# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' #TrackingRef 'Compiled.cif' # SUBMISSION DETAILS _journal_coden_Cambridge 0222 _publ_contact_author_name 'Laurence K. Thompson' _publ_contact_author_address ; Department of Chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; _publ_contact_author_email lk.thompson@mun.ca _publ_contact_author_phone 1-709-864-8750 _publ_contact_author_fax 1-709-864-3702 _publ_section_title ; Complexes of ditopic carbo- and thio-carbohydrazone ligands - mononuclear, 1D chain, dinuclear and tetranuclear examples. ; _publ_section_abstract ; Please see full paper. ; loop_ _publ_author_name _publ_author_address 'Santokh S. Tandon' ; Department of Chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; 'John L. Lee' ; Department of Chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; 'Marie-Claire Dul' ; Department of Chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; 'Louise N. Dawe ' ; Department of Chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; 'Laurence K. Thompson ' ; Department of Chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; data_1 _database_code_depnum_ccdc_archive 'CCDC 798363' #TrackingRef 'Compiled.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C12 H14 O2 N6)2 Co2 (C H3 O)](Cl O4) (H2 O)1.8' _chemical_formula_sum 'C25 H34.60 Cl Co2 N12 O10.80' _chemical_formula_weight 829.34 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' 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 28.548(9) _cell_length_b 16.552(5) _cell_length_c 16.073(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.443(5) _cell_angle_gamma 90.00 _cell_volume 7069(4) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 13615 _cell_measurement_theta_min 2.1720 _cell_measurement_theta_max 30.8409 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3408 _exptl_absorpt_coefficient_mu 1.086 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9772 _exptl_absorpt_correction_T_min 0.8870 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 46312 _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 26.50 _reflns_number_total 7297 _reflns_number_gt 6660 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.1251P)^2^+61.7391P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7297 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.1033 _refine_ls_wR_factor_ref 0.2746 _refine_ls_wR_factor_gt 0.2672 _refine_ls_goodness_of_fit_ref 1.196 _refine_ls_restrained_S_all 1.196 _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 Co1 Co 0.13088(3) 0.01865(5) 0.73604(5) 0.0289(3) Uani 1 1 d . . . Co2 Co 0.22709(3) 0.12180(5) 0.82516(5) 0.0296(3) Uani 1 1 d . . . Cl1 Cl 0.35614(14) 0.12722(18) 0.6004(2) 0.0878(9) Uani 1 1 d . . . O1 O 0.22494(19) -0.0156(3) 0.6146(3) 0.0440(12) Uani 1 1 d . . . O2 O 0.27633(18) 0.2745(3) 0.8558(3) 0.0398(11) Uani 1 1 d . . . O3 O 0.13098(18) 0.1787(3) 0.9392(3) 0.0410(11) Uani 1 1 d . . . O4 O 0.04191(17) -0.0109(3) 0.5899(3) 0.0366(10) Uani 1 1 d . . . O5 O 0.19983(16) 0.0137(3) 0.8269(3) 0.0315(9) Uani 1 1 d . . . O6 O 0.3316(6) 0.0565(8) 0.6002(9) 0.159(6) Uani 1 1 d . . . O7 O 0.3612(5) 0.1381(7) 0.5162(7) 0.130(4) Uani 1 1 d . . . O8 O 0.3288(5) 0.1910(7) 0.6178(8) 0.132(4) Uani 1 1 d . . . O9 O 0.4056(5) 0.1245(7) 0.6711(8) 0.144(5) Uani 1 1 d . . . O10 O 0.0303(4) 0.3620(6) 0.4499(10) 0.073(4) Uani 0.60 1 d P A 1 O12 O 0.0516(10) 0.4609(16) 0.7877(17) 0.139(8) Uiso 0.50 1 d P B 1 O11 O 0.0459(9) 0.3168(11) 0.4980(15) 0.089(7) Uani 0.40 1 d P C 2 O13 O 0.0000 0.449(3) 0.7500 0.191(17) Uiso 0.50 2 d SP D 2 N1 N 0.09708(19) -0.0416(3) 0.8012(3) 0.0313(11) Uani 1 1 d . . . N2 N 0.1352(2) -0.0847(3) 0.6914(3) 0.0326(11) Uani 1 1 d . . . N3 N 0.1617(2) -0.0872(3) 0.6353(4) 0.0409(13) Uani 1 1 d . . . H8 H 0.1775 -0.1280 0.6366 0.083 Uiso 1 1 d . . . N4 N 0.1657(2) 0.0495(3) 0.6603(3) 0.0323(11) Uani 1 1 d . . . N5 N 0.1998(2) 0.1129(3) 0.6992(3) 0.0305(11) Uani 1 1 d . . . N6 N 0.2483(2) 0.2236(3) 0.7966(3) 0.0333(11) Uani 1 1 d . . . N7 N 0.2951(2) 0.0811(3) 0.8528(4) 0.0355(12) Uani 1 1 d . . . N8 N 0.2513(2) 0.1398(3) 0.9491(3) 0.0331(11) Uani 1 1 d . . . N9 N 0.2163(2) 0.1720(3) 0.9783(3) 0.0333(12) Uani 1 1 d . . . H22 H 0.2218 0.1769 1.0304 0.057 Uiso 1 1 d . . . N10 N 0.1662(2) 0.1640(3) 0.8304(3) 0.0309(11) Uani 1 1 d . . . N11 N 0.1239(2) 0.1240(3) 0.7705(4) 0.0325(11) Uani 1 1 d . . . N12 N 0.0668(2) 0.0416(3) 0.6467(3) 0.0331(11) Uani 1 1 d . . . C1 C 0.0813(3) -0.0144(4) 0.8646(5) 0.0369(14) Uani 1 1 d . . . H1 H 0.0859 0.0410 0.8809 0.044 Uiso 1 1 calc R . . C2 C 0.0583(3) -0.0645(5) 0.9075(5) 0.0439(16) Uani 1 1 d . . . H2 H 0.0483 -0.0442 0.9537 0.053 Uiso 1 1 calc R . . C3 C 0.0503(3) -0.1446(5) 0.8815(5) 0.0461(17) Uani 1 1 d . . . H3 H 0.0334 -0.1798 0.9080 0.055 Uiso 1 1 calc R . . C4 C 0.0675(3) -0.1734(4) 0.8157(5) 0.0411(15) Uani 1 1 d . . . H4 H 0.0634 -0.2287 0.7985 0.049 Uiso 1 1 calc R . . C5 C 0.0904(2) -0.1203(4) 0.7761(4) 0.0340(14) Uani 1 1 d . . . C6 C 0.1121(3) -0.1439(4) 0.7095(4) 0.0349(14) Uani 1 1 d . . . C7 C 0.1085(3) -0.2258(4) 0.6709(6) 0.0503(19) Uani 1 1 d . . . H5 H 0.0746 -0.2474 0.6583 0.060 Uiso 1 1 calc R . . H6 H 0.1333 -0.2612 0.7135 0.060 Uiso 1 1 calc R . . H7 H 0.1151 -0.2231 0.6153 0.060 Uiso 1 1 calc R . . C8 C 0.1888(3) -0.0157(4) 0.6366(4) 0.0383(15) Uani 1 1 d . . . C9 C 0.2049(3) 0.1740(4) 0.6540(4) 0.0385(15) Uani 1 1 d . . . C10 C 0.1835(4) 0.1793(5) 0.5551(5) 0.062(2) Uani 1 1 d . . . H9 H 0.1767 0.1248 0.5297 0.075 Uiso 1 1 calc R . . H10 H 0.2075 0.2064 0.5339 0.075 Uiso 1 1 calc R . . H11 H 0.1521 0.2103 0.5363 0.075 Uiso 1 1 calc R . . C11 C 0.2343(3) 0.2390(4) 0.7102(4) 0.0392(15) Uani 1 1 d . . . C12 C 0.2485(4) 0.3143(5) 0.6766(5) 0.057(2) Uani 1 1 d . . . H12 H 0.2512 0.3042 0.6185 0.068 Uiso 1 1 calc R . . H13 H 0.2809 0.3333 0.7190 0.068 Uiso 1 1 calc R . . H14 H 0.2227 0.3556 0.6699 0.068 Uiso 1 1 calc R . . C13 C 0.3155(3) 0.0521(5) 0.7972(6) 0.0483(18) Uani 1 1 d . . . H15 H 0.2955 0.0490 0.7353 0.058 Uiso 1 1 calc R . . C14 C 0.3651(4) 0.0259(7) 0.8262(7) 0.070(3) Uani 1 1 d . . . H16 H 0.3785 0.0020 0.7860 0.084 Uiso 1 1 calc R . . C15 C 0.3942(4) 0.0357(7) 0.9153(7) 0.074(3) Uani 1 1 d . . . H17 H 0.4290 0.0221 0.9363 0.088 Uiso 1 1 calc R . . C16 C 0.3735(3) 0.0651(7) 0.9735(6) 0.061(2) Uani 1 1 d . . . H18 H 0.3931 0.0694 1.0355 0.073 Uiso 1 1 calc R . . C17 C 0.3242(3) 0.0881(5) 0.9412(5) 0.0418(16) Uani 1 1 d . . . C18 C 0.2967(3) 0.1215(4) 0.9967(4) 0.0355(14) Uani 1 1 d . . . C19 C 0.3194(3) 0.1282(5) 1.0963(5) 0.0446(17) Uani 1 1 d . . . H19 H 0.3457 0.0871 1.1199 0.054 Uiso 1 1 calc R . . H20 H 0.2932 0.1197 1.1213 0.054 Uiso 1 1 calc R . . H21 H 0.3341 0.1820 1.1129 0.054 Uiso 1 1 calc R . . C20 C 0.1672(3) 0.1710(4) 0.9167(4) 0.0346(14) Uani 1 1 d . . . C21 C 0.0842(3) 0.1639(4) 0.7197(4) 0.0363(14) Uani 1 1 d . . . C22 C 0.0494(3) 0.1155(4) 0.6502(5) 0.0361(14) Uani 1 1 d . . . C23 C -0.0002(3) 0.1436(5) 0.5850(5) 0.0445(17) Uani 1 1 d . . . H26 H 0.0040 0.1964 0.5608 0.053 Uiso 1 1 calc R . . H27 H -0.0243 0.1485 0.6152 0.053 Uiso 1 1 calc R . . H28 H -0.0128 0.1045 0.5360 0.053 Uiso 1 1 calc R . . C24 C 0.2090(3) -0.0251(4) 0.9087(4) 0.0379(15) Uani 1 1 d . . . H29 H 0.2452 -0.0252 0.9436 0.045 Uiso 1 1 calc R . . H30 H 0.1967 -0.0809 0.8979 0.045 Uiso 1 1 calc R . . H31 H 0.1914 0.0036 0.9420 0.045 Uiso 1 1 calc R . . C25 C 0.0762(3) 0.2520(4) 0.7308(6) 0.054(2) Uani 1 1 d . . . H23 H 0.1089 0.2795 0.7543 0.065 Uiso 1 1 calc R . . H24 H 0.0587 0.2590 0.7727 0.065 Uiso 1 1 calc R . . H25 H 0.0559 0.2753 0.6728 0.065 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 0.0339(5) 0.0258(4) 0.0275(5) -0.0022(3) 0.0118(4) -0.0011(3) Co2 0.0335(5) 0.0297(5) 0.0259(4) -0.0009(3) 0.0112(4) -0.0029(3) Cl1 0.112(2) 0.0726(17) 0.0823(19) 0.0036(14) 0.0399(18) -0.0069(16) O1 0.048(3) 0.046(3) 0.048(3) -0.008(2) 0.030(2) -0.006(2) O2 0.047(3) 0.040(3) 0.034(2) -0.004(2) 0.016(2) -0.014(2) O3 0.043(3) 0.043(3) 0.039(3) -0.008(2) 0.018(2) -0.002(2) O4 0.038(2) 0.033(2) 0.033(2) -0.0058(18) 0.006(2) -0.0090(19) O5 0.034(2) 0.034(2) 0.028(2) -0.0024(17) 0.0129(18) -0.0022(18) O6 0.225(14) 0.134(10) 0.148(10) -0.036(8) 0.103(10) -0.103(10) O7 0.190(12) 0.124(8) 0.105(7) 0.039(6) 0.087(8) 0.036(8) O8 0.157(10) 0.126(9) 0.133(9) 0.010(7) 0.078(8) 0.061(8) O9 0.137(10) 0.122(9) 0.118(8) 0.006(7) -0.018(7) 0.002(7) O10 0.061(6) 0.021(4) 0.142(12) -0.032(6) 0.043(7) -0.012(4) O11 0.16(2) 0.036(8) 0.124(16) 0.004(10) 0.110(16) 0.000(11) N1 0.027(3) 0.035(3) 0.031(3) 0.002(2) 0.008(2) 0.001(2) N2 0.039(3) 0.033(3) 0.029(3) -0.001(2) 0.015(2) 0.002(2) N3 0.060(4) 0.032(3) 0.042(3) -0.003(2) 0.032(3) -0.004(3) N4 0.036(3) 0.028(3) 0.030(3) -0.006(2) 0.009(2) -0.006(2) N5 0.032(3) 0.034(3) 0.026(3) -0.004(2) 0.011(2) -0.005(2) N6 0.038(3) 0.034(3) 0.026(3) -0.003(2) 0.009(2) -0.006(2) N7 0.036(3) 0.034(3) 0.037(3) 0.003(2) 0.015(2) 0.001(2) N8 0.043(3) 0.030(3) 0.026(3) -0.002(2) 0.012(2) -0.005(2) N9 0.042(3) 0.031(3) 0.030(3) -0.004(2) 0.017(2) -0.003(2) N10 0.035(3) 0.030(3) 0.026(2) -0.005(2) 0.010(2) -0.003(2) N11 0.037(3) 0.029(3) 0.030(3) -0.005(2) 0.009(2) 0.001(2) N12 0.036(3) 0.035(3) 0.026(3) 0.001(2) 0.009(2) -0.004(2) C1 0.039(4) 0.037(3) 0.037(3) 0.001(3) 0.017(3) -0.001(3) C2 0.046(4) 0.048(4) 0.042(4) 0.008(3) 0.021(3) 0.009(3) C3 0.045(4) 0.049(4) 0.050(4) 0.012(3) 0.024(3) 0.000(3) C4 0.042(4) 0.033(3) 0.050(4) 0.000(3) 0.018(3) -0.003(3) C5 0.034(3) 0.031(3) 0.036(3) -0.002(3) 0.011(3) 0.001(3) C6 0.041(4) 0.025(3) 0.038(3) -0.001(3) 0.014(3) -0.003(3) C7 0.067(5) 0.032(4) 0.058(5) -0.011(3) 0.030(4) -0.007(3) C8 0.046(4) 0.038(4) 0.033(3) -0.005(3) 0.016(3) 0.000(3) C9 0.046(4) 0.038(4) 0.032(3) -0.001(3) 0.013(3) -0.009(3) C10 0.092(7) 0.054(5) 0.035(4) 0.001(3) 0.016(4) -0.021(5) C11 0.047(4) 0.036(3) 0.031(3) 0.002(3) 0.011(3) -0.009(3) C12 0.072(6) 0.048(4) 0.041(4) 0.006(3) 0.009(4) -0.020(4) C13 0.048(4) 0.052(4) 0.051(4) 0.002(4) 0.026(4) 0.006(3) C14 0.056(5) 0.098(8) 0.062(6) 0.006(5) 0.031(5) 0.021(5) C15 0.046(5) 0.106(8) 0.072(6) 0.016(6) 0.026(5) 0.026(5) C16 0.041(4) 0.092(7) 0.046(4) 0.007(4) 0.010(4) 0.012(4) C17 0.041(4) 0.043(4) 0.041(4) 0.004(3) 0.014(3) 0.000(3) C18 0.042(4) 0.031(3) 0.030(3) 0.000(2) 0.009(3) -0.006(3) C19 0.043(4) 0.046(4) 0.036(4) 0.003(3) 0.005(3) -0.005(3) C20 0.044(4) 0.029(3) 0.033(3) -0.001(2) 0.016(3) 0.001(3) C21 0.038(3) 0.032(3) 0.038(3) -0.006(3) 0.013(3) 0.000(3) C22 0.042(4) 0.029(3) 0.038(3) 0.000(3) 0.014(3) -0.001(3) C23 0.037(4) 0.041(4) 0.049(4) 0.000(3) 0.009(3) 0.002(3) C24 0.046(4) 0.035(3) 0.031(3) 0.005(3) 0.011(3) -0.001(3) C25 0.055(5) 0.035(4) 0.054(5) -0.008(3) -0.001(4) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N11 1.862(5) . ? Co1 N2 1.876(5) . ? Co1 N4 1.902(5) . ? Co1 N12 1.906(5) . ? Co1 N1 1.940(5) . ? Co1 O5 1.978(4) . ? Co2 N8 1.878(5) . ? Co2 N5 1.891(5) . ? Co2 N6 1.902(5) . ? Co2 N10 1.904(5) . ? Co2 N7 1.947(6) . ? Co2 O5 1.956(4) . ? Cl1 O6 1.363(10) . ? Cl1 O8 1.399(10) . ? Cl1 O7 1.424(9) . ? Cl1 O9 1.453(11) . ? O1 C8 1.209(8) . ? O2 N6 1.303(7) . ? O3 C20 1.221(8) . ? O4 N12 1.272(7) . ? O5 C24 1.400(8) . ? N1 C1 1.333(8) . ? N1 C5 1.357(8) . ? N2 C6 1.274(8) . ? N2 N3 1.374(7) . ? N3 C8 1.410(9) . ? N3 H8 0.8073 . ? N4 C8 1.387(9) . ? N4 N5 1.411(7) . ? N5 C9 1.285(9) . ? N6 C11 1.322(8) . ? N7 C13 1.323(9) . ? N7 C17 1.363(9) . ? N8 C18 1.278(9) . ? N8 N9 1.360(8) . ? N9 C20 1.388(9) . ? N9 H22 0.7972 . ? N10 C20 1.382(8) . ? N10 N11 1.405(7) . ? N11 C21 1.308(9) . ? N12 C22 1.329(9) . ? C1 C2 1.387(10) . ? C1 H1 0.9500 . ? C2 C3 1.384(11) . ? C2 H2 0.9500 . ? C3 C4 1.401(10) . ? C3 H3 0.9500 . ? C4 C5 1.383(10) . ? C4 H4 0.9500 . ? C5 C6 1.471(9) . ? C6 C7 1.479(9) . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C7 H7 0.9800 . ? C9 C11 1.456(9) . ? C9 C10 1.483(10) . ? C10 H9 0.9800 . ? C10 H10 0.9800 . ? C10 H11 0.9800 . ? C11 C12 1.473(10) . ? C12 H12 0.9800 . ? C12 H13 0.9800 . ? C12 H14 0.9800 . ? C13 C14 1.389(12) . ? C13 H15 0.9500 . ? C14 C15 1.377(14) . ? C14 H16 0.9500 . ? C15 C16 1.367(13) . ? C15 H17 0.9500 . ? C16 C17 1.363(11) . ? C16 H18 0.9500 . ? C17 C18 1.493(10) . ? C18 C19 1.494(9) . ? C19 H19 0.9800 . ? C19 H20 0.9800 . ? C19 H21 0.9800 . ? C21 C22 1.437(9) . ? C21 C25 1.497(9) . ? C22 C23 1.495(10) . ? C23 H26 0.9800 . ? C23 H27 0.9800 . ? C23 H28 0.9800 . ? C24 H29 0.9800 . ? C24 H30 0.9800 . ? C24 H31 0.9800 . ? C25 H23 0.9800 . ? C25 H24 0.9800 . ? C25 H25 0.9800 . ? 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 N11 Co1 N2 175.2(2) . . ? N11 Co1 N4 94.4(2) . . ? N2 Co1 N4 82.9(2) . . ? N11 Co1 N12 81.9(2) . . ? N2 Co1 N12 94.2(2) . . ? N4 Co1 N12 92.7(2) . . ? N11 Co1 N1 101.1(2) . . ? N2 Co1 N1 81.6(2) . . ? N4 Co1 N1 164.5(2) . . ? N12 Co1 N1 88.8(2) . . ? N11 Co1 O5 90.3(2) . . ? N2 Co1 O5 93.3(2) . . ? N4 Co1 O5 82.6(2) . . ? N12 Co1 O5 170.6(2) . . ? N1 Co1 O5 97.9(2) . . ? N8 Co2 N5 174.8(2) . . ? N8 Co2 N6 95.1(2) . . ? N5 Co2 N6 81.6(2) . . ? N8 Co2 N10 83.3(2) . . ? N5 Co2 N10 92.9(2) . . ? N6 Co2 N10 93.6(2) . . ? N8 Co2 N7 82.1(2) . . ? N5 Co2 N7 101.8(2) . . ? N6 Co2 N7 89.0(2) . . ? N10 Co2 N7 165.3(2) . . ? N8 Co2 O5 97.1(2) . . ? N5 Co2 O5 86.2(2) . . ? N6 Co2 O5 167.7(2) . . ? N10 Co2 O5 87.7(2) . . ? N7 Co2 O5 92.8(2) . . ? O6 Cl1 O8 109.0(9) . . ? O6 Cl1 O7 109.6(8) . . ? O8 Cl1 O7 110.6(7) . . ? O6 Cl1 O9 109.0(8) . . ? O8 Cl1 O9 108.7(8) . . ? O7 Cl1 O9 109.9(8) . . ? C24 O5 Co2 119.6(4) . . ? C24 O5 Co1 120.4(4) . . ? Co2 O5 Co1 104.2(2) . . ? C1 N1 C5 120.1(6) . . ? C1 N1 Co1 127.8(5) . . ? C5 N1 Co1 112.1(4) . . ? C6 N2 N3 125.6(6) . . ? C6 N2 Co1 120.2(5) . . ? N3 N2 Co1 114.1(4) . . ? N2 N3 C8 113.2(5) . . ? N2 N3 H8 116.3 . . ? C8 N3 H8 113.9 . . ? C8 N4 N5 112.4(5) . . ? C8 N4 Co1 112.2(4) . . ? N5 N4 Co1 110.6(4) . . ? C9 N5 N4 122.5(5) . . ? C9 N5 Co2 117.1(4) . . ? N4 N5 Co2 118.7(4) . . ? O2 N6 C11 120.8(5) . . ? O2 N6 Co2 124.1(4) . . ? C11 N6 Co2 115.1(4) . . ? C13 N7 C17 118.9(6) . . ? C13 N7 Co2 128.3(5) . . ? C17 N7 Co2 112.7(5) . . ? C18 N8 N9 126.8(6) . . ? C18 N8 Co2 119.9(5) . . ? N9 N8 Co2 113.3(4) . . ? N8 N9 C20 115.3(5) . . ? N8 N9 H22 120.9 . . ? C20 N9 H22 120.7 . . ? C20 N10 N11 115.1(5) . . ? C20 N10 Co2 113.0(4) . . ? N11 N10 Co2 111.5(4) . . ? C21 N11 N10 121.4(5) . . ? C21 N11 Co1 116.7(4) . . ? N10 N11 Co1 119.1(4) . . ? O4 N12 C22 122.7(6) . . ? O4 N12 Co1 122.3(4) . . ? C22 N12 Co1 115.0(4) . . ? N1 C1 C2 122.1(7) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 118.5(7) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 119.3(7) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 119.1(7) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 120.8(6) . . ? N1 C5 C6 114.9(6) . . ? C4 C5 C6 124.2(6) . . ? N2 C6 C5 110.6(6) . . ? N2 C6 C7 124.9(6) . . ? C5 C6 C7 124.4(6) . . ? C6 C7 H5 109.5 . . ? C6 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C6 C7 H7 109.5 . . ? H5 C7 H7 109.5 . . ? H6 C7 H7 109.5 . . ? O1 C8 N4 128.5(7) . . ? O1 C8 N3 121.2(6) . . ? N4 C8 N3 110.2(6) . . ? N5 C9 C11 113.0(6) . . ? N5 C9 C10 124.4(6) . . ? C11 C9 C10 122.6(6) . . ? C9 C10 H9 109.5 . . ? C9 C10 H10 109.5 . . ? H9 C10 H10 109.5 . . ? C9 C10 H11 109.5 . . ? H9 C10 H11 109.5 . . ? H10 C10 H11 109.5 . . ? N6 C11 C9 113.2(6) . . ? N6 C11 C12 122.0(6) . . ? C9 C11 C12 124.8(6) . . ? C11 C12 H12 109.5 . . ? C11 C12 H13 109.5 . . ? H12 C12 H13 109.5 . . ? C11 C12 H14 109.5 . . ? H12 C12 H14 109.5 . . ? H13 C12 H14 109.5 . . ? N7 C13 C14 122.2(8) . . ? N7 C13 H15 118.9 . . ? C14 C13 H15 118.9 . . ? C15 C14 C13 117.8(9) . . ? C15 C14 H16 121.1 . . ? C13 C14 H16 121.1 . . ? C16 C15 C14 120.4(8) . . ? C16 C15 H17 119.8 . . ? C14 C15 H17 119.8 . . ? C17 C16 C15 119.0(8) . . ? C17 C16 H18 120.5 . . ? C15 C16 H18 120.5 . . ? C16 C17 N7 121.6(7) . . ? C16 C17 C18 124.8(7) . . ? N7 C17 C18 113.6(6) . . ? N8 C18 C17 111.7(6) . . ? N8 C18 C19 124.8(7) . . ? C17 C18 C19 123.5(6) . . ? C18 C19 H19 109.5 . . ? C18 C19 H20 109.5 . . ? H19 C19 H20 109.5 . . ? C18 C19 H21 109.5 . . ? H19 C19 H21 109.5 . . ? H20 C19 H21 109.5 . . ? O3 C20 N10 126.7(6) . . ? O3 C20 N9 122.0(6) . . ? N10 C20 N9 111.3(5) . . ? N11 C21 C22 113.5(6) . . ? N11 C21 C25 123.5(6) . . ? C22 C21 C25 122.9(6) . . ? N12 C22 C21 112.5(6) . . ? N12 C22 C23 122.0(6) . . ? C21 C22 C23 125.5(6) . . ? C22 C23 H26 109.5 . . ? C22 C23 H27 109.5 . . ? H26 C23 H27 109.5 . . ? C22 C23 H28 109.5 . . ? H26 C23 H28 109.5 . . ? H27 C23 H28 109.5 . . ? O5 C24 H29 109.5 . . ? O5 C24 H30 109.5 . . ? H29 C24 H30 109.5 . . ? O5 C24 H31 109.5 . . ? H29 C24 H31 109.5 . . ? H30 C24 H31 109.5 . . ? C21 C25 H23 109.5 . . ? C21 C25 H24 109.5 . . ? H23 C25 H24 109.5 . . ? C21 C25 H25 109.5 . . ? H23 C25 H25 109.5 . . ? H24 C25 H25 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.356 _refine_diff_density_min -1.339 _refine_diff_density_rms 0.148 data_2 _database_code_depnum_ccdc_archive 'CCDC 798364' #TrackingRef 'Compiled.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H8 N4 Ni O5, 2(H2 O), 0.5(H2 O)' _chemical_formula_sum 'C7 H13 N4 Ni O7.50' _chemical_formula_weight 331.90 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' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 14.584(9) _cell_length_b 7.305(4) _cell_length_c 12.245(7) _cell_angle_alpha 90.00 _cell_angle_beta 107.787(7) _cell_angle_gamma 90.00 _cell_volume 1242.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 3764 _cell_measurement_theta_min 1.7466 _cell_measurement_theta_max 29.5127 _exptl_crystal_description Prism _exptl_crystal_colour 'Light Blue' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 1.604 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9761 _exptl_absorpt_correction_T_min 0.8553 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 15333 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 26.48 _reflns_number_total 2553 _reflns_number_gt 2535 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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. Collection, solution and refinement proceeded normally. H (9-12) were initially introduced in difference map positions and refined positionally, with fixed thermal parameters. Subsequently, they were refined on a riding model. All other hydrogen atoms were introduced in calculated positions with isotropic thermal parameters set twenty percent greater than those of their bonding partners and were refined on the riding model. Protons on the half-occupancy lattice water molecule, O(8), could not be located in difference maps, and were therefore, omitted from the model. All non-hydrogen atoms were refined anisotropically. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+9.0443P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0105(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2553 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1591 _refine_ls_wR_factor_gt 0.1589 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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 Ni1 Ni 0.25305(4) 0.55207(8) 0.34376(5) 0.0161(2) Uani 1 1 d . . . O1 O 0.3416(2) 0.4589(5) 0.4948(3) 0.0230(7) Uani 1 1 d . . . O2 O 0.4704(2) 0.2829(5) 0.5657(3) 0.0227(7) Uani 1 1 d . . . O3 O 0.2865(3) 0.4560(5) -0.0134(3) 0.0304(9) Uani 1 1 d . . . O4 O 0.0164(3) 0.8578(6) 0.2947(3) 0.0367(10) Uani 1 1 d . . . O5 O 0.1509(2) 0.7021(5) 0.3814(3) 0.0251(7) Uani 1 1 d . . . O6 O 0.1716(2) 0.3134(5) 0.3233(4) 0.0330(9) Uani 1 1 d . . . H9 H 0.1835 0.2105 0.3337 0.040 Uiso 1 1 d . . . H10 H 0.1135 0.3144 0.2931 0.040 Uiso 1 1 d . . . O7 O 0.3375(2) 0.7886(5) 0.3561(3) 0.0241(7) Uani 1 1 d . . . H11 H 0.3253 0.8541 0.4048 0.029 Uiso 1 1 d . . . H12 H 0.3961 0.7681 0.3771 0.029 Uiso 1 1 d . . . O8 O 0.2443(8) 0.4563(12) 0.6792(8) 0.048(2) Uani 0.50 1 d P . . N1 N 0.3478(3) 0.4128(5) 0.2850(3) 0.0188(8) Uani 1 1 d . . . N2 N 0.3430(3) 0.4004(6) 0.1729(3) 0.0227(9) Uani 1 1 d . . . H4 H 0.3875 0.3335 0.1571 0.027 Uiso 1 1 calc R . . N3 N 0.1992(3) 0.5831(6) 0.0869(3) 0.0259(9) Uani 1 1 d . . . H5 H 0.1611 0.6256 0.0216 0.031 Uiso 1 1 calc R . . N4 N 0.1759(3) 0.6254(6) 0.1843(3) 0.0209(8) Uani 1 1 d . . . C1 C 0.4079(3) 0.3597(7) 0.4837(4) 0.0200(9) Uani 1 1 d . . . C2 C 0.4139(3) 0.3271(6) 0.3632(4) 0.0210(9) Uani 1 1 d . . . C3 C 0.4912(4) 0.2079(8) 0.3454(5) 0.0304(11) Uani 1 1 d . . . H1 H 0.5528 0.2732 0.3700 0.036 Uiso 1 1 calc R . . H2 H 0.4755 0.1766 0.2639 0.036 Uiso 1 1 calc R . . H3 H 0.4960 0.0955 0.3905 0.036 Uiso 1 1 calc R . . C4 C 0.2769(4) 0.4801(7) 0.0823(4) 0.0243(10) Uani 1 1 d . . . C5 C 0.0995(3) 0.7170(7) 0.1774(4) 0.0243(10) Uani 1 1 d . . . C6 C 0.0281(5) 0.7838(11) 0.0681(5) 0.0452(16) Uani 1 1 d . . . H6 H -0.0022 0.6787 0.0211 0.054 Uiso 1 1 calc R . . H7 H 0.0614 0.8587 0.0256 0.054 Uiso 1 1 calc R . . H8 H -0.0214 0.8575 0.0864 0.054 Uiso 1 1 calc R . . C7 C 0.0860(3) 0.7635(7) 0.2935(4) 0.0227(10) 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 0.0137(3) 0.0219(4) 0.0128(3) -0.0001(2) 0.0041(2) 0.0014(2) O1 0.0183(15) 0.0306(19) 0.0194(16) 0.0046(14) 0.0049(13) 0.0038(14) O2 0.0147(14) 0.0332(19) 0.0181(15) 0.0066(14) 0.0021(12) 0.0027(13) O3 0.047(2) 0.032(2) 0.0173(17) 0.0088(14) 0.0161(16) 0.0197(17) O4 0.0262(18) 0.056(3) 0.0279(19) -0.0031(19) 0.0080(15) 0.0145(18) O5 0.0194(15) 0.036(2) 0.0177(16) -0.0042(14) 0.0030(13) 0.0015(14) O6 0.0185(16) 0.0271(19) 0.049(2) 0.0120(17) 0.0038(16) -0.0028(14) O7 0.0175(15) 0.0228(17) 0.0304(18) -0.0018(14) 0.0046(13) 0.0005(13) O8 0.079(7) 0.028(4) 0.049(5) -0.003(4) 0.039(5) 0.006(4) N1 0.0173(18) 0.0214(19) 0.0179(18) -0.0038(15) 0.0058(15) -0.0040(15) N2 0.028(2) 0.029(2) 0.0137(18) 0.0032(16) 0.0095(16) 0.0079(17) N3 0.027(2) 0.036(2) 0.0165(19) 0.0051(17) 0.0091(16) 0.0147(18) N4 0.0219(19) 0.025(2) 0.0160(18) 0.0004(16) 0.0062(15) 0.0002(16) C1 0.016(2) 0.023(2) 0.020(2) 0.0013(18) 0.0039(17) -0.0036(17) C2 0.015(2) 0.022(2) 0.023(2) -0.0008(18) 0.0029(17) -0.0014(17) C3 0.031(3) 0.034(3) 0.027(3) 0.002(2) 0.011(2) 0.012(2) C4 0.028(2) 0.024(2) 0.022(2) 0.0032(19) 0.0100(19) 0.007(2) C5 0.022(2) 0.030(3) 0.022(2) 0.002(2) 0.0080(18) 0.0030(19) C6 0.043(3) 0.066(4) 0.026(3) 0.009(3) 0.009(2) 0.027(3) C7 0.017(2) 0.031(2) 0.020(2) -0.0024(19) 0.0050(17) 0.0027(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N4 2.006(4) . ? Ni1 O5 2.013(4) . ? Ni1 N1 2.017(4) . ? Ni1 O1 2.023(3) . ? Ni1 O6 2.081(4) . ? Ni1 O7 2.101(4) . ? O1 C1 1.248(6) . ? O2 C1 1.262(6) . ? O3 C4 1.234(6) . ? O4 C7 1.231(6) . ? O5 C7 1.279(6) . ? O6 H9 0.7731 . ? O6 H10 0.8141 . ? O7 H11 0.8256 . ? O7 H12 0.8271 . ? N1 C2 1.294(6) . ? N1 N2 1.356(5) . ? N2 C4 1.358(6) . ? N2 H4 0.8800 . ? N3 N4 1.371(6) . ? N3 C4 1.376(6) . ? N3 H5 0.8800 . ? N4 C5 1.281(6) . ? C1 C2 1.524(7) . ? C2 C3 1.492(7) . ? C3 H1 0.9800 . ? C3 H2 0.9800 . ? C3 H3 0.9800 . ? C5 C6 1.504(7) . ? C5 C7 1.532(7) . ? C6 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? 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 N4 Ni1 O5 81.00(15) . . ? N4 Ni1 N1 91.64(17) . . ? O5 Ni1 N1 172.59(15) . . ? N4 Ni1 O1 172.47(15) . . ? O5 Ni1 O1 106.53(14) . . ? N1 Ni1 O1 80.84(15) . . ? N4 Ni1 O6 88.68(16) . . ? O5 Ni1 O6 92.77(16) . . ? N1 Ni1 O6 87.87(16) . . ? O1 Ni1 O6 90.56(15) . . ? N4 Ni1 O7 89.56(15) . . ? O5 Ni1 O7 89.68(14) . . ? N1 Ni1 O7 89.41(15) . . ? O1 Ni1 O7 90.82(14) . . ? O6 Ni1 O7 176.73(15) . . ? C1 O1 Ni1 113.3(3) . . ? C7 O5 Ni1 114.1(3) . . ? Ni1 O6 H9 134.7 . . ? Ni1 O6 H10 121.6 . . ? H9 O6 H10 103.5 . . ? Ni1 O7 H11 106.1 . . ? Ni1 O7 H12 113.6 . . ? H11 O7 H12 108.1 . . ? C2 N1 N2 120.9(4) . . ? C2 N1 Ni1 114.6(3) . . ? N2 N1 Ni1 124.4(3) . . ? N1 N2 C4 127.1(4) . . ? N1 N2 H4 116.5 . . ? C4 N2 H4 116.5 . . ? N4 N3 C4 125.8(4) . . ? N4 N3 H5 117.1 . . ? C4 N3 H5 117.1 . . ? C5 N4 N3 120.1(4) . . ? C5 N4 Ni1 115.0(3) . . ? N3 N4 Ni1 124.9(3) . . ? O1 C1 O2 124.5(4) . . ? O1 C1 C2 118.1(4) . . ? O2 C1 C2 117.3(4) . . ? N1 C2 C3 126.8(4) . . ? N1 C2 C1 113.0(4) . . ? C3 C2 C1 120.1(4) . . ? C2 C3 H1 109.5 . . ? C2 C3 H2 109.5 . . ? H1 C3 H2 109.5 . . ? C2 C3 H3 109.5 . . ? H1 C3 H3 109.5 . . ? H2 C3 H3 109.5 . . ? O3 C4 N2 117.2(4) . . ? O3 C4 N3 116.8(4) . . ? N2 C4 N3 126.0(4) . . ? N4 C5 C6 125.5(5) . . ? N4 C5 C7 114.2(4) . . ? C6 C5 C7 120.2(4) . . ? C5 C6 H6 109.5 . . ? C5 C6 H7 109.5 . . ? H6 C6 H7 109.5 . . ? C5 C6 H8 109.5 . . ? H6 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? O4 C7 O5 126.0(5) . . ? O4 C7 C5 118.4(4) . . ? O5 C7 C5 115.6(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.875 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.139 data_4 _database_code_depnum_ccdc_archive 'CCDC 798366' #TrackingRef 'Compiled.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H8 Cu N4 O5, H2 O' _chemical_formula_sum 'C7 H10 Cu N4 O6' _chemical_formula_weight 309.73 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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 10.216(6) _cell_length_b 5.797(4) _cell_length_c 17.111(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.005(6) _cell_angle_gamma 90.00 _cell_volume 1013.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 3504 _cell_measurement_theta_min 2.3043 _cell_measurement_theta_max 29.5803 _exptl_crystal_description Prism _exptl_crystal_colour Blue _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.030 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 2.187 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.8794 _exptl_absorpt_correction_T_min 0.6257 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 8314 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 26.50 _reflns_number_total 2072 _reflns_number_gt 2040 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.0330P)^2^+0.9850P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2072 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0245 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0633 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.009960(19) 0.68678(3) 0.329579(12) 0.01292(9) Uani 1 1 d . . . O1 O 1.16402(12) 0.8725(2) 0.35094(7) 0.0158(3) Uani 1 1 d . . . O2 O 1.35195(13) 0.8544(2) 0.41963(8) 0.0213(3) Uani 1 1 d . . . O3 O 0.88310(12) 0.0049(2) 0.43955(8) 0.0187(3) Uani 1 1 d . . . O4 O 0.70468(13) 0.9534(2) 0.22189(8) 0.0220(3) Uani 1 1 d . . . O5 O 0.91309(12) 0.8926(2) 0.26005(7) 0.0149(3) Uani 1 1 d . . . O6 O 0.41010(14) 0.5946(3) 0.08996(9) 0.0358(4) Uani 1 1 d . . . H9 H 0.4780 0.5192 0.0943 0.043 Uiso 1 1 d . . . H10 H 0.3909 0.5799 0.0436 0.043 Uiso 1 1 d . . . N1 N 1.08738(14) 0.4856(2) 0.41007(8) 0.0124(3) Uani 1 1 d . . . N2 N 1.03585(15) 0.2797(3) 0.43321(9) 0.0138(3) Uani 1 1 d . . . H4 H 1.0728 0.1870 0.4632 0.016 Uiso 1 1 d . . . N3 N 0.82420(15) 0.3124(2) 0.36946(9) 0.0143(3) Uani 1 1 d . . . H5 H 0.7485 0.2591 0.3681 0.017 Uiso 1 1 d . . . N4 N 0.84444(14) 0.5178(2) 0.33191(8) 0.0122(3) Uani 1 1 d . . . C1 C 1.24520(18) 0.7752(3) 0.39776(10) 0.0146(3) Uani 1 1 d . . . C2 C 1.20480(17) 0.5416(3) 0.43080(10) 0.0136(3) Uani 1 1 d . . . C3 C 1.29837(17) 0.3988(3) 0.47733(11) 0.0193(4) Uani 1 1 d . . . H1 H 1.3759 0.4910 0.4910 0.023 Uiso 1 1 calc R . . H2 H 1.3246 0.2647 0.4465 0.023 Uiso 1 1 calc R . . H3 H 1.2563 0.3466 0.5252 0.023 Uiso 1 1 calc R . . C4 C 0.91413(18) 0.1958(3) 0.41387(10) 0.0136(4) Uani 1 1 d . . . C5 C 0.75012(17) 0.6123(3) 0.29268(10) 0.0140(3) Uani 1 1 d . . . C6 C 0.61539(18) 0.5210(3) 0.28255(12) 0.0219(4) Uani 1 1 d . . . H6 H 0.6192 0.3611 0.2641 0.026 Uiso 1 1 calc R . . H7 H 0.5673 0.6151 0.2441 0.026 Uiso 1 1 calc R . . H8 H 0.5706 0.5263 0.3327 0.026 Uiso 1 1 calc R . . C7 C 0.78898(18) 0.8379(3) 0.25442(10) 0.0142(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 Cu1 0.01164(13) 0.01106(13) 0.01599(13) 0.00350(7) -0.00158(9) -0.00235(7) O1 0.0150(6) 0.0129(6) 0.0196(6) 0.0013(5) 0.0000(5) -0.0026(5) O2 0.0167(7) 0.0216(7) 0.0253(7) 0.0004(6) -0.0031(5) -0.0083(5) O3 0.0190(6) 0.0129(6) 0.0241(7) 0.0074(5) -0.0038(5) -0.0047(5) O4 0.0160(6) 0.0222(7) 0.0279(7) 0.0103(6) 0.0007(5) 0.0040(5) O5 0.0136(6) 0.0138(6) 0.0174(6) 0.0048(5) 0.0003(5) -0.0006(5) O6 0.0205(7) 0.0562(11) 0.0306(8) -0.0150(8) -0.0044(6) 0.0189(7) N1 0.0141(7) 0.0092(7) 0.0140(7) 0.0000(5) 0.0018(5) -0.0013(5) N2 0.0126(7) 0.0114(7) 0.0171(7) 0.0046(6) -0.0021(6) -0.0011(6) N3 0.0116(7) 0.0113(7) 0.0200(8) 0.0050(5) -0.0009(6) -0.0040(5) N4 0.0138(7) 0.0090(7) 0.0138(7) 0.0009(5) 0.0015(5) -0.0007(5) C1 0.0152(8) 0.0131(8) 0.0156(8) -0.0024(7) 0.0039(7) -0.0017(7) C2 0.0140(8) 0.0122(8) 0.0146(8) -0.0023(6) 0.0017(6) -0.0007(6) C3 0.0159(8) 0.0165(9) 0.0252(9) 0.0017(7) -0.0033(7) -0.0001(7) C4 0.0157(9) 0.0119(8) 0.0132(8) -0.0007(6) 0.0013(7) -0.0001(6) C5 0.0128(8) 0.0137(8) 0.0155(8) 0.0012(7) 0.0011(6) 0.0006(7) C6 0.0143(9) 0.0208(9) 0.0305(10) 0.0079(8) -0.0040(7) -0.0020(7) C7 0.0156(8) 0.0127(8) 0.0144(8) 0.0011(6) 0.0034(7) 0.0004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.9364(15) . ? Cu1 O5 1.9437(14) . ? Cu1 N4 1.9553(17) . ? Cu1 N1 1.9606(16) . ? Cu1 O5 2.4332(15) 2_745 ? O1 C1 1.275(2) . ? O2 C1 1.235(2) . ? O3 C4 1.235(2) . ? O4 C7 1.218(2) . ? O5 C7 1.309(2) . ? O5 Cu1 2.4332(15) 2_755 ? O6 H9 0.8217 . ? O6 H10 0.8179 . ? N1 C2 1.287(2) . ? N1 N2 1.366(2) . ? N2 C4 1.370(2) . ? N2 H4 0.8297 . ? N3 C4 1.361(2) . ? N3 N4 1.370(2) . ? N3 H5 0.8330 . ? N4 C5 1.287(2) . ? C1 C2 1.527(3) . ? C2 C3 1.485(2) . ? C3 H1 0.9800 . ? C3 H2 0.9800 . ? C3 H3 0.9800 . ? C5 C6 1.482(3) . ? C5 C7 1.519(2) . ? C6 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? 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 O1 Cu1 O5 100.22(6) . . ? O1 Cu1 N4 167.18(6) . . ? O5 Cu1 N4 83.63(7) . . ? O1 Cu1 N1 83.20(7) . . ? O5 Cu1 N1 171.88(6) . . ? N4 Cu1 N1 91.49(7) . . ? O1 Cu1 O5 103.78(6) . 2_745 ? O5 Cu1 O5 102.19(5) . 2_745 ? N4 Cu1 O5 87.18(6) . 2_745 ? N1 Cu1 O5 83.98(7) . 2_745 ? C1 O1 Cu1 112.98(12) . . ? C7 O5 Cu1 112.23(11) . . ? C7 O5 Cu1 116.53(10) . 2_755 ? Cu1 O5 Cu1 130.50(7) . 2_755 ? H9 O6 H10 102.7 . . ? C2 N1 N2 120.18(15) . . ? C2 N1 Cu1 113.97(12) . . ? N2 N1 Cu1 124.79(12) . . ? N1 N2 C4 126.36(15) . . ? N1 N2 H4 124.9 . . ? C4 N2 H4 108.7 . . ? C4 N3 N4 125.95(15) . . ? C4 N3 H5 116.6 . . ? N4 N3 H5 117.2 . . ? C5 N4 N3 119.79(15) . . ? C5 N4 Cu1 114.57(12) . . ? N3 N4 Cu1 125.63(11) . . ? O2 C1 O1 125.96(17) . . ? O2 C1 C2 117.41(16) . . ? O1 C1 C2 116.61(16) . . ? N1 C2 C3 126.54(16) . . ? N1 C2 C1 112.23(15) . . ? C3 C2 C1 121.14(15) . . ? C2 C3 H1 109.5 . . ? C2 C3 H2 109.5 . . ? H1 C3 H2 109.5 . . ? C2 C3 H3 109.5 . . ? H1 C3 H3 109.5 . . ? H2 C3 H3 109.5 . . ? O3 C4 N3 117.96(16) . . ? O3 C4 N2 118.02(16) . . ? N3 C4 N2 124.00(16) . . ? N4 C5 C6 126.45(17) . . ? N4 C5 C7 113.12(15) . . ? C6 C5 C7 120.43(15) . . ? C5 C6 H6 109.5 . . ? C5 C6 H7 109.5 . . ? H6 C6 H7 109.5 . . ? C5 C6 H8 109.5 . . ? H6 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? O4 C7 O5 125.23(17) . . ? O4 C7 C5 118.84(16) . . ? O5 C7 C5 115.93(15) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.439 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.069 data_5 _database_code_depnum_ccdc_archive 'CCDC 798367' #TrackingRef 'Compiled.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H28 N16 Ni4 O16 S4, 2(H12 Ni O6), 4.5(H2 O)' _chemical_formula_sum 'C28 H61 N16 Ni6 O32.50 S4' _chemical_formula_weight 1622.32 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n m c' _symmetry_space_group_name_Hall '-P 4ac 2a' _symmetry_Int_Tables_number 137 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x, z+1/2' '-x+1/2, -y+1/2, z' 'y, -x+1/2, z+1/2' '-x+1/2, y, z' 'y, x, z+1/2' 'x, -y+1/2, z' '-y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'y-1/2, -x, -z-1/2' 'x-1/2, y-1/2, -z' '-y, x-1/2, -z-1/2' 'x-1/2, -y, -z' '-y, -x, -z-1/2' '-x, y-1/2, -z' 'y-1/2, x-1/2, -z-1/2' _cell_length_a 15.808(3) _cell_length_b 15.808(3) _cell_length_c 11.932(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2981.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 12467 _cell_measurement_theta_min 2.4968 _cell_measurement_theta_max 30.6157 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1666 _exptl_absorpt_coefficient_mu 2.098 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.8558 _exptl_absorpt_correction_T_min 0.7311 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 42940 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0074 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 26.49 _reflns_number_total 1658 _reflns_number_gt 1658 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SIR92 (J. Appl. Cryst., 1994, 27, 435)' _computing_structure_refinement 'SHELXL-97 (Acta Cryst. 2008. A64, 112-122)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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. All hydrogen atoms were located in difference map positions. They were initially refined positionally with fixed displacement ellipses (1.2 times that of their bonding partner) and distance and angle restraints. In the final round of least squares they were refned on a riding model. ; _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^)+(0.0654P)^2^+5.8217P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1658 _refine_ls_number_parameters 112 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1175 _refine_ls_wR_factor_gt 0.1175 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.166 _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 0.59885(2) 0.09885(2) 0.7500 0.01291(19) Uani 1 2 d S . . Ni2 Ni 0.2500 0.2500 0.70549(6) 0.0196(2) Uani 1 4 d S . . S1 S 0.7500 0.09722(6) 0.76906(8) 0.0167(2) Uani 1 2 d S . . O1 O 0.47060(12) 0.10454(12) 0.79195(16) 0.0177(4) Uani 1 1 d . . . O2 O 0.38864(13) 0.12309(15) 0.94330(18) 0.0250(5) Uani 1 1 d . . . O3 O 0.2500 0.1561(3) 0.5890(3) 0.0397(9) Uani 1 2 d S . . H5 H 0.2015 0.1529 0.5439 0.047 Uiso 1 1 d . . . O4 O 0.38058(18) 0.2500 0.7008(3) 0.0233(6) Uani 1 2 d S . . H6 H 0.4099 0.2982 0.7225 0.029 Uiso 1 1 d . . . O5 O 0.2500 0.1537(2) 0.8206(3) 0.0329(8) Uani 1 2 d S . . H7 H 0.2947 0.1495 0.8728 0.040 Uiso 1 1 d . . . O6 O 0.5369(2) 0.2500 0.3115(3) 0.0411(9) Uani 1 2 d S . . H8 H 0.5442 0.2500 0.2307 0.049 Uiso 1 2 d S . . H9 H 0.4752 0.2500 0.3148 0.049 Uiso 1 2 d S . . O7 O 0.7500 0.2500 0.2500 0.18(2) Uani 0.50 8 d SP . . H10 H 0.7828 0.2500 0.1791 0.198 Uiso 0.25 2 d SP . . N1 N 0.60441(14) 0.09261(14) 0.9177(2) 0.0148(5) Uani 1 1 d . . . N2 N 0.67894(14) 0.08592(17) 0.97489(19) 0.0215(5) Uani 1 1 d . . . H4 H 0.6803 0.0801 1.0482 0.026 Uiso 0.50 1 calc PR . . C1 C 0.45879(17) 0.10994(16) 0.8982(2) 0.0180(5) Uani 1 1 d . . . C2 C 0.53513(17) 0.10072(16) 0.9724(2) 0.0167(5) Uani 1 1 d . . . C3 C 0.52793(19) 0.1061(2) 1.0971(2) 0.0243(6) Uani 1 1 d . . . H1 H 0.5486 0.1613 1.1225 0.029 Uiso 1 1 calc R . . H2 H 0.5619 0.0611 1.1314 0.029 Uiso 1 1 calc R . . H3 H 0.4686 0.0994 1.1191 0.029 Uiso 1 1 calc R . . C4 C 0.7500 0.0886(2) 0.9132(3) 0.0169(7) Uani 1 2 d S . . 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 0.0133(2) 0.0133(2) 0.0122(3) -0.00005(11) 0.00005(11) 0.00040(15) Ni2 0.0158(4) 0.0232(4) 0.0198(4) 0.000 0.000 0.000 S1 0.0126(5) 0.0226(5) 0.0149(4) 0.0009(3) 0.000 0.000 O1 0.0155(9) 0.0209(9) 0.0168(9) 0.0012(7) 0.0023(7) 0.0008(7) O2 0.0164(9) 0.0364(12) 0.0222(10) -0.0012(9) 0.0016(8) 0.0048(8) O3 0.0234(15) 0.058(2) 0.0381(19) -0.0256(18) 0.000 0.000 O4 0.0157(13) 0.0241(14) 0.0301(16) 0.000 -0.0019(11) 0.000 O5 0.0180(14) 0.047(2) 0.0339(17) 0.0177(15) 0.000 0.000 O6 0.046(2) 0.049(2) 0.0287(17) 0.000 -0.0058(15) 0.000 O7 0.053(10) 0.053(10) 0.44(8) 0.000 0.000 0.000 N1 0.0129(11) 0.0156(10) 0.0159(12) 0.0011(8) -0.0001(8) -0.0002(7) N2 0.0145(12) 0.0335(13) 0.0166(11) 0.0025(10) -0.0019(9) -0.0007(9) C1 0.0156(12) 0.0173(12) 0.0212(13) -0.0012(10) 0.0015(10) 0.0002(9) C2 0.0173(13) 0.0175(12) 0.0152(12) 0.0006(9) 0.0015(10) -0.0002(9) C3 0.0212(14) 0.0363(16) 0.0154(13) 0.0001(11) 0.0031(11) 0.0010(12) C4 0.0167(18) 0.0189(17) 0.0150(17) -0.0003(14) 0.000 0.000 _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 N1 2.005(3) . ? Ni1 N1 2.005(3) 16_657 ? Ni1 O1 2.0901(19) 16_657 ? Ni1 O1 2.0902(19) . ? Ni1 S1 2.4003(5) 10_667 ? Ni1 S1 2.4003(6) . ? Ni2 O3 2.034(3) 3 ? Ni2 O3 2.034(3) . ? Ni2 O5 2.051(3) 3 ? Ni2 O5 2.051(3) . ? Ni2 O4 2.065(3) 3 ? Ni2 O4 2.065(3) . ? S1 C4 1.725(4) . ? S1 Ni1 2.4004(5) 12_657 ? O1 C1 1.284(4) . ? O2 C1 1.250(3) . ? O3 H5 0.9386 . ? O4 H6 0.9281 . ? O5 H7 0.9439 . ? O6 H8 0.9711 . ? O6 H9 0.9761 . ? O7 H10 0.9925 . ? N1 C2 1.281(4) . ? N1 N2 1.366(3) . ? N2 C4 1.344(3) . ? N2 H4 0.8800 . ? C1 C2 1.504(4) . ? C2 C3 1.494(4) . ? C3 H1 0.9800 . ? C3 H2 0.9800 . ? C3 H3 0.9800 . ? C4 N2 1.344(3) 5_655 ? 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 N1 Ni1 N1 179.58(13) . 16_657 ? N1 Ni1 O1 100.92(8) . 16_657 ? N1 Ni1 O1 78.80(8) 16_657 16_657 ? N1 Ni1 O1 78.80(8) . . ? N1 Ni1 O1 100.92(8) 16_657 . ? O1 Ni1 O1 98.09(10) 16_657 . ? N1 Ni1 S1 98.27(7) . 10_667 ? N1 Ni1 S1 82.02(7) 16_657 10_667 ? O1 Ni1 S1 160.61(6) 16_657 10_667 ? O1 Ni1 S1 88.25(5) . 10_667 ? N1 Ni1 S1 82.03(7) . . ? N1 Ni1 S1 98.27(7) 16_657 . ? O1 Ni1 S1 88.25(5) 16_657 . ? O1 Ni1 S1 160.61(6) . . ? S1 Ni1 S1 91.74(5) 10_667 . ? O3 Ni2 O3 93.8(2) 3 . ? O3 Ni2 O5 85.14(16) 3 3 ? O3 Ni2 O5 178.95(16) . 3 ? O3 Ni2 O5 178.95(16) 3 . ? O3 Ni2 O5 85.14(16) . . ? O5 Ni2 O5 95.9(2) 3 . ? O3 Ni2 O4 88.95(6) 3 3 ? O3 Ni2 O4 88.95(6) . 3 ? O5 Ni2 O4 91.03(6) 3 3 ? O5 Ni2 O4 91.03(6) . 3 ? O3 Ni2 O4 88.95(6) 3 . ? O3 Ni2 O4 88.95(6) . . ? O5 Ni2 O4 91.03(6) 3 . ? O5 Ni2 O4 91.03(6) . . ? O4 Ni2 O4 176.92(17) 3 . ? C4 S1 Ni1 95.47(2) . . ? C4 S1 Ni1 95.47(2) . 12_657 ? Ni1 S1 Ni1 169.06(5) . 12_657 ? C1 O1 Ni1 112.36(17) . . ? Ni2 O3 H5 115.5 . . ? Ni2 O4 H6 119.4 . . ? Ni2 O5 H7 119.6 . . ? H8 O6 H9 99.1 . . ? C2 N1 N2 119.4(2) . . ? C2 N1 Ni1 117.76(19) . . ? N2 N1 Ni1 122.71(17) . . ? C4 N2 N1 116.4(2) . . ? C4 N2 H4 121.8 . . ? N1 N2 H4 121.8 . . ? O2 C1 O1 124.4(3) . . ? O2 C1 C2 118.3(2) . . ? O1 C1 C2 117.3(2) . . ? N1 C2 C3 125.3(3) . . ? N1 C2 C1 113.3(2) . . ? C3 C2 C1 121.3(2) . . ? C2 C3 H1 109.5 . . ? C2 C3 H2 109.5 . . ? H1 C3 H2 109.5 . . ? C2 C3 H3 109.5 . . ? H1 C3 H3 109.5 . . ? H2 C3 H3 109.5 . . ? N2 C4 N2 113.4(3) . 5_655 ? N2 C4 S1 123.27(17) . . ? N2 C4 S1 123.27(17) 5_655 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.315 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.115 data_6 _database_code_depnum_ccdc_archive 'CCDC 798368' #TrackingRef 'Compiled.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H15 Cl2 Co N6 O3, 0.75(C3H3N)' _chemical_formula_sum 'C10.50 H17.25 Cl2 Co N6.75 O3' _chemical_formula_weight 415.88 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' 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 12.4448(14) _cell_length_b 12.8355(14) _cell_length_c 10.6625(12) _cell_angle_alpha 90.00 _cell_angle_beta 97.964(2) _cell_angle_gamma 90.00 _cell_volume 1686.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7084 _cell_measurement_theta_min 2.3596 _cell_measurement_theta_max 30.8114 _exptl_crystal_description Prism _exptl_crystal_colour 'Light Brown' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 1.358 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9041 _exptl_absorpt_correction_T_min 0.8091 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 21693 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0149 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 26.49 _reflns_number_total 3472 _reflns_number_gt 3441 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _refine_special_details ; H(1) was initially introduced in its difference map position and refined positionally, with a fixed thermal parameters. Subsequently, it was refined on a riding model. All other hydrogen atoms were introduced in calculated positions with isotropic thermal parameters set twenty percent greater than those of their bonding partners and were refined on the riding model. 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^)+(0.0586P)^2^+3.1426P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3472 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Co1 Co 0.78044(2) 0.97948(2) 0.73610(3) 0.01374(13) Uani 1 1 d . . . Cl1 Cl 0.86169(5) 1.09400(5) 0.87422(6) 0.02270(16) Uani 1 1 d . . . Cl2 Cl 0.69214(5) 0.86048(5) 0.60495(6) 0.02219(16) Uani 1 1 d . . . O1 O 0.97069(15) 0.96996(15) 0.62057(18) 0.0209(4) Uani 1 1 d . . . O3 O 0.56900(15) 0.89017(15) 1.02429(18) 0.0243(4) Uani 1 1 d . . . O4 O 0.83321(15) 1.09485(15) 0.52539(17) 0.0226(4) Uani 1 1 d . . . H1 H 0.8898 1.0453 0.5535 0.025 Uiso 1 1 d . . . N1 N 0.76161(17) 1.08038(17) 0.60711(19) 0.0175(4) Uani 1 1 d . . . N2 N 0.91760(17) 0.93056(16) 0.70965(19) 0.0164(4) Uani 1 1 d . . . N3 N 0.71947(18) 0.85957(17) 0.9403(2) 0.0204(5) Uani 1 1 d . . . H9 H 0.7295 0.8052 0.9908 0.025 Uiso 1 1 calc R . . N4 N 0.79795(17) 0.87877(16) 0.86528(19) 0.0159(4) Uani 1 1 d . . . N5 N 0.59585(18) 0.99889(18) 0.8682(2) 0.0194(4) Uani 1 1 d . . . H8 H 0.5381 1.0335 0.8838 0.023 Uiso 1 1 calc R . . N6 N 0.64536(17) 1.03368(16) 0.76922(19) 0.0164(4) Uani 1 1 d . . . N7 N 0.6435(4) 1.0847(4) 0.2206(5) 0.0559(12) Uani 0.75 1 d P . . C1 C 0.6739(2) 1.1349(2) 0.5973(2) 0.0201(5) Uani 1 1 d . . . C2 C 0.6435(2) 1.2156(2) 0.4986(3) 0.0307(6) Uani 1 1 d . . . H2 H 0.6942 1.2131 0.4362 0.037 Uiso 1 1 calc R . . H3 H 0.6464 1.2846 0.5383 0.037 Uiso 1 1 calc R . . H4 H 0.5697 1.2022 0.4564 0.037 Uiso 1 1 calc R . . C3 C 0.6053(2) 1.10820(19) 0.6956(2) 0.0178(5) Uani 1 1 d . . . C4 C 0.5023(2) 1.1662(2) 0.7023(3) 0.0242(6) Uani 1 1 d . . . H5 H 0.4536 1.1576 0.6226 0.029 Uiso 1 1 calc R . . H6 H 0.5184 1.2404 0.7166 0.029 Uiso 1 1 calc R . . H7 H 0.4673 1.1388 0.7723 0.029 Uiso 1 1 calc R . . C5 C 0.6267(2) 0.91633(19) 0.9451(2) 0.0178(5) Uani 1 1 d . . . C6 C 0.8896(2) 0.83015(19) 0.8809(2) 0.0170(5) Uani 1 1 d . . . C7 C 0.9236(2) 0.7517(2) 0.9814(3) 0.0240(5) Uani 1 1 d . . . H10 H 0.9288 0.7852 1.0647 0.029 Uiso 1 1 calc R . . H11 H 0.9945 0.7230 0.9697 0.029 Uiso 1 1 calc R . . H12 H 0.8700 0.6955 0.9762 0.029 Uiso 1 1 calc R . . C8 C 0.9615(2) 0.86092(19) 0.7891(2) 0.0170(5) Uani 1 1 d . . . C9 C 1.0735(2) 0.8196(2) 0.7900(3) 0.0241(6) Uani 1 1 d . . . H13 H 1.1211 0.8485 0.8626 0.029 Uiso 1 1 calc R . . H14 H 1.1006 0.8397 0.7115 0.029 Uiso 1 1 calc R . . H15 H 1.0724 0.7435 0.7966 0.029 Uiso 1 1 calc R . . C10 C 0.7056(4) 1.0201(4) 0.2411(5) 0.0410(11) Uani 0.75 1 d P . . C11 C 0.7811(4) 0.9342(4) 0.2671(5) 0.0467(12) Uani 0.75 1 d P . . H16 H 0.7828 0.9118 0.3552 0.056 Uiso 0.75 1 calc PR . . H17 H 0.8538 0.9569 0.2533 0.056 Uiso 0.75 1 calc PR . . H18 H 0.7578 0.8760 0.2103 0.056 Uiso 0.75 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01399(19) 0.0143(2) 0.01344(19) 0.00023(11) 0.00358(13) 0.00035(11) Cl1 0.0269(3) 0.0196(3) 0.0209(3) -0.0043(2) 0.0008(2) -0.0028(2) Cl2 0.0196(3) 0.0222(3) 0.0243(3) -0.0078(2) 0.0011(2) -0.0007(2) O1 0.0180(9) 0.0274(10) 0.0193(9) 0.0057(7) 0.0099(7) 0.0006(7) O3 0.0229(9) 0.0254(10) 0.0271(10) 0.0066(8) 0.0128(8) 0.0040(8) O4 0.0229(9) 0.0273(10) 0.0202(9) 0.0066(7) 0.0118(7) 0.0032(8) N1 0.0191(10) 0.0194(10) 0.0150(9) -0.0004(8) 0.0059(8) -0.0016(8) N2 0.0171(10) 0.0170(10) 0.0157(10) -0.0013(8) 0.0043(8) -0.0021(8) N3 0.0201(10) 0.0193(11) 0.0239(11) 0.0082(8) 0.0101(9) 0.0045(8) N4 0.0163(10) 0.0155(10) 0.0168(10) 0.0002(8) 0.0058(8) -0.0003(8) N5 0.0185(11) 0.0218(10) 0.0200(11) 0.0057(9) 0.0097(9) 0.0058(8) N6 0.0163(10) 0.0188(10) 0.0149(10) 0.0008(8) 0.0050(8) 0.0004(8) N7 0.041(2) 0.053(3) 0.068(3) -0.005(2) -0.013(2) -0.003(2) C1 0.0207(12) 0.0247(13) 0.0153(11) 0.0013(10) 0.0041(9) -0.0010(10) C2 0.0332(15) 0.0326(15) 0.0281(14) 0.0144(12) 0.0110(12) 0.0114(12) C3 0.0203(12) 0.0167(11) 0.0171(11) 0.0003(9) 0.0048(9) 0.0019(9) C4 0.0227(13) 0.0274(14) 0.0231(13) 0.0047(11) 0.0051(10) 0.0074(11) C5 0.0186(11) 0.0177(11) 0.0180(11) 0.0014(9) 0.0054(9) 0.0000(9) C6 0.0164(11) 0.0181(12) 0.0172(11) -0.0017(9) 0.0045(9) -0.0035(9) C7 0.0198(12) 0.0254(14) 0.0270(13) 0.0092(11) 0.0042(10) 0.0017(10) C8 0.0181(12) 0.0155(12) 0.0176(11) -0.0023(9) 0.0036(9) -0.0006(9) C9 0.0178(12) 0.0317(14) 0.0240(13) 0.0029(11) 0.0071(10) 0.0059(11) C10 0.040(3) 0.037(3) 0.041(2) -0.0019(19) -0.010(2) -0.012(2) C11 0.037(2) 0.039(3) 0.055(3) -0.010(2) -0.026(2) 0.002(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 Co1 N2 1.876(2) . ? Co1 N4 1.880(2) . ? Co1 N1 1.880(2) . ? Co1 N6 1.897(2) . ? Co1 Cl1 2.2225(7) . ? Co1 Cl2 2.2518(7) . ? O1 N2 1.330(3) . ? O3 C5 1.229(3) . ? O4 N1 1.343(3) . ? O4 H1 0.9653 . ? N1 C1 1.289(3) . ? N2 C8 1.299(3) . ? N3 N4 1.368(3) . ? N3 C5 1.372(3) . ? N3 H9 0.8800 . ? N4 C6 1.290(3) . ? N5 C5 1.362(3) . ? N5 N6 1.369(3) . ? N5 H8 0.8800 . ? N6 C3 1.293(3) . ? N7 C10 1.134(7) . ? C1 C3 1.480(3) . ? C1 C2 1.488(4) . ? C2 H2 0.9800 . ? C2 H3 0.9800 . ? C2 H4 0.9800 . ? C3 C4 1.493(3) . ? C4 H5 0.9800 . ? C4 H6 0.9800 . ? C4 H7 0.9800 . ? C6 C8 1.469(3) . ? C6 C7 1.489(4) . ? C7 H10 0.9800 . ? C7 H11 0.9800 . ? C7 H12 0.9800 . ? C8 C9 1.489(3) . ? C9 H13 0.9800 . ? C9 H14 0.9800 . ? C9 H15 0.9800 . ? C10 C11 1.450(7) . ? C11 H16 0.9800 . ? C11 H17 0.9800 . ? C11 H18 0.9800 . ? 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 N2 Co1 N4 82.21(9) . . ? N2 Co1 N1 98.30(9) . . ? N4 Co1 N1 179.48(9) . . ? N2 Co1 N6 177.06(9) . . ? N4 Co1 N6 97.56(9) . . ? N1 Co1 N6 81.93(9) . . ? N2 Co1 Cl1 88.92(7) . . ? N4 Co1 Cl1 88.47(7) . . ? N1 Co1 Cl1 91.62(7) . . ? N6 Co1 Cl1 88.15(7) . . ? N2 Co1 Cl2 93.18(7) . . ? N4 Co1 Cl2 89.17(7) . . ? N1 Co1 Cl2 90.71(7) . . ? N6 Co1 Cl2 89.74(7) . . ? Cl1 Co1 Cl2 176.61(3) . . ? N1 O4 H1 103.2 . . ? C1 N1 O4 120.2(2) . . ? C1 N1 Co1 116.86(17) . . ? O4 N1 Co1 122.91(16) . . ? C8 N2 O1 121.4(2) . . ? C8 N2 Co1 116.22(17) . . ? O1 N2 Co1 122.17(16) . . ? N4 N3 C5 126.8(2) . . ? N4 N3 H9 116.6 . . ? C5 N3 H9 116.6 . . ? C6 N4 N3 121.8(2) . . ? C6 N4 Co1 115.95(17) . . ? N3 N4 Co1 122.21(16) . . ? C5 N5 N6 126.7(2) . . ? C5 N5 H8 116.6 . . ? N6 N5 H8 116.6 . . ? C3 N6 N5 122.2(2) . . ? C3 N6 Co1 115.80(17) . . ? N5 N6 Co1 121.94(16) . . ? N1 C1 C3 112.4(2) . . ? N1 C1 C2 124.4(2) . . ? C3 C1 C2 123.1(2) . . ? C1 C2 H2 109.5 . . ? C1 C2 H3 109.5 . . ? H2 C2 H3 109.5 . . ? C1 C2 H4 109.5 . . ? H2 C2 H4 109.5 . . ? H3 C2 H4 109.5 . . ? N6 C3 C1 112.9(2) . . ? N6 C3 C4 126.9(2) . . ? C1 C3 C4 120.1(2) . . ? C3 C4 H5 109.5 . . ? C3 C4 H6 109.5 . . ? H5 C4 H6 109.5 . . ? C3 C4 H7 109.5 . . ? H5 C4 H7 109.5 . . ? H6 C4 H7 109.5 . . ? O3 C5 N5 118.9(2) . . ? O3 C5 N3 117.1(2) . . ? N5 C5 N3 124.0(2) . . ? N4 C6 C8 113.2(2) . . ? N4 C6 C7 125.3(2) . . ? C8 C6 C7 121.5(2) . . ? C6 C7 H10 109.5 . . ? C6 C7 H11 109.5 . . ? H10 C7 H11 109.5 . . ? C6 C7 H12 109.5 . . ? H10 C7 H12 109.5 . . ? H11 C7 H12 109.5 . . ? N2 C8 C6 112.3(2) . . ? N2 C8 C9 123.9(2) . . ? C6 C8 C9 123.8(2) . . ? C8 C9 H13 109.5 . . ? C8 C9 H14 109.5 . . ? H13 C9 H14 109.5 . . ? C8 C9 H15 109.5 . . ? H13 C9 H15 109.5 . . ? H14 C9 H15 109.5 . . ? N7 C10 C11 177.4(5) . . ? C10 C11 H16 109.5 . . ? C10 C11 H17 109.5 . . ? H16 C11 H17 109.5 . . ? C10 C11 H18 109.5 . . ? H16 C11 H18 109.5 . . ? H17 C11 H18 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.783 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.096 data_7 _database_code_depnum_ccdc_archive 'CCDC 798369' #TrackingRef 'Compiled.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H15 Br2 Co N6 O3, 0.7(C2 H3 N)' _chemical_formula_sum 'C10.40 H17.10 Br2 Co N6.70 O3 ' _chemical_formula_weight 502.73 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' Br Br -0.2901 2.4595 '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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5454(10) _cell_length_b 10.1776(13) _cell_length_c 10.7934(13) _cell_angle_alpha 82.511(7) _cell_angle_beta 71.639(6) _cell_angle_gamma 82.963(7) _cell_volume 880.02(19) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5250 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 29.72 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 494.80 _exptl_absorpt_coefficient_mu 5.552 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1807 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; Shape and scale corrections using equivalent reflections. Shape function based on spherical harmonics. Highest even and odd order for spherical harmonics: 4 and 1 Laue group: -1 Friedel opposites are equivalent. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 5789 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 26.50 _reflns_number_total 3538 _reflns_number_gt 3202 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'TwinSolve (Rigaku/MSC Inc., 2005)' _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'TwinSolve (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.1290P)^2^+6.7771P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3538 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2263 _refine_ls_wR_factor_gt 0.2190 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _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 Br1 Br 0.38141(9) 0.93238(7) 0.32653(7) 0.0238(3) Uani 1 1 d . . . Br2 Br 0.27437(9) 0.55764(7) 0.15469(7) 0.0252(3) Uani 1 1 d . . . Co1 Co 0.32686(10) 0.74238(8) 0.24272(8) 0.0147(3) Uani 1 1 d . . . O1 O 0.2544(7) 0.5983(6) 0.4934(5) 0.0269(12) Uani 1 1 d . . . O2 O 0.1969(7) 1.0104(7) -0.0783(6) 0.0419(17) Uani 1 1 d . . . O3 O 0.5465(7) 0.5841(6) 0.3580(5) 0.0323(13) Uani 1 1 d . . . N1 N 0.1954(7) 0.6816(6) 0.4097(6) 0.0210(12) Uani 1 1 d . . . N2 N 0.1206(7) 0.8287(6) 0.2328(5) 0.0162(11) Uani 1 1 d . . . N3 N 0.1057(7) 0.9056(6) 0.1225(6) 0.0196(12) Uani 1 1 d . . . H7 H 0.0058 0.9416 0.1251 0.024 Uiso 1 1 calc R . . N4 N 0.3897(8) 0.8813(7) -0.0136(6) 0.0290(15) Uani 1 1 d . . . H8 H 0.4581 0.9023 -0.0919 0.035 Uiso 1 1 calc R . . N5 N 0.4555(7) 0.8004(6) 0.0735(6) 0.0196(12) Uani 1 1 d . . . N6 N 0.5309(7) 0.6570(6) 0.2524(6) 0.0202(12) Uani 1 1 d . . . N7 N 0.1377(17) 0.766(2) 0.806(2) 0.090(7) Uani 0.70 1 d P . . C1 C -0.0817(10) 0.6861(10) 0.5699(7) 0.035(2) Uani 1 1 d . . . H1 H -0.0268 0.6698 0.6384 0.042 Uiso 1 1 calc R . . H2 H -0.1297 0.6052 0.5645 0.042 Uiso 1 1 calc R . . H3 H -0.1696 0.7585 0.5914 0.042 Uiso 1 1 calc R . . C2 C 0.0413(9) 0.7236(8) 0.4417(7) 0.0224(14) Uani 1 1 d . . . C3 C -0.0036(9) 0.8102(7) 0.3373(7) 0.0201(14) Uani 1 1 d . . . C4 C -0.1764(10) 0.8685(10) 0.3547(8) 0.036(2) Uani 1 1 d . . . H4 H -0.1922 0.9542 0.3912 0.043 Uiso 1 1 calc R . . H5 H -0.2533 0.8079 0.4149 0.043 Uiso 1 1 calc R . . H6 H -0.1975 0.8818 0.2697 0.043 Uiso 1 1 calc R . . C5 C 0.2291(9) 0.9319(8) 0.0095(7) 0.0266(16) Uani 1 1 d . . . C6 C 0.7300(9) 0.7786(8) -0.0904(8) 0.0257(16) Uani 1 1 d . . . H9 H 0.7299 0.7076 -0.1436 0.031 Uiso 1 1 calc R . . H10 H 0.8408 0.7792 -0.0820 0.031 Uiso 1 1 calc R . . H11 H 0.6990 0.8646 -0.1329 0.031 Uiso 1 1 calc R . . C7 C 0.6094(8) 0.7554(7) 0.0413(7) 0.0197(13) Uani 1 1 d . . . C8 C 0.6563(8) 0.6731(7) 0.1447(8) 0.0218(14) Uani 1 1 d . . . C9 C 0.8237(10) 0.6071(9) 0.1349(9) 0.0336(19) Uani 1 1 d . . . H12 H 0.8809 0.5890 0.0439 0.040 Uiso 1 1 calc R . . H13 H 0.8140 0.5233 0.1917 0.040 Uiso 1 1 calc R . . H14 H 0.8869 0.6655 0.1626 0.040 Uiso 1 1 calc R . . C10 C 0.2703(19) 0.7464(13) 0.7487(16) 0.044(3) Uani 0.70 1 d P . . C11 C 0.4400(14) 0.7375(13) 0.6714(14) 0.039(3) Uani 0.70 1 d P . . H15 H 0.4934 0.6504 0.6929 0.047 Uiso 0.70 1 calc PR . . H16 H 0.4957 0.8078 0.6900 0.047 Uiso 0.70 1 calc PR . . H17 H 0.4476 0.7480 0.5782 0.047 Uiso 0.70 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0256(4) 0.0214(4) 0.0259(4) -0.0066(3) -0.0085(3) -0.0014(3) Br2 0.0273(4) 0.0198(4) 0.0296(4) -0.0065(3) -0.0082(3) -0.0031(3) Co1 0.0142(5) 0.0148(5) 0.0149(5) 0.0004(4) -0.0057(4) 0.0010(4) O1 0.028(3) 0.030(3) 0.019(2) 0.011(2) -0.009(2) 0.006(2) O2 0.022(3) 0.069(5) 0.028(3) 0.019(3) -0.009(2) 0.005(3) O3 0.023(3) 0.045(4) 0.025(3) 0.010(3) -0.012(2) 0.008(2) N1 0.023(3) 0.020(3) 0.021(3) 0.005(2) -0.011(2) -0.002(2) N2 0.016(3) 0.017(3) 0.017(3) 0.002(2) -0.010(2) 0.002(2) N3 0.012(2) 0.029(3) 0.018(3) 0.001(2) -0.008(2) 0.003(2) N4 0.020(3) 0.041(4) 0.016(3) 0.009(3) 0.003(2) 0.002(3) N5 0.020(3) 0.019(3) 0.020(3) -0.001(2) -0.008(2) 0.000(2) N6 0.021(3) 0.017(3) 0.024(3) 0.002(2) -0.012(2) 0.001(2) N7 0.029(7) 0.130(17) 0.105(14) -0.062(13) 0.011(8) -0.018(8) C1 0.029(4) 0.051(5) 0.017(3) 0.013(3) -0.003(3) -0.005(4) C2 0.021(3) 0.025(4) 0.019(3) 0.002(3) -0.008(3) 0.003(3) C3 0.021(3) 0.020(3) 0.019(3) 0.003(3) -0.009(3) 0.000(3) C4 0.024(4) 0.056(6) 0.019(3) 0.001(4) -0.001(3) 0.010(4) C5 0.023(4) 0.036(4) 0.015(3) 0.007(3) -0.006(3) 0.008(3) C6 0.020(3) 0.020(4) 0.030(4) 0.003(3) -0.002(3) 0.003(3) C7 0.020(3) 0.018(3) 0.021(3) -0.002(3) -0.006(3) 0.002(3) C8 0.015(3) 0.020(3) 0.035(4) -0.011(3) -0.012(3) 0.003(3) C9 0.022(4) 0.040(5) 0.036(4) 0.000(4) -0.013(3) 0.012(3) C10 0.045(8) 0.026(6) 0.067(9) -0.016(6) -0.023(7) -0.002(5) C11 0.023(5) 0.035(7) 0.053(8) -0.031(6) 0.009(5) -0.009(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 Br1 Co1 2.3911(11) . ? Br2 Co1 2.3622(11) . ? Co1 N1 1.870(6) . ? Co1 N5 1.872(6) . ? Co1 N6 1.878(6) . ? Co1 N2 1.898(5) . ? O1 N1 1.331(7) . ? O2 C5 1.235(9) . ? O3 N6 1.311(8) . ? N1 C2 1.285(9) . ? N2 C3 1.293(9) . ? N2 N3 1.369(8) . ? N3 C5 1.359(9) . ? N3 H7 0.8800 . ? N4 C5 1.363(9) . ? N4 N5 1.377(9) . ? N4 H8 0.8800 . ? N5 C7 1.290(9) . ? N6 C8 1.317(10) . ? N7 C10 1.12(2) . ? C1 C2 1.486(10) . ? C1 H1 0.9800 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? C2 C3 1.458(9) . ? C3 C4 1.486(10) . ? C4 H4 0.9800 . ? C4 H5 0.9800 . ? C4 H6 0.9800 . ? C6 C7 1.479(10) . ? C6 H9 0.9800 . ? C6 H10 0.9800 . ? C6 H11 0.9800 . ? C7 C8 1.436(10) . ? C8 C9 1.482(9) . ? C9 H12 0.9800 . ? C9 H13 0.9800 . ? C9 H14 0.9800 . ? C10 C11 1.425(18) . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C11 H17 0.9800 . ? 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 N1 Co1 N5 178.5(2) . . ? N1 Co1 N6 98.3(3) . . ? N5 Co1 N6 82.3(3) . . ? N1 Co1 N2 81.8(2) . . ? N5 Co1 N2 97.7(2) . . ? N6 Co1 N2 180.0(3) . . ? N1 Co1 Br2 90.5(2) . . ? N5 Co1 Br2 88.07(19) . . ? N6 Co1 Br2 90.71(19) . . ? N2 Co1 Br2 89.28(18) . . ? N1 Co1 Br1 90.8(2) . . ? N5 Co1 Br1 90.62(19) . . ? N6 Co1 Br1 89.67(19) . . ? N2 Co1 Br1 90.34(18) . . ? Br2 Co1 Br1 178.57(4) . . ? C2 N1 O1 120.1(6) . . ? C2 N1 Co1 116.8(5) . . ? O1 N1 Co1 123.1(5) . . ? C3 N2 N3 122.7(6) . . ? C3 N2 Co1 115.4(5) . . ? N3 N2 Co1 121.9(4) . . ? C5 N3 N2 126.7(6) . . ? C5 N3 H7 116.7 . . ? N2 N3 H7 116.7 . . ? C5 N4 N5 126.4(6) . . ? C5 N4 H8 116.8 . . ? N5 N4 H8 116.8 . . ? C7 N5 N4 121.7(6) . . ? C7 N5 Co1 115.7(5) . . ? N4 N5 Co1 122.5(5) . . ? O3 N6 C8 122.4(6) . . ? O3 N6 Co1 122.3(5) . . ? C8 N6 Co1 115.3(5) . . ? C2 C1 H1 109.5 . . ? C2 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? C2 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? N1 C2 C3 113.0(6) . . ? N1 C2 C1 124.3(7) . . ? C3 C2 C1 122.6(6) . . ? N2 C3 C2 113.1(6) . . ? N2 C3 C4 125.7(6) . . ? C2 C3 C4 121.3(6) . . ? C3 C4 H4 109.5 . . ? C3 C4 H5 109.5 . . ? H4 C4 H5 109.5 . . ? C3 C4 H6 109.5 . . ? H4 C4 H6 109.5 . . ? H5 C4 H6 109.5 . . ? O2 C5 N3 118.6(7) . . ? O2 C5 N4 116.6(7) . . ? N3 C5 N4 124.7(6) . . ? C7 C6 H9 109.5 . . ? C7 C6 H10 109.5 . . ? H9 C6 H10 109.5 . . ? C7 C6 H11 109.5 . . ? H9 C6 H11 109.5 . . ? H10 C6 H11 109.5 . . ? N5 C7 C8 114.0(6) . . ? N5 C7 C6 124.9(7) . . ? C8 C7 C6 121.0(6) . . ? N6 C8 C7 112.6(6) . . ? N6 C8 C9 121.7(7) . . ? C7 C8 C9 125.6(7) . . ? C8 C9 H12 109.5 . . ? C8 C9 H13 109.5 . . ? H12 C9 H13 109.5 . . ? C8 C9 H14 109.5 . . ? H12 C9 H14 109.5 . . ? H13 C9 H14 109.5 . . ? N7 C10 C11 173.5(18) . . ? C10 C11 H15 109.5 . . ? C10 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? C10 C11 H17 109.5 . . ? H15 C11 H17 109.5 . . ? H16 C11 H17 109.5 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.151 _refine_diff_density_min -1.791 _refine_diff_density_rms 0.254 data_8 _database_code_depnum_ccdc_archive 'CCDC 798370' #TrackingRef 'Compiled.cif' # start Validation Reply Form _vrf_CHEMW03_8 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: This structure was Squeezed. As a result, nine water molecules per formula unit are not present in the model, however, they have been included in the formula for the calculation of intensive properties (density, etc...) The treated via Squeeze is discussed further under "platon_squeeze_ details". ; _vrf_PLAT306_8 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O49 RESPONSE: O49 is a lattice solvent molecule for which the protons could not be located in difference map positions, and were therefore omitted from the model. This atom is further discussed under refine_special_details. ; _vrf_PLAT043_8 ; PROBLEM: Check Reported Molecular Weight ................ 1888.00 RESPONSE: This structure was Squeezed. As a result, nine water molecules per formula unit are not present in the model, however, they have been included in the formula for the calculation of intensive properties (density, etc...) The treated via Squeeze is discussed further under "platon_squeeze_ details". ; _vrf_PLAT044_8 ; PROBLEM: Calculated and Reported Dx Differ .............. ? RESPONSE: This structure was Squeezed. As a result, nine water molecules per formula unit are not present in the model, however, they have been included in the formula for the calculation of intensive properties (density, etc...) The treated via Squeeze is discussed further under "platon_squeeze_ details". ; _vrf_PLAT731_8 ; PROBLEM: Bond Calc 1.402(17), Rep 1.402(2) ...... 8.50 su-Ra RESPONSE: A DFIX instruction was used to restrain this bond length. This warning reflects this treatment since calculated s.u.'s are based on reported variances only. (http://journals.iucr.org-PLAT731) The use of restraints is further discussed under "refine_special_details". ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C36 H60 N24 Ni4 O8 S4), 4(Cl O4), 9.5(H2 O)' _chemical_formula_sum 'C36 H78 Cl4 N24 Ni4 O33.50 S4' _chemical_formula_weight 1888.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.241(3) _cell_length_b 22.657(5) _cell_length_c 24.327(4) _cell_angle_alpha 80.500(11) _cell_angle_beta 77.768(15) _cell_angle_gamma 88.138(16) _cell_volume 8097(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 31371 _cell_measurement_theta_min 2.4247 _cell_measurement_theta_max 31.0047 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3896 _exptl_absorpt_coefficient_mu 1.242 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9313 _exptl_absorpt_correction_T_min 0.8280 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 62773 _diffrn_reflns_av_R_equivalents 0.0808 _diffrn_reflns_av_sigmaI/netI 0.1129 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.50 _reflns_number_total 28333 _reflns_number_gt 18856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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. On average, each ligand in this structure bears a charge of (-1) has has 15 hydrogen atoms. OH and NH hydrogen atoms (on average, 3 per ligand) could not be located in difference map positions and so they were omitted from the model. They were included in the formula for charge balance purposes and for the calculation of intensive properties. Bond distances and angles were restrained (DFIX and DANG) in the treatment of the two perchlorate anions containing Cl3 and Cl5. ; _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^)+(0.1462P)^2^+32.7023P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28333 _refine_ls_number_parameters 1741 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1467 _refine_ls_R_factor_gt 0.1153 _refine_ls_wR_factor_ref 0.3256 _refine_ls_wR_factor_gt 0.2965 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.093 0.407 1.000 1377.0 288.7 2 0.236 0.778 0.860 12.2 9.1 3 0.500 0.000 0.500 162.2 27.1 4 0.500 0.500 0.000 130.8 36.8 5 0.764 0.222 0.140 12.2 9.3 _platon_squeeze_details ; The Platon Squeeze procedure was applied to recover 317 electrons per unit cell in five voids (total volume 1694.4 ^A^3); that is 92.75 electrons per formula unit. Disordered lattice solvent water molecules (approx. 9) were present prior to the application of Squeeze, however, a good point atom model could not be achieved. Note that one lattice solvent water molecule, O49 was not removed via Squeeze, but rather, was left in the model as it makes significant H-bonding interactions with ligands from both grid moieties in the asymmetric unit. The application of Squeeze gave a good improvement in the data statistics and allowed for a full anisotropic refinement of the structure. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; 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 0.95329(9) 0.48707(5) 0.28082(5) 0.0473(3) Uani 1 1 d . . . Ni2 Ni 0.69370(8) 0.59839(5) 0.29172(5) 0.0459(3) Uani 1 1 d . . . Ni3 Ni 0.54464(8) 0.44185(5) 0.24283(5) 0.0469(3) Uani 1 1 d . . . Ni4 Ni 0.78708(8) 0.31871(5) 0.26984(5) 0.0465(3) Uani 1 1 d . . . Ni5 Ni 0.48699(8) -0.05846(5) 0.26719(5) 0.0441(3) Uani 1 1 d . . . Ni6 Ni 0.29403(8) 0.11186(5) 0.27229(5) 0.0421(3) Uani 1 1 d . . . Ni7 Ni 0.07462(8) 0.00409(5) 0.22927(5) 0.0434(3) Uani 1 1 d . . . Ni8 Ni 0.26955(8) -0.15931(5) 0.21408(5) 0.0445(3) Uani 1 1 d . . . Cl1 Cl 0.7142(2) 0.89051(15) 0.11030(12) 0.0716(8) Uani 1 1 d . . . Cl2 Cl 0.5763(3) 0.38350(16) 0.53946(13) 0.0889(10) Uani 1 1 d D . . Cl3 Cl 0.6972(5) 0.3258(4) 0.0197(2) 0.181(3) Uani 1 1 d D . . Cl4 Cl 0.1027(2) 0.37418(13) 0.43955(12) 0.0730(8) Uani 1 1 d . . . Cl5 Cl -0.1389(3) 0.12433(18) 0.50270(13) 0.0889(10) Uani 1 1 d . . . Cl6 Cl -0.0739(2) 0.13335(13) 0.06451(11) 0.0650(7) Uani 1 1 d . . . Cl7 Cl 0.2346(2) 0.35617(15) 0.03993(12) 0.0740(8) Uani 1 1 d . . . Cl8 Cl 0.3497(2) 0.16527(14) 0.46958(13) 0.0698(7) Uani 1 1 d . . . S1 S 0.84361(18) 0.56174(12) 0.27394(10) 0.0541(6) Uani 1 1 d . . . S2 S 0.6214(2) 0.51342(12) 0.27723(10) 0.0601(7) Uani 1 1 d . . . S3 S 0.65886(17) 0.36693(11) 0.23927(10) 0.0507(6) Uani 1 1 d . . . S4 S 0.8589(2) 0.40538(12) 0.28311(10) 0.0594(7) Uani 1 1 d . . . S5 S 0.37920(17) 0.02109(11) 0.27663(10) 0.0493(6) Uani 1 1 d . . . S6 S 0.17479(16) 0.07800(11) 0.23715(9) 0.0473(5) Uani 1 1 d . . . S7 S 0.18123(17) -0.07428(10) 0.23371(9) 0.0473(5) Uani 1 1 d . . . S8 S 0.40804(16) -0.12033(10) 0.22361(10) 0.0459(5) Uani 1 1 d . . . O1 O 1.1280(5) 0.4120(4) 0.2897(3) 0.071(2) Uani 1 1 d . . . O2 O 0.5210(5) 0.6759(4) 0.3153(3) 0.070(2) Uani 1 1 d . . . O3 O 0.7691(5) 0.7168(3) 0.3147(3) 0.0573(17) Uani 1 1 d . . . O4 O 0.4100(5) 0.3664(3) 0.2008(3) 0.0622(19) Uani 1 1 d . . . O5 O 0.3805(5) 0.5303(4) 0.2332(3) 0.078(2) Uani 1 1 d . . . O6 O 0.9366(5) 0.2337(3) 0.3060(3) 0.068(2) Uani 1 1 d . . . O7 O 0.7202(5) 0.1926(3) 0.2590(3) 0.0547(16) Uani 1 1 d . . . O8 O 1.1030(5) 0.5787(4) 0.2800(3) 0.071(2) Uani 1 1 d . . . O9 O 0.6447(5) -0.1547(3) 0.2640(3) 0.0575(17) Uani 1 1 d . . . O10 O 0.1912(4) 0.2347(3) 0.2723(3) 0.0517(16) Uani 1 1 d . . . O11 O 0.4377(5) 0.1779(3) 0.3160(3) 0.0555(17) Uani 1 1 d . . . O12 O -0.0808(5) -0.0768(3) 0.2160(3) 0.068(2) Uani 1 1 d . . . O13 O -0.0808(4) 0.0978(3) 0.2228(3) 0.0542(16) Uani 1 1 d . . . O14 O 0.3514(5) -0.2835(3) 0.1867(3) 0.0571(17) Uani 1 1 d . . . O15 O 0.1057(5) -0.2285(3) 0.1949(3) 0.067(2) Uani 1 1 d . . . O16 O 0.6323(5) -0.0021(4) 0.3166(3) 0.065(2) Uani 1 1 d . . . O17 O 0.7253(9) 0.9437(5) 0.0703(4) 0.130(4) Uani 1 1 d . . . O18 O 0.7296(6) 0.9065(4) 0.1624(3) 0.081(2) Uani 1 1 d . . . O19 O 0.6270(5) 0.8666(4) 0.1188(4) 0.087(3) Uani 1 1 d . . . O20 O 0.7806(7) 0.8509(6) 0.0869(5) 0.129(5) Uani 1 1 d . . . O21 O 0.5487(15) 0.4381(10) 0.5081(7) 0.275(15) Uani 1 1 d D . . O22 O 0.5584(9) 0.3995(6) 0.5906(4) 0.151(6) Uani 1 1 d D . . O23 O 0.5070(8) 0.3432(5) 0.5324(5) 0.129(4) Uani 1 1 d . . . O24 O 0.6562(12) 0.3798(9) 0.5046(9) 0.239(12) Uani 1 1 d D . . O25 O 0.695(2) 0.3871(5) -0.0016(11) 0.41(2) Uani 1 1 d DU . . O26 O 0.6565(7) 0.3126(5) 0.0800(4) 0.118(4) Uani 1 1 d D . . O27 O 0.7896(11) 0.3066(10) 0.0082(8) 0.234(10) Uani 1 1 d D . . O28 O 0.6496(16) 0.2950(15) -0.0058(9) 0.39(2) Uani 1 1 d D . . O29 O 0.0531(7) 0.3643(5) 0.3972(4) 0.116(4) Uani 1 1 d . . . O30 O 0.1326(12) 0.4324(5) 0.4200(5) 0.169(7) Uani 1 1 d . . . O31 O 0.1655(7) 0.3301(5) 0.4390(5) 0.118(4) Uani 1 1 d . . . O32 O 0.0450(10) 0.3688(5) 0.4943(5) 0.147(5) Uani 1 1 d . . . O33 O -0.0862(7) 0.1289(4) 0.4482(4) 0.096(3) Uani 1 1 d . . . O34 O -0.1918(19) 0.0790(14) 0.5161(9) 0.38(2) Uani 1 1 d D . . O35 O -0.1667(13) 0.1765(12) 0.5187(10) 0.303(15) Uani 1 1 d D . . O36 O -0.0761(14) 0.1090(13) 0.5383(6) 0.301(16) Uani 1 1 d D . . O37 O -0.0242(8) 0.1133(5) 0.1073(4) 0.120(4) Uani 1 1 d . . . O38 O -0.0753(12) 0.1947(5) 0.0561(8) 0.183(7) Uani 1 1 d . . . O39 O -0.1653(10) 0.1241(9) 0.0810(6) 0.195(8) Uani 1 1 d . . . O40 O -0.0356(12) 0.1122(9) 0.0170(5) 0.229(11) Uani 1 1 d . . . O41 O 0.3196(6) 0.3278(4) 0.0195(5) 0.098(3) Uani 1 1 d . . . O42 O 0.1940(6) 0.3254(5) 0.0957(4) 0.096(3) Uani 1 1 d . . . O43 O 0.1780(7) 0.3527(5) 0.0004(4) 0.097(3) Uani 1 1 d . . . O44 O 0.2465(7) 0.4176(4) 0.0427(4) 0.095(3) Uani 1 1 d . . . O45 O 0.3659(10) 0.1278(6) 0.4263(4) 0.142(5) Uani 1 1 d . . . O46 O 0.3186(8) 0.1240(6) 0.5186(4) 0.128(4) Uani 1 1 d . . . O47 O 0.2865(8) 0.2063(6) 0.4561(11) 0.239(12) Uani 1 1 d . . . O48 O 0.4313(7) 0.1907(6) 0.4692(5) 0.116(4) Uani 1 1 d . . . O49 O 0.2965(5) 0.2802(3) 0.1752(3) 0.0628(19) Uani 1 1 d . . . N1 N 1.0736(6) 0.4408(4) 0.2558(4) 0.055(2) Uani 1 1 d . . . N2 N 0.9803(6) 0.5099(4) 0.1944(3) 0.054(2) Uani 1 1 d . . . N3 N 0.9235(6) 0.5431(4) 0.1686(3) 0.052(2) Uani 1 1 d . . . N4 N 0.8012(6) 0.6037(3) 0.1724(3) 0.056(2) Uani 1 1 d . . . N5 N 0.7325(5) 0.6282(3) 0.2071(3) 0.0451(18) Uani 1 1 d . . . N6 N 0.5911(5) 0.6568(3) 0.2762(3) 0.0484(18) Uani 1 1 d . . . N7 N 0.7329(6) 0.6605(3) 0.3363(3) 0.0506(19) Uani 1 1 d . . . N8 N 0.6571(5) 0.5598(4) 0.3747(3) 0.0506(19) Uani 1 1 d . . . N9 N 0.6197(6) 0.5036(3) 0.3888(3) 0.056(2) Uani 1 1 d . . . N10 N 0.5332(5) 0.4368(4) 0.3680(3) 0.0507(19) Uani 1 1 d . . . N11 N 0.5001(5) 0.4164(3) 0.3262(3) 0.0436(17) Uani 1 1 d . . . N12 N 0.4462(5) 0.3805(3) 0.2457(3) 0.0469(18) Uani 1 1 d . . . N13 N 0.4638(6) 0.5086(4) 0.2101(4) 0.058(2) Uani 1 1 d . . . N14 N 0.6108(5) 0.4669(3) 0.1622(3) 0.0454(18) Uani 1 1 d . . . N15 N 0.6950(6) 0.4430(4) 0.1387(3) 0.057(2) Uani 1 1 d . . . N16 N 0.8000(6) 0.3755(3) 0.1499(3) 0.0494(19) Uani 1 1 d . . . N17 N 0.8393(5) 0.3344(3) 0.1856(3) 0.0495(19) Uani 1 1 d . . . N18 N 0.9064(6) 0.2699(4) 0.2622(4) 0.056(2) Uani 1 1 d . . . N19 N 0.7175(5) 0.2380(4) 0.2909(3) 0.0507(19) Uani 1 1 d . . . N20 N 0.7333(5) 0.3149(3) 0.3528(3) 0.0402(16) Uani 1 1 d . . . N21 N 0.7424(5) 0.3610(3) 0.3808(3) 0.0458(18) Uani 1 1 d . . . N22 N 0.8387(6) 0.4308(3) 0.3913(3) 0.053(2) Uani 1 1 d . . . N23 N 0.9084(6) 0.4690(3) 0.3645(3) 0.0509(19) Uani 1 1 d . . . N24 N 1.0292(6) 0.5430(4) 0.3105(4) 0.054(2) Uani 1 1 d . . . N25 N 0.5643(5) -0.1321(3) 0.2918(3) 0.0468(18) Uani 1 1 d . . . N26 N 0.4232(5) -0.0878(3) 0.3471(3) 0.0460(18) Uani 1 1 d . . . N27 N 0.3485(6) -0.0595(3) 0.3734(3) 0.053(2) Uani 1 1 d . . . N28 N 0.2625(5) 0.0220(4) 0.3778(3) 0.0514(19) Uani 1 1 d . . . N29 N 0.2425(5) 0.0768(3) 0.3534(3) 0.0390(16) Uani 1 1 d . . . N30 N 0.2093(5) 0.1794(3) 0.3018(3) 0.0453(18) Uani 1 1 d . . . N31 N 0.4048(5) 0.1644(3) 0.2703(3) 0.0503(19) Uani 1 1 d . . . N32 N 0.3418(4) 0.1379(3) 0.1895(3) 0.0396(16) Uani 1 1 d . . . N33 N 0.3088(5) 0.1184(3) 0.1468(3) 0.0465(18) Uani 1 1 d . . . N34 N 0.1979(5) 0.0673(3) 0.1266(3) 0.0488(19) Uani 1 1 d . . . N35 N 0.1205(5) 0.0312(3) 0.1467(3) 0.0457(18) Uani 1 1 d . . . N36 N -0.0054(6) -0.0410(3) 0.1913(3) 0.053(2) Uani 1 1 d . . . N37 N -0.0362(5) 0.0573(3) 0.2558(3) 0.0459(18) Uani 1 1 d . . . N38 N 0.0409(5) -0.0237(3) 0.3127(3) 0.0434(17) Uani 1 1 d . . . N39 N 0.0864(5) -0.0701(3) 0.3406(3) 0.0504(19) Uani 1 1 d . . . N40 N 0.1755(6) -0.1495(4) 0.3324(3) 0.060(2) Uani 1 1 d . . . N41 N 0.2245(5) -0.1862(4) 0.2971(3) 0.0505(19) Uani 1 1 d . . . N42 N 0.3161(5) -0.2466(3) 0.2259(3) 0.0473(18) Uani 1 1 d . . . N43 N 0.1784(6) -0.1900(3) 0.1727(4) 0.054(2) Uani 1 1 d . . . N44 N 0.3172(5) -0.1224(3) 0.1329(3) 0.0470(18) Uani 1 1 d . . . N45 N 0.3816(5) -0.0804(3) 0.1162(3) 0.0457(18) Uani 1 1 d . . . N46 N 0.4862(5) -0.0303(3) 0.1444(3) 0.0440(17) Uani 1 1 d . . . N47 N 0.5333(5) -0.0239(3) 0.1847(3) 0.0440(17) Uani 1 1 d . . . N48 N 0.5928(6) -0.0054(4) 0.2706(3) 0.052(2) Uani 1 1 d . . . C1 C 1.2042(11) 0.4369(8) 0.1799(6) 0.129(7) Uani 1 1 d . . . H1A H 1.2305 0.4166 0.2114 0.154 Uiso 1 1 calc R . . H1B H 1.2401 0.4724 0.1608 0.154 Uiso 1 1 calc R . . H1C H 1.2038 0.4096 0.1526 0.154 Uiso 1 1 calc R . . C2 C 1.1112(8) 0.4551(6) 0.2025(5) 0.071(3) Uani 1 1 d . . . C3 C 1.0520(8) 0.4880(5) 0.1677(4) 0.063(3) Uani 1 1 d . . . C4 C 1.0788(11) 0.4975(7) 0.1041(5) 0.105(5) Uani 1 1 d . . . H4A H 1.0286 0.4868 0.0883 0.126 Uiso 1 1 calc R . . H4B H 1.1307 0.4722 0.0925 0.126 Uiso 1 1 calc R . . H4C H 1.0948 0.5396 0.0899 0.126 Uiso 1 1 calc R . . C5 C 0.8523(7) 0.5712(4) 0.2006(4) 0.048(2) Uani 1 1 d . . . C6 C 0.6937(9) 0.6925(5) 0.1218(5) 0.072(3) Uani 1 1 d . . . H6A H 0.7485 0.6758 0.1010 0.086 Uiso 1 1 calc R . . H6B H 0.6987 0.7362 0.1160 0.086 Uiso 1 1 calc R . . H6C H 0.6420 0.6814 0.1076 0.086 Uiso 1 1 calc R . . C7 C 0.6811(7) 0.6677(4) 0.1851(4) 0.056(3) Uani 1 1 d . . . C8 C 0.6053(6) 0.6892(4) 0.2256(4) 0.048(2) Uani 1 1 d . . . C9 C 0.5512(8) 0.7401(5) 0.2082(5) 0.070(3) Uani 1 1 d . . . H9A H 0.5247 0.7320 0.1768 0.084 Uiso 1 1 calc R . . H9B H 0.5892 0.7759 0.1955 0.084 Uiso 1 1 calc R . . H9C H 0.5033 0.7466 0.2405 0.084 Uiso 1 1 calc R . . C10 C 0.7371(9) 0.6834(5) 0.4310(5) 0.068(3) Uani 1 1 d . . . H10A H 0.7945 0.6718 0.4417 0.081 Uiso 1 1 calc R . . H10B H 0.6889 0.6783 0.4653 0.081 Uiso 1 1 calc R . . H10C H 0.7399 0.7254 0.4127 0.081 Uiso 1 1 calc R . . C11 C 0.7186(7) 0.6448(5) 0.3907(4) 0.052(2) Uani 1 1 d . . . C12 C 0.6815(7) 0.5856(4) 0.4126(4) 0.052(2) Uani 1 1 d . . . C13 C 0.6699(9) 0.5572(5) 0.4752(4) 0.066(3) Uani 1 1 d . . . H13A H 0.6104 0.5671 0.4961 0.079 Uiso 1 1 calc R . . H13B H 0.7162 0.5725 0.4916 0.079 Uiso 1 1 calc R . . H13C H 0.6756 0.5136 0.4780 0.079 Uiso 1 1 calc R . . C14 C 0.5888(7) 0.4821(4) 0.3481(4) 0.051(2) Uani 1 1 d . . . C15 C 0.4058(7) 0.3447(4) 0.4034(4) 0.056(3) Uani 1 1 d . . . H15A H 0.4495 0.3507 0.4263 0.067 Uiso 1 1 calc R . . H15B H 0.3978 0.3018 0.4045 0.067 Uiso 1 1 calc R . . H15C H 0.3482 0.3624 0.4190 0.067 Uiso 1 1 calc R . . C16 C 0.4392(6) 0.3741(4) 0.3431(4) 0.045(2) Uani 1 1 d . . . C17 C 0.4030(6) 0.3575(4) 0.2965(4) 0.046(2) Uani 1 1 d . . . C18 C 0.3256(8) 0.3170(5) 0.3068(4) 0.067(3) Uani 1 1 d . . . H18A H 0.2714 0.3367 0.3248 0.080 Uiso 1 1 calc R . . H18B H 0.3362 0.2802 0.3320 0.080 Uiso 1 1 calc R . . H18C H 0.3175 0.3071 0.2705 0.080 Uiso 1 1 calc R . . C19 C 0.4536(10) 0.5875(6) 0.1302(5) 0.094(5) Uani 1 1 d . . . H19A H 0.4273 0.5751 0.1005 0.112 Uiso 1 1 calc R . . H19B H 0.4983 0.6190 0.1129 0.112 Uiso 1 1 calc R . . H19C H 0.4062 0.6029 0.1582 0.112 Uiso 1 1 calc R . . C20 C 0.4975(7) 0.5355(5) 0.1590(4) 0.057(3) Uani 1 1 d . . . C21 C 0.5819(8) 0.5138(5) 0.1312(5) 0.065(3) Uani 1 1 d . . . C22 C 0.6329(10) 0.5398(6) 0.0744(5) 0.089(4) Uani 1 1 d . . . H22A H 0.6867 0.5597 0.0784 0.107 Uiso 1 1 calc R . . H22B H 0.5953 0.5689 0.0556 0.107 Uiso 1 1 calc R . . H22C H 0.6505 0.5079 0.0515 0.107 Uiso 1 1 calc R . . C23 C 0.7214(7) 0.3982(5) 0.1729(4) 0.051(2) Uani 1 1 d . . . C24 C 0.9611(8) 0.3172(5) 0.1061(5) 0.070(3) Uani 1 1 d . . . H24A H 0.9646 0.2794 0.0912 0.084 Uiso 1 1 calc R . . H24B H 1.0219 0.3317 0.1037 0.084 Uiso 1 1 calc R . . H24C H 0.9292 0.3469 0.0835 0.084 Uiso 1 1 calc R . . C25 C 0.9122(8) 0.3076(4) 0.1663(4) 0.057(3) Uani 1 1 d . . . C26 C 0.9498(6) 0.2673(4) 0.2105(4) 0.046(2) Uani 1 1 d . . . C27 C 1.0277(7) 0.2313(5) 0.1965(4) 0.061(3) Uani 1 1 d . . . H27A H 1.0397 0.2069 0.2314 0.073 Uiso 1 1 calc R . . H27B H 1.0795 0.2572 0.1783 0.073 Uiso 1 1 calc R . . H27C H 1.0174 0.2050 0.1703 0.073 Uiso 1 1 calc R . . C28 C 0.6356(7) 0.1649(4) 0.3697(4) 0.055(2) Uani 1 1 d . . . H28A H 0.6715 0.1331 0.3529 0.066 Uiso 1 1 calc R . . H28B H 0.5747 0.1640 0.3626 0.066 Uiso 1 1 calc R . . H28C H 0.6328 0.1585 0.4109 0.066 Uiso 1 1 calc R . . C29 C 0.6782(6) 0.2246(4) 0.3431(4) 0.049(2) Uani 1 1 d . . . C30 C 0.6794(7) 0.2713(5) 0.3791(4) 0.058(3) Uani 1 1 d . . . C31 C 0.6278(8) 0.2662(5) 0.4379(4) 0.073(3) Uani 1 1 d . . . H31A H 0.6692 0.2641 0.4640 0.087 Uiso 1 1 calc R . . H31B H 0.5909 0.2299 0.4473 0.087 Uiso 1 1 calc R . . H31C H 0.5889 0.3012 0.4417 0.087 Uiso 1 1 calc R . . C32 C 0.8145(6) 0.4012(4) 0.3545(4) 0.048(2) Uani 1 1 d . . . C33 C 0.9036(8) 0.4968(5) 0.4587(4) 0.066(3) Uani 1 1 d . . . H33A H 0.8387 0.4896 0.4672 0.079 Uiso 1 1 calc R . . H33B H 0.9156 0.5348 0.4700 0.079 Uiso 1 1 calc R . . H33C H 0.9328 0.4641 0.4798 0.079 Uiso 1 1 calc R . . C34 C 0.9401(6) 0.4996(4) 0.3954(4) 0.049(2) Uani 1 1 d . . . C35 C 1.0150(6) 0.5386(5) 0.3654(4) 0.050(2) Uani 1 1 d . . . C36 C 1.0697(7) 0.5691(6) 0.3949(5) 0.072(3) Uani 1 1 d . . . H36A H 1.1238 0.5455 0.3987 0.087 Uiso 1 1 calc R . . H36B H 1.0349 0.5733 0.4328 0.087 Uiso 1 1 calc R . . H36C H 1.0869 0.6088 0.3729 0.087 Uiso 1 1 calc R . . C37 C 0.5831(8) -0.2101(4) 0.3721(5) 0.060(3) Uani 1 1 d . . . H37A H 0.6342 -0.2217 0.3441 0.072 Uiso 1 1 calc R . . H37B H 0.5422 -0.2443 0.3868 0.072 Uiso 1 1 calc R . . H37C H 0.6048 -0.1978 0.4037 0.072 Uiso 1 1 calc R . . C38 C 0.5341(6) -0.1589(4) 0.3442(4) 0.047(2) Uani 1 1 d . . . C39 C 0.4509(7) -0.1345(4) 0.3739(4) 0.051(2) Uani 1 1 d . . . C40 C 0.4097(9) -0.1643(6) 0.4341(5) 0.081(4) Uani 1 1 d . . . H40A H 0.4244 -0.1410 0.4615 0.098 Uiso 1 1 calc R . . H40B H 0.4337 -0.2049 0.4409 0.098 Uiso 1 1 calc R . . H40C H 0.3443 -0.1663 0.4387 0.098 Uiso 1 1 calc R . . C41 C 0.3284(6) -0.0061(4) 0.3455(4) 0.045(2) Uani 1 1 d . . . C42 C 0.1407(7) 0.0891(5) 0.4444(4) 0.055(2) Uani 1 1 d . . . H42A H 0.1244 0.0467 0.4499 0.066 Uiso 1 1 calc R . . H42B H 0.0864 0.1130 0.4534 0.066 Uiso 1 1 calc R . . H42C H 0.1811 0.0946 0.4695 0.066 Uiso 1 1 calc R . . C43 C 0.1867(6) 0.1088(4) 0.3840(4) 0.046(2) Uani 1 1 d . . . C44 C 0.1684(6) 0.1680(4) 0.3534(4) 0.0403(19) Uani 1 1 d . . . C45 C 0.1035(8) 0.2102(5) 0.3849(5) 0.069(3) Uani 1 1 d . . . H45A H 0.1197 0.2128 0.4214 0.083 Uiso 1 1 calc R . . H45B H 0.0421 0.1948 0.3920 0.083 Uiso 1 1 calc R . . H45C H 0.1071 0.2501 0.3617 0.083 Uiso 1 1 calc R . . C46 C 0.5271(7) 0.2284(5) 0.2109(5) 0.063(3) Uani 1 1 d . . . H46A H 0.5084 0.2699 0.2127 0.075 Uiso 1 1 calc R . . H46B H 0.5638 0.2258 0.1731 0.075 Uiso 1 1 calc R . . H46C H 0.5624 0.2149 0.2400 0.075 Uiso 1 1 calc R . . C47 C 0.4461(6) 0.1895(4) 0.2215(4) 0.051(2) Uani 1 1 d . . . C48 C 0.4121(7) 0.1723(4) 0.1731(4) 0.048(2) Uani 1 1 d . . . C49 C 0.4553(8) 0.1974(5) 0.1127(4) 0.063(3) Uani 1 1 d . . . H49A H 0.4577 0.1664 0.0887 0.075 Uiso 1 1 calc R . . H49B H 0.5164 0.2109 0.1112 0.075 Uiso 1 1 calc R . . H49C H 0.4200 0.2313 0.0987 0.075 Uiso 1 1 calc R . . C50 C 0.2293(6) 0.0892(4) 0.1691(4) 0.044(2) Uani 1 1 d . . . C51 C 0.1250(8) 0.0159(5) 0.0470(4) 0.061(3) Uani 1 1 d . . . H51A H 0.1044 0.0542 0.0290 0.074 Uiso 1 1 calc R . . H51B H 0.1030 -0.0168 0.0316 0.074 Uiso 1 1 calc R . . H51C H 0.1908 0.0153 0.0391 0.074 Uiso 1 1 calc R . . C52 C 0.0896(7) 0.0080(4) 0.1099(4) 0.047(2) Uani 1 1 d . . . C53 C 0.0105(7) -0.0305(4) 0.1371(4) 0.052(2) Uani 1 1 d . . . C54 C -0.0528(9) -0.0524(6) 0.1028(4) 0.081(4) Uani 1 1 d . . . H54A H -0.1052 -0.0721 0.1292 0.097 Uiso 1 1 calc R . . H54B H -0.0209 -0.0809 0.0794 0.097 Uiso 1 1 calc R . . H54C H -0.0725 -0.0182 0.0781 0.097 Uiso 1 1 calc R . . C55 C -0.1510(7) 0.0815(5) 0.3367(4) 0.062(3) Uani 1 1 d . . . H55A H -0.1363 0.1016 0.3663 0.074 Uiso 1 1 calc R . . H55B H -0.2003 0.0531 0.3537 0.074 Uiso 1 1 calc R . . H55C H -0.1693 0.1113 0.3073 0.074 Uiso 1 1 calc R . . C56 C -0.0688(7) 0.0479(4) 0.3101(4) 0.049(2) Uani 1 1 d . . . C57 C -0.0224(7) 0.0033(4) 0.3448(4) 0.050(2) Uani 1 1 d . . . C58 C -0.0539(9) -0.0105(5) 0.4073(4) 0.073(3) Uani 1 1 d . . . H58A H -0.1138 -0.0285 0.4162 0.088 Uiso 1 1 calc R . . H58B H -0.0564 0.0265 0.4235 0.088 Uiso 1 1 calc R . . H58C H -0.0122 -0.0386 0.4235 0.088 Uiso 1 1 calc R . . C59 C 0.1471(6) -0.0997(4) 0.3051(4) 0.044(2) Uani 1 1 d . . . C60 C 0.2283(9) -0.2635(5) 0.3819(4) 0.068(3) Uani 1 1 d . . . H60A H 0.2243 -0.2305 0.4038 0.082 Uiso 1 1 calc R . . H60B H 0.2780 -0.2899 0.3897 0.082 Uiso 1 1 calc R . . H60C H 0.1720 -0.2862 0.3931 0.082 Uiso 1 1 calc R . . C61 C 0.2448(7) -0.2385(4) 0.3189(5) 0.057(3) Uani 1 1 d . . . C62 C 0.2931(6) -0.2763(5) 0.2784(4) 0.050(2) Uani 1 1 d . . . C63 C 0.3060(7) -0.3397(4) 0.2951(5) 0.059(3) Uani 1 1 d . . . H63A H 0.2547 -0.3618 0.2902 0.071 Uiso 1 1 calc R . . H63B H 0.3111 -0.3478 0.3351 0.071 Uiso 1 1 calc R . . H63C H 0.3611 -0.3525 0.2712 0.071 Uiso 1 1 calc R . . C64 C 0.1480(7) -0.1984(5) 0.0801(5) 0.069(3) Uani 1 1 d . . . H64A H 0.1052 -0.2293 0.1021 0.082 Uiso 1 1 calc R . . H64B H 0.1909 -0.2157 0.0510 0.082 Uiso 1 1 calc R . . H64C H 0.1156 -0.1655 0.0616 0.082 Uiso 1 1 calc R . . C65 C 0.1963(7) -0.1756(4) 0.1182(4) 0.052(2) Uani 1 1 d . . . C66 C 0.2743(7) -0.1344(4) 0.0946(4) 0.045(2) Uani 1 1 d . . . C67 C 0.2992(7) -0.1113(5) 0.0323(4) 0.062(3) Uani 1 1 d . . . H67A H 0.3467 -0.0812 0.0251 0.074 Uiso 1 1 calc R . . H67B H 0.2465 -0.0932 0.0192 0.074 Uiso 1 1 calc R . . H67C H 0.3209 -0.1444 0.0117 0.074 Uiso 1 1 calc R . . C68 C 0.4262(6) -0.0764(4) 0.1570(4) 0.047(2) Uani 1 1 d . . . C69 C 0.6266(8) 0.0583(5) 0.1187(5) 0.070(3) Uani 1 1 d . . . H69A H 0.6152 0.0405 0.0868 0.084 Uiso 1 1 calc R . . H69B H 0.6911 0.0659 0.1132 0.084 Uiso 1 1 calc R . . H69C H 0.5938 0.0961 0.1204 0.084 Uiso 1 1 calc R . . C70 C 0.5959(6) 0.0165(4) 0.1728(4) 0.048(2) Uani 1 1 d . . . C71 C 0.6380(6) 0.0201(4) 0.2238(4) 0.048(2) Uani 1 1 d . . . C72 C 0.7277(9) 0.0507(6) 0.2150(5) 0.081(4) Uani 1 1 d . . . H72A H 0.7225 0.0813 0.2397 0.098 Uiso 1 1 calc R . . H72B H 0.7462 0.0696 0.1751 0.098 Uiso 1 1 calc R . . H72C H 0.7727 0.0211 0.2246 0.098 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 0.0552(8) 0.0495(7) 0.0368(6) -0.0036(5) -0.0107(5) -0.0031(5) Ni2 0.0485(7) 0.0503(7) 0.0383(6) -0.0045(5) -0.0088(5) -0.0063(5) Ni3 0.0546(7) 0.0471(7) 0.0381(6) -0.0035(5) -0.0097(5) -0.0069(5) Ni4 0.0542(7) 0.0455(7) 0.0367(6) -0.0029(5) -0.0052(5) -0.0044(5) Ni5 0.0469(7) 0.0475(7) 0.0373(6) -0.0032(5) -0.0098(5) -0.0026(5) Ni6 0.0445(7) 0.0443(7) 0.0371(6) -0.0049(5) -0.0086(5) -0.0039(5) Ni7 0.0453(7) 0.0496(7) 0.0350(6) -0.0058(5) -0.0081(5) -0.0043(5) Ni8 0.0499(7) 0.0460(7) 0.0380(6) -0.0052(5) -0.0110(5) -0.0022(5) Cl1 0.0726(19) 0.091(2) 0.0506(15) -0.0114(13) -0.0089(13) -0.0146(15) Cl2 0.112(3) 0.086(2) 0.0503(17) 0.0029(15) 0.0143(17) -0.0015(19) Cl3 0.161(5) 0.308(9) 0.076(3) -0.049(4) -0.031(3) 0.094(6) Cl4 0.100(2) 0.0621(17) 0.0524(16) -0.0111(12) -0.0050(15) 0.0026(16) Cl5 0.101(3) 0.105(3) 0.0512(17) -0.0098(16) 0.0019(17) 0.016(2) Cl6 0.0753(19) 0.0719(18) 0.0481(14) -0.0068(12) -0.0171(13) 0.0106(14) Cl7 0.076(2) 0.083(2) 0.0561(16) 0.0040(14) -0.0110(14) -0.0015(15) Cl8 0.0714(19) 0.0727(18) 0.0635(17) -0.0051(13) -0.0125(14) -0.0138(15) S1 0.0584(16) 0.0694(16) 0.0338(12) -0.0071(10) -0.0106(10) 0.0098(12) S2 0.0811(19) 0.0604(16) 0.0366(13) -0.0013(10) -0.0086(12) -0.0240(14) S3 0.0557(15) 0.0526(14) 0.0400(12) -0.0003(10) -0.0072(10) -0.0015(11) S4 0.0751(18) 0.0632(16) 0.0376(13) -0.0092(11) -0.0025(12) -0.0214(13) S5 0.0549(14) 0.0526(14) 0.0360(12) -0.0014(9) -0.0047(10) 0.0024(11) S6 0.0519(14) 0.0516(14) 0.0380(12) -0.0073(9) -0.0075(10) -0.0084(11) S7 0.0559(14) 0.0461(13) 0.0363(12) -0.0028(9) -0.0044(10) -0.0003(10) S8 0.0505(14) 0.0459(13) 0.0404(12) -0.0019(9) -0.0112(10) -0.0014(10) O1 0.083(6) 0.081(5) 0.055(4) -0.010(4) -0.031(4) 0.035(4) O2 0.062(5) 0.091(6) 0.058(5) -0.023(4) -0.003(4) 0.001(4) O3 0.062(4) 0.055(4) 0.054(4) -0.004(3) -0.008(3) -0.016(3) O4 0.077(5) 0.064(4) 0.050(4) -0.007(3) -0.023(4) -0.009(4) O5 0.068(5) 0.099(6) 0.062(5) -0.006(4) -0.012(4) 0.017(4) O6 0.073(5) 0.078(5) 0.051(4) 0.002(4) -0.018(4) -0.010(4) O7 0.064(4) 0.051(4) 0.055(4) -0.014(3) -0.020(3) 0.000(3) O8 0.069(5) 0.080(5) 0.057(5) -0.007(4) 0.000(4) -0.017(4) O9 0.060(4) 0.059(4) 0.050(4) -0.003(3) -0.013(3) 0.015(3) O10 0.059(4) 0.033(3) 0.065(4) -0.003(3) -0.020(3) 0.001(3) O11 0.055(4) 0.068(4) 0.045(4) -0.007(3) -0.014(3) -0.016(3) O12 0.060(5) 0.085(5) 0.059(4) -0.002(4) -0.014(4) -0.039(4) O13 0.053(4) 0.051(4) 0.057(4) -0.006(3) -0.011(3) 0.009(3) O14 0.067(5) 0.049(4) 0.062(4) -0.023(3) -0.016(3) 0.007(3) O15 0.067(5) 0.079(5) 0.055(4) -0.012(4) -0.007(4) -0.023(4) O16 0.052(4) 0.102(6) 0.048(4) -0.018(4) -0.020(3) -0.017(4) O17 0.181(12) 0.102(8) 0.087(7) 0.023(6) 0.000(7) -0.063(8) O18 0.079(6) 0.117(7) 0.037(4) -0.013(4) 0.006(4) -0.011(5) O19 0.048(5) 0.109(7) 0.104(7) 0.004(5) -0.028(4) -0.023(4) O20 0.080(7) 0.215(13) 0.112(8) -0.098(9) -0.022(6) 0.050(7) O21 0.33(3) 0.32(3) 0.173(16) 0.153(17) -0.163(18) -0.22(2) O22 0.172(12) 0.191(13) 0.080(7) -0.068(8) 0.045(7) -0.081(10) O23 0.132(9) 0.104(8) 0.133(10) -0.027(7) 0.023(8) -0.048(7) O24 0.210(18) 0.25(2) 0.223(19) -0.123(17) 0.120(16) -0.134(17) O25 0.51(3) 0.38(3) 0.27(2) 0.14(2) -0.10(2) 0.24(3) O26 0.112(8) 0.163(11) 0.066(6) -0.017(6) 0.005(6) 0.020(7) O27 0.149(14) 0.32(3) 0.188(17) -0.002(16) 0.034(13) 0.065(16) O28 0.28(3) 0.78(7) 0.146(17) -0.16(3) -0.047(16) -0.22(4) O29 0.097(7) 0.162(10) 0.073(6) 0.036(6) -0.027(5) 0.009(7) O30 0.275(18) 0.079(8) 0.116(10) -0.024(6) 0.055(10) -0.032(9) O31 0.081(7) 0.124(9) 0.154(10) -0.014(7) -0.048(7) 0.042(6) O32 0.224(14) 0.093(8) 0.090(8) -0.027(6) 0.049(8) 0.016(8) O33 0.105(7) 0.087(6) 0.076(6) -0.015(5) 0.032(5) -0.016(5) O34 0.44(4) 0.49(4) 0.182(18) -0.18(2) 0.16(2) -0.39(4) O35 0.179(17) 0.44(4) 0.34(3) -0.28(3) -0.005(18) 0.09(2) O36 0.25(2) 0.51(4) 0.077(10) 0.040(16) 0.010(12) 0.20(3) O37 0.149(10) 0.162(10) 0.050(5) -0.015(6) -0.032(6) 0.059(8) O38 0.250(18) 0.064(8) 0.254(19) -0.015(9) -0.099(15) -0.009(9) O39 0.120(11) 0.32(2) 0.138(12) 0.044(13) -0.064(10) -0.056(13) O40 0.273(19) 0.37(2) 0.085(8) -0.126(12) -0.095(10) 0.229(18) O41 0.072(6) 0.072(6) 0.146(9) -0.015(6) -0.018(6) 0.013(5) O42 0.079(6) 0.130(8) 0.065(5) 0.020(5) -0.009(5) -0.020(5) O43 0.106(7) 0.115(8) 0.079(6) -0.012(5) -0.048(6) 0.023(6) O44 0.127(8) 0.056(5) 0.080(6) -0.017(4) 0.029(5) -0.001(5) O45 0.201(13) 0.171(11) 0.053(6) -0.011(6) -0.018(7) -0.102(10) O46 0.148(10) 0.169(11) 0.049(5) 0.010(6) 0.008(6) -0.053(9) O47 0.078(8) 0.101(10) 0.48(3) 0.064(14) -0.016(13) 0.009(7) O48 0.080(7) 0.173(11) 0.108(8) -0.042(7) -0.029(6) -0.033(7) O49 0.073(5) 0.063(4) 0.049(4) 0.004(3) -0.014(3) -0.007(4) N1 0.057(5) 0.049(5) 0.062(5) -0.014(4) -0.018(4) 0.017(4) N2 0.067(6) 0.060(5) 0.033(4) -0.007(3) -0.008(4) 0.008(4) N3 0.067(5) 0.063(5) 0.030(4) -0.008(3) -0.018(4) 0.021(4) N4 0.079(6) 0.041(4) 0.040(4) 0.000(3) 0.004(4) 0.013(4) N5 0.043(4) 0.039(4) 0.050(4) -0.003(3) -0.001(3) -0.020(3) N6 0.044(4) 0.045(4) 0.055(5) -0.015(4) 0.000(4) -0.003(3) N7 0.062(5) 0.034(4) 0.056(5) -0.003(3) -0.015(4) -0.009(4) N8 0.039(4) 0.071(5) 0.037(4) -0.004(4) 0.000(3) -0.009(4) N9 0.078(6) 0.040(4) 0.051(5) 0.008(3) -0.023(4) -0.019(4) N10 0.056(5) 0.056(5) 0.041(4) -0.006(3) -0.012(4) -0.007(4) N11 0.041(4) 0.049(4) 0.039(4) -0.012(3) -0.002(3) -0.005(3) N12 0.052(5) 0.046(4) 0.043(4) -0.003(3) -0.014(4) -0.001(3) N13 0.054(5) 0.055(5) 0.063(6) -0.010(4) -0.010(4) 0.003(4) N14 0.055(5) 0.039(4) 0.044(4) -0.008(3) -0.013(4) -0.007(3) N15 0.066(6) 0.065(5) 0.040(4) -0.002(4) -0.018(4) 0.009(4) N16 0.060(5) 0.041(4) 0.045(4) -0.005(3) -0.009(4) 0.000(4) N17 0.053(5) 0.044(4) 0.050(5) -0.010(3) -0.005(4) -0.002(4) N18 0.051(5) 0.058(5) 0.058(5) 0.004(4) -0.020(4) 0.002(4) N19 0.045(5) 0.058(5) 0.052(5) -0.012(4) -0.014(4) -0.003(4) N20 0.039(4) 0.034(4) 0.052(4) -0.005(3) -0.022(3) 0.007(3) N21 0.051(5) 0.042(4) 0.047(4) -0.013(3) -0.009(3) -0.007(3) N22 0.061(5) 0.048(5) 0.051(5) -0.001(3) -0.014(4) -0.016(4) N23 0.061(5) 0.041(4) 0.055(5) -0.011(3) -0.018(4) -0.006(4) N24 0.053(5) 0.049(5) 0.058(5) -0.005(4) -0.008(4) -0.002(4) N25 0.059(5) 0.037(4) 0.048(4) 0.000(3) -0.025(4) 0.009(3) N26 0.045(4) 0.054(5) 0.037(4) -0.002(3) -0.007(3) 0.006(4) N27 0.061(5) 0.042(4) 0.048(5) 0.000(3) 0.000(4) 0.011(4) N28 0.052(5) 0.057(5) 0.046(4) -0.009(4) -0.012(4) 0.012(4) N29 0.042(4) 0.041(4) 0.036(4) -0.008(3) -0.010(3) -0.005(3) N30 0.044(4) 0.047(4) 0.045(4) -0.010(3) -0.006(3) -0.011(3) N31 0.054(5) 0.051(5) 0.048(5) -0.005(3) -0.018(4) -0.003(4) N32 0.029(4) 0.031(4) 0.059(5) -0.007(3) -0.011(3) -0.003(3) N33 0.053(5) 0.053(5) 0.033(4) -0.003(3) -0.010(3) -0.008(4) N34 0.039(4) 0.055(5) 0.056(5) -0.018(4) -0.010(4) -0.005(3) N35 0.047(5) 0.052(5) 0.041(4) -0.008(3) -0.014(3) -0.007(3) N36 0.067(5) 0.045(4) 0.044(5) -0.003(3) -0.006(4) -0.015(4) N37 0.042(4) 0.047(4) 0.048(5) -0.003(3) -0.013(3) -0.004(3) N38 0.037(4) 0.047(4) 0.047(4) -0.012(3) -0.008(3) -0.004(3) N39 0.058(5) 0.046(4) 0.043(4) 0.002(3) -0.012(4) 0.020(4) N40 0.083(6) 0.051(5) 0.047(5) -0.006(4) -0.019(4) 0.014(4) N41 0.055(5) 0.050(5) 0.043(4) -0.007(3) -0.001(4) -0.016(4) N42 0.052(5) 0.039(4) 0.058(5) -0.006(3) -0.030(4) 0.006(3) N43 0.059(5) 0.042(4) 0.062(5) -0.008(4) -0.016(4) -0.002(4) N44 0.042(4) 0.044(4) 0.052(5) 0.003(3) -0.013(4) 0.004(3) N45 0.048(5) 0.048(4) 0.040(4) -0.006(3) -0.005(3) -0.013(3) N46 0.040(4) 0.056(5) 0.035(4) -0.001(3) -0.009(3) -0.007(3) N47 0.045(4) 0.046(4) 0.039(4) -0.007(3) -0.005(3) -0.005(3) N48 0.064(5) 0.061(5) 0.036(4) -0.015(4) -0.017(4) -0.003(4) C1 0.141(15) 0.167(17) 0.063(9) -0.009(9) -0.011(9) 0.093(13) C2 0.069(8) 0.097(9) 0.046(6) -0.021(6) -0.005(5) 0.009(6) C3 0.072(7) 0.070(7) 0.047(6) -0.014(5) -0.010(5) 0.028(6) C4 0.124(12) 0.140(13) 0.035(6) 0.000(7) -0.001(7) 0.061(10) C5 0.067(6) 0.035(5) 0.039(5) -0.002(4) -0.012(4) 0.009(4) C6 0.086(9) 0.054(7) 0.067(7) -0.003(5) -0.006(6) 0.019(6) C7 0.067(7) 0.043(5) 0.049(6) 0.009(4) -0.007(5) -0.005(5) C8 0.048(6) 0.055(6) 0.050(6) -0.023(4) -0.021(4) 0.007(4) C9 0.077(8) 0.062(7) 0.070(8) -0.012(5) -0.013(6) 0.016(6) C10 0.084(8) 0.054(6) 0.069(7) -0.001(5) -0.030(6) -0.016(6) C11 0.050(6) 0.058(6) 0.050(6) -0.004(4) -0.015(4) 0.000(4) C12 0.059(6) 0.051(6) 0.041(5) 0.004(4) -0.004(4) -0.003(5) C13 0.092(9) 0.069(7) 0.047(6) -0.009(5) -0.035(6) -0.009(6) C14 0.053(6) 0.056(6) 0.043(5) 0.007(4) -0.019(4) -0.011(5) C15 0.068(7) 0.056(6) 0.041(5) 0.000(4) -0.009(5) -0.019(5) C16 0.046(5) 0.038(5) 0.047(5) 0.001(4) -0.008(4) -0.003(4) C17 0.054(6) 0.040(5) 0.048(5) -0.009(4) -0.018(4) 0.005(4) C18 0.070(7) 0.083(8) 0.042(6) -0.002(5) 0.000(5) -0.027(6) C19 0.103(10) 0.099(10) 0.058(7) 0.020(7) -0.003(7) 0.039(8) C20 0.055(6) 0.071(7) 0.048(6) 0.000(5) -0.021(5) 0.004(5) C21 0.080(8) 0.049(6) 0.060(7) -0.005(5) -0.007(6) 0.005(5) C22 0.098(10) 0.088(9) 0.064(8) 0.004(6) 0.002(7) 0.028(8) C23 0.060(6) 0.066(6) 0.030(5) -0.002(4) -0.021(4) -0.006(5) C24 0.068(7) 0.079(8) 0.056(7) -0.007(5) 0.001(5) -0.007(6) C25 0.084(8) 0.048(6) 0.038(5) 0.002(4) -0.013(5) -0.012(5) C26 0.052(6) 0.043(5) 0.044(5) -0.009(4) -0.005(4) -0.017(4) C27 0.050(6) 0.072(7) 0.055(6) -0.007(5) -0.004(5) 0.007(5) C28 0.058(6) 0.054(6) 0.046(5) -0.003(4) -0.001(5) -0.008(5) C29 0.047(5) 0.052(6) 0.047(5) -0.001(4) -0.014(4) -0.010(4) C30 0.067(7) 0.065(7) 0.040(5) -0.002(4) -0.012(5) 0.011(5) C31 0.086(8) 0.079(8) 0.045(6) -0.008(5) 0.008(5) -0.031(6) C32 0.045(5) 0.060(6) 0.033(5) -0.007(4) 0.006(4) -0.017(4) C33 0.072(7) 0.095(8) 0.025(5) -0.017(5) 0.011(4) -0.028(6) C34 0.042(5) 0.054(6) 0.046(5) 0.006(4) -0.011(4) -0.005(4) C35 0.046(6) 0.068(6) 0.041(5) -0.014(4) -0.019(4) 0.013(5) C36 0.051(7) 0.106(10) 0.060(7) -0.003(6) -0.016(5) -0.018(6) C37 0.079(8) 0.040(5) 0.066(7) -0.001(4) -0.033(6) 0.018(5) C38 0.052(6) 0.047(5) 0.050(6) -0.012(4) -0.023(4) -0.001(4) C39 0.053(6) 0.058(6) 0.038(5) -0.001(4) -0.010(4) 0.011(5) C40 0.086(9) 0.078(8) 0.059(7) 0.015(6) 0.009(6) 0.013(7) C41 0.033(5) 0.048(5) 0.059(6) -0.007(4) -0.021(4) 0.006(4) C42 0.046(6) 0.059(6) 0.053(6) -0.007(4) 0.005(4) 0.004(4) C43 0.046(5) 0.045(5) 0.044(5) 0.005(4) -0.008(4) 0.001(4) C44 0.038(5) 0.031(4) 0.058(6) -0.012(4) -0.019(4) 0.002(3) C45 0.071(7) 0.053(6) 0.070(7) -0.006(5) 0.007(6) 0.016(5) C46 0.061(7) 0.066(7) 0.064(7) -0.007(5) -0.016(5) -0.026(5) C47 0.041(5) 0.044(5) 0.063(6) -0.004(4) -0.005(4) -0.001(4) C48 0.061(6) 0.035(5) 0.043(5) 0.004(4) -0.010(4) 0.002(4) C49 0.080(8) 0.059(6) 0.045(6) -0.006(5) -0.004(5) -0.023(5) C50 0.034(5) 0.039(5) 0.063(6) -0.007(4) -0.018(4) 0.003(4) C51 0.071(7) 0.069(7) 0.047(6) -0.012(5) -0.013(5) -0.015(6) C52 0.063(6) 0.040(5) 0.037(5) -0.007(4) -0.006(4) 0.008(4) C53 0.073(7) 0.035(5) 0.054(6) -0.016(4) -0.024(5) 0.009(4) C54 0.093(9) 0.114(10) 0.041(6) 0.010(6) -0.031(6) -0.057(8) C55 0.058(6) 0.070(7) 0.051(6) 0.002(5) -0.009(5) 0.010(5) C56 0.055(6) 0.042(5) 0.052(6) -0.009(4) -0.012(4) -0.008(4) C57 0.061(6) 0.045(5) 0.043(5) -0.006(4) -0.008(4) 0.000(4) C58 0.111(10) 0.069(7) 0.031(5) 0.003(5) -0.007(5) 0.025(7) C59 0.041(5) 0.043(5) 0.045(5) -0.009(4) 0.000(4) -0.007(4) C60 0.093(9) 0.050(6) 0.052(6) 0.008(5) -0.006(6) 0.005(6) C61 0.060(6) 0.032(5) 0.071(7) 0.004(4) -0.002(5) -0.013(4) C62 0.029(5) 0.071(7) 0.056(6) -0.007(5) -0.023(4) -0.010(4) C63 0.056(6) 0.038(5) 0.086(8) -0.009(5) -0.021(5) -0.009(4) C64 0.048(6) 0.086(8) 0.077(8) -0.016(6) -0.018(5) -0.021(6) C65 0.056(6) 0.052(6) 0.055(6) -0.012(4) -0.027(5) 0.009(4) C66 0.061(6) 0.040(5) 0.038(5) -0.005(4) -0.021(4) 0.004(4) C67 0.053(6) 0.090(8) 0.042(5) -0.003(5) -0.014(5) -0.005(5) C68 0.045(5) 0.053(6) 0.043(5) -0.002(4) -0.017(4) 0.002(4) C69 0.065(7) 0.084(8) 0.057(7) 0.012(6) -0.018(5) -0.023(6) C70 0.054(6) 0.059(6) 0.029(4) -0.001(4) -0.009(4) -0.005(5) C71 0.036(5) 0.064(6) 0.049(6) -0.015(4) -0.013(4) -0.002(4) C72 0.104(10) 0.086(9) 0.060(7) 0.004(6) -0.037(7) -0.043(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N23 1.983(8) . ? Ni1 N2 2.036(7) . ? Ni1 N24 2.053(8) . ? Ni1 N1 2.108(8) . ? Ni1 S1 2.351(3) . ? Ni1 S4 2.367(3) . ? Ni2 N5 2.023(7) . ? Ni2 N8 2.030(7) . ? Ni2 N6 2.071(8) . ? Ni2 N7 2.084(8) . ? Ni2 S2 2.361(3) . ? Ni2 S1 2.382(3) . ? Ni3 N11 1.990(7) . ? Ni3 N14 2.005(8) . ? Ni3 N12 2.061(8) . ? Ni3 N13 2.083(9) . ? Ni3 S2 2.384(3) . ? Ni3 S3 2.390(3) . ? Ni4 N20 2.001(8) . ? Ni4 N17 2.012(8) . ? Ni4 N19 2.077(8) . ? Ni4 N18 2.088(8) . ? Ni4 S4 2.378(3) . ? Ni4 S3 2.403(3) . ? Ni5 N26 1.995(7) . ? Ni5 N47 2.015(7) . ? Ni5 N48 2.067(8) . ? Ni5 N25 2.090(7) . ? Ni5 S8 2.383(3) . ? Ni5 S5 2.405(3) . ? Ni6 N32 1.986(7) . ? Ni6 N29 2.001(7) . ? Ni6 N31 2.084(8) . ? Ni6 N30 2.090(8) . ? Ni6 S6 2.364(3) . ? Ni6 S5 2.395(3) . ? Ni7 N35 1.983(7) . ? Ni7 N38 1.984(7) . ? Ni7 N36 2.064(8) . ? Ni7 N37 2.095(8) . ? Ni7 S6 2.359(3) . ? Ni7 S7 2.372(3) . ? Ni8 N41 1.990(8) . ? Ni8 N44 2.004(8) . ? Ni8 N42 2.075(7) . ? Ni8 N43 2.077(8) . ? Ni8 S7 2.369(3) . ? Ni8 S8 2.384(3) . ? Cl1 O17 1.409(10) . ? Cl1 O19 1.412(8) . ? Cl1 O20 1.421(10) . ? Cl1 O18 1.441(8) . ? Cl2 O22 1.323(10) . ? Cl2 O24 1.338(12) . ? Cl2 O21 1.442(19) . ? Cl2 O23 1.473(11) . ? Cl3 O28 1.329(17) . ? Cl3 O25 1.402(2) . ? Cl3 O27 1.444(15) . ? Cl3 O26 1.450(10) . ? Cl4 O31 1.360(10) . ? Cl4 O30 1.384(11) . ? Cl4 O32 1.421(10) . ? Cl4 O29 1.449(11) . ? Cl5 O34 1.282(16) . ? Cl5 O35 1.33(2) . ? Cl5 O33 1.386(8) . ? Cl5 O36 1.420(18) . ? Cl6 O40 1.335(10) . ? Cl6 O38 1.371(12) . ? Cl6 O39 1.379(14) . ? Cl6 O37 1.421(9) . ? Cl7 O44 1.424(9) . ? Cl7 O43 1.434(9) . ? Cl7 O42 1.439(8) . ? Cl7 O41 1.454(9) . ? Cl8 O47 1.369(13) . ? Cl8 O48 1.384(9) . ? Cl8 O46 1.394(9) . ? Cl8 O45 1.436(12) . ? S1 C5 1.739(9) . ? S2 C14 1.725(9) . ? S3 C23 1.741(9) . ? S4 C32 1.712(9) . ? S5 C41 1.710(10) . ? S6 C50 1.669(10) . ? S7 C59 1.711(9) . ? S8 C68 1.728(9) . ? O1 N1 1.367(10) . ? O2 N6 1.383(10) . ? O3 N7 1.381(9) . ? O4 N12 1.408(10) . ? O5 N13 1.384(11) . ? O6 N18 1.383(10) . ? O7 N19 1.383(10) . ? O8 N24 1.406(10) . ? O9 N25 1.395(10) . ? O10 N30 1.388(9) . ? O11 N31 1.392(9) . ? O12 N36 1.395(10) . ? O13 N37 1.378(9) . ? O14 N42 1.383(10) . ? O15 N43 1.390(10) . ? O16 N48 1.391(9) . ? N1 C2 1.295(13) . ? N2 C3 1.277(13) . ? N2 N3 1.320(11) . ? N3 C5 1.396(12) . ? N4 C5 1.280(12) . ? N4 N5 1.365(11) . ? N5 C7 1.296(12) . ? N6 C8 1.303(12) . ? N7 C11 1.285(12) . ? N8 C12 1.292(12) . ? N8 N9 1.373(10) . ? N9 C14 1.346(12) . ? N10 C14 1.314(11) . ? N10 N11 1.376(10) . ? N11 C16 1.309(11) . ? N12 C17 1.303(11) . ? N13 C20 1.296(12) . ? N14 C21 1.318(13) . ? N14 N15 1.419(11) . ? N15 C23 1.312(12) . ? N16 C23 1.335(13) . ? N16 N17 1.378(11) . ? N17 C25 1.286(13) . ? N18 C26 1.300(12) . ? N19 C29 1.276(11) . ? N20 C30 1.297(12) . ? N20 N21 1.362(9) . ? N21 C32 1.421(11) . ? N22 C32 1.320(12) . ? N22 N23 1.372(10) . ? N23 C34 1.276(12) . ? N24 C35 1.294(12) . ? N25 C38 1.311(12) . ? N26 C39 1.258(11) . ? N26 N27 1.377(10) . ? N27 C41 1.345(11) . ? N28 N29 1.342(10) . ? N28 C41 1.350(12) . ? N29 C43 1.294(11) . ? N30 C44 1.265(11) . ? N31 C47 1.270(12) . ? N32 C48 1.298(11) . ? N32 N33 1.387(10) . ? N33 C50 1.360(11) . ? N34 C50 1.394(11) . ? N34 N35 1.409(10) . ? N35 C52 1.284(11) . ? N36 C53 1.272(12) . ? N37 C56 1.292(11) . ? N38 C57 1.309(12) . ? N38 N39 1.401(10) . ? N39 C59 1.366(11) . ? N40 C59 1.322(12) . ? N40 N41 1.381(11) . ? N41 C61 1.271(12) . ? N42 C62 1.323(12) . ? N43 C65 1.284(12) . ? N44 C66 1.313(11) . ? N44 N45 1.340(10) . ? N45 C68 1.333(11) . ? N46 N47 1.360(10) . ? N46 C68 1.362(11) . ? N47 C70 1.297(11) . ? N48 C71 1.257(12) . ? C1 C2 1.480(18) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.468(15) . ? C3 C4 1.494(14) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 C7 1.523(14) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.477(14) . ? C8 C9 1.454(14) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.491(14) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.447(13) . ? C12 C13 1.527(13) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 C16 1.497(12) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.466(12) . ? C17 C18 1.472(13) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.484(15) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.435(15) . ? C21 C22 1.470(15) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C24 C25 1.481(14) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.490(14) . ? C26 C27 1.432(14) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.504(12) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.482(14) . ? C30 C31 1.468(13) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C33 C34 1.514(12) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.455(13) . ? C35 C36 1.464(14) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.505(12) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.461(13) . ? C39 C40 1.518(13) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C42 C43 1.487(12) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.472(12) . ? C44 C45 1.530(13) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.492(13) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.493(14) . ? C48 C49 1.503(12) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C51 C52 1.494(12) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.481(14) . ? C53 C54 1.542(13) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.524(14) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.470(13) . ? C57 C58 1.478(13) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C60 C61 1.514(14) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.475(14) . ? C62 C63 1.446(13) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.462(13) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.490(14) . ? C66 C67 1.490(12) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C69 C70 1.485(13) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C71 1.529(12) . ? C71 C72 1.511(14) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? 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 N23 Ni1 N2 171.4(3) . . ? N23 Ni1 N24 77.5(3) . . ? N2 Ni1 N24 106.4(3) . . ? N23 Ni1 N1 111.0(3) . . ? N2 Ni1 N1 77.2(3) . . ? N24 Ni1 N1 86.5(3) . . ? N23 Ni1 S1 90.3(2) . . ? N2 Ni1 S1 82.1(2) . . ? N24 Ni1 S1 90.5(2) . . ? N1 Ni1 S1 157.2(2) . . ? N23 Ni1 S4 81.9(2) . . ? N2 Ni1 S4 95.0(3) . . ? N24 Ni1 S4 158.2(2) . . ? N1 Ni1 S4 94.7(2) . . ? S1 Ni1 S4 96.35(11) . . ? N5 Ni2 N8 174.1(3) . . ? N5 Ni2 N6 77.9(3) . . ? N8 Ni2 N6 106.0(3) . . ? N5 Ni2 N7 108.9(3) . . ? N8 Ni2 N7 76.1(3) . . ? N6 Ni2 N7 87.2(3) . . ? N5 Ni2 S2 92.9(2) . . ? N8 Ni2 S2 82.4(2) . . ? N6 Ni2 S2 94.6(2) . . ? N7 Ni2 S2 158.0(2) . . ? N5 Ni2 S1 79.3(2) . . ? N8 Ni2 S1 97.8(2) . . ? N6 Ni2 S1 154.4(2) . . ? N7 Ni2 S1 89.6(2) . . ? S2 Ni2 S1 97.81(11) . . ? N11 Ni3 N14 170.0(3) . . ? N11 Ni3 N12 77.4(3) . . ? N14 Ni3 N12 110.0(3) . . ? N11 Ni3 N13 111.1(3) . . ? N14 Ni3 N13 76.4(3) . . ? N12 Ni3 N13 88.6(3) . . ? N11 Ni3 S2 80.8(2) . . ? N14 Ni3 S2 92.7(2) . . ? N12 Ni3 S2 156.4(2) . . ? N13 Ni3 S2 91.0(3) . . ? N11 Ni3 S3 92.1(2) . . ? N14 Ni3 S3 81.1(2) . . ? N12 Ni3 S3 92.3(2) . . ? N13 Ni3 S3 156.3(3) . . ? S2 Ni3 S3 97.39(11) . . ? N20 Ni4 N17 172.4(3) . . ? N20 Ni4 N19 76.7(3) . . ? N17 Ni4 N19 109.7(3) . . ? N20 Ni4 N18 108.2(3) . . ? N17 Ni4 N18 76.6(3) . . ? N19 Ni4 N18 88.3(3) . . ? N20 Ni4 S4 82.8(2) . . ? N17 Ni4 S4 91.1(2) . . ? N19 Ni4 S4 158.7(2) . . ? N18 Ni4 S4 92.4(2) . . ? N20 Ni4 S3 94.2(2) . . ? N17 Ni4 S3 82.0(2) . . ? N19 Ni4 S3 89.5(2) . . ? N18 Ni4 S3 156.4(2) . . ? S4 Ni4 S3 98.13(11) . . ? N26 Ni5 N47 171.3(3) . . ? N26 Ni5 N48 107.7(3) . . ? N47 Ni5 N48 77.2(3) . . ? N26 Ni5 N25 77.3(3) . . ? N47 Ni5 N25 110.4(3) . . ? N48 Ni5 N25 87.0(3) . . ? N26 Ni5 S8 96.1(2) . . ? N47 Ni5 S8 80.4(2) . . ? N48 Ni5 S8 154.6(2) . . ? N25 Ni5 S8 89.6(2) . . ? N26 Ni5 S5 82.2(2) . . ? N47 Ni5 S5 90.5(2) . . ? N48 Ni5 S5 93.6(2) . . ? N25 Ni5 S5 158.6(2) . . ? S8 Ni5 S5 98.50(9) . . ? N32 Ni6 N29 173.5(3) . . ? N32 Ni6 N31 76.5(3) . . ? N29 Ni6 N31 108.6(3) . . ? N32 Ni6 N30 107.5(3) . . ? N29 Ni6 N30 76.8(3) . . ? N31 Ni6 N30 89.5(3) . . ? N32 Ni6 S6 81.4(2) . . ? N29 Ni6 S6 94.1(2) . . ? N31 Ni6 S6 156.0(2) . . ? N30 Ni6 S6 88.3(2) . . ? N32 Ni6 S5 94.2(2) . . ? N29 Ni6 S5 81.8(2) . . ? N31 Ni6 S5 93.0(2) . . ? N30 Ni6 S5 158.1(2) . . ? S6 Ni6 S5 97.93(10) . . ? N35 Ni7 N38 174.5(3) . . ? N35 Ni7 N36 76.5(3) . . ? N38 Ni7 N36 107.5(3) . . ? N35 Ni7 N37 107.7(3) . . ? N38 Ni7 N37 76.4(3) . . ? N36 Ni7 N37 88.5(3) . . ? N35 Ni7 S6 82.3(2) . . ? N38 Ni7 S6 94.1(2) . . ? N36 Ni7 S6 157.7(2) . . ? N37 Ni7 S6 91.3(2) . . ? N35 Ni7 S7 93.1(2) . . ? N38 Ni7 S7 82.9(2) . . ? N36 Ni7 S7 94.0(3) . . ? N37 Ni7 S7 159.0(2) . . ? S6 Ni7 S7 94.07(10) . . ? N41 Ni8 N44 173.0(3) . . ? N41 Ni8 N42 77.4(3) . . ? N44 Ni8 N42 108.3(3) . . ? N41 Ni8 N43 106.8(3) . . ? N44 Ni8 N43 78.1(3) . . ? N42 Ni8 N43 86.9(3) . . ? N41 Ni8 S7 82.1(3) . . ? N44 Ni8 S7 92.7(2) . . ? N42 Ni8 S7 158.4(2) . . ? N43 Ni8 S7 92.8(2) . . ? N41 Ni8 S8 95.3(2) . . ? N44 Ni8 S8 80.5(2) . . ? N42 Ni8 S8 92.0(2) . . ? N43 Ni8 S8 157.0(2) . . ? S7 Ni8 S8 96.55(9) . . ? O17 Cl1 O19 111.4(7) . . ? O17 Cl1 O20 105.0(8) . . ? O19 Cl1 O20 111.3(7) . . ? O17 Cl1 O18 105.9(6) . . ? O19 Cl1 O18 110.6(5) . . ? O20 Cl1 O18 112.5(6) . . ? O22 Cl2 O24 128.5(12) . . ? O22 Cl2 O21 97.9(12) . . ? O24 Cl2 O21 96.0(11) . . ? O22 Cl2 O23 111.9(7) . . ? O24 Cl2 O23 114.6(9) . . ? O21 Cl2 O23 98.6(8) . . ? O28 Cl3 O25 110.5(16) . . ? O28 Cl3 O27 109.2(15) . . ? O25 Cl3 O27 107.9(14) . . ? O28 Cl3 O26 105.5(13) . . ? O25 Cl3 O26 111.9(13) . . ? O27 Cl3 O26 111.8(9) . . ? O31 Cl4 O30 117.6(9) . . ? O31 Cl4 O32 110.0(8) . . ? O30 Cl4 O32 111.4(7) . . ? O31 Cl4 O29 104.9(7) . . ? O30 Cl4 O29 101.9(9) . . ? O32 Cl4 O29 110.4(8) . . ? O34 Cl5 O35 120.1(17) . . ? O34 Cl5 O33 113.3(9) . . ? O35 Cl5 O33 114.7(13) . . ? O34 Cl5 O36 102.8(16) . . ? O35 Cl5 O36 98.8(14) . . ? O33 Cl5 O36 103.3(8) . . ? O40 Cl6 O38 111.9(13) . . ? O40 Cl6 O39 114.3(12) . . ? O38 Cl6 O39 97.5(12) . . ? O40 Cl6 O37 109.0(7) . . ? O38 Cl6 O37 108.3(9) . . ? O39 Cl6 O37 115.2(8) . . ? O44 Cl7 O43 108.3(6) . . ? O44 Cl7 O42 109.3(6) . . ? O43 Cl7 O42 110.5(6) . . ? O44 Cl7 O41 111.5(6) . . ? O43 Cl7 O41 107.9(6) . . ? O42 Cl7 O41 109.4(6) . . ? O47 Cl8 O48 113.5(8) . . ? O47 Cl8 O46 113.6(9) . . ? O48 Cl8 O46 113.1(7) . . ? O47 Cl8 O45 106.7(12) . . ? O48 Cl8 O45 106.9(7) . . ? O46 Cl8 O45 101.8(7) . . ? C5 S1 Ni1 97.9(3) . . ? C5 S1 Ni2 93.6(3) . . ? Ni1 S1 Ni2 153.41(13) . . ? C14 S2 Ni2 96.9(3) . . ? C14 S2 Ni3 95.0(3) . . ? Ni2 S2 Ni3 166.87(13) . . ? C23 S3 Ni3 95.7(4) . . ? C23 S3 Ni4 93.3(3) . . ? Ni3 S3 Ni4 151.94(12) . . ? C32 S4 Ni1 93.2(3) . . ? C32 S4 Ni4 97.1(3) . . ? Ni1 S4 Ni4 168.38(13) . . ? C41 S5 Ni6 94.6(3) . . ? C41 S5 Ni5 95.4(3) . . ? Ni6 S5 Ni5 168.67(12) . . ? C50 S6 Ni7 97.1(3) . . ? C50 S6 Ni6 94.8(3) . . ? Ni7 S6 Ni6 153.03(12) . . ? C59 S7 Ni8 95.3(3) . . ? C59 S7 Ni7 96.1(3) . . ? Ni8 S7 Ni7 162.09(12) . . ? C68 S8 Ni5 96.8(3) . . ? C68 S8 Ni8 93.6(3) . . ? Ni5 S8 Ni8 149.51(12) . . ? C2 N1 O1 115.2(9) . . ? C2 N1 Ni1 114.1(7) . . ? O1 N1 Ni1 127.9(6) . . ? C3 N2 N3 123.4(8) . . ? C3 N2 Ni1 116.1(7) . . ? N3 N2 Ni1 120.5(6) . . ? N2 N3 C5 119.9(7) . . ? C5 N4 N5 112.1(8) . . ? C7 N5 N4 119.7(8) . . ? C7 N5 Ni2 116.2(7) . . ? N4 N5 Ni2 123.6(6) . . ? C8 N6 O2 114.8(8) . . ? C8 N6 Ni2 115.1(6) . . ? O2 N6 Ni2 128.2(6) . . ? C11 N7 O3 116.5(8) . . ? C11 N7 Ni2 115.4(6) . . ? O3 N7 Ni2 128.0(6) . . ? C12 N8 N9 120.9(8) . . ? C12 N8 Ni2 118.1(6) . . ? N9 N8 Ni2 120.3(6) . . ? C14 N9 N8 117.2(7) . . ? C14 N10 N11 112.9(7) . . ? C16 N11 N10 116.6(7) . . ? C16 N11 Ni3 118.4(6) . . ? N10 N11 Ni3 124.9(5) . . ? C17 N12 O4 114.8(7) . . ? C17 N12 Ni3 115.6(6) . . ? O4 N12 Ni3 128.8(5) . . ? C20 N13 O5 113.6(8) . . ? C20 N13 Ni3 114.7(7) . . ? O5 N13 Ni3 131.7(7) . . ? C21 N14 N15 116.7(8) . . ? C21 N14 Ni3 118.8(7) . . ? N15 N14 Ni3 123.8(6) . . ? C23 N15 N14 113.4(8) . . ? C23 N16 N17 116.7(7) . . ? C25 N17 N16 120.9(8) . . ? C25 N17 Ni4 118.7(7) . . ? N16 N17 Ni4 120.3(6) . . ? C26 N18 O6 117.1(8) . . ? C26 N18 Ni4 116.1(7) . . ? O6 N18 Ni4 126.1(6) . . ? C29 N19 O7 115.0(8) . . ? C29 N19 Ni4 115.2(6) . . ? O7 N19 Ni4 128.8(6) . . ? C30 N20 N21 118.6(8) . . ? C30 N20 Ni4 119.4(6) . . ? N21 N20 Ni4 121.4(5) . . ? N20 N21 C32 115.7(7) . . ? C32 N22 N23 110.3(7) . . ? C34 N23 N22 117.1(8) . . ? C34 N23 Ni1 117.7(6) . . ? N22 N23 Ni1 124.8(6) . . ? C35 N24 O8 115.4(8) . . ? C35 N24 Ni1 115.3(7) . . ? O8 N24 Ni1 128.6(6) . . ? C38 N25 O9 115.1(7) . . ? C38 N25 Ni5 113.3(6) . . ? O9 N25 Ni5 131.5(5) . . ? C39 N26 N27 118.8(8) . . ? C39 N26 Ni5 118.9(6) . . ? N27 N26 Ni5 122.2(6) . . ? C41 N27 N26 116.1(8) . . ? N29 N28 C41 114.7(8) . . ? C43 N29 N28 118.0(7) . . ? C43 N29 Ni6 118.3(6) . . ? N28 N29 Ni6 123.7(6) . . ? C44 N30 O10 115.9(7) . . ? C44 N30 Ni6 115.5(6) . . ? O10 N30 Ni6 128.7(5) . . ? C47 N31 O11 114.9(8) . . ? C47 N31 Ni6 116.6(7) . . ? O11 N31 Ni6 128.4(6) . . ? C48 N32 N33 116.3(7) . . ? C48 N32 Ni6 119.4(6) . . ? N33 N32 Ni6 124.2(5) . . ? C50 N33 N32 110.0(7) . . ? C50 N34 N35 114.3(7) . . ? C52 N35 N34 117.5(8) . . ? C52 N35 Ni7 120.0(6) . . ? N34 N35 Ni7 121.4(5) . . ? C53 N36 O12 114.2(8) . . ? C53 N36 Ni7 115.8(7) . . ? O12 N36 Ni7 129.6(6) . . ? C56 N37 O13 116.9(8) . . ? C56 N37 Ni7 114.6(6) . . ? O13 N37 Ni7 128.3(6) . . ? C57 N38 N39 116.7(8) . . ? C57 N38 Ni7 120.7(6) . . ? N39 N38 Ni7 122.4(6) . . ? C59 N39 N38 114.5(7) . . ? C59 N40 N41 114.2(8) . . ? C61 N41 N40 118.8(8) . . ? C61 N41 Ni8 118.5(7) . . ? N40 N41 Ni8 122.6(6) . . ? C62 N42 O14 112.6(7) . . ? C62 N42 Ni8 115.3(7) . . ? O14 N42 Ni8 130.6(6) . . ? C65 N43 O15 115.2(8) . . ? C65 N43 Ni8 115.3(7) . . ? O15 N43 Ni8 129.2(6) . . ? C66 N44 N45 117.7(8) . . ? C66 N44 Ni8 117.2(6) . . ? N45 N44 Ni8 124.5(6) . . ? C68 N45 N44 112.1(7) . . ? N47 N46 C68 117.0(7) . . ? C70 N47 N46 119.0(7) . . ? C70 N47 Ni5 118.0(6) . . ? N46 N47 Ni5 120.9(5) . . ? C71 N48 O16 113.4(8) . . ? C71 N48 Ni5 116.8(6) . . ? O16 N48 Ni5 128.6(6) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 113.8(10) . . ? N1 C2 C1 121.5(11) . . ? C3 C2 C1 124.7(10) . . ? N2 C3 C2 116.8(9) . . ? N2 C3 C4 122.8(10) . . ? C2 C3 C4 120.2(10) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N4 C5 N3 116.2(8) . . ? N4 C5 S1 126.1(7) . . ? N3 C5 S1 117.7(7) . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N5 C7 C8 115.9(8) . . ? N5 C7 C6 124.8(10) . . ? C8 C7 C6 119.3(9) . . ? N6 C8 C9 125.1(9) . . ? N6 C8 C7 113.4(8) . . ? C9 C8 C7 121.5(9) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N7 C11 C12 116.0(9) . . ? N7 C11 C10 124.6(9) . . ? C12 C11 C10 119.5(9) . . ? N8 C12 C11 113.7(8) . . ? N8 C12 C13 123.4(9) . . ? C11 C12 C13 122.9(9) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N10 C14 N9 113.5(8) . . ? N10 C14 S2 125.4(7) . . ? N9 C14 S2 121.1(7) . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N11 C16 C17 113.4(8) . . ? N11 C16 C15 125.6(8) . . ? C17 C16 C15 120.9(8) . . ? N12 C17 C16 114.4(8) . . ? N12 C17 C18 123.2(8) . . ? C16 C17 C18 122.4(8) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N13 C20 C21 116.8(9) . . ? N13 C20 C19 122.7(10) . . ? C21 C20 C19 120.4(10) . . ? N14 C21 C20 112.6(9) . . ? N14 C21 C22 122.2(10) . . ? C20 C21 C22 125.2(10) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N15 C23 N16 112.8(8) . . ? N15 C23 S3 124.8(8) . . ? N16 C23 S3 122.3(7) . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N17 C25 C24 124.8(10) . . ? N17 C25 C26 114.7(9) . . ? C24 C25 C26 120.4(10) . . ? N18 C26 C27 124.3(9) . . ? N18 C26 C25 113.2(9) . . ? C27 C26 C25 122.4(9) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N19 C29 C30 116.0(8) . . ? N19 C29 C28 124.3(9) . . ? C30 C29 C28 119.6(8) . . ? N20 C30 C31 125.3(10) . . ? N20 C30 C29 111.8(8) . . ? C31 C30 C29 122.9(9) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N22 C32 N21 111.9(7) . . ? N22 C32 S4 128.6(7) . . ? N21 C32 S4 119.5(7) . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N23 C34 C35 115.1(9) . . ? N23 C34 C33 123.6(8) . . ? C35 C34 C33 121.3(8) . . ? N24 C35 C34 113.7(9) . . ? N24 C35 C36 123.5(10) . . ? C34 C35 C36 122.8(9) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C38 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N25 C38 C39 115.3(8) . . ? N25 C38 C37 122.2(9) . . ? C39 C38 C37 122.5(9) . . ? N26 C39 C38 114.9(8) . . ? N26 C39 C40 126.4(9) . . ? C38 C39 C40 118.6(9) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N27 C41 N28 111.8(8) . . ? N27 C41 S5 123.4(7) . . ? N28 C41 S5 124.8(7) . . ? C43 C42 H42A 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C43 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N29 C43 C44 114.0(8) . . ? N29 C43 C42 125.2(8) . . ? C44 C43 C42 120.7(8) . . ? N30 C44 C43 115.4(8) . . ? N30 C44 C45 125.4(8) . . ? C43 C44 C45 119.2(8) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C47 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N31 C47 C46 124.9(10) . . ? N31 C47 C48 113.9(8) . . ? C46 C47 C48 120.9(9) . . ? N32 C48 C47 113.2(8) . . ? N32 C48 C49 126.3(9) . . ? C47 C48 C49 120.3(8) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N33 C50 N34 110.1(8) . . ? N33 C50 S6 127.4(7) . . ? N34 C50 S6 122.4(7) . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N35 C52 C53 111.7(8) . . ? N35 C52 C51 127.4(9) . . ? C53 C52 C51 120.8(8) . . ? N36 C53 C52 115.1(8) . . ? N36 C53 C54 121.9(9) . . ? C52 C53 C54 122.8(9) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 H55A 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C56 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N37 C56 C57 116.5(9) . . ? N37 C56 C55 121.8(9) . . ? C57 C56 C55 121.7(9) . . ? N38 C57 C56 111.3(8) . . ? N38 C57 C58 127.6(9) . . ? C56 C57 C58 120.8(9) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N40 C59 N39 112.1(8) . . ? N40 C59 S7 124.7(7) . . ? N39 C59 S7 123.1(7) . . ? C61 C60 H60A 109.5 . . ? C61 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C61 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N41 C61 C62 115.9(9) . . ? N41 C61 C60 126.0(10) . . ? C62 C61 C60 118.0(9) . . ? N42 C62 C63 125.2(10) . . ? N42 C62 C61 112.5(9) . . ? C63 C62 C61 122.1(9) . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 H64A 109.5 . . ? C65 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C65 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N43 C65 C64 124.5(10) . . ? N43 C65 C66 115.0(8) . . ? C64 C65 C66 120.4(9) . . ? N44 C66 C67 125.2(9) . . ? N44 C66 C65 114.2(8) . . ? C67 C66 C65 120.6(8) . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N45 C68 N46 114.4(8) . . ? N45 C68 S8 125.7(7) . . ? N46 C68 S8 119.8(7) . . ? C70 C69 H69A 109.5 . . ? C70 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C70 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N47 C70 C69 128.5(8) . . ? N47 C70 C71 112.1(8) . . ? C69 C70 C71 119.4(8) . . ? N48 C71 C72 125.9(9) . . ? N48 C71 C70 114.0(8) . . ? C72 C71 C70 120.1(8) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.909 _refine_diff_density_min -1.154 _refine_diff_density_rms 0.133 data_3 _database_code_depnum_ccdc_archive 'CCDC 807545' #TrackingRef 'Compiled.cif' # start Validation Reply Form _vrf_CHEMW03_3 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: This structure was Squeezed. As a result, three methanol, eight water and 0.5 hydroxide ions per formula unit are not present in the model, however, they have been included in the formula for the calculation of intensive properties (density, etc...) The treatment via Squeeze is discussed further under "platon_squeeze_details". ; _vrf_PLAT430_3 ; PROBLEM: Short Inter D...A Contact O27 .. O27 .. 2.49 Ang. RESPONSE: This atom is a 0.25-occupancy H2O molecule which is part of a disordered [Ni(H2O)6] cation. Hydrogen atoms could not be located in difference map positions and were therefore omitted from the model. They were included in the formula for the calculation of intensive properties (density, etc...) ; _vrf_PLAT043_3 ; PROBLEM: Check Reported Molecular Weight ................ 1602.68 RESPONSE: This structure was Squeezed. As a result, three methanol, eight water and 0.5 hydroxide ions per formula unit are not present in the model, however, they have been included in the formula for the calculation of intensive properties (density, etc...) The treatment via Squeeze is discussed further under "platon_squeeze_details". ; _vrf_PLAT044_3 ; PROBLEM: Calculated and Reported Dx Differ .............. ? RESPONSE: This structure was Squeezed. As a result, three methanol, eight water and 0.5 hydroxide ions per formula unit are not present in the model, however, they have been included in the formula for the calculation of intensive properties (density, etc...) The treatment via Squeeze is discussed further under "platon_squeeze_details". ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H30 N16 Ni4 O20, 1.25(H12 Ni O6), 3(C H4 O), 0.5(H O), 8 (H2 O)' _chemical_formula_sum 'C31 H73.50 N16 Ni5.25 O39' _chemical_formula_weight 1602.68 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' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P -3 1 c' _symmetry_space_group_name_Hall '-P 3 2c' _symmetry_Int_Tables_number 163 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, z+1/2' 'x-y, -y, z+1/2' '-x, -x+y, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, -z-1/2' '-x+y, y, -z-1/2' 'x, x-y, -z-1/2' _cell_length_a 28.4916(8) _cell_length_b 28.4916(8) _cell_length_c 30.0145(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 21100.6(13) _cell_formula_units_Z 12 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 63080 _cell_measurement_theta_min 1.9711 _cell_measurement_theta_max 29.8218 _exptl_crystal_description Prism _exptl_crystal_colour 'Light Green' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9966 _exptl_absorpt_coefficient_mu 1.477 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.8984 _exptl_absorpt_correction_T_min 0.7755 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 146241 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 26.50 _reflns_number_total 14570 _reflns_number_gt 13448 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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. In the structure, a Ni(H2O)6 cation sits on a special position. The site-occupancy of that position is 0.5, and the occupancy of the Ni atom on that site was found to be 0.5. That is, a 0.25 occupancy Ni(H2O)6 cation is present in the asymmetric unit. This is deliberate, and does not reflect a redundant site-occupancy error. ; _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^)+(0.0860P)^2^+45.8705P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14570 _refine_ls_number_parameters 736 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1797 _refine_ls_wR_factor_gt 0.1735 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.021 -0.033 0.000 7365 1670 ' ' 2 0.401 0.200 0.750 15 8 ' ' 3 0.799 0.201 0.750 16 7 ' ' 4 0.201 0.401 0.250 15 7 ' ' 5 0.799 0.599 0.750 16 9 ' ' 6 0.200 0.799 0.250 16 8 ' ' 7 0.599 0.799 0.250 16 8 ' ' _platon_squeeze_details ; The Platon Squeeze procedure was applied to recover 1717 electrons per unit cell in seven voids (total volume 7459 ^A^3); that is 143 electrons per formula unit (with Z=12). Disordered lattice solvent methanol (approx. 3) and water molecules (approx. 8) were present prior to the application of Squeeze, however, a good point atom model could not be achieved. Additionally, in order for the charge of the 0.25-occupancy [Ni(H2O)6] cation to be balanced, a 0.5-occupancy hydroxide molecule must additionally be present. The application of Squeeze gave a good improvement in the data statistics and allowed for a full anisotropic refinement of the structure. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; 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 0.61969(2) 1.01750(2) 0.38028(2) 0.03642(15) Uani 1 1 d . . . Ni2 Ni 0.616377(19) 1.027327(19) 0.513916(17) 0.02703(13) Uani 1 1 d . . . Ni3 Ni 0.65983(2) 0.91107(2) 0.521836(18) 0.03050(14) Uani 1 1 d . . . Ni4 Ni 0.62372(2) 0.88085(2) 0.396609(19) 0.03507(15) Uani 1 1 d . . . Ni5 Ni 0.65388(3) 0.95097(3) 0.20348(2) 0.0567(2) Uani 1 1 d . . . Ni6 Ni 0.43688(3) 0.87375(7) 0.7500 0.0505(5) Uani 0.50 2 d SPD . . O1 O 0.61265(16) 1.00772(17) 0.31177(11) 0.0535(9) Uani 1 1 d . . . O2 O 0.5485(2) 0.9741(3) 0.25962(14) 0.0967(19) Uani 1 1 d . . . O3 O 0.58978(11) 1.00302(11) 0.44769(9) 0.0302(6) Uani 1 1 d . . . O4 O 0.55518(13) 0.96750(13) 0.63608(10) 0.0420(7) Uani 1 1 d . . . O5 O 0.61246(11) 1.01852(12) 0.58238(10) 0.0342(6) Uani 1 1 d . . . O6 O 0.60207(11) 1.09100(11) 0.51307(10) 0.0311(6) Uani 1 1 d . . . O7 O 0.64537(13) 1.18082(12) 0.50254(14) 0.0493(9) Uani 1 1 d . . . O8 O 0.66787(10) 0.99115(10) 0.51099(9) 0.0285(6) Uani 1 1 d . . . O9 O 0.76570(14) 0.85581(13) 0.50762(17) 0.0636(12) Uani 1 1 d . . . O10 O 0.68732(11) 0.85455(11) 0.51593(11) 0.0365(7) Uani 1 1 d . . . O11 O 0.67677(12) 0.92268(12) 0.58834(11) 0.0404(7) Uani 1 1 d . . . O12 O 0.63497(16) 0.90041(15) 0.65413(12) 0.0558(9) Uani 1 1 d . . . O13 O 0.61245(11) 0.88329(11) 0.46525(10) 0.0328(6) Uani 1 1 d . . . O14 O 0.5271(2) 0.8342(2) 0.28801(15) 0.105(2) Uani 1 1 d . . . O15 O 0.60097(15) 0.86763(14) 0.33020(11) 0.0502(8) Uani 1 1 d . . . O16 O 0.63114(14) 0.81177(13) 0.40290(11) 0.0442(8) Uani 1 1 d . . . O17 O 0.69556(15) 0.78946(13) 0.41130(13) 0.0508(8) Uani 1 1 d . . . O18 O 0.65168(11) 0.96443(11) 0.38944(10) 0.0353(6) Uani 1 1 d . . . O19 O 0.6881(2) 1.17996(18) 0.3627(2) 0.116(2) Uani 1 1 d . . . O20 O 0.62604(16) 1.09339(15) 0.37345(15) 0.0597(10) Uani 1 1 d . . . O21 O 0.6823(2) 0.8972(2) 0.20105(14) 0.0783(14) Uani 1 1 d . . . O22 O 0.63098(17) 1.00780(18) 0.20563(12) 0.0583(10) Uani 1 1 d . . . O23 O 0.57456(18) 0.88883(18) 0.20812(13) 0.0643(10) Uani 1 1 d . . . O24 O 0.66164(16) 0.95596(17) 0.27337(12) 0.0579(10) Uani 1 1 d . . . O25 O 0.73263(17) 1.0153(2) 0.19844(14) 0.0766(13) Uani 1 1 d . . . O26 O 0.6452(2) 0.9464(2) 0.13628(13) 0.0763(14) Uani 1 1 d . . . O27 O 0.4552(5) 0.9393(6) 0.7892(5) 0.040(3) Uani 0.25 1 d P A 1 O28 O 0.4081(6) 0.8329(6) 0.6887(5) 0.052(3) Uani 0.25 1 d P A 1 O29 O 0.4809(6) 0.8445(6) 0.7596(5) 0.049(3) Uani 0.25 1 d P A 1 O30 O 0.4564(5) 0.9154(5) 0.8107(4) 0.036(3) Uani 0.25 1 d PD A 2 O31 O 0.4377(7) 0.8101(5) 0.7154(5) 0.066(4) Uani 0.25 1 d PD A 2 O32 O 0.5224(4) 0.8964(5) 0.7616(4) 0.038(3) Uani 0.25 1 d PD A 2 N1 N 0.54053(15) 0.96862(15) 0.37351(12) 0.0373(8) Uani 1 1 d . . . N2 N 0.50786(14) 0.94861(14) 0.41031(12) 0.0341(7) Uani 1 1 d . . . N3 N 0.51100(13) 0.94865(13) 0.48536(11) 0.0292(7) Uani 1 1 d . . . H4 H 0.4761 0.9251 0.4862 0.035 Uiso 1 1 calc R . . N4 N 0.54112(13) 0.96814(13) 0.52276(11) 0.0281(7) Uani 1 1 d . . . N5 N 0.69073(13) 1.08972(13) 0.50243(12) 0.0285(7) Uani 1 1 d . . . N6 N 0.73172(13) 1.07869(13) 0.49725(12) 0.0296(7) Uani 1 1 d . . . H11 H 0.7651 1.1037 0.4906 0.036 Uiso 1 1 calc R . . N7 N 0.75497(13) 1.01252(12) 0.49928(13) 0.0328(8) Uani 1 1 d . . . H12 H 0.7891 1.0365 0.4939 0.039 Uiso 1 1 calc R . . N8 N 0.73692(13) 0.95851(13) 0.50417(13) 0.0329(8) Uani 1 1 d . . . N9 N 0.58625(13) 0.87303(13) 0.54688(12) 0.0316(7) Uani 1 1 d . . . N10 N 0.54256(13) 0.85051(13) 0.51800(11) 0.0299(7) Uani 1 1 d . . . N11 N 0.52381(14) 0.83919(15) 0.44340(13) 0.0377(8) Uani 1 1 d . . . H19 H 0.4887 0.8225 0.4487 0.045 Uiso 1 1 calc R . . N12 N 0.54416(15) 0.84702(14) 0.40204(13) 0.0381(8) Uani 1 1 d . . . N13 N 0.70388(15) 0.91271(15) 0.39388(13) 0.0392(8) Uani 1 1 d . . . N14 N 0.73373(15) 0.96702(15) 0.38902(15) 0.0451(10) Uani 1 1 d . . . H26 H 0.7693 0.9848 0.3870 0.054 Uiso 1 1 calc R . . N15 N 0.73264(16) 1.04547(16) 0.38394(16) 0.0493(10) Uani 1 1 d . . . H27 H 0.7683 1.0645 0.3832 0.059 Uiso 1 1 calc R . . N16 N 0.69935(16) 1.06668(15) 0.38151(14) 0.0415(9) Uani 1 1 d . . . C1 C 0.5624(3) 0.9808(3) 0.29955(17) 0.0596(15) Uani 1 1 d . . . C2 C 0.5203(2) 0.9572(2) 0.33454(16) 0.0450(11) Uani 1 1 d . . . C3 C 0.4621(2) 0.9241(3) 0.3231(2) 0.0660(16) Uani 1 1 d . . . H1 H 0.4527 0.8862 0.3193 0.079 Uiso 1 1 calc R . . H2 H 0.4550 0.9374 0.2953 0.079 Uiso 1 1 calc R . . H3 H 0.4402 0.9267 0.3471 0.079 Uiso 1 1 calc R . . C4 C 0.53850(15) 0.96805(16) 0.44591(13) 0.0287(8) Uani 1 1 d . . . C5 C 0.46704(17) 0.90863(18) 0.57266(15) 0.0383(10) Uani 1 1 d . . . H5 H 0.4529 0.8826 0.5480 0.046 Uiso 1 1 calc R . . H6 H 0.4438 0.9246 0.5770 0.046 Uiso 1 1 calc R . . H7 H 0.4674 0.8899 0.6000 0.046 Uiso 1 1 calc R . . C6 C 0.52297(15) 0.95207(16) 0.56215(14) 0.0298(8) Uani 1 1 d . . . C7 C 0.56614(17) 0.98119(17) 0.59661(14) 0.0340(9) Uani 1 1 d . . . C8 C 0.64387(16) 1.13705(16) 0.50565(15) 0.0346(9) Uani 1 1 d . . . C9 C 0.69714(16) 1.13733(16) 0.49932(15) 0.0318(8) Uani 1 1 d . . . C10 C 0.74880(18) 1.18814(17) 0.4915(2) 0.0464(12) Uani 1 1 d . . . H8 H 0.7654 1.2044 0.5202 0.056 Uiso 1 1 calc R . . H9 H 0.7418 1.2135 0.4746 0.056 Uiso 1 1 calc R . . H10 H 0.7734 1.1802 0.4746 0.056 Uiso 1 1 calc R . . C11 C 0.71643(15) 1.02577(15) 0.50327(14) 0.0293(8) Uani 1 1 d . . . C12 C 0.82854(19) 0.9705(2) 0.5019(2) 0.0632(17) Uani 1 1 d . . . H13 H 0.8417 1.0063 0.5153 0.076 Uiso 1 1 calc R . . H14 H 0.8398 0.9747 0.4706 0.076 Uiso 1 1 calc R . . H15 H 0.8438 0.9513 0.5181 0.076 Uiso 1 1 calc R . . C13 C 0.76883(17) 0.93909(17) 0.50462(18) 0.0406(10) Uani 1 1 d . . . C14 C 0.73794(17) 0.87813(17) 0.51016(18) 0.0413(11) Uani 1 1 d . . . C15 C 0.6347(2) 0.89953(18) 0.61268(16) 0.0400(10) Uani 1 1 d . . . C16 C 0.58083(18) 0.86885(17) 0.58930(15) 0.0368(9) Uani 1 1 d . . . C17 C 0.5287(2) 0.8379(2) 0.61446(18) 0.0486(12) Uani 1 1 d . . . H16 H 0.5356 0.8260 0.6431 0.058 Uiso 1 1 calc R . . H17 H 0.5032 0.8062 0.5971 0.058 Uiso 1 1 calc R . . H18 H 0.5131 0.8612 0.6197 0.058 Uiso 1 1 calc R . . C18 C 0.56179(16) 0.85914(15) 0.47712(15) 0.0332(9) Uani 1 1 d . . . C19 C 0.4546(3) 0.8011(3) 0.3653(2) 0.087(2) Uani 1 1 d . . . H20 H 0.4411 0.7620 0.3667 0.104 Uiso 1 1 calc R . . H21 H 0.4422 0.8095 0.3375 0.104 Uiso 1 1 calc R . . H22 H 0.4407 0.8119 0.3908 0.104 Uiso 1 1 calc R . . C20 C 0.5149(2) 0.8310(2) 0.36644(19) 0.0567(14) Uani 1 1 d . . . C21 C 0.5507(3) 0.8451(2) 0.32528(19) 0.0631(16) Uani 1 1 d . . . C22 C 0.6801(2) 0.82263(18) 0.40426(16) 0.0417(10) Uani 1 1 d . . . C23 C 0.7234(2) 0.88093(19) 0.39717(17) 0.0446(11) Uani 1 1 d . . . C24 C 0.7818(2) 0.8973(2) 0.3944(3) 0.0660(17) Uani 1 1 d . . . H23 H 0.7887 0.8730 0.4129 0.079 Uiso 1 1 calc R . . H24 H 0.8040 0.9346 0.4051 0.079 Uiso 1 1 calc R . . H25 H 0.7913 0.8949 0.3634 0.079 Uiso 1 1 calc R . . C25 C 0.70359(17) 0.99134(18) 0.38757(16) 0.0394(10) Uani 1 1 d . . . C26 C 0.7770(2) 1.1582(2) 0.3710(3) 0.0737(19) Uani 1 1 d . . . H28 H 0.7965 1.1405 0.3595 0.088 Uiso 1 1 calc R . . H29 H 0.7915 1.1739 0.4003 0.088 Uiso 1 1 calc R . . H30 H 0.7817 1.1869 0.3504 0.088 Uiso 1 1 calc R . . C27 C 0.7182(2) 1.1174(2) 0.3751(2) 0.0544(13) Uani 1 1 d . . . C28 C 0.6746(2) 1.1313(2) 0.3706(2) 0.0626(16) 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 0.0324(3) 0.0330(3) 0.0446(3) 0.0055(2) 0.0057(2) 0.0169(2) Ni2 0.0201(2) 0.0213(2) 0.0390(3) -0.00100(19) -0.00204(19) 0.00975(19) Ni3 0.0224(2) 0.0206(2) 0.0466(3) -0.0010(2) -0.0017(2) 0.0094(2) Ni4 0.0321(3) 0.0272(3) 0.0436(3) -0.0006(2) 0.0015(2) 0.0131(2) Ni5 0.0649(5) 0.0782(5) 0.0448(4) 0.0116(3) 0.0034(3) 0.0491(4) Ni6 0.0716(10) 0.0285(8) 0.0371(9) 0.000 0.0072(8) 0.0142(4) O1 0.057(2) 0.072(3) 0.0418(18) 0.0127(17) 0.0107(16) 0.040(2) O2 0.087(3) 0.174(6) 0.037(2) 0.016(3) 0.004(2) 0.072(4) O3 0.0230(13) 0.0275(14) 0.0387(15) -0.0001(11) -0.0005(11) 0.0115(11) O4 0.0378(17) 0.0426(18) 0.0398(17) 0.0007(13) -0.0035(13) 0.0157(14) O5 0.0252(14) 0.0363(16) 0.0386(15) -0.0034(12) -0.0043(12) 0.0134(12) O6 0.0234(13) 0.0256(14) 0.0457(16) -0.0026(12) -0.0026(11) 0.0133(12) O7 0.0338(17) 0.0253(15) 0.093(3) 0.0019(16) 0.0032(17) 0.0177(13) O8 0.0205(13) 0.0198(12) 0.0462(16) 0.0024(11) -0.0001(11) 0.0108(11) O9 0.0319(17) 0.0217(16) 0.139(4) -0.0027(19) -0.005(2) 0.0146(14) O10 0.0277(15) 0.0213(13) 0.0588(19) 0.0034(13) -0.0024(13) 0.0111(12) O11 0.0347(16) 0.0335(16) 0.0461(17) -0.0016(13) -0.0045(13) 0.0119(13) O12 0.058(2) 0.052(2) 0.050(2) -0.0048(17) -0.0048(17) 0.0215(18) O13 0.0240(13) 0.0239(14) 0.0470(17) 0.0020(12) 0.0015(12) 0.0094(11) O14 0.085(3) 0.108(4) 0.052(3) 0.017(3) -0.022(2) -0.005(3) O15 0.052(2) 0.0410(19) 0.0461(19) 0.0012(15) -0.0031(16) 0.0149(17) O16 0.0484(19) 0.0320(16) 0.0532(19) 0.0012(14) 0.0064(15) 0.0209(15) O17 0.055(2) 0.0351(18) 0.065(2) -0.0015(15) -0.0051(17) 0.0246(16) O18 0.0271(14) 0.0282(14) 0.0477(17) 0.0025(12) 0.0035(12) 0.0116(12) O19 0.103(4) 0.045(3) 0.216(7) 0.049(3) 0.072(4) 0.049(3) O20 0.056(2) 0.043(2) 0.090(3) 0.0243(19) 0.023(2) 0.0323(19) O21 0.109(4) 0.105(4) 0.061(3) 0.016(2) 0.007(2) 0.084(3) O22 0.067(2) 0.078(3) 0.0429(19) 0.0044(18) -0.0004(17) 0.047(2) O23 0.070(3) 0.074(3) 0.051(2) -0.0043(19) -0.0020(19) 0.037(2) O24 0.062(2) 0.075(3) 0.0433(19) 0.0105(18) -0.0004(17) 0.039(2) O25 0.055(2) 0.100(4) 0.054(2) 0.017(2) 0.0061(19) 0.024(2) O26 0.113(4) 0.125(4) 0.041(2) 0.012(2) 0.005(2) 0.097(4) O27 0.035(7) 0.039(7) 0.044(7) -0.025(6) -0.002(5) 0.017(6) O28 0.060(9) 0.051(8) 0.055(8) -0.013(7) -0.006(7) 0.035(7) O29 0.055(8) 0.046(8) 0.055(8) -0.002(6) -0.008(7) 0.034(7) O30 0.037(7) 0.026(6) 0.055(8) 0.001(6) 0.006(6) 0.024(5) O31 0.075(11) 0.040(8) 0.077(11) -0.001(7) 0.021(9) 0.024(8) O32 0.033(6) 0.033(6) 0.046(7) -0.010(5) 0.011(5) 0.016(5) N1 0.038(2) 0.040(2) 0.0373(19) 0.0022(15) -0.0030(15) 0.0226(17) N2 0.0290(17) 0.0352(18) 0.0370(18) -0.0024(15) -0.0010(14) 0.0152(15) N3 0.0200(15) 0.0261(16) 0.0378(18) -0.0008(13) -0.0019(13) 0.0087(13) N4 0.0210(15) 0.0248(16) 0.0382(18) 0.0006(13) -0.0010(13) 0.0112(13) N5 0.0214(15) 0.0215(15) 0.0434(19) -0.0030(13) -0.0034(13) 0.0112(13) N6 0.0197(15) 0.0190(15) 0.049(2) 0.0002(14) 0.0006(14) 0.0085(13) N7 0.0176(15) 0.0143(14) 0.063(2) -0.0012(14) -0.0012(15) 0.0056(12) N8 0.0264(17) 0.0182(15) 0.053(2) -0.0041(14) -0.0025(15) 0.0105(13) N9 0.0279(17) 0.0196(15) 0.048(2) 0.0002(14) -0.0005(14) 0.0122(14) N10 0.0226(16) 0.0265(16) 0.0390(18) 0.0022(14) 0.0014(13) 0.0112(14) N11 0.0248(17) 0.0333(19) 0.047(2) 0.0032(16) -0.0001(15) 0.0086(15) N12 0.0346(19) 0.0280(18) 0.046(2) 0.0001(15) -0.0054(16) 0.0117(15) N13 0.038(2) 0.0337(19) 0.050(2) 0.0044(16) 0.0027(16) 0.0208(17) N14 0.0274(18) 0.0285(19) 0.074(3) 0.0049(18) 0.0070(18) 0.0097(15) N15 0.0294(19) 0.031(2) 0.081(3) 0.0007(19) 0.0067(19) 0.0103(16) N16 0.036(2) 0.0286(18) 0.061(2) 0.0087(17) 0.0110(18) 0.0168(16) C1 0.064(4) 0.094(5) 0.037(3) 0.002(3) -0.005(2) 0.052(4) C2 0.049(3) 0.059(3) 0.038(2) 0.003(2) -0.004(2) 0.036(3) C3 0.056(3) 0.088(5) 0.061(3) -0.019(3) -0.023(3) 0.041(3) C4 0.0240(18) 0.0276(19) 0.038(2) 0.0002(15) -0.0035(15) 0.0157(16) C5 0.032(2) 0.041(2) 0.042(2) 0.0096(19) 0.0019(18) 0.0181(19) C6 0.0230(18) 0.0247(18) 0.045(2) -0.0026(16) -0.0051(16) 0.0142(16) C7 0.036(2) 0.034(2) 0.038(2) -0.0008(17) -0.0019(17) 0.0218(19) C8 0.0249(19) 0.026(2) 0.052(2) -0.0024(18) -0.0042(17) 0.0126(17) C9 0.0242(19) 0.0233(19) 0.048(2) -0.0051(17) -0.0054(17) 0.0119(16) C10 0.029(2) 0.023(2) 0.086(4) 0.002(2) 0.001(2) 0.0125(18) C11 0.0218(18) 0.0207(18) 0.043(2) -0.0047(15) -0.0040(16) 0.0090(15) C12 0.030(2) 0.029(2) 0.134(6) 0.000(3) 0.003(3) 0.017(2) C13 0.023(2) 0.023(2) 0.074(3) -0.005(2) -0.007(2) 0.0101(17) C14 0.028(2) 0.024(2) 0.073(3) 0.000(2) -0.006(2) 0.0140(18) C15 0.047(3) 0.028(2) 0.048(3) -0.0062(18) -0.006(2) 0.020(2) C16 0.037(2) 0.030(2) 0.048(3) 0.0048(18) 0.0056(19) 0.0200(19) C17 0.042(3) 0.046(3) 0.063(3) 0.017(2) 0.014(2) 0.026(2) C18 0.030(2) 0.0182(17) 0.054(3) -0.0025(17) -0.0049(18) 0.0142(16) C19 0.049(3) 0.096(5) 0.070(4) 0.023(4) -0.017(3) 0.002(3) C20 0.048(3) 0.045(3) 0.060(3) 0.010(2) -0.011(2) 0.010(2) C21 0.074(4) 0.043(3) 0.050(3) 0.009(2) -0.010(3) 0.013(3) C22 0.052(3) 0.031(2) 0.045(2) 0.0010(18) 0.005(2) 0.023(2) C23 0.042(3) 0.038(2) 0.059(3) 0.008(2) 0.012(2) 0.025(2) C24 0.047(3) 0.051(3) 0.108(5) 0.011(3) 0.008(3) 0.031(3) C25 0.028(2) 0.034(2) 0.053(3) -0.0022(19) 0.0026(18) 0.0134(18) C26 0.053(3) 0.025(2) 0.129(6) 0.006(3) 0.014(4) 0.009(2) C27 0.054(3) 0.037(3) 0.069(4) 0.007(2) 0.014(3) 0.021(2) C28 0.059(3) 0.043(3) 0.093(4) 0.018(3) 0.031(3) 0.031(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.981(4) . ? Ni1 N16 1.984(4) . ? Ni1 O1 2.071(4) . ? Ni1 O20 2.088(3) . ? Ni1 O18 2.138(3) . ? Ni1 O3 2.154(3) . ? Ni2 N4 1.974(3) . ? Ni2 N5 2.000(3) . ? Ni2 O6 2.049(3) . ? Ni2 O5 2.066(3) . ? Ni2 O3 2.117(3) . ? Ni2 O8 2.176(3) . ? Ni3 N9 1.965(3) . ? Ni3 N8 1.991(3) . ? Ni3 O11 2.041(3) . ? Ni3 O13 2.065(3) . ? Ni3 O10 2.121(3) . ? Ni3 O8 2.200(3) . ? Ni4 N12 1.977(4) . ? Ni4 N13 1.993(4) . ? Ni4 O15 2.071(3) . ? Ni4 O16 2.090(3) . ? Ni4 O13 2.092(3) . ? Ni4 O18 2.111(3) . ? Ni5 O22 2.027(4) . ? Ni5 O26 2.028(4) . ? Ni5 O21 2.062(4) . ? Ni5 O23 2.064(5) . ? Ni5 O25 2.074(5) . ? Ni5 O24 2.107(4) . ? Ni6 O29 1.843(13) . ? Ni6 O29 1.843(13) 11_557 ? Ni6 O27 2.042(11) . ? Ni6 O27 2.042(11) 11_557 ? Ni6 O30 2.091(11) 11_557 ? Ni6 O30 2.091(11) . ? Ni6 O31 2.099(12) . ? Ni6 O31 2.099(12) 11_557 ? Ni6 O28 2.112(14) . ? Ni6 O28 2.112(14) 11_557 ? Ni6 O32 2.214(10) 11_557 ? Ni6 O32 2.214(10) . ? O1 C1 1.293(7) . ? O2 C1 1.247(7) . ? O3 C4 1.294(5) . ? O4 C7 1.238(5) . ? O5 C7 1.285(5) . ? O6 C8 1.276(5) . ? O7 C8 1.230(5) . ? O8 C11 1.255(5) . ? O9 C14 1.241(5) . ? O10 C14 1.262(5) . ? O11 C15 1.271(6) . ? O12 C15 1.244(6) . ? O13 C18 1.300(5) . ? O14 C21 1.261(7) . ? O15 C21 1.252(7) . ? O16 C22 1.269(6) . ? O17 C22 1.245(6) . ? O18 C25 1.282(5) . ? O19 C28 1.261(7) . ? O20 C28 1.263(7) . ? N1 C2 1.272(6) . ? N1 N2 1.371(5) . ? N2 C4 1.314(5) . ? N3 N4 1.352(5) . ? N3 C4 1.374(5) . ? N3 H4 0.8800 . ? N4 C6 1.280(5) . ? N5 C9 1.279(5) . ? N5 N6 1.362(4) . ? N6 C11 1.356(5) . ? N6 H11 0.8800 . ? N7 C11 1.333(5) . ? N7 N8 1.365(4) . ? N7 H12 0.8800 . ? N8 C13 1.279(5) . ? N9 C16 1.281(6) . ? N9 N10 1.383(5) . ? N10 C18 1.316(6) . ? N11 N12 1.341(5) . ? N11 C18 1.379(5) . ? N11 H19 0.8800 . ? N12 C20 1.291(6) . ? N13 C23 1.281(6) . ? N13 N14 1.350(5) . ? N14 C25 1.347(6) . ? N14 H26 0.8800 . ? N15 C25 1.341(6) . ? N15 N16 1.358(5) . ? N15 H27 0.8800 . ? N16 C27 1.279(6) . ? C1 C2 1.480(8) . ? C2 C3 1.480(7) . ? C3 H1 0.9800 . ? C3 H2 0.9800 . ? C3 H3 0.9800 . ? C5 C6 1.483(6) . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C5 H7 0.9800 . ? C6 C7 1.500(6) . ? C8 C9 1.526(6) . ? C9 C10 1.479(6) . ? C10 H8 0.9800 . ? C10 H9 0.9800 . ? C10 H10 0.9800 . ? C12 C13 1.476(6) . ? C12 H13 0.9800 . ? C12 H14 0.9800 . ? C12 H15 0.9800 . ? C13 C14 1.513(6) . ? C15 C16 1.506(6) . ? C16 C17 1.499(6) . ? C17 H16 0.9800 . ? C17 H17 0.9800 . ? C17 H18 0.9800 . ? C19 C20 1.489(8) . ? C19 H20 0.9800 . ? C19 H21 0.9800 . ? C19 H22 0.9800 . ? C20 C21 1.523(9) . ? C22 C23 1.509(7) . ? C23 C24 1.490(7) . ? C24 H23 0.9800 . ? C24 H24 0.9800 . ? C24 H25 0.9800 . ? C26 C27 1.491(8) . ? C26 H28 0.9800 . ? C26 H29 0.9800 . ? C26 H30 0.9800 . ? C27 C28 1.489(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 N1 Ni1 N16 175.19(16) . . ? N1 Ni1 O1 78.71(15) . . ? N16 Ni1 O1 96.49(17) . . ? N1 Ni1 O20 101.34(15) . . ? N16 Ni1 O20 78.12(15) . . ? O1 Ni1 O20 89.67(17) . . ? N1 Ni1 O18 104.72(13) . . ? N16 Ni1 O18 75.84(13) . . ? O1 Ni1 O18 94.55(13) . . ? O20 Ni1 O18 153.93(14) . . ? N1 Ni1 O3 76.07(13) . . ? N16 Ni1 O3 108.73(14) . . ? O1 Ni1 O3 154.75(14) . . ? O20 Ni1 O3 96.42(14) . . ? O18 Ni1 O3 90.66(11) . . ? N4 Ni2 N5 176.25(14) . . ? N4 Ni2 O6 98.40(12) . . ? N5 Ni2 O6 78.59(12) . . ? N4 Ni2 O5 78.05(13) . . ? N5 Ni2 O5 104.37(13) . . ? O6 Ni2 O5 95.58(12) . . ? N4 Ni2 O3 77.79(12) . . ? N5 Ni2 O3 100.12(13) . . ? O6 Ni2 O3 94.65(11) . . ? O5 Ni2 O3 154.88(11) . . ? N4 Ni2 O8 107.60(12) . . ? N5 Ni2 O8 75.45(11) . . ? O6 Ni2 O8 153.99(11) . . ? O5 Ni2 O8 89.48(11) . . ? O3 Ni2 O8 91.31(10) . . ? N9 Ni3 N8 170.68(15) . . ? N9 Ni3 O11 79.39(14) . . ? N8 Ni3 O11 93.40(14) . . ? N9 Ni3 O13 77.90(13) . . ? N8 Ni3 O13 109.21(14) . . ? O11 Ni3 O13 157.29(12) . . ? N9 Ni3 O10 108.08(12) . . ? N8 Ni3 O10 78.02(12) . . ? O11 Ni3 O10 93.31(13) . . ? O13 Ni3 O10 93.38(12) . . ? N9 Ni3 O8 99.07(12) . . ? N8 Ni3 O8 75.47(12) . . ? O11 Ni3 O8 94.76(12) . . ? O13 Ni3 O8 89.14(11) . . ? O10 Ni3 O8 152.67(11) . . ? N12 Ni4 N13 177.01(16) . . ? N12 Ni4 O15 79.19(15) . . ? N13 Ni4 O15 103.08(16) . . ? N12 Ni4 O16 99.47(14) . . ? N13 Ni4 O16 78.48(14) . . ? O15 Ni4 O16 94.90(14) . . ? N12 Ni4 O13 77.13(13) . . ? N13 Ni4 O13 100.68(14) . . ? O15 Ni4 O13 156.15(13) . . ? O16 Ni4 O13 91.82(12) . . ? N12 Ni4 O18 104.62(13) . . ? N13 Ni4 O18 77.40(13) . . ? O15 Ni4 O18 90.82(13) . . ? O16 Ni4 O18 155.88(13) . . ? O13 Ni4 O18 92.33(11) . . ? O22 Ni5 O26 90.29(16) . . ? O22 Ni5 O21 176.3(2) . . ? O26 Ni5 O21 89.87(17) . . ? O22 Ni5 O23 91.80(17) . . ? O26 Ni5 O23 88.09(19) . . ? O21 Ni5 O23 91.9(2) . . ? O22 Ni5 O25 86.3(2) . . ? O26 Ni5 O25 91.5(2) . . ? O21 Ni5 O25 90.0(2) . . ? O23 Ni5 O25 178.0(2) . . ? O22 Ni5 O24 88.81(15) . . ? O26 Ni5 O24 178.94(16) . . ? O21 Ni5 O24 91.05(16) . . ? O23 Ni5 O24 91.36(16) . . ? O25 Ni5 O24 88.99(16) . . ? O29 Ni6 O29 133.8(9) . 11_557 ? O29 Ni6 O27 113.7(6) . . ? O29 Ni6 O27 102.6(6) 11_557 . ? O29 Ni6 O27 102.6(6) . 11_557 ? O29 Ni6 O27 113.7(6) 11_557 11_557 ? O27 Ni6 O27 75.3(9) . 11_557 ? O29 Ni6 O30 108.3(6) . 11_557 ? O29 Ni6 O30 94.1(5) 11_557 11_557 ? O27 Ni6 O30 96.7(7) . 11_557 ? O27 Ni6 O30 26.5(5) 11_557 11_557 ? O29 Ni6 O30 94.1(5) . . ? O29 Ni6 O30 108.3(6) 11_557 . ? O27 Ni6 O30 26.5(5) . . ? O27 Ni6 O30 96.7(7) 11_557 . ? O30 Ni6 O30 121.2(7) 11_557 . ? O29 Ni6 O31 52.0(7) . . ? O29 Ni6 O31 91.7(7) 11_557 . ? O27 Ni6 O31 165.2(6) . . ? O27 Ni6 O31 102.5(6) 11_557 . ? O30 Ni6 O31 85.9(6) 11_557 . ? O30 Ni6 O31 143.7(6) . . ? O29 Ni6 O31 91.7(7) . 11_557 ? O29 Ni6 O31 52.0(7) 11_557 11_557 ? O27 Ni6 O31 102.5(6) . 11_557 ? O27 Ni6 O31 165.2(6) 11_557 11_557 ? O30 Ni6 O31 143.7(6) 11_557 11_557 ? O30 Ni6 O31 85.9(6) . 11_557 ? O31 Ni6 O31 83.2(9) . 11_557 ? O29 Ni6 O28 93.0(6) . . ? O29 Ni6 O28 64.8(6) 11_557 . ? O27 Ni6 O28 149.0(6) . . ? O27 Ni6 O28 84.1(6) 11_557 . ? O30 Ni6 O28 58.5(6) 11_557 . ? O30 Ni6 O28 172.5(5) . . ? O31 Ni6 O28 42.4(6) . . ? O31 Ni6 O28 91.4(7) 11_557 . ? O29 Ni6 O28 64.8(6) . 11_557 ? O29 Ni6 O28 93.0(6) 11_557 11_557 ? O27 Ni6 O28 84.1(6) . 11_557 ? O27 Ni6 O28 149.0(6) 11_557 11_557 ? O30 Ni6 O28 172.5(5) 11_557 11_557 ? O30 Ni6 O28 58.5(6) . 11_557 ? O31 Ni6 O28 91.4(6) . 11_557 ? O31 Ni6 O28 42.4(6) 11_557 11_557 ? O28 Ni6 O28 123.0(8) . 11_557 ? O29 Ni6 O32 171.5(6) . 11_557 ? O29 Ni6 O32 37.7(5) 11_557 11_557 ? O27 Ni6 O32 72.5(5) . 11_557 ? O27 Ni6 O32 84.3(5) 11_557 11_557 ? O30 Ni6 O32 75.8(4) 11_557 11_557 ? O30 Ni6 O32 89.8(5) . 11_557 ? O31 Ni6 O32 122.2(6) . 11_557 ? O31 Ni6 O32 81.1(6) 11_557 11_557 ? O28 Ni6 O32 82.8(5) . 11_557 ? O28 Ni6 O32 111.5(5) 11_557 11_557 ? O29 Ni6 O32 37.7(5) . . ? O29 Ni6 O32 171.5(6) 11_557 . ? O27 Ni6 O32 84.3(5) . . ? O27 Ni6 O32 72.5(5) 11_557 . ? O30 Ni6 O32 89.8(5) 11_557 . ? O30 Ni6 O32 75.8(4) . . ? O31 Ni6 O32 81.0(5) . . ? O31 Ni6 O32 122.2(6) 11_557 . ? O28 Ni6 O32 111.5(5) . . ? O28 Ni6 O32 82.8(5) 11_557 . ? O32 Ni6 O32 150.8(6) 11_557 . ? C1 O1 Ni1 111.4(3) . . ? C4 O3 Ni2 111.9(2) . . ? C4 O3 Ni1 107.2(2) . . ? Ni2 O3 Ni1 140.98(14) . . ? C7 O5 Ni2 113.7(3) . . ? C8 O6 Ni2 114.6(2) . . ? C11 O8 Ni2 112.0(2) . . ? C11 O8 Ni3 110.2(2) . . ? Ni2 O8 Ni3 137.73(13) . . ? C14 O10 Ni3 111.4(3) . . ? C15 O11 Ni3 113.1(3) . . ? C18 O13 Ni3 108.5(3) . . ? C18 O13 Ni4 113.6(3) . . ? Ni3 O13 Ni4 137.81(14) . . ? C21 O15 Ni4 112.4(4) . . ? C22 O16 Ni4 112.9(3) . . ? C25 O18 Ni4 110.5(3) . . ? C25 O18 Ni1 110.1(3) . . ? Ni4 O18 Ni1 139.22(14) . . ? C28 O20 Ni1 112.6(3) . . ? C2 N1 N2 120.5(4) . . ? C2 N1 Ni1 119.0(3) . . ? N2 N1 Ni1 120.5(3) . . ? C4 N2 N1 108.0(3) . . ? N4 N3 C4 115.7(3) . . ? N4 N3 H4 122.2 . . ? C4 N3 H4 122.2 . . ? C6 N4 N3 124.1(3) . . ? C6 N4 Ni2 120.1(3) . . ? N3 N4 Ni2 115.7(2) . . ? C9 N5 N6 123.5(3) . . ? C9 N5 Ni2 118.8(3) . . ? N6 N5 Ni2 117.7(2) . . ? C11 N6 N5 113.9(3) . . ? C11 N6 H11 123.0 . . ? N5 N6 H11 123.0 . . ? C11 N7 N8 114.2(3) . . ? C11 N7 H12 122.9 . . ? N8 N7 H12 122.9 . . ? C13 N8 N7 122.7(3) . . ? C13 N8 Ni3 119.0(3) . . ? N7 N8 Ni3 117.4(2) . . ? C16 N9 N10 122.7(4) . . ? C16 N9 Ni3 118.5(3) . . ? N10 N9 Ni3 118.7(3) . . ? C18 N10 N9 107.7(3) . . ? N12 N11 C18 115.2(4) . . ? N12 N11 H19 122.4 . . ? C18 N11 H19 122.4 . . ? C20 N12 N11 123.9(4) . . ? C20 N12 Ni4 119.0(4) . . ? N11 N12 Ni4 116.9(3) . . ? C23 N13 N14 124.8(4) . . ? C23 N13 Ni4 118.6(3) . . ? N14 N13 Ni4 116.6(3) . . ? C25 N14 N13 113.2(4) . . ? C25 N14 H26 123.4 . . ? N13 N14 H26 123.4 . . ? C25 N15 N16 110.5(4) . . ? C25 N15 H27 124.8 . . ? N16 N15 H27 124.8 . . ? C27 N16 N15 121.2(4) . . ? C27 N16 Ni1 118.8(4) . . ? N15 N16 Ni1 119.6(3) . . ? O2 C1 O1 122.5(6) . . ? O2 C1 C2 119.2(6) . . ? O1 C1 C2 118.3(4) . . ? N1 C2 C3 126.6(5) . . ? N1 C2 C1 112.0(5) . . ? C3 C2 C1 121.4(5) . . ? C2 C3 H1 109.5 . . ? C2 C3 H2 109.5 . . ? H1 C3 H2 109.5 . . ? C2 C3 H3 109.5 . . ? H1 C3 H3 109.5 . . ? H2 C3 H3 109.5 . . ? O3 C4 N2 127.9(4) . . ? O3 C4 N3 118.1(3) . . ? N2 C4 N3 114.0(3) . . ? C6 C5 H5 109.5 . . ? C6 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C6 C5 H7 109.5 . . ? H5 C5 H7 109.5 . . ? H6 C5 H7 109.5 . . ? N4 C6 C5 124.6(4) . . ? N4 C6 C7 111.5(4) . . ? C5 C6 C7 123.8(4) . . ? O4 C7 O5 124.9(4) . . ? O4 C7 C6 118.5(4) . . ? O5 C7 C6 116.6(4) . . ? O7 C8 O6 126.7(4) . . ? O7 C8 C9 117.1(4) . . ? O6 C8 C9 116.2(3) . . ? N5 C9 C10 126.5(4) . . ? N5 C9 C8 111.8(3) . . ? C10 C9 C8 121.7(3) . . ? C9 C10 H8 109.5 . . ? C9 C10 H9 109.5 . . ? H8 C10 H9 109.5 . . ? C9 C10 H10 109.5 . . ? H8 C10 H10 109.5 . . ? H9 C10 H10 109.5 . . ? O8 C11 N7 122.3(3) . . ? O8 C11 N6 120.9(3) . . ? N7 C11 N6 116.8(3) . . ? C13 C12 H13 109.5 . . ? C13 C12 H14 109.5 . . ? H13 C12 H14 109.5 . . ? C13 C12 H15 109.5 . . ? H13 C12 H15 109.5 . . ? H14 C12 H15 109.5 . . ? N8 C13 C12 126.2(4) . . ? N8 C13 C14 111.5(4) . . ? C12 C13 C14 122.3(4) . . ? O9 C14 O10 126.0(4) . . ? O9 C14 C13 115.3(4) . . ? O10 C14 C13 118.7(4) . . ? O12 C15 O11 124.7(5) . . ? O12 C15 C16 118.2(4) . . ? O11 C15 C16 117.1(4) . . ? N9 C16 C17 126.4(4) . . ? N9 C16 C15 111.6(4) . . ? C17 C16 C15 122.0(4) . . ? C16 C17 H16 109.5 . . ? C16 C17 H17 109.5 . . ? H16 C17 H17 109.5 . . ? C16 C17 H18 109.5 . . ? H16 C17 H18 109.5 . . ? H17 C17 H18 109.5 . . ? O13 C18 N10 127.1(4) . . ? O13 C18 N11 116.9(4) . . ? N10 C18 N11 116.1(4) . . ? C20 C19 H20 109.5 . . ? C20 C19 H21 109.5 . . ? H20 C19 H21 109.5 . . ? C20 C19 H22 109.5 . . ? H20 C19 H22 109.5 . . ? H21 C19 H22 109.5 . . ? N12 C20 C19 125.4(6) . . ? N12 C20 C21 110.4(5) . . ? C19 C20 C21 124.1(5) . . ? O15 C21 O14 124.3(6) . . ? O15 C21 C20 118.9(5) . . ? O14 C21 C20 116.8(6) . . ? O17 C22 O16 125.7(4) . . ? O17 C22 C23 117.0(4) . . ? O16 C22 C23 117.2(4) . . ? N13 C23 C24 125.9(5) . . ? N13 C23 C22 112.6(4) . . ? C24 C23 C22 121.5(4) . . ? C23 C24 H23 109.5 . . ? C23 C24 H24 109.5 . . ? H23 C24 H24 109.5 . . ? C23 C24 H25 109.5 . . ? H23 C24 H25 109.5 . . ? H24 C24 H25 109.5 . . ? O18 C25 N15 123.7(4) . . ? O18 C25 N14 122.2(4) . . ? N15 C25 N14 114.1(4) . . ? C27 C26 H28 109.5 . . ? C27 C26 H29 109.5 . . ? H28 C26 H29 109.5 . . ? C27 C26 H30 109.5 . . ? H28 C26 H30 109.5 . . ? H29 C26 H30 109.5 . . ? N16 C27 C28 112.3(5) . . ? N16 C27 C26 124.5(5) . . ? C28 C27 C26 123.1(5) . . ? O19 C28 O20 123.7(6) . . ? O19 C28 C27 118.3(6) . . ? O20 C28 C27 117.9(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.257 _refine_diff_density_min -1.250 _refine_diff_density_rms 0.097