26 C21 C22 115.5(12) . . ? C26 C21 C20 118.8(11) . . ? C22 C21 C20 125.8(11) . . ? C23 C22 C21 123.0(12) . . ? C23 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? C24 C23 C22 121.0(11) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 118.0(12) . . ? C23 C24 H24 121.0 . . ? C25 C24 H24 121.0 . . ? C24 C25 C26 120.0(11) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 122.5(10) . . ? C21 C26 N4 122.8(12) . . ? C25 C26 N4 114.6(11) . . ? C32 C27 C28 116.9(11) . . ? C32 C27 C33 121.5(10) . . ? C28 C27 C33 121.5(11) . . ? C29 C28 C27 120.6(12) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C30 C29 C28 120.6(12) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 120.1(13) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 118.1(12) . . ? C32 C31 H31 120.9 . . ? C30 C31 H31 120.9 . . ? C27 C32 C31 123.7(10) . . ? C27 C32 N7 118.1(10) . . ? C31 C32 N7 118.2(10) . . ? N5 C33 C27 112.7(8) . . ? N5 C33 H33A 109.1 . . ? C27 C33 H33A 109.1 . . ? N5 C33 H33B 109.1 . . ? C27 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? C35 C34 N5 111.1(8) . . ? C35 C34 H34A 109.4 . . ? N5 C34 H34A 109.4 . . ? C35 C34 H34B 109.4 . . ? N5 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? O5 C35 C34 109.9(9) . . ? O5 C35 H35A 109.7 . . ? C34 C35 H35A 109.7 . . ? O5 C35 H35B 109.7 . . ? C34 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? C37 C36 O5 112.7(9) . . ? C37 C36 H36A 109.1 . . ? O5 C36 H36A 109.1 . . ? C37 C36 H36B 109.1 . . ? O5 C36 H36B 109.1 . . ? H36A C36 H36B 107.8 . . ? C36 C37 O6 113.8(9) . . ? C36 C37 H37A 108.8 . . ? O6 C37 H37A 108.8 . . ? C36 C37 H37B 108.8 . . ? O6 C37 H37B 108.8 . . ? H37A C37 H37B 107.7 . . ? O6 C38 C39 106.5(10) . . ? O6 C38 H38A 110.4 . . ? C39 C38 H38A 110.4 . . ? O6 C38 H38B 110.4 . . ? C39 C38 H38B 110.4 . . ? H38A C38 H38B 108.6 . . ? N6 C39 C38 111.6(9) . . ? N6 C39 H39A 109.3 . . ? C38 C39 H39A 109.3 . . ? N6 C39 H39B 109.3 . . ? C38 C39 H39B 109.3 . . ? H39A C39 H39B 108.0 . . ? N6 C40 C41 110.9(9) . . ? N6 C40 H40A 109.5 . . ? C41 C40 H40A 109.5 . . ? N6 C40 H40B 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? O8 C41 C40 106.5(8) . . ? O8 C41 H41A 110.4 . . ? C40 C41 H41A 110.4 . . ? O8 C41 H41B 110.4 . . ? C40 C41 H41B 110.4 . . ? H41A C41 H41B 108.6 . . ? O8 C42 C43 113.3(9) . . ? O8 C42 H42A 108.9 . . ? C43 C42 H42A 108.9 . . ? O8 C42 H42B 108.9 . . ? C43 C42 H42B 108.9 . . ? H42A C42 H42B 107.7 . . ? O7 C43 C42 109.7(7) . . ? O7 C43 H43A 109.7 . . ? C42 C43 H43A 109.7 . . ? O7 C43 H43B 109.7 . . ? C42 C43 H43B 109.7 . . ? H43A C43 H43B 108.2 . . ? O7 C44 C45 108.9(7) . . ? O7 C44 H44A 109.9 . . ? C45 C44 H44A 109.9 . . ? O7 C44 H44B 109.9 . . ? C45 C44 H44B 109.9 . . ? H44A C44 H44B 108.3 . . ? N5 C45 C44 112.4(8) . . ? N5 C45 H45A 109.1 . . ? C44 C45 H45A 109.1 . . ? N5 C45 H45B 109.1 . . ? C44 C45 H45B 109.1 . . ? H45A C45 H45B 107.9 . . ? N6 C46 C47 113.3(10) . . ? N6 C46 H46A 108.9 . . ? C47 C46 H46A 108.9 . . ? N6 C46 H46B 108.9 . . ? C47 C46 H46B 108.9 . . ? H46A C46 H46B 107.7 . . ? C48 C47 C52 118.5(11) . . ? C48 C47 C46 117.4(12) . . ? C52 C47 C46 124.1(10) . . ? C49 C48 C47 122.5(13) . . ? C49 C48 H48 118.7 . . ? C47 C48 H48 118.7 . . ? C48 C49 C50 117.9(12) . . ? C48 C49 H49 121.0 . . ? C50 C49 H49 121.0 . . ? C49 C50 C51 121.3(13) . . ? C49 C50 H50 119.4 . . ? C51 C50 H50 119.4 . . ? C50 C51 C52 119.4(12) . . ? C50 C51 H51 120.3 . . ? C52 C51 H51 120.3 . . ? C47 C52 C51 120.1(11) . . ? C47 C52 N8 115.5(11) . . ? C51 C52 N8 124.3(11) . . ? 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 Co2 O1W Co1 N1S -144.5(4) . . . . ? Co2 O1W Co1 N1 16.0(16) . . . . ? Co2 O1W Co1 N3 130.1(4) . . . . ? Co2 O1W Co1 O3 26.4(4) . . . . ? Co2 O1W Co1 O1 -61.3(4) . . . . ? O1W Co1 O1 C10 3.4(10) . . . . ? N1S Co1 O1 C10 95.1(10) . . . . ? N1 Co1 O1 C10 -163.0(10) . . . . ? N3 Co1 O1 C10 148.2(10) . . . . ? O3 Co1 O1 C10 -83.3(9) . . . . ? O1W Co1 O1 C9 178.5(6) . . . . ? N1S Co1 O1 C9 -89.8(7) . . . . ? N1 Co1 O1 C9 12.1(6) . . . . ? N3 Co1 O1 C9 -36.7(11) . . . . ? O3 Co1 O1 C9 91.7(7) . . . . ? O1W Co1 N1 C19 6.4(17) . . . . ? N1S Co1 N1 C19 166.7(7) . . . . ? N3 Co1 N1 C19 -108.3(7) . . . . ? O3 Co1 N1 C19 -4.1(6) . . . . ? O1 Co1 N1 C19 86.6(7) . . . . ? O1W Co1 N1 C8 -113.0(13) . . . . ? N1S Co1 N1 C8 47.3(7) . . . . ? N3 Co1 N1 C8 132.4(6) . . . . ? O3 Co1 N1 C8 -123.5(6) . . . . ? O1 Co1 N1 C8 -32.8(6) . . . . ? O1W Co1 N1 C7 128.6(12) . . . . ? N1S Co1 N1 C7 -71.1(7) . . . . ? N3 Co1 N1 C7 14.0(6) . . . . ? O3 Co1 N1 C7 118.1(6) . . . . ? O1 Co1 N1 C7 -151.2(6) . . . . ? Co1 O1W Co2 O4 -69.8(4) . . . . ? Co1 O1W Co2 N4 168.6(5) . . . . ? Co1 O1W Co2 O2 56.2(4) . . . . ? O1W Co2 O2 C11 33.1(8) . . . . ? O4 Co2 O2 C11 139.2(7) . . . . ? N4 Co2 O2 C11 -67.4(8) . . . . ? N2 Co2 O2 C11 -152.8(8) . . . . ? O1W Co2 O2 C12 -177.6(8) . . . . ? O4 Co2 O2 C12 -71.6(8) . . . . ? N4 Co2 O2 C12 81.9(8) . . . . ? N2 Co2 O2 C12 -3.5(8) . . . . ? O4 Co2 N2 C13 107.3(7) . . . . ? N4 Co2 N2 C13 -133.0(8) . . . . ? O2 Co2 N2 C13 -21.1(7) . . . . ? O4 Co2 N2 C14 -13.3(6) . . . . ? N4 Co2 N2 C14 106.5(7) . . . . ? O2 Co2 N2 C14 -141.6(7) . . . . ? O4 Co2 N2 C20 -136.9(8) . . . . ? N4 Co2 N2 C20 -17.2(8) . . . . ? O2 Co2 N2 C20 94.8(8) . . . . ? C6 C1 C2 C3 -2.1(19) . . . . ? C7 C1 C2 C3 176.2(12) . . . . ? Co4 O2W Co3 N2S -145.1(4) . . . . ? Co4 O2W Co3 N5 12.9(14) . . . . ? Co4 O2W Co3 N7 128.8(4) . . . . ? Co4 O2W Co3 O5 -61.2(4) . . . . ? Co4 O2W Co3 O7 25.7(4) . . . . ? O1W Co1 O3 C17 77.8(7) . . . . ? N1 Co1 O3 C17 -104.6(7) . . . . ? N3 Co1 O3 C17 -17.3(7) . . . . ? O1 Co1 O3 C17 178.7(7) . . . . ? O1W Co1 O3 C18 -148.4(6) . . . . ? N1 Co1 O3 C18 29.1(6) . . . . ? N3 Co1 O3 C18 116.4(6) . . . . ? O1 Co1 O3 C18 -47.6(6) . . . . ? O1W Co1 N3 C6 -126.7(6) . . . . ? N1S Co1 N3 C6 140.7(7) . . . . ? N1 Co1 N3 C6 40.9(7) . . . . ? O3 Co1 N3 C6 -38.3(7) . . . . ? O1 Co1 N3 C6 87.9(10) . . . . ? C1 C2 C3 C4 0(2) . . . . ? Co3 O2W Co4 N8 168.8(5) . . . . ? Co3 O2W Co4 O8 -69.4(4) . . . . ? Co3 O2W Co4 O6 57.3(4) . . . . ? O1W Co2 N4 C26 149.1(9) . . . . ? O4 Co2 N4 C26 42.0(11) . . . . ? O2 Co2 N4 C26 -113.0(9) . . . . ? N2 Co2 N4 C26 -33.8(10) . . . . ? O1W Co2 O4 C15 157.2(6) . . . . ? N4 Co2 O4 C15 -97.1(7) . . . . ? O2 Co2 O4 C15 54.5(7) . . . . ? N2 Co2 O4 C15 -14.8(7) . . . . ? O1W Co2 O4 C16 9.4(6) . . . . ? N4 Co2 O4 C16 115.1(6) . . . . ? O2 Co2 O4 C16 -93.3(7) . . . . ? N2 Co2 O4 C16 -162.6(6) . . . . ? C2 C3 C4 C5 2(2) . . . . ? O2W Co3 O5 C36 -0.5(9) . . . . ? N2S Co3 O5 C36 91.2(9) . . . . ? N5 Co3 O5 C36 -166.6(9) . . . . ? N7 Co3 O5 C36 146.5(10) . . . . ? O7 Co3 O5 C36 -86.8(9) . . . . ? O2W Co3 O5 C35 179.5(6) . . . . ? N2S Co3 O5 C35 -88.7(6) . . . . ? N5 Co3 O5 C35 13.4(6) . . . . ? N7 Co3 O5 C35 -33.5(11) . . . . ? O7 Co3 O5 C35 93.2(6) . . . . ? O2W Co3 N5 C33 132.2(11) . . . . ? N2S Co3 N5 C33 -70.2(7) . . . . ? N7 Co3 N5 C33 15.6(6) . . . . ? O5 Co3 N5 C33 -150.9(7) . . . . ? O7 Co3 N5 C33 119.2(6) . . . . ? O2W Co3 N5 C45 9.5(16) . . . . ? N2S Co3 N5 C45 167.2(6) . . . . ? N7 Co3 N5 C45 -107.1(6) . . . . ? O5 Co3 N5 C45 86.4(6) . . . . ? O7 Co3 N5 C45 -3.5(6) . . . . ? O2W Co3 N5 C34 -112.4(12) . . . . ? N2S Co3 N5 C34 45.3(7) . . . . ? N7 Co3 N5 C34 131.0(6) . . . . ? O5 Co3 N5 C34 -35.5(6) . . . . ? O7 Co3 N5 C34 -125.4(6) . . . . ? C3 C4 C5 C6 -1.2(19) . . . . ? O2W Co4 O6 C38 -175.6(8) . . . . ? N8 Co4 O6 C38 85.1(9) . . . . ? O8 Co4 O6 C38 -70.3(9) . . . . ? N6 Co4 O6 C38 -1.5(8) . . . . ? O2W Co4 O6 C37 33.5(7) . . . . ? N8 Co4 O6 C37 -65.9(8) . . . . ? O8 Co4 O6 C37 138.7(7) . . . . ? N6 Co4 O6 C37 -152.4(8) . . . . ? N8 Co4 N6 C40 106.7(7) . . . . ? O8 Co4 N6 C40 -13.1(7) . . . . ? O6 Co4 N6 C40 -142.3(7) . . . . ? N8 Co4 N6 C39 -134.8(7) . . . . ? O8 Co4 N6 C39 105.3(7) . . . . ? O6 Co4 N6 C39 -23.8(7) . . . . ? N8 Co4 N6 C46 -14.3(8) . . . . ? O8 Co4 N6 C46 -134.2(8) . . . . ? O6 Co4 N6 C46 96.7(8) . . . . ? C2 C1 C6 C5 2.8(16) . . . . ? C7 C1 C6 C5 -175.4(9) . . . . ? C2 C1 C6 N3 179.8(10) . . . . ? C7 C1 C6 N3 1.6(15) . . . . ? C4 C5 C6 C1 -1.2(16) . . . . ? C4 C5 C6 N3 -177.9(10) . . . . ? Co1 N3 C6 C1 -54.2(11) . . . . ? Co1 N3 C6 C5 122.6(10) . . . . ? O2W Co3 O7 C43 80.0(7) . . . . ? N5 Co3 O7 C43 -103.1(7) . . . . ? N7 Co3 O7 C43 -15.4(7) . . . . ? O5 Co3 O7 C43 179.9(7) . . . . ? O2W Co3 O7 C44 -147.1(6) . . . . ? N5 Co3 O7 C44 29.8(6) . . . . ? N7 Co3 O7 C44 117.5(6) . . . . ? O5 Co3 O7 C44 -47.3(6) . . . . ? O2W Co3 N7 C32 -128.8(7) . . . . ? N2S Co3 N7 C32 138.8(7) . . . . ? N5 Co3 N7 C32 38.6(7) . . . . ? O5 Co3 N7 C32 83.9(10) . . . . ? O7 Co3 N7 C32 -40.7(7) . . . . ? C6 C1 C7 N1 64.5(12) . . . . ? C2 C1 C7 N1 -113.7(11) . . . . ? C19 N1 C7 C1 61.7(10) . . . . ? C8 N1 C7 C1 -177.1(8) . . . . ? Co1 N1 C7 C1 -62.0(9) . . . . ? O2W Co4 O8 C41 156.4(6) . . . . ? N8 Co4 O8 C41 -98.9(7) . . . . ? O6 Co4 O8 C41 54.5(7) . . . . ? N6 Co4 O8 C41 -14.3(6) . . . . ? O2W Co4 O8 C42 9.3(7) . . . . ? N8 Co4 O8 C42 114.0(7) . . . . ? O6 Co4 O8 C42 -92.6(7) . . . . ? N6 Co4 O8 C42 -161.4(7) . . . . ? O2W Co4 N8 C52 145.9(10) . . . . ? O8 Co4 N8 C52 39.7(11) . . . . ? O6 Co4 N8 C52 -117.3(10) . . . . ? N6 Co4 N8 C52 -38.4(10) . . . . ? C19 N1 C8 C9 -64.5(10) . . . . ? C7 N1 C8 C9 175.2(8) . . . . ? Co1 N1 C8 C9 55.4(9) . . . . ? C10 O1 C9 C8 -170.6(8) . . . . ? Co1 O1 C9 C8 13.0(10) . . . . ? N1 C8 C9 O1 -45.4(11) . . . . ? C9 O1 C10 C11 178.3(9) . . . . ? Co1 O1 C10 C11 -6.5(15) . . . . ? C12 O2 C11 C10 94.2(12) . . . . ? Co2 O2 C11 C10 -116.8(9) . . . . ? O1 C10 C11 O2 75.6(12) . . . . ? C11 O2 C12 C13 177.8(9) . . . . ? Co2 O2 C12 C13 27.2(12) . . . . ? C14 N2 C13 C12 163.3(10) . . . . ? C20 N2 C13 C12 -74.7(12) . . . . ? Co2 N2 C13 C12 44.9(12) . . . . ? O2 C12 C13 N2 -48.9(13) . . . . ? C13 N2 C14 C15 -76.8(12) . . . . ? C20 N2 C14 C15 163.1(10) . . . . ? Co2 N2 C14 C15 38.3(11) . . . . ? C16 O4 C15 C14 -171.9(8) . . . . ? Co2 O4 C15 C14 38.5(10) . . . . ? N2 C14 C15 O4 -49.2(12) . . . . ? C15 O4 C16 C17 -68.5(10) . . . . ? Co2 O4 C16 C17 79.7(8) . . . . ? C18 O3 C17 C16 170.4(8) . . . . ? Co1 O3 C17 C16 -59.5(10) . . . . ? O4 C16 C17 O3 -56.8(10) . . . . ? C17 O3 C18 C19 91.3(9) . . . . ? Co1 O3 C18 C19 -49.3(8) . . . . ? C8 N1 C19 C18 93.8(10) . . . . ? C7 N1 C19 C18 -145.5(9) . . . . ? Co1 N1 C19 C18 -21.7(11) . . . . ? O3 C18 C19 N1 49.8(11) . . . . ? C13 N2 C20 C21 177.0(9) . . . . ? C14 N2 C20 C21 -59.7(13) . . . . ? Co2 N2 C20 C21 63.2(11) . . . . ? N2 C20 C21 C26 -60.2(15) . . . . ? N2 C20 C21 C22 120.9(12) . . . . ? C26 C21 C22 C23 0.9(18) . . . . ? C20 C21 C22 C23 179.8(12) . . . . ? C21 C22 C23 C24 -1(2) . . . . ? C22 C23 C24 C25 0.6(18) . . . . ? C23 C24 C25 C26 -0.9(16) . . . . ? C22 C21 C26 C25 -1.2(17) . . . . ? C20 C21 C26 C25 179.7(10) . . . . ? C22 C21 C26 N4 175.6(10) . . . . ? C20 C21 C26 N4 -3.5(17) . . . . ? C24 C25 C26 C21 1.3(17) . . . . ? C24 C25 C26 N4 -175.7(9) . . . . ? Co2 N4 C26 C21 51.3(14) . . . . ? Co2 N4 C26 C25 -131.6(9) . . . . ? C32 C27 C28 C29 -3.5(16) . . . . ? C33 C27 C28 C29 175.3(10) . . . . ? C27 C28 C29 C30 1.3(19) . . . . ? C28 C29 C30 C31 1(2) . . . . ? C29 C30 C31 C32 -1.3(19) . . . . ? C28 C27 C32 C31 3.5(16) . . . . ? C33 C27 C32 C31 -175.3(10) . . . . ? C28 C27 C32 N7 -178.7(9) . . . . ? C33 C27 C32 N7 2.5(15) . . . . ? C30 C31 C32 C27 -1.1(17) . . . . ? C30 C31 C32 N7 -178.9(10) . . . . ? Co3 N7 C32 C27 -52.7(11) . . . . ? Co3 N7 C32 C31 125.2(9) . . . . ? C45 N5 C33 C27 60.3(10) . . . . ? C34 N5 C33 C27 -177.3(8) . . . . ? Co3 N5 C33 C27 -63.4(9) . . . . ? C32 C27 C33 N5 64.8(13) . . . . ? C28 C27 C33 N5 -113.8(11) . . . . ? C33 N5 C34 C35 175.1(9) . . . . ? C45 N5 C34 C35 -64.5(11) . . . . ? Co3 N5 C34 C35 56.6(9) . . . . ? C36 O5 C35 C34 -167.0(8) . . . . ? Co3 O5 C35 C34 13.0(10) . . . . ? N5 C34 C35 O5 -46.2(11) . . . . ? C35 O5 C36 C37 179.4(9) . . . . ? Co3 O5 C36 C37 -0.6(15) . . . . ? O5 C36 C37 O6 69.1(14) . . . . ? C38 O6 C37 C36 94.2(12) . . . . ? Co4 O6 C37 C36 -114.1(10) . . . . ? C37 O6 C38 C39 -179.6(9) . . . . ? Co4 O6 C38 C39 26.5(13) . . . . ? C40 N6 C39 C38 163.3(10) . . . . ? C46 N6 C39 C38 -74.2(12) . . . . ? Co4 N6 C39 C38 46.8(12) . . . . ? O6 C38 C39 N6 -49.0(14) . . . . ? C39 N6 C40 C41 -76.9(12) . . . . ? C46 N6 C40 C41 159.8(9) . . . . ? Co4 N6 C40 C41 37.5(11) . . . . ? C42 O8 C41 C40 -172.7(9) . . . . ? Co4 O8 C41 C40 37.8(10) . . . . ? N6 C40 C41 O8 -49.0(12) . . . . ? C41 O8 C42 C43 -69.2(10) . . . . ? Co4 O8 C42 C43 78.2(9) . . . . ? C44 O7 C43 C42 168.9(8) . . . . ? Co3 O7 C43 C42 -62.0(10) . . . . ? O8 C42 C43 O7 -53.8(11) . . . . ? C43 O7 C44 C45 89.1(9) . . . . ? Co3 O7 C44 C45 -49.9(8) . . . . ? C33 N5 C45 C44 -146.7(8) . . . . ? C34 N5 C45 C44 94.3(10) . . . . ? Co3 N5 C45 C44 -22.8(10) . . . . ? O7 C44 C45 N5 51.2(11) . . . . ? C40 N6 C46 C47 -61.6(12) . . . . ? C39 N6 C46 C47 175.1(9) . . . . ? Co4 N6 C46 C47 58.3(11) . . . . ? N6 C46 C47 C48 121.9(11) . . . . ? N6 C46 C47 C52 -61.1(14) . . . . ? C52 C47 C48 C49 1.4(18) . . . . ? C46 C47 C48 C49 178.6(12) . . . . ? C47 C48 C49 C50 2(2) . . . . ? C48 C49 C50 C51 -1(2) . . . . ? C49 C50 C51 C52 -3.1(18) . . . . ? C48 C47 C52 C51 -5.5(17) . . . . ? C46 C47 C52 C51 177.5(10) . . . . ? C48 C47 C52 N8 177.7(10) . . . . ? C46 C47 C52 N8 0.7(16) . . . . ? C50 C51 C52 C47 6.3(17) . . . . ? C50 C51 C52 N8 -177.1(10) . . . . ? Co4 N8 C52 C47 50.2(14) . . . . ? Co4 N8 C52 C51 -126.5(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W O17A 0.86 2.15 2.992(14) 166.2 . O2W H2W O22A 0.85 2.22 3.046(16) 164.8 . O2W H2W O23B 0.85 2.63 3.20(3) 125.9 . N3 H3A O26B 0.90 2.27 3.14(2) 162.2 . N3 H3A O27 0.90 2.45 3.259(14) 150.4 . N3 H3B O15 0.90 2.31 3.164(11) 158.6 . N4 H4A O18A 0.90 2.61 3.25(2) 129.0 . N4 H4B O17B 0.90 2.47 3.03(3) 121.2 . N4 H4B O28B 0.90 2.57 3.25(2) 133.2 . N4 H4B O17A 0.90 2.55 3.181(18) 127.9 . N7 H7NA O30 0.90 2.39 3.205(14) 150.1 . N7 H7NA O29A 0.90 2.47 3.35(3) 164.9 . N7 H7NB O9 0.90 2.33 3.185(11) 158.1 1_655 N8 H8NA O21A 0.90 2.30 2.902(18) 124.3 . N8 H8NB O22B 0.90 2.29 3.01(3) 136.2 . _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.809 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.070 data_compound1 _database_code_depnum_ccdc_archive 'CCDC 265325' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H52 N8 Ni2 O4, 4(Cl O4), 2(C2 H3 N) ' _chemical_formula_sum 'C38 H58 Cl4 N10 Ni2 O20' _chemical_formula_weight 1234.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.032(2) _cell_length_b 11.376(3) _cell_length_c 11.665(2) _cell_angle_alpha 86.993(4) _cell_angle_beta 65.913(4) _cell_angle_gamma 81.707(4) _cell_volume 1322.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.996 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8181 _exptl_absorpt_correction_T_max 0.8489 _exptl_absorpt_process_details 'Sadabs (Scheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7859 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.10 _reflns_number_total 5667 _reflns_number_gt 3558 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0922P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5667 _refine_ls_number_parameters 355 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1044 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1704 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.62489(5) 0.28370(4) 1.00706(5) 0.03858(19) Uani 1 1 d . . . Cl1 Cl 0.79141(13) -0.16411(11) 1.07076(14) 0.0661(4) Uani 1 1 d DU . . O1 O 0.7490(3) 0.4200(2) 0.9499(3) 0.0505(7) Uani 1 1 d . . . N1 N 0.5300(4) 0.1314(3) 1.0704(3) 0.0428(8) Uani 1 1 d . . . H2N H 0.480(4) 0.128(3) 1.039(3) 0.027(11) Uiso 1 1 d . . . H1N H 0.599(4) 0.074(4) 1.039(4) 0.044(12) Uiso 1 1 d . . . N1S N 0.5747(4) 0.2977(3) 0.8568(3) 0.0497(9) Uani 1 1 d . . . C1 C 0.6696(5) 0.1720(4) 1.2212(4) 0.0512(11) Uani 1 1 d . . . H1A H 0.7308 0.1135 1.1595 0.061 Uiso 1 1 calc R . . H1B H 0.7019 0.1753 1.2867 0.061 Uiso 1 1 calc R . . C1S C 0.5604(5) 0.2784(4) 0.7710(5) 0.0554(12) Uani 1 1 d . . . Cl2 Cl 0.90607(16) 0.26982(13) 1.45849(14) 0.0781(4) Uani 1 1 d . . . O2 O 0.5525(3) 0.6034(2) 0.8758(3) 0.0434(7) Uani 1 1 d . . . N2 N 0.6707(3) 0.2916(3) 1.1594(3) 0.0426(8) Uani 1 1 d . . . C2 C 0.5339(5) 0.1328(3) 1.2773(4) 0.0478(10) Uani 1 1 d . . . N2S N 0.7974(4) 0.1704(3) 0.8978(4) 0.0533(9) Uani 1 1 d . . . C2S C 0.5429(7) 0.2538(6) 0.6579(5) 0.094(2) Uani 1 1 d . . . H2S1 H 0.5246 0.3273 0.6199 0.113 Uiso 1 1 calc R . . H2S2 H 0.4693 0.2090 0.6793 0.113 Uiso 1 1 calc R . . H2S3 H 0.6233 0.2088 0.5999 0.113 Uiso 1 1 calc R . . C3S C 0.8846(5) 0.1075(4) 0.8311(4) 0.0523(11) Uani 1 1 d . . . C3 C 0.4697(6) 0.1161(4) 1.4061(5) 0.0607(13) Uani 1 1 d . . . H3 H 0.5131 0.1278 1.4572 0.073 Uiso 1 1 calc R . . C4 C 0.3433(7) 0.0826(5) 1.4597(5) 0.0797(17) Uani 1 1 d . . . H4 H 0.3025 0.0724 1.5461 0.096 Uiso 1 1 calc R . . O4A O 0.800(2) -0.2815(7) 1.080(2) 0.146(7) Uani 0.69(3) 1 d PDU A 1 O4B O 0.859(2) -0.256(3) 0.986(5) 0.164(16) Uani 0.31(3) 1 d PDU A 2 C4S C 0.9956(5) 0.0242(5) 0.7479(5) 0.0782(16) Uani 1 1 d . . . H4S1 H 1.0781 0.0415 0.7482 0.094 Uiso 1 1 calc R . . H4S2 H 0.9995 0.0318 0.6642 0.094 Uiso 1 1 calc R . . H4S3 H 0.9821 -0.0554 0.7767 0.094 Uiso 1 1 calc R . . O5 O 0.9000(5) -0.0985(5) 1.0252(6) 0.1329(19) Uani 1 1 d . A . C5 C 0.2773(6) 0.0645(5) 1.3864(5) 0.0753(15) Uani 1 1 d . . . H5 H 0.1921 0.0415 1.4222 0.090 Uiso 1 1 calc R . . O6 O 0.6904(4) -0.1134(3) 1.0332(4) 0.0935(13) Uani 1 1 d . A . C6 C 0.3396(5) 0.0808(4) 1.2581(5) 0.0575(12) Uani 1 1 d . . . H6 H 0.2949 0.0703 1.2077 0.069 Uiso 1 1 calc R . . O7 O 0.7452(8) -0.1310(7) 1.2036(6) 0.171(3) Uani 1 1 d . A . C7 C 0.4664(4) 0.1124(3) 1.2043(4) 0.0432(10) Uani 1 1 d . . . C8 C 0.8092(5) 0.3230(4) 1.1101(5) 0.0535(11) Uani 1 1 d . . . H8A H 0.8722 0.2552 1.0655 0.064 Uiso 1 1 calc R . . H8B H 0.8297 0.3418 1.1798 0.064 Uiso 1 1 calc R . . O8 O 0.9442(7) 0.1663(5) 1.5089(7) 0.164(3) Uani 1 1 d . . . C9 C 0.8260(5) 0.4285(4) 1.0221(5) 0.0630(13) Uani 1 1 d . . . H9A H 0.7950 0.5021 1.0701 0.076 Uiso 1 1 calc R . . H9B H 0.9198 0.4281 0.9667 0.076 Uiso 1 1 calc R . . O9 O 0.8208(6) 0.2388(7) 1.4062(5) 0.168(3) Uani 1 1 d . . . C10 C 0.7758(4) 0.5017(4) 0.8470(4) 0.0482(10) Uani 1 1 d . . . H10A H 0.7710 0.4635 0.7769 0.058 Uiso 1 1 calc R . . H10B H 0.8662 0.5205 0.8206 0.058 Uiso 1 1 calc R . . O10 O 1.0206(7) 0.3115(7) 1.3711(6) 0.178(3) Uani 1 1 d . . . C11 C 0.6805(4) 0.6143(4) 0.8789(4) 0.0462(10) Uani 1 1 d . . . H11A H 0.6652 0.6401 0.9622 0.055 Uiso 1 1 calc R . . H11B H 0.7213 0.6752 0.8202 0.055 Uiso 1 1 calc R . . O11 O 0.8363(6) 0.3540(5) 1.5558(5) 0.1326(19) Uani 1 1 d . . . C12 C 0.5628(5) 0.6012(4) 0.7483(4) 0.0510(11) Uani 1 1 d . . . H12A H 0.6141 0.5273 0.7072 0.061 Uiso 1 1 calc R . . H12B H 0.6078 0.6665 0.7011 0.061 Uiso 1 1 calc R . . C13 C 0.4228(5) 0.6124(4) 0.7535(4) 0.0533(11) Uani 1 1 d . . . H13A H 0.4262 0.6285 0.6698 0.064 Uiso 1 1 calc R . . H13B H 0.3881 0.5374 0.7803 0.064 Uiso 1 1 calc R . . C1W C 0.7661(14) 0.5958(8) 1.4025(11) 0.142(4) Uani 1 1 d . . . N1W N 0.6606(13) 0.5659(9) 1.4248(11) 0.190(5) Uani 1 1 d . . . C2W C 0.8833(10) 0.6327(9) 1.3883(11) 0.169(4) Uani 1 1 d . . . H2W1 H 0.9028 0.6089 1.4598 0.253 Uiso 1 1 calc R . . H2W2 H 0.8756 0.7176 1.3813 0.253 Uiso 1 1 calc R . . H2W3 H 0.9544 0.5975 1.3137 0.253 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 Ni1 0.0447(3) 0.0326(3) 0.0450(3) -0.0032(2) -0.0251(3) -0.0028(2) Cl1 0.0621(8) 0.0516(7) 0.0964(10) 0.0055(7) -0.0451(8) -0.0067(6) O1 0.0545(18) 0.0428(16) 0.069(2) 0.0108(14) -0.0384(16) -0.0136(14) N1 0.046(2) 0.039(2) 0.050(2) -0.0050(16) -0.026(2) -0.0040(17) N1S 0.059(2) 0.049(2) 0.049(2) 0.0005(17) -0.030(2) -0.0086(18) C1 0.068(3) 0.039(2) 0.061(3) 0.006(2) -0.043(3) -0.002(2) C1S 0.060(3) 0.060(3) 0.054(3) -0.004(2) -0.031(3) -0.009(2) Cl2 0.0859(10) 0.0729(9) 0.0727(9) -0.0041(7) -0.0315(8) -0.0027(8) O2 0.0469(17) 0.0395(15) 0.0478(17) -0.0061(12) -0.0245(14) 0.0003(13) N2 0.050(2) 0.0357(17) 0.052(2) -0.0018(15) -0.0320(18) -0.0038(15) C2 0.061(3) 0.035(2) 0.052(3) 0.0018(19) -0.030(2) 0.0020(19) N2S 0.055(2) 0.045(2) 0.060(2) -0.0026(18) -0.025(2) -0.0011(19) C2S 0.101(5) 0.141(6) 0.059(3) -0.013(4) -0.048(4) -0.024(4) C3S 0.050(3) 0.057(3) 0.054(3) -0.003(2) -0.025(2) -0.008(2) C3 0.081(4) 0.052(3) 0.055(3) 0.005(2) -0.037(3) -0.001(3) C4 0.090(5) 0.072(4) 0.057(3) 0.010(3) -0.015(3) 0.001(3) O4A 0.226(15) 0.034(3) 0.258(16) 0.019(6) -0.186(14) -0.002(6) O4B 0.074(12) 0.12(2) 0.33(3) -0.13(2) -0.110(17) 0.038(11) C4S 0.062(3) 0.093(4) 0.067(4) -0.025(3) -0.016(3) 0.006(3) O5 0.105(4) 0.134(5) 0.178(5) 0.022(4) -0.069(4) -0.046(3) C5 0.062(3) 0.083(4) 0.072(4) 0.016(3) -0.019(3) -0.013(3) O6 0.097(3) 0.069(2) 0.149(4) -0.016(2) -0.090(3) 0.009(2) C6 0.059(3) 0.050(3) 0.066(3) 0.004(2) -0.028(3) -0.008(2) O7 0.221(7) 0.196(7) 0.124(5) -0.005(4) -0.093(5) -0.050(6) C7 0.053(3) 0.0284(19) 0.049(3) 0.0009(17) -0.023(2) -0.0012(18) C8 0.056(3) 0.050(3) 0.073(3) 0.003(2) -0.044(3) -0.010(2) O8 0.195(6) 0.100(4) 0.201(6) 0.043(4) -0.098(5) 0.005(4) C9 0.065(3) 0.060(3) 0.084(4) 0.009(3) -0.046(3) -0.023(2) O9 0.136(5) 0.277(8) 0.123(4) -0.067(5) -0.081(4) -0.010(5) C10 0.043(2) 0.044(2) 0.055(3) 0.001(2) -0.018(2) -0.0044(19) O10 0.154(6) 0.184(6) 0.127(5) 0.011(4) 0.024(4) -0.063(5) C11 0.048(3) 0.040(2) 0.056(3) 0.0010(19) -0.026(2) -0.0078(19) O11 0.131(4) 0.135(4) 0.115(4) -0.060(3) -0.031(3) -0.002(4) C12 0.067(3) 0.040(2) 0.049(3) -0.0083(19) -0.030(2) 0.008(2) C13 0.070(3) 0.044(2) 0.055(3) -0.010(2) -0.036(3) -0.002(2) C1W 0.231(13) 0.084(6) 0.188(10) -0.002(6) -0.166(11) -0.013(7) N1W 0.252(13) 0.153(8) 0.245(11) -0.013(7) -0.189(11) 0.000(8) C2W 0.112(7) 0.134(8) 0.243(12) -0.031(8) -0.053(8) -0.009(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1S 2.035(4) . ? Ni1 N2 2.045(3) . ? Ni1 N2S 2.095(4) . ? Ni1 N1 2.098(4) . ? Ni1 O1 2.117(3) . ? Ni1 O2 2.150(3) 2_667 ? Cl1 O4A 1.327(7) . ? Cl1 O4B 1.387(14) . ? Cl1 O6 1.397(4) . ? Cl1 O5 1.404(5) . ? Cl1 O7 1.471(6) . ? O1 C9 1.433(5) . ? O1 C10 1.436(5) . ? N1 C7 1.446(5) . ? N1 H2N 0.78(4) . ? N1 H1N 0.89(4) . ? N1S C1S 1.112(5) . ? C1 C2 1.493(6) . ? C1 N2 1.505(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1S C2S 1.455(6) . ? Cl2 O8 1.377(5) . ? Cl2 O10 1.390(6) . ? Cl2 O9 1.403(5) . ? Cl2 O11 1.410(5) . ? O2 C12 1.447(5) . ? O2 C11 1.450(5) . ? O2 Ni1 2.150(3) 2_667 ? N2 C8 1.488(5) . ? N2 C13 1.492(5) 2_667 ? C2 C7 1.386(6) . ? C2 C3 1.391(6) . ? N2S C3S 1.137(6) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? C3S C4S 1.460(7) . ? C3 C4 1.377(8) . ? C3 H3 0.9300 . ? C4 C5 1.368(8) . ? C4 H4 0.9300 . ? C4S H4S1 0.9600 . ? C4S H4S2 0.9600 . ? C4S H4S3 0.9600 . ? C5 C6 1.384(7) . ? C5 H5 0.9300 . ? C6 C7 1.373(6) . ? C6 H6 0.9300 . ? C8 C9 1.519(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.493(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.508(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N2 1.492(5) 2_667 ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C1W N1W 1.181(14) . ? C1W C2W 1.361(13) . ? C2W H2W1 0.9600 . ? C2W H2W2 0.9600 . ? C2W H2W3 0.9600 . ? 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 N1S Ni1 N2 173.05(13) . . ? N1S Ni1 N2S 87.90(15) . . ? N2 Ni1 N2S 96.65(14) . . ? N1S Ni1 N1 91.77(15) . . ? N2 Ni1 N1 93.68(14) . . ? N2S Ni1 N1 87.37(15) . . ? N1S Ni1 O1 95.47(13) . . ? N2 Ni1 O1 79.70(12) . . ? N2S Ni1 O1 85.61(13) . . ? N1 Ni1 O1 169.72(13) . . ? N1S Ni1 O2 93.52(13) . 2_667 ? N2 Ni1 O2 82.04(12) . 2_667 ? N2S Ni1 O2 178.23(12) . 2_667 ? N1 Ni1 O2 91.53(13) . 2_667 ? O1 Ni1 O2 95.30(11) . 2_667 ? O4A Cl1 O4B 46.6(18) . . ? O4A Cl1 O6 113.4(6) . . ? O4B Cl1 O6 103.6(16) . . ? O4A Cl1 O5 125.7(10) . . ? O4B Cl1 O5 93.6(16) . . ? O6 Cl1 O5 110.8(3) . . ? O4A Cl1 O7 100.3(10) . . ? O4B Cl1 O7 143(3) . . ? O6 Cl1 O7 106.1(4) . . ? O5 Cl1 O7 96.3(4) . . ? C9 O1 C10 113.8(3) . . ? C9 O1 Ni1 114.6(2) . . ? C10 O1 Ni1 131.5(2) . . ? C7 N1 Ni1 118.4(3) . . ? C7 N1 H2N 111(3) . . ? Ni1 N1 H2N 109(3) . . ? C7 N1 H1N 107(3) . . ? Ni1 N1 H1N 101(3) . . ? H2N N1 H1N 109(4) . . ? C1S N1S Ni1 163.6(4) . . ? C2 C1 N2 113.1(3) . . ? C2 C1 H1A 109.0 . . ? N2 C1 H1A 109.0 . . ? C2 C1 H1B 109.0 . . ? N2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N1S C1S C2S 179.4(6) . . ? O8 Cl2 O10 108.5(5) . . ? O8 Cl2 O9 105.1(5) . . ? O10 Cl2 O9 113.7(4) . . ? O8 Cl2 O11 108.8(4) . . ? O10 Cl2 O11 110.0(4) . . ? O9 Cl2 O11 110.5(4) . . ? C12 O2 C11 111.4(3) . . ? C12 O2 Ni1 110.9(2) . 2_667 ? C11 O2 Ni1 120.0(2) . 2_667 ? C8 N2 C13 108.9(3) . 2_667 ? C8 N2 C1 108.6(3) . . ? C13 N2 C1 113.0(3) 2_667 . ? C8 N2 Ni1 106.2(3) . . ? C13 N2 Ni1 109.5(2) 2_667 . ? C1 N2 Ni1 110.4(2) . . ? C7 C2 C3 117.2(5) . . ? C7 C2 C1 121.9(4) . . ? C3 C2 C1 120.9(4) . . ? C3S N2S Ni1 173.2(4) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N2S C3S C4S 178.5(5) . . ? C4 C3 C2 121.7(5) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 120.3(5) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? C4 C5 C6 118.9(5) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C7 C6 C5 120.9(5) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C2 121.0(4) . . ? C6 C7 N1 120.6(4) . . ? C2 C7 N1 118.3(4) . . ? N2 C8 C9 111.8(3) . . ? N2 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N2 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? O1 C9 C8 108.3(3) . . ? O1 C9 H9A 110.0 . . ? C8 C9 H9A 110.0 . . ? O1 C9 H9B 110.0 . . ? C8 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? O1 C10 C11 113.2(4) . . ? O1 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? O1 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.8 . . ? O2 C11 C10 113.6(3) . . ? O2 C11 H11A 108.9 . . ? C10 C11 H11A 108.9 . . ? O2 C11 H11B 108.9 . . ? C10 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? O2 C12 C13 107.9(4) . . ? O2 C12 H12A 110.1 . . ? C13 C12 H12A 110.1 . . ? O2 C12 H12B 110.1 . . ? C13 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? N2 C13 C12 112.9(3) 2_667 . ? N2 C13 H13A 109.0 2_667 . ? C12 C13 H13A 109.0 . . ? N2 C13 H13B 109.0 2_667 . ? C12 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? N1W C1W C2W 174.7(14) . . ? C1W C2W H2W1 109.5 . . ? C1W C2W H2W2 109.5 . . ? H2W1 C2W H2W2 109.5 . . ? C1W C2W H2W3 109.5 . . ? H2W1 C2W H2W3 109.5 . . ? H2W2 C2W H2W3 109.5 . . ? 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 N1S Ni1 O1 C9 -170.3(3) . . . . ? N2 Ni1 O1 C9 14.8(3) . . . . ? N2S Ni1 O1 C9 -82.8(3) . . . . ? N1 Ni1 O1 C9 -35.7(9) . . . . ? O2 Ni1 O1 C9 95.7(3) 2_667 . . . ? N1S Ni1 O1 C10 5.7(3) . . . . ? N2 Ni1 O1 C10 -169.2(3) . . . . ? N2S Ni1 O1 C10 93.2(3) . . . . ? N1 Ni1 O1 C10 140.3(7) . . . . ? O2 Ni1 O1 C10 -88.3(3) 2_667 . . . ? N1S Ni1 N1 C7 -146.5(3) . . . . ? N2 Ni1 N1 C7 29.2(3) . . . . ? N2S Ni1 N1 C7 125.7(3) . . . . ? O1 Ni1 N1 C7 78.7(8) . . . . ? O2 Ni1 N1 C7 -52.9(3) 2_667 . . . ? N2S Ni1 N1S C1S 36.0(13) . . . . ? N1 Ni1 N1S C1S -51.3(13) . . . . ? O1 Ni1 N1S C1S 121.4(13) . . . . ? O2 Ni1 N1S C1S -143.0(13) 2_667 . . . ? C2 C1 N2 C8 178.5(4) . . . . ? C2 C1 N2 C13 57.5(5) . . . 2_667 ? C2 C1 N2 Ni1 -65.4(4) . . . . ? N2S Ni1 N2 C8 51.1(3) . . . . ? N1 Ni1 N2 C8 138.9(3) . . . . ? O1 Ni1 N2 C8 -33.2(2) . . . . ? O2 Ni1 N2 C8 -130.1(3) 2_667 . . . ? N2S Ni1 N2 C13 168.5(3) . . . 2_667 ? N1 Ni1 N2 C13 -103.7(3) . . . 2_667 ? O1 Ni1 N2 C13 84.2(3) . . . 2_667 ? O2 Ni1 N2 C13 -12.7(3) 2_667 . . 2_667 ? N2S Ni1 N2 C1 -66.4(3) . . . . ? N1 Ni1 N2 C1 21.4(3) . . . . ? O1 Ni1 N2 C1 -150.7(3) . . . . ? O2 Ni1 N2 C1 112.4(3) 2_667 . . . ? N2 C1 C2 C7 63.0(5) . . . . ? N2 C1 C2 C3 -116.5(4) . . . . ? C7 C2 C3 C4 -1.1(7) . . . . ? C1 C2 C3 C4 178.5(4) . . . . ? C2 C3 C4 C5 0.2(8) . . . . ? C3 C4 C5 C6 -0.3(8) . . . . ? C4 C5 C6 C7 1.3(8) . . . . ? C5 C6 C7 C2 -2.3(7) . . . . ? C5 C6 C7 N1 -178.9(4) . . . . ? C3 C2 C7 C6 2.1(6) . . . . ? C1 C2 C7 C6 -177.5(4) . . . . ? C3 C2 C7 N1 178.8(4) . . . . ? C1 C2 C7 N1 -0.7(6) . . . . ? Ni1 N1 C7 C6 133.3(4) . . . . ? Ni1 N1 C7 C2 -43.4(5) . . . . ? C13 N2 C8 C9 -69.0(5) 2_667 . . . ? C1 N2 C8 C9 167.5(4) . . . . ? Ni1 N2 C8 C9 48.8(4) . . . . ? C10 O1 C9 C8 -169.0(4) . . . . ? Ni1 O1 C9 C8 7.7(5) . . . . ? N2 C8 C9 O1 -37.0(6) . . . . ? C9 O1 C10 C11 -94.7(4) . . . . ? Ni1 O1 C10 C11 89.3(4) . . . . ? C12 O2 C11 C10 -76.2(4) . . . . ? Ni1 O2 C11 C10 151.9(3) 2_667 . . . ? O1 C10 C11 O2 -79.5(4) . . . . ? C11 O2 C12 C13 -169.8(3) . . . . ? Ni1 O2 C12 C13 -33.4(4) 2_667 . . . ? O2 C12 C13 N2 46.3(5) . . . 2_667 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H2N O6 0.78(4) 2.38(4) 3.160(5) 173(4) 2_657 N1 H1N O6 0.89(4) 2.22(4) 3.025(5) 151(4) . _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.517 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.080