# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_complex1 _database_code_depnum_ccdc_archive 'CCDC 924183' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H76 Ni6 O26, 4(C H4 O)' _chemical_formula_sum 'C74 H92 Ni6 O30' _chemical_formula_weight 1813.74 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.578(6) _cell_length_b 27.265(19) _cell_length_c 15.964(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.540(13) _cell_angle_gamma 90.00 _cell_volume 3722(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 765 _cell_measurement_theta_min 2.614 _cell_measurement_theta_max 22.372 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.575 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5716 _exptl_absorpt_correction_T_max 0.8584 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18414 _diffrn_reflns_av_R_equivalents 0.1019 _diffrn_reflns_av_unetI/netI 0.1561 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.12 _reflns_number_total 6638 _reflns_number_gt 3355 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0969P)^2^+3.5707P] 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 6638 _refine_ls_number_parameters 507 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1609 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.2265 _refine_ls_wR_factor_gt 0.1694 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 -0.03697(14) 0.04511(4) 0.85577(7) 0.0305(3) Uani 1 1 d . . . Ni2 Ni 0.11570(13) 0.03991(4) 1.03458(7) 0.0275(3) Uani 1 1 d . . . Ni3 Ni 0.15887(15) 0.13177(4) 0.92653(7) 0.0316(3) Uani 1 1 d . . . O9 O 0.1817(7) 0.0579(2) 0.9205(3) 0.0281(14) Uani 1 1 d . . . O10 O -0.1048(7) 0.0347(2) 0.9729(3) 0.0283(14) Uani 1 1 d . . . O3 O -0.0560(7) 0.1185(2) 0.8649(4) 0.0322(15) Uani 1 1 d . . . O7 O -0.0244(7) -0.0290(2) 0.8551(3) 0.0299(14) Uani 1 1 d . . . O8 O 0.1017(7) 0.1123(2) 1.0500(3) 0.0302(15) Uani 1 1 d . . . O4 O -0.2621(7) 0.0451(2) 0.8080(4) 0.0356(16) Uani 1 1 d . . . O6 O 0.0520(7) 0.0487(2) 0.7435(4) 0.0348(15) Uani 1 1 d . . . O11 O 0.2363(8) 0.1320(2) 0.8040(4) 0.0391(16) Uani 1 1 d . . . O2 O 0.1063(8) 0.2032(2) 0.9193(4) 0.0363(16) Uani 1 1 d . . . O1 O 0.2532(8) 0.2825(2) 0.9404(4) 0.0475(18) Uani 1 1 d . . . H1 H 0.2361 0.2527 0.9486 0.071 Uiso 1 1 calc R . . C10 C -0.2553(11) 0.1266(3) 0.7511(6) 0.034(2) Uani 1 1 d . . . C30 C 0.0483(11) 0.1357(3) 1.1163(6) 0.032(2) Uani 1 1 d . . . O5 O -0.0167(9) 0.0938(2) 0.5986(4) 0.0488(19) Uani 1 1 d . . . H5 H -0.0232 0.0888 0.6502 0.073 Uiso 1 1 calc R . . C29 C 0.0492(12) 0.1871(4) 1.1130(6) 0.043(3) Uani 1 1 d . . . H17 H 0.0859 0.2026 1.0650 0.051 Uiso 1 1 calc R . . C6 C -0.0110(12) 0.2784(3) 0.8771(6) 0.038(2) Uani 1 1 d . . . C23 C 0.0689(11) -0.0387(3) 0.7241(5) 0.036(2) Uani 1 1 d . . . H29 H 0.1004 -0.0620 0.6846 0.043 Uiso 1 1 calc R . . C21 C 0.1373(12) 0.0201(4) 0.6145(6) 0.039(2) Uani 1 1 d . . . C8 C -0.1278(12) 0.1984(3) 0.8271(6) 0.034(2) Uani 1 1 d . . . H8 H -0.2055 0.2178 0.7973 0.041 Uiso 1 1 calc R . . C25 C -0.0042(10) 0.1124(3) 1.1872(5) 0.029(2) Uani 1 1 d . . . C7 C -0.0136(12) 0.2234(3) 0.8755(6) 0.035(2) Uani 1 1 d . . . C11 C -0.3102(12) 0.1572(4) 0.6840(6) 0.038(2) Uani 1 1 d . . . H11 H -0.2671 0.1892 0.6802 0.046 Uiso 1 1 calc R . . C15 C -0.3143(11) 0.0775(3) 0.7542(6) 0.034(2) Uani 1 1 d . . . C22 C 0.0821(11) 0.0095(4) 0.6996(6) 0.035(2) Uani 1 1 d . . . C9 C -0.1421(12) 0.1479(3) 0.8168(5) 0.033(2) Uani 1 1 d . . . C14 C -0.4356(12) 0.0644(3) 0.6943(5) 0.036(2) Uani 1 1 d . . . H14 H -0.4827 0.0330 0.6978 0.043 Uiso 1 1 calc R . . C20 C 0.2394(12) -0.0126(4) 0.5778(6) 0.044(3) Uani 1 1 d . . . H27 H 0.2779 -0.0403 0.6090 0.053 Uiso 1 1 calc R . . C2 C 0.1217(13) 0.3554(4) 0.9083(7) 0.047(3) Uani 1 1 d . . . H1A H 0.2142 0.3724 0.9277 0.057 Uiso 1 1 calc R . . C24 C 0.0165(10) -0.0590(3) 0.7979(5) 0.026(2) Uani 1 1 d . . . C26 C -0.0556(12) 0.1436(3) 1.2529(6) 0.040(2) Uani 1 1 d . . . H20 H -0.0923 0.1287 1.3014 0.047 Uiso 1 1 calc R . . C17 C 0.1216(13) 0.0664(4) 0.4867(6) 0.050(3) Uani 1 1 d . . . H24 H 0.0800 0.0933 0.4542 0.060 Uiso 1 1 calc R . . C1 C 0.1183(11) 0.3047(3) 0.9095(5) 0.032(2) Uani 1 1 d . . . C4 C -0.1383(14) 0.3558(4) 0.8479(7) 0.054(3) Uani 1 1 d . . . H3 H -0.2277 0.3736 0.8261 0.064 Uiso 1 1 calc R . . C18 C 0.2229(12) 0.0329(4) 0.4518(6) 0.045(3) Uani 1 1 d . . . H23 H 0.2484 0.0369 0.3954 0.054 Uiso 1 1 calc R . . C12 C -0.4231(12) 0.1425(3) 0.6243(6) 0.038(2) Uani 1 1 d . . . H12 H -0.4565 0.1637 0.5792 0.046 Uiso 1 1 calc R . . C5 C -0.1434(13) 0.3060(4) 0.8471(6) 0.048(3) Uani 1 1 d . . . H4 H -0.2363 0.2897 0.8263 0.057 Uiso 1 1 calc R . . C27 C -0.0536(13) 0.1937(3) 1.2483(6) 0.045(3) Uani 1 1 d . . . H19 H -0.0873 0.2133 1.2928 0.054 Uiso 1 1 calc R . . C16 C 0.0828(12) 0.0602(4) 0.5681(6) 0.041(3) Uani 1 1 d . . . C19 C 0.2847(14) -0.0053(4) 0.4982(6) 0.049(3) Uani 1 1 d . . . H22 H 0.3583 -0.0266 0.4757 0.059 Uiso 1 1 calc R . . C13 C -0.4891(12) 0.0961(4) 0.6302(6) 0.040(3) Uani 1 1 d . . . H13 H -0.5709 0.0861 0.5903 0.048 Uiso 1 1 calc R . . C28 C -0.0002(12) 0.2158(3) 1.1756(6) 0.044(3) Uani 1 1 d . . . H18 H 0.0013 0.2505 1.1704 0.052 Uiso 1 1 calc R . . C3 C -0.0088(14) 0.3811(4) 0.8790(7) 0.051(3) Uani 1 1 d . . . H2 H -0.0092 0.4160 0.8803 0.061 Uiso 1 1 calc R . . O12 O 0.3803(7) 0.1492(2) 0.9777(4) 0.0392(16) Uani 1 1 d . . . C32 C -0.2250(10) 0.0654(3) 1.0006(5) 0.030(2) Uani 1 1 d . . . H32A H -0.2000 0.0998 0.9897 0.045 Uiso 1 1 calc R . . H32B H -0.2327 0.0607 1.0609 0.045 Uiso 1 1 calc R . . H32C H -0.3250 0.0569 0.9700 0.045 Uiso 1 1 calc R . . C31 C 0.3237(11) 0.0371(3) 0.8938(6) 0.038(2) Uani 1 1 d . . . H31A H 0.3898 0.0260 0.9431 0.057 Uiso 1 1 calc R . . H31B H 0.3797 0.0619 0.8636 0.057 Uiso 1 1 calc R . . H31C H 0.2982 0.0091 0.8566 0.057 Uiso 1 1 calc R . . O15 O 0.4344(10) 0.2069(4) 0.1076(6) 0.091(3) Uani 1 1 d . . . H13A H 0.3541 0.2005 0.1324 0.137 Uiso 1 1 calc R . . C34 C 0.5059(12) 0.1662(4) 0.9297(6) 0.049(3) Uani 1 1 d . . . H34A H 0.5246 0.1422 0.8861 0.074 Uiso 1 1 calc R . . H34B H 0.6012 0.1703 0.9672 0.074 Uiso 1 1 calc R . . H34C H 0.4770 0.1978 0.9035 0.074 Uiso 1 1 calc R . . C33 C 0.2439(14) 0.1733(4) 0.7468(6) 0.056(3) Uani 1 1 d . . . H33A H 0.1379 0.1850 0.7303 0.084 Uiso 1 1 calc R . . H33B H 0.2942 0.1629 0.6966 0.084 Uiso 1 1 calc R . . H33C H 0.3048 0.1999 0.7748 0.084 Uiso 1 1 calc R . . C37 C 0.5710(18) 0.1940(5) 0.1604(8) 0.090(5) Uani 1 1 d . . . H35A H 0.6318 0.2237 0.1752 0.134 Uiso 1 1 calc R . . H35B H 0.6351 0.1712 0.1305 0.134 Uiso 1 1 calc R . . H35C H 0.5397 0.1784 0.2118 0.134 Uiso 1 1 calc R . . O13 O 0.3385(7) 0.0302(2) 1.1000(3) 0.0313(15) Uani 1 1 d . . . C35 C 0.4148(12) 0.0685(4) 1.1488(7) 0.049(3) Uani 1 1 d . . . H37A H 0.4474 0.0944 1.1114 0.074 Uiso 1 1 calc R . . H37B H 0.5070 0.0552 1.1813 0.074 Uiso 1 1 calc R . . H37C H 0.3425 0.0822 1.1873 0.074 Uiso 1 1 calc R . . O14 O 0.5268(13) 0.2990(4) 0.0750(6) 0.096(3) Uani 1 1 d . . . H14A H 0.4478 0.3143 0.0545 0.145 Uiso 1 1 calc R . . C36 C 0.6401(19) 0.2976(5) 0.0164(10) 0.101(5) Uani 1 1 d . . . H36A H 0.5941 0.3093 -0.0382 0.151 Uiso 1 1 calc R . . H36B H 0.6771 0.2639 0.0107 0.151 Uiso 1 1 calc R . . H36C H 0.7281 0.3188 0.0356 0.151 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 0.0354(8) 0.0281(7) 0.0288(6) -0.0012(5) 0.0085(6) 0.0024(6) Ni2 0.0292(7) 0.0267(6) 0.0275(6) -0.0036(5) 0.0082(5) 0.0024(5) Ni3 0.0378(8) 0.0271(6) 0.0311(6) -0.0008(5) 0.0098(6) 0.0009(6) O9 0.029(4) 0.028(3) 0.028(3) -0.006(3) 0.005(3) 0.004(3) O10 0.030(4) 0.026(3) 0.029(3) -0.005(3) 0.007(3) 0.004(3) O3 0.034(4) 0.027(3) 0.036(3) 0.003(3) 0.001(3) -0.001(3) O7 0.037(4) 0.026(3) 0.028(3) -0.006(3) 0.010(3) 0.001(3) O8 0.035(4) 0.028(3) 0.029(3) -0.007(3) 0.013(3) 0.002(3) O4 0.038(4) 0.032(4) 0.035(3) -0.007(3) -0.004(3) -0.003(3) O6 0.043(4) 0.029(4) 0.032(3) -0.003(3) 0.006(3) -0.004(3) O11 0.047(4) 0.035(4) 0.036(4) 0.005(3) 0.013(3) -0.002(3) O2 0.044(4) 0.028(4) 0.038(4) -0.001(3) 0.010(3) 0.000(3) O1 0.048(5) 0.035(4) 0.059(4) 0.002(4) 0.000(4) -0.010(3) C10 0.035(6) 0.036(6) 0.034(5) -0.007(4) 0.008(5) 0.000(5) C30 0.026(6) 0.035(5) 0.036(5) -0.002(5) 0.001(4) 0.001(4) O5 0.067(5) 0.039(4) 0.043(4) 0.002(3) 0.019(4) 0.013(4) C29 0.052(7) 0.040(6) 0.038(5) -0.005(5) 0.016(5) 0.008(5) C6 0.040(7) 0.038(6) 0.035(5) -0.002(4) 0.008(5) -0.002(5) C23 0.044(7) 0.032(5) 0.032(5) 0.001(4) 0.009(5) -0.006(5) C21 0.048(7) 0.037(6) 0.034(5) -0.006(5) 0.009(5) -0.002(5) C8 0.042(6) 0.031(5) 0.032(5) 0.002(4) 0.015(5) 0.002(5) C25 0.028(6) 0.030(5) 0.030(5) -0.006(4) 0.002(4) 0.008(4) C7 0.041(7) 0.036(6) 0.030(5) -0.005(4) 0.015(5) 0.002(5) C11 0.048(7) 0.038(6) 0.031(5) -0.003(5) 0.015(5) -0.003(5) C15 0.032(6) 0.040(6) 0.031(5) 0.002(5) 0.006(5) 0.009(5) C22 0.030(6) 0.043(6) 0.034(5) -0.007(5) 0.009(5) 0.002(5) C9 0.040(6) 0.035(6) 0.028(5) 0.002(4) 0.020(5) 0.002(5) C14 0.048(7) 0.030(5) 0.031(5) -0.013(4) 0.007(5) 0.006(5) C20 0.060(8) 0.033(6) 0.043(6) -0.006(5) 0.022(6) -0.007(5) C2 0.041(7) 0.045(7) 0.058(7) 0.006(5) 0.010(6) -0.004(5) C24 0.029(6) 0.026(5) 0.024(5) -0.001(4) 0.004(4) 0.002(4) C26 0.047(7) 0.035(6) 0.039(5) -0.005(4) 0.017(5) -0.001(5) C17 0.066(8) 0.051(7) 0.034(6) 0.003(5) 0.006(6) 0.000(6) C1 0.031(6) 0.033(5) 0.030(5) -0.004(4) -0.003(5) -0.002(5) C4 0.057(8) 0.032(6) 0.071(8) -0.004(5) 0.003(7) 0.015(5) C18 0.051(7) 0.051(7) 0.036(6) -0.011(5) 0.022(5) -0.006(6) C12 0.049(7) 0.037(6) 0.030(5) 0.006(4) 0.010(5) 0.007(5) C5 0.055(8) 0.031(6) 0.056(7) -0.006(5) 0.002(6) 0.002(5) C27 0.061(8) 0.032(6) 0.046(6) -0.013(5) 0.024(6) -0.003(5) C16 0.046(7) 0.041(6) 0.036(6) -0.003(5) 0.006(5) 0.003(5) C19 0.069(9) 0.042(6) 0.042(6) -0.013(5) 0.035(6) 0.000(6) C13 0.042(7) 0.044(6) 0.035(5) -0.008(5) 0.004(5) 0.010(5) C28 0.064(8) 0.018(5) 0.052(6) -0.004(5) 0.029(6) -0.008(5) C3 0.060(8) 0.037(6) 0.056(7) 0.000(5) 0.006(6) 0.000(6) O12 0.035(4) 0.041(4) 0.043(4) 0.000(3) 0.015(3) -0.008(3) C32 0.028(6) 0.027(5) 0.035(5) -0.013(4) 0.009(4) 0.006(4) C31 0.044(7) 0.030(5) 0.041(5) -0.001(4) 0.016(5) 0.003(5) O15 0.053(6) 0.150(9) 0.074(6) -0.040(6) 0.019(5) -0.034(6) C34 0.039(7) 0.056(7) 0.054(7) -0.004(5) 0.010(6) 0.003(5) C33 0.078(9) 0.043(6) 0.051(6) 0.020(5) 0.036(6) 0.012(6) C37 0.102(13) 0.105(12) 0.063(8) 0.000(8) 0.014(9) -0.046(10) O13 0.031(4) 0.035(4) 0.028(3) -0.009(3) 0.000(3) -0.001(3) C35 0.043(7) 0.040(6) 0.063(7) -0.008(5) -0.007(6) 0.003(5) O14 0.112(9) 0.107(9) 0.072(6) 0.002(5) 0.017(6) 0.025(7) C36 0.106(14) 0.089(11) 0.110(12) -0.020(9) 0.031(11) -0.022(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O6 2.006(6) . ? Ni1 O3 2.014(6) . ? Ni1 O4 2.020(6) . ? Ni1 O10 2.022(6) . ? Ni1 O7 2.024(6) . ? Ni1 O9 2.098(6) . ? Ni2 O8 1.994(6) . ? Ni2 O7 2.005(6) 3_557 ? Ni2 O9 2.010(6) . ? Ni2 O10 2.039(6) 3_557 ? Ni2 O10 2.067(6) . ? Ni2 O13 2.120(6) . ? Ni3 O2 2.000(6) . ? Ni3 O9 2.026(6) . ? Ni3 O3 2.051(6) . ? Ni3 O12 2.063(7) . ? Ni3 O11 2.115(6) . ? Ni3 O8 2.135(6) . ? O9 C31 1.439(10) . ? O10 C32 1.425(9) . ? O10 Ni2 2.039(6) 3_557 ? O3 C9 1.299(11) . ? O7 C24 1.295(9) . ? O7 Ni2 2.005(6) 3_557 ? O8 C30 1.347(10) . ? O4 C15 1.286(10) . ? O6 C22 1.316(10) . ? O11 C33 1.456(10) . ? O2 C7 1.317(11) . ? O1 C1 1.362(11) . ? O1 H1 0.8400 . ? C10 C11 1.409(13) . ? C10 C15 1.435(12) . ? C10 C9 1.490(13) . ? C30 C25 1.403(12) . ? C30 C29 1.403(13) . ? O5 C16 1.368(11) . ? O5 H5 0.8400 . ? C29 C28 1.362(13) . ? C29 H17 0.9500 . ? C6 C1 1.386(13) . ? C6 C5 1.414(14) . ? C6 C7 1.499(12) . ? C23 C22 1.377(12) . ? C23 C24 1.408(12) . ? C23 H29 0.9500 . ? C21 C16 1.381(13) . ? C21 C20 1.409(13) . ? C21 C22 1.501(12) . ? C8 C7 1.379(13) . ? C8 C9 1.390(12) . ? C8 H8 0.9500 . ? C25 C26 1.447(12) . ? C25 C24 1.479(12) 3_557 ? C11 C12 1.364(13) . ? C11 H11 0.9500 . ? C15 C14 1.402(13) . ? C14 C13 1.389(13) . ? C14 H14 0.9500 . ? C20 C19 1.374(13) . ? C20 H27 0.9500 . ? C2 C3 1.371(14) . ? C2 C1 1.384(13) . ? C2 H1A 0.9500 . ? C24 C25 1.479(12) 3_557 ? C26 C27 1.369(12) . ? C26 H20 0.9500 . ? C17 C16 1.377(13) . ? C17 C18 1.406(14) . ? C17 H24 0.9500 . ? C4 C5 1.359(13) . ? C4 C3 1.367(15) . ? C4 H3 0.9500 . ? C18 C19 1.360(14) . ? C18 H23 0.9500 . ? C12 C13 1.392(13) . ? C12 H12 0.9500 . ? C5 H4 0.9500 . ? C27 C28 1.416(13) . ? C27 H19 0.9500 . ? C19 H22 0.9500 . ? C13 H13 0.9500 . ? C28 H18 0.9500 . ? C3 H2 0.9500 . ? O12 C34 1.446(11) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? O15 C37 1.433(15) . ? O15 H13A 0.8400 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C37 H35A 0.9800 . ? C37 H35B 0.9800 . ? C37 H35C 0.9800 . ? O13 C35 1.431(11) . ? C35 H37A 0.9800 . ? C35 H37B 0.9800 . ? C35 H37C 0.9800 . ? O14 C36 1.402(15) . ? O14 H14A 0.8400 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 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 O6 Ni1 O3 93.1(2) . . ? O6 Ni1 O4 94.7(3) . . ? O3 Ni1 O4 86.9(2) . . ? O6 Ni1 O10 172.4(2) . . ? O3 Ni1 O10 92.4(2) . . ? O4 Ni1 O10 90.7(2) . . ? O6 Ni1 O7 91.2(2) . . ? O3 Ni1 O7 175.7(2) . . ? O4 Ni1 O7 92.8(2) . . ? O10 Ni1 O7 83.3(2) . . ? O6 Ni1 O9 92.5(2) . . ? O3 Ni1 O9 82.7(2) . . ? O4 Ni1 O9 167.7(2) . . ? O10 Ni1 O9 83.0(2) . . ? O7 Ni1 O9 97.1(2) . . ? O8 Ni2 O7 90.4(2) . 3_557 ? O8 Ni2 O9 83.9(2) . . ? O7 Ni2 O9 171.6(2) 3_557 . ? O8 Ni2 O10 172.6(2) . 3_557 ? O7 Ni2 O10 83.4(2) 3_557 3_557 ? O9 Ni2 O10 101.8(2) . 3_557 ? O8 Ni2 O10 93.7(2) . . ? O7 Ni2 O10 90.1(2) 3_557 . ? O9 Ni2 O10 84.2(2) . . ? O10 Ni2 O10 82.4(2) 3_557 . ? O8 Ni2 O13 97.1(2) . . ? O7 Ni2 O13 87.1(2) 3_557 . ? O9 Ni2 O13 99.7(2) . . ? O10 Ni2 O13 86.6(2) 3_557 . ? O10 Ni2 O13 168.8(2) . . ? O2 Ni3 O9 170.8(3) . . ? O2 Ni3 O3 87.4(3) . . ? O9 Ni3 O3 83.6(2) . . ? O2 Ni3 O12 89.7(3) . . ? O9 Ni3 O12 99.1(2) . . ? O3 Ni3 O12 174.0(2) . . ? O2 Ni3 O11 91.7(2) . . ? O9 Ni3 O11 85.4(2) . . ? O3 Ni3 O11 83.9(2) . . ? O12 Ni3 O11 91.1(3) . . ? O2 Ni3 O8 103.2(2) . . ? O9 Ni3 O8 80.0(2) . . ? O3 Ni3 O8 97.8(2) . . ? O12 Ni3 O8 87.9(2) . . ? O11 Ni3 O8 165.1(2) . . ? C31 O9 Ni2 118.6(5) . . ? C31 O9 Ni3 119.6(5) . . ? Ni2 O9 Ni3 99.5(2) . . ? C31 O9 Ni1 122.2(5) . . ? Ni2 O9 Ni1 95.8(2) . . ? Ni3 O9 Ni1 95.9(2) . . ? C32 O10 Ni1 118.1(5) . . ? C32 O10 Ni2 125.0(5) . 3_557 ? Ni1 O10 Ni2 95.8(2) . 3_557 ? C32 O10 Ni2 118.0(5) . . ? Ni1 O10 Ni2 96.4(2) . . ? Ni2 O10 Ni2 97.6(2) 3_557 . ? C9 O3 Ni1 128.0(6) . . ? C9 O3 Ni3 128.5(6) . . ? Ni1 O3 Ni3 97.8(3) . . ? C24 O7 Ni2 132.2(5) . 3_557 ? C24 O7 Ni1 130.7(5) . . ? Ni2 O7 Ni1 96.8(2) 3_557 . ? C30 O8 Ni2 126.4(6) . . ? C30 O8 Ni3 136.5(6) . . ? Ni2 O8 Ni3 96.4(2) . . ? C15 O4 Ni1 121.6(6) . . ? C22 O6 Ni1 122.7(6) . . ? C33 O11 Ni3 128.0(6) . . ? C7 O2 Ni3 126.9(6) . . ? C1 O1 H1 109.5 . . ? C11 C10 C15 118.8(9) . . ? C11 C10 C9 117.7(8) . . ? C15 C10 C9 123.4(8) . . ? O8 C30 C25 124.8(8) . . ? O8 C30 C29 116.1(8) . . ? C25 C30 C29 119.0(8) . . ? C16 O5 H5 109.5 . . ? C28 C29 C30 122.9(10) . . ? C28 C29 H17 118.6 . . ? C30 C29 H17 118.6 . . ? C1 C6 C5 116.6(9) . . ? C1 C6 C7 122.3(9) . . ? C5 C6 C7 121.1(9) . . ? C22 C23 C24 130.7(9) . . ? C22 C23 H29 114.6 . . ? C24 C23 H29 114.6 . . ? C16 C21 C20 118.2(9) . . ? C16 C21 C22 121.3(9) . . ? C20 C21 C22 120.3(9) . . ? C7 C8 C9 127.5(9) . . ? C7 C8 H8 116.3 . . ? C9 C8 H8 116.3 . . ? C30 C25 C26 117.1(8) . . ? C30 C25 C24 127.3(8) . 3_557 ? C26 C25 C24 115.6(8) . 3_557 ? O2 C7 C8 125.5(9) . . ? O2 C7 C6 113.5(8) . . ? C8 C7 C6 120.8(9) . . ? C12 C11 C10 122.2(9) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? O4 C15 C14 118.8(9) . . ? O4 C15 C10 124.0(9) . . ? C14 C15 C10 117.3(8) . . ? O6 C22 C23 126.9(8) . . ? O6 C22 C21 114.5(8) . . ? C23 C22 C21 118.7(8) . . ? O3 C9 C8 120.0(9) . . ? O3 C9 C10 119.0(8) . . ? C8 C9 C10 121.0(9) . . ? C13 C14 C15 121.9(9) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C19 C20 C21 121.6(10) . . ? C19 C20 H27 119.2 . . ? C21 C20 H27 119.2 . . ? C3 C2 C1 119.9(10) . . ? C3 C2 H1A 120.1 . . ? C1 C2 H1A 120.1 . . ? O7 C24 C23 117.6(8) . . ? O7 C24 C25 118.8(7) . 3_557 ? C23 C24 C25 123.7(8) . 3_557 ? C27 C26 C25 122.9(9) . . ? C27 C26 H20 118.6 . . ? C25 C26 H20 118.6 . . ? C16 C17 C18 119.7(10) . . ? C16 C17 H24 120.1 . . ? C18 C17 H24 120.1 . . ? O1 C1 C2 115.5(9) . . ? O1 C1 C6 122.5(8) . . ? C2 C1 C6 122.0(9) . . ? C5 C4 C3 122.2(11) . . ? C5 C4 H3 118.9 . . ? C3 C4 H3 118.9 . . ? C19 C18 C17 120.6(9) . . ? C19 C18 H23 119.7 . . ? C17 C18 H23 119.7 . . ? C11 C12 C13 119.4(9) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C4 C5 C6 120.4(10) . . ? C4 C5 H4 119.8 . . ? C6 C5 H4 119.8 . . ? C26 C27 C28 118.3(9) . . ? C26 C27 H19 120.9 . . ? C28 C27 H19 120.9 . . ? O5 C16 C17 117.3(9) . . ? O5 C16 C21 122.2(9) . . ? C17 C16 C21 120.5(9) . . ? C18 C19 C20 119.2(10) . . ? C18 C19 H22 120.4 . . ? C20 C19 H22 120.4 . . ? C14 C13 C12 120.1(9) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C29 C28 C27 119.9(9) . . ? C29 C28 H18 120.1 . . ? C27 C28 H18 120.1 . . ? C2 C3 C4 118.9(10) . . ? C2 C3 H2 120.5 . . ? C4 C3 H2 120.5 . . ? C34 O12 Ni3 124.4(6) . . ? O10 C32 H32A 109.5 . . ? O10 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O10 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O9 C31 H31A 109.5 . . ? O9 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O9 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 O15 H13A 109.5 . . ? O12 C34 H34A 109.5 . . ? O12 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O12 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O11 C33 H33A 109.5 . . ? O11 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O11 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O15 C37 H35A 109.5 . . ? O15 C37 H35B 109.5 . . ? H35A C37 H35B 109.5 . . ? O15 C37 H35C 109.5 . . ? H35A C37 H35C 109.5 . . ? H35B C37 H35C 109.5 . . ? C35 O13 Ni2 122.2(5) . . ? O13 C35 H37A 109.5 . . ? O13 C35 H37B 109.5 . . ? H37A C35 H37B 109.5 . . ? O13 C35 H37C 109.5 . . ? H37A C35 H37C 109.5 . . ? H37B C35 H37C 109.5 . . ? C36 O14 H14A 109.5 . . ? O14 C36 H36A 109.5 . . ? O14 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O14 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.12 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.351 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.135 data_complex2 _database_code_depnum_ccdc_archive 'CCDC 924184' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H76 Co Ni5 O26, 4(C H4 O)' _chemical_formula_sum 'C74 H92 Co Ni5 O30' _chemical_formula_weight 1813.96 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' O O 0.0106 0.0060 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.5016(7) _cell_length_b 27.218(2) _cell_length_c 16.0744(12) _cell_angle_alpha 90.00 _cell_angle_beta 94.700(2) _cell_angle_gamma 90.00 _cell_volume 3707.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6393 _cell_measurement_theta_min 2.518 _cell_measurement_theta_max 23.109 _exptl_crystal_description needles _exptl_crystal_colour 'light brown' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1886 _exptl_absorpt_coefficient_mu 1.551 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5759 _exptl_absorpt_correction_T_max 0.8604 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19910 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_unetI/netI 0.0369 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6901 _reflns_number_gt 5601 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0631P)^2^+3.6327P] 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 6901 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 Ni3 Ni 0.3377(2) 0.13188(10) 0.57213(13) 0.0137(6) Uani 0.50 1 d P A 1 Co1 Co 0.3322(4) 0.13275(14) 0.5707(2) 0.0577(13) Uani 0.50 1 d P A 2 Ni1 Ni 0.53623(5) 0.045603(15) 0.64380(3) 0.02818(14) Uani 1 1 d . A . Ni2 Ni 0.38394(5) 0.039792(15) 0.46492(3) 0.02618(14) Uani 1 1 d . . . O9 O 0.3152(3) 0.05819(8) 0.57878(14) 0.0268(5) Uani 1 1 d . . . O10 O 0.6045(3) 0.03487(8) 0.52693(14) 0.0261(5) Uani 1 1 d . . . O3 O 0.5531(3) 0.11893(8) 0.63559(14) 0.0307(5) Uani 1 1 d . . . O7 O 0.5219(3) -0.02859(8) 0.64438(14) 0.0285(5) Uani 1 1 d . . . O8 O 0.3970(3) 0.11213(8) 0.44837(14) 0.0289(5) Uani 1 1 d . . . O4 O 0.7609(3) 0.04522(9) 0.69082(16) 0.0338(6) Uani 1 1 d . . . O6 O 0.4470(3) 0.04856(8) 0.75584(15) 0.0331(6) Uani 1 1 d . . . O2 O 0.3944(3) 0.20365(9) 0.58154(16) 0.0363(6) Uani 1 1 d . . . O13 O 0.1596(3) 0.03024(9) 0.39998(15) 0.0320(6) Uani 1 1 d . . . O11 O 0.2547(3) 0.13210(9) 0.69643(16) 0.0405(6) Uani 1 1 d . . . O12 O 0.1140(3) 0.15188(10) 0.52205(16) 0.0402(6) Uani 1 1 d . . . O5 O 0.5184(4) 0.09454(10) 0.90063(17) 0.0480(7) Uani 1 1 d . . . H1 H 0.5220 0.0908 0.8489 0.072 Uiso 1 1 calc R . . C10 C 0.7523(4) 0.12707(13) 0.7486(2) 0.0329(8) Uani 1 1 d . . . O1 O 0.2443(3) 0.28279(10) 0.5596(2) 0.0487(7) Uani 1 1 d . . . H5 H 0.2583 0.2523 0.5586 0.073 Uiso 1 1 calc R . . C29 C 0.4507(4) 0.18734(13) 0.3859(2) 0.0353(8) Uani 1 1 d . . . H31 H 0.4145 0.2033 0.4334 0.042 Uiso 1 1 calc R A . C30 C 0.4499(4) 0.13537(13) 0.3837(2) 0.0290(8) Uani 1 1 d . A . C7 C 0.5124(4) 0.22417(13) 0.6248(2) 0.0323(8) Uani 1 1 d . A . C23 C 0.4332(5) -0.03857(13) 0.7761(2) 0.0361(9) Uani 1 1 d . . . H9 H 0.4067 -0.0621 0.8164 0.043 Uiso 1 1 calc R A . C22 C 0.4159(4) 0.00998(14) 0.7989(2) 0.0340(8) Uani 1 1 d . A . C21 C 0.3620(5) 0.01985(14) 0.8834(2) 0.0351(9) Uani 1 1 d . . . C6 C 0.5118(5) 0.27913(13) 0.6228(2) 0.0357(9) Uani 1 1 d . . . C25 C 0.5059(4) 0.11198(13) 0.3118(2) 0.0314(8) Uani 1 1 d . . . C8 C 0.6276(5) 0.19924(13) 0.6732(2) 0.0358(9) Uani 1 1 d . . . H18 H 0.7067 0.2187 0.7025 0.043 Uiso 1 1 calc R A . C24 C 0.4844(4) -0.05834(13) 0.7019(2) 0.0304(8) Uani 1 1 d . . . C26 C 0.5564(5) 0.14339(14) 0.2486(2) 0.0405(9) Uani 1 1 d . A . H28 H 0.5949 0.1287 0.2007 0.049 Uiso 1 1 calc R . . C2 C 0.3794(5) 0.35647(14) 0.5913(3) 0.0451(10) Uani 1 1 d . . . H5A H 0.2880 0.3738 0.5698 0.054 Uiso 1 1 calc R A . C11 C 0.8083(5) 0.15721(14) 0.8167(2) 0.0363(9) Uani 1 1 d . A . H21 H 0.7659 0.1893 0.8207 0.044 Uiso 1 1 calc R . . C1 C 0.3786(5) 0.30502(14) 0.5908(2) 0.0361(9) Uani 1 1 d . A . C15 C 0.8131(4) 0.07793(13) 0.7463(2) 0.0332(8) Uani 1 1 d . A . C14 C 0.9352(5) 0.06453(14) 0.8067(2) 0.0368(9) Uani 1 1 d . . . H24 H 0.9825 0.0331 0.8033 0.044 Uiso 1 1 calc R A . C9 C 0.6404(4) 0.14820(13) 0.6835(2) 0.0310(8) Uani 1 1 d . A . C20 C 0.2596(5) -0.01210(14) 0.9198(2) 0.0423(10) Uani 1 1 d . A . H12 H 0.2175 -0.0393 0.8884 0.051 Uiso 1 1 calc R . . C18 C 0.2796(5) 0.03337(16) 1.0456(3) 0.0474(11) Uani 1 1 d . A . H14 H 0.2545 0.0373 1.1018 0.057 Uiso 1 1 calc R . . C27 C 0.5529(5) 0.19346(14) 0.2528(3) 0.0448(10) Uani 1 1 d . . . H29 H 0.5856 0.2129 0.2082 0.054 Uiso 1 1 calc R A . C19 C 0.2175(5) -0.00542(15) 0.9998(3) 0.0454(10) Uani 1 1 d . . . H13 H 0.1462 -0.0274 1.0230 0.055 Uiso 1 1 calc R A . C12 C 0.9204(5) 0.14203(14) 0.8766(2) 0.0396(9) Uani 1 1 d . . . H22 H 0.9526 0.1629 0.9223 0.048 Uiso 1 1 calc R A . C28 C 0.5007(5) 0.21562(14) 0.3236(3) 0.0426(10) Uani 1 1 d . A . H30 H 0.4999 0.2504 0.3283 0.051 Uiso 1 1 calc R . . C17 C 0.3781(5) 0.06685(15) 1.0117(2) 0.0451(10) Uani 1 1 d . . . H15 H 0.4181 0.0940 1.0439 0.054 Uiso 1 1 calc R A . C5 C 0.6433(5) 0.30635(15) 0.6531(3) 0.0448(10) Uani 1 1 d . A . H2 H 0.7361 0.2896 0.6744 0.054 Uiso 1 1 calc R . . C13 C 0.9876(5) 0.09542(15) 0.8701(2) 0.0408(9) Uani 1 1 d . A . H23 H 1.0699 0.0852 0.9099 0.049 Uiso 1 1 calc R . . C16 C 0.4189(5) 0.06068(14) 0.9298(2) 0.0388(9) Uani 1 1 d . A . C4 C 0.6419(6) 0.35722(15) 0.6529(3) 0.0507(11) Uani 1 1 d . . . H3 H 0.7325 0.3751 0.6742 0.061 Uiso 1 1 calc R A . C3 C 0.5080(5) 0.38180(15) 0.6217(3) 0.0493(11) Uani 1 1 d . A . H4 H 0.5062 0.4167 0.6217 0.059 Uiso 1 1 calc R . . C32 C 0.7262(4) 0.06556(12) 0.5002(2) 0.0314(8) Uani 1 1 d . A . H35A H 0.7010 0.1000 0.5108 0.047 Uiso 1 1 calc R . . H35B H 0.7347 0.0608 0.4403 0.047 Uiso 1 1 calc R . . H35C H 0.8268 0.0570 0.5310 0.047 Uiso 1 1 calc R . . C31 C 0.1729(5) 0.03677(14) 0.6048(2) 0.0373(9) Uani 1 1 d . A . H36A H 0.1131 0.0617 0.6328 0.056 Uiso 1 1 calc R . . H36B H 0.1997 0.0096 0.6435 0.056 Uiso 1 1 calc R . . H36C H 0.1088 0.0243 0.5559 0.056 Uiso 1 1 calc R . . C35 C 0.0832(5) 0.06903(14) 0.3524(3) 0.0464(10) Uani 1 1 d . A . H37A H 0.0566 0.0956 0.3899 0.070 Uiso 1 1 calc R . . H37B H -0.0135 0.0565 0.3223 0.070 Uiso 1 1 calc R . . H37C H 0.1541 0.0816 0.3122 0.070 Uiso 1 1 calc R . . C34 C -0.0116(5) 0.16801(16) 0.5696(3) 0.0499(11) Uani 1 1 d . A . H34A H -0.0271 0.1441 0.6138 0.075 Uiso 1 1 calc R . . H34B H -0.1090 0.1709 0.5329 0.075 Uiso 1 1 calc R . . H34C H 0.0154 0.2000 0.5947 0.075 Uiso 1 1 calc R . . C33 C 0.2491(6) 0.17283(15) 0.7516(3) 0.0538(12) Uani 1 1 d . A . H33A H 0.3555 0.1798 0.7770 0.081 Uiso 1 1 calc R . . H33B H 0.1795 0.1650 0.7955 0.081 Uiso 1 1 calc R . . H33C H 0.2084 0.2017 0.7204 0.081 Uiso 1 1 calc R . . O15 O 1.0643(4) 0.20908(15) 0.3898(2) 0.0789(12) Uani 1 1 d . . . H14A H 1.0889 0.1869 0.4249 0.118 Uiso 1 1 calc R . . O14 O 0.4649(5) 0.19950(17) 0.9238(2) 0.0870(12) Uani 1 1 d . . . H15A H 0.5553 0.1937 0.9469 0.130 Uiso 1 1 calc R . . C37 C 0.9288(8) 0.1943(2) 0.3386(4) 0.0842(19) Uani 1 1 d . . . H39A H 0.8485 0.1820 0.3737 0.126 Uiso 1 1 calc R . . H39B H 0.9577 0.1683 0.3006 0.126 Uiso 1 1 calc R . . H39C H 0.8866 0.2225 0.3061 0.126 Uiso 1 1 calc R . . C36 C 0.3548(8) 0.2008(2) 0.9849(4) 0.0868(18) Uani 1 1 d . . . H38A H 0.4107 0.1986 1.0405 0.130 Uiso 1 1 calc R . . H38B H 0.2818 0.1730 0.9764 0.130 Uiso 1 1 calc R . . H38C H 0.2953 0.2316 0.9801 0.130 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 Ni3 0.0078(7) 0.0195(14) 0.0135(10) 0.0030(9) -0.0014(7) -0.0004(7) Co1 0.092(2) 0.027(2) 0.058(2) -0.0030(16) 0.0282(17) 0.0027(16) Ni1 0.0345(3) 0.0247(2) 0.0260(3) 0.00110(17) 0.00624(19) -0.00106(19) Ni2 0.0304(3) 0.0229(2) 0.0260(2) 0.00225(17) 0.00686(18) -0.00124(18) O9 0.0283(13) 0.0263(12) 0.0268(12) 0.0027(10) 0.0079(10) -0.0012(10) O10 0.0270(13) 0.0261(12) 0.0258(12) 0.0026(9) 0.0057(9) -0.0037(10) O3 0.0344(14) 0.0255(12) 0.0321(13) 0.0002(10) 0.0027(11) -0.0004(10) O7 0.0366(14) 0.0239(12) 0.0259(13) 0.0025(9) 0.0086(10) -0.0003(10) O8 0.0356(14) 0.0224(12) 0.0295(13) 0.0031(10) 0.0084(10) 0.0007(10) O4 0.0345(14) 0.0321(14) 0.0343(14) -0.0002(11) -0.0011(11) 0.0003(11) O6 0.0430(16) 0.0282(13) 0.0289(13) 0.0004(10) 0.0090(11) -0.0001(11) O2 0.0452(16) 0.0276(13) 0.0363(14) 0.0008(11) 0.0052(12) 0.0009(12) O13 0.0315(14) 0.0299(13) 0.0347(14) 0.0060(10) 0.0030(10) 0.0012(11) O11 0.0532(18) 0.0338(14) 0.0361(15) -0.0041(11) 0.0130(12) 0.0023(13) O12 0.0351(15) 0.0432(15) 0.0431(16) 0.0021(12) 0.0084(12) 0.0048(12) O5 0.064(2) 0.0451(16) 0.0367(16) -0.0043(13) 0.0163(14) -0.0126(15) C10 0.037(2) 0.034(2) 0.0287(18) 0.0010(15) 0.0070(15) -0.0053(16) O1 0.0464(18) 0.0332(15) 0.065(2) -0.0022(14) -0.0031(14) 0.0021(13) C29 0.041(2) 0.0279(19) 0.038(2) 0.0025(16) 0.0138(17) 0.0014(16) C30 0.0258(19) 0.0308(18) 0.0308(19) 0.0063(15) 0.0043(14) -0.0021(15) C7 0.039(2) 0.0287(18) 0.0303(19) -0.0002(15) 0.0112(16) -0.0017(16) C23 0.048(2) 0.0300(19) 0.031(2) 0.0062(15) 0.0108(17) -0.0003(17) C22 0.038(2) 0.037(2) 0.0277(19) 0.0038(15) 0.0074(15) 0.0012(17) C21 0.039(2) 0.034(2) 0.033(2) 0.0051(16) 0.0059(16) 0.0074(17) C6 0.044(2) 0.0302(19) 0.034(2) 0.0021(15) 0.0128(16) -0.0017(17) C25 0.034(2) 0.0291(18) 0.0317(19) 0.0053(15) 0.0035(15) 0.0002(15) C8 0.041(2) 0.0322(19) 0.035(2) -0.0037(15) 0.0045(16) -0.0069(17) C24 0.0286(19) 0.0318(18) 0.0307(19) 0.0072(15) 0.0025(15) -0.0014(15) C26 0.053(3) 0.034(2) 0.037(2) 0.0011(16) 0.0156(18) -0.0008(18) C2 0.049(3) 0.034(2) 0.053(3) -0.0001(18) 0.009(2) 0.0046(19) C11 0.043(2) 0.033(2) 0.034(2) -0.0006(16) 0.0097(17) -0.0060(17) C1 0.041(2) 0.033(2) 0.035(2) 0.0005(16) 0.0083(16) 0.0015(17) C15 0.036(2) 0.036(2) 0.0286(19) 0.0023(15) 0.0058(15) -0.0048(16) C14 0.041(2) 0.034(2) 0.036(2) 0.0060(16) 0.0045(17) -0.0026(17) C9 0.035(2) 0.0310(19) 0.0284(19) -0.0004(14) 0.0116(15) -0.0027(16) C20 0.054(3) 0.034(2) 0.040(2) 0.0049(17) 0.0144(19) 0.0044(19) C18 0.057(3) 0.056(3) 0.030(2) 0.0066(19) 0.0113(19) 0.009(2) C27 0.059(3) 0.031(2) 0.047(2) 0.0100(17) 0.020(2) 0.0013(19) C19 0.058(3) 0.039(2) 0.041(2) 0.0115(18) 0.019(2) 0.004(2) C12 0.048(2) 0.038(2) 0.034(2) 0.0007(16) 0.0042(17) -0.0065(18) C28 0.054(3) 0.0244(19) 0.052(2) 0.0041(17) 0.018(2) 0.0043(18) C17 0.057(3) 0.044(2) 0.035(2) -0.0004(18) 0.0055(19) 0.004(2) C5 0.044(2) 0.034(2) 0.056(3) 0.0059(18) 0.0042(19) -0.0034(18) C13 0.044(2) 0.045(2) 0.034(2) 0.0073(17) 0.0012(17) -0.0070(19) C16 0.047(2) 0.035(2) 0.035(2) 0.0026(17) 0.0079(17) 0.0020(18) C4 0.052(3) 0.034(2) 0.066(3) 0.002(2) 0.004(2) -0.006(2) C3 0.055(3) 0.030(2) 0.064(3) 0.0003(19) 0.012(2) 0.002(2) C32 0.036(2) 0.0263(18) 0.0334(19) 0.0027(15) 0.0085(15) -0.0070(15) C31 0.040(2) 0.033(2) 0.040(2) 0.0026(16) 0.0127(17) -0.0017(17) C35 0.048(3) 0.037(2) 0.053(3) 0.0098(19) -0.007(2) 0.0002(19) C34 0.043(3) 0.049(3) 0.058(3) 0.001(2) 0.011(2) -0.001(2) C33 0.078(3) 0.039(2) 0.049(3) -0.0081(19) 0.032(2) -0.003(2) O15 0.058(2) 0.107(3) 0.073(3) 0.039(2) 0.0144(19) 0.026(2) O14 0.107(3) 0.088(3) 0.067(3) -0.005(2) 0.013(2) 0.010(3) C37 0.099(5) 0.095(5) 0.059(3) 0.010(3) 0.008(3) 0.038(4) C36 0.094(5) 0.072(4) 0.096(5) -0.012(3) 0.014(4) -0.014(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ni3 O2 2.015(4) . ? Ni3 O9 2.018(3) . ? Ni3 O3 2.053(3) . ? Ni3 O12 2.076(3) . ? Ni3 O8 2.160(3) . ? Ni3 O11 2.173(3) . ? Co1 O2 2.005(5) . ? Co1 O12 2.021(4) . ? Co1 O9 2.039(4) . ? Co1 O3 2.106(4) . ? Co1 O8 2.159(5) . ? Co1 O11 2.176(5) . ? Ni1 O4 1.996(2) . ? Ni1 O3 2.006(2) . ? Ni1 O6 2.012(2) . ? Ni1 O7 2.023(2) . ? Ni1 O10 2.032(2) . ? Ni1 O9 2.102(2) . ? Ni2 O8 1.991(2) . ? Ni2 O7 2.013(2) 3_656 ? Ni2 O9 2.029(2) . ? Ni2 O10 2.038(2) 3_656 ? Ni2 O10 2.054(2) . ? Ni2 O13 2.114(2) . ? O9 C31 1.436(4) . ? O10 C32 1.424(4) . ? O10 Ni2 2.038(2) 3_656 ? O3 C9 1.298(4) . ? O7 C24 1.289(4) . ? O7 Ni2 2.013(2) 3_656 ? O8 C30 1.327(4) . ? O4 C15 1.311(4) . ? O6 C22 1.297(4) . ? O2 C7 1.298(4) . ? O13 C35 1.428(4) . ? O11 C33 1.423(5) . ? O12 C34 1.433(5) . ? O5 C16 1.360(5) . ? O5 H1 0.8400 . ? C10 C11 1.419(5) . ? C10 C15 1.435(5) . ? C10 C9 1.472(5) . ? O1 C1 1.352(5) . ? O1 H5 0.8400 . ? C29 C28 1.359(5) . ? C29 C30 1.415(5) . ? C29 H31 0.9500 . ? C30 C25 1.435(5) . ? C7 C8 1.379(5) . ? C7 C6 1.496(5) . ? C23 C22 1.382(5) . ? C23 C24 1.410(5) . ? C23 H9 0.9500 . ? C22 C21 1.492(5) . ? C21 C20 1.394(5) . ? C21 C16 1.402(5) . ? C6 C5 1.395(5) . ? C6 C1 1.396(5) . ? C25 C26 1.420(5) . ? C25 C24 1.480(5) 3_656 ? C8 C9 1.402(5) . ? C8 H18 0.9500 . ? C24 C25 1.480(5) 3_656 ? C26 C27 1.365(5) . ? C26 H28 0.9500 . ? C2 C3 1.350(6) . ? C2 C1 1.400(5) . ? C2 H5A 0.9500 . ? C11 C12 1.362(5) . ? C11 H21 0.9500 . ? C15 C14 1.411(5) . ? C14 C13 1.367(5) . ? C14 H24 0.9500 . ? C20 C19 1.375(5) . ? C20 H12 0.9500 . ? C18 C19 1.368(6) . ? C18 C17 1.380(6) . ? C18 H14 0.9500 . ? C27 C28 1.392(6) . ? C27 H29 0.9500 . ? C19 H13 0.9500 . ? C12 C13 1.399(6) . ? C12 H22 0.9500 . ? C28 H30 0.9500 . ? C17 C16 1.400(5) . ? C17 H15 0.9500 . ? C5 C4 1.385(6) . ? C5 H2 0.9500 . ? C13 H23 0.9500 . ? C4 C3 1.379(6) . ? C4 H3 0.9500 . ? C3 H4 0.9500 . ? C32 H35A 0.9800 . ? C32 H35B 0.9800 . ? C32 H35C 0.9800 . ? C31 H36A 0.9800 . ? C31 H36B 0.9800 . ? C31 H36C 0.9800 . ? C35 H37A 0.9800 . ? C35 H37B 0.9800 . ? C35 H37C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? O15 C37 1.417(7) . ? O15 H14A 0.8400 . ? O14 C36 1.411(7) . ? O14 H15A 0.8400 . ? C37 H39A 0.9800 . ? C37 H39B 0.9800 . ? C37 H39C 0.9800 . ? C36 H38A 0.9800 . ? C36 H38B 0.9800 . ? C36 H38C 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 O2 Ni3 O9 169.27(14) . . ? O2 Ni3 O3 86.03(12) . . ? O9 Ni3 O3 83.54(12) . . ? O2 Ni3 O12 88.91(14) . . ? O9 Ni3 O12 101.16(13) . . ? O3 Ni3 O12 171.67(17) . . ? O2 Ni3 O8 103.76(14) . . ? O9 Ni3 O8 80.31(12) . . ? O3 Ni3 O8 98.56(13) . . ? O12 Ni3 O8 89.06(12) . . ? O2 Ni3 O11 91.27(14) . . ? O9 Ni3 O11 85.11(13) . . ? O3 Ni3 O11 83.52(12) . . ? O12 Ni3 O11 89.99(13) . . ? O8 Ni3 O11 164.92(16) . . ? O2 Co1 O12 90.75(19) . . ? O2 Co1 O9 166.4(2) . . ? O12 Co1 O9 102.33(19) . . ? O2 Co1 O3 84.86(17) . . ? O12 Co1 O3 172.1(2) . . ? O9 Co1 O3 81.69(16) . . ? O2 Co1 O8 104.1(2) . . ? O12 Co1 O8 90.53(17) . . ? O9 Co1 O8 79.87(16) . . ? O3 Co1 O8 96.94(18) . . ? O2 Co1 O11 91.43(18) . . ? O12 Co1 O11 91.35(18) . . ? O9 Co1 O11 84.51(17) . . ? O3 Co1 O11 82.18(16) . . ? O8 Co1 O11 164.3(2) . . ? O4 Ni1 O3 87.63(10) . . ? O4 Ni1 O6 94.63(11) . . ? O3 Ni1 O6 93.06(10) . . ? O4 Ni1 O7 92.83(10) . . ? O3 Ni1 O7 176.38(10) . . ? O6 Ni1 O7 90.49(9) . . ? O4 Ni1 O10 90.71(10) . . ? O3 Ni1 O10 93.14(9) . . ? O6 Ni1 O10 171.98(10) . . ? O7 Ni1 O10 83.26(9) . . ? O4 Ni1 O9 167.93(9) . . ? O3 Ni1 O9 82.59(9) . . ? O6 Ni1 O9 92.94(10) . . ? O7 Ni1 O9 96.50(9) . . ? O10 Ni1 O9 82.82(9) . . ? O8 Ni2 O7 90.15(9) . 3_656 ? O8 Ni2 O9 84.25(9) . . ? O7 Ni2 O9 171.59(9) 3_656 . ? O8 Ni2 O10 172.55(9) . 3_656 ? O7 Ni2 O10 83.36(9) 3_656 3_656 ? O9 Ni2 O10 101.78(9) . 3_656 ? O8 Ni2 O10 94.05(9) . . ? O7 Ni2 O10 90.06(9) 3_656 . ? O9 Ni2 O10 84.10(9) . . ? O10 Ni2 O10 82.33(9) 3_656 . ? O8 Ni2 O13 96.52(9) . . ? O7 Ni2 O13 87.57(10) 3_656 . ? O9 Ni2 O13 99.27(9) . . ? O10 Ni2 O13 86.90(9) 3_656 . ? O10 Ni2 O13 169.17(9) . . ? C31 O9 Ni3 120.3(2) . . ? C31 O9 Ni2 118.3(2) . . ? Ni3 O9 Ni2 99.32(12) . . ? C31 O9 Co1 119.2(2) . . ? Ni3 O9 Co1 1.46(14) . . ? Ni2 O9 Co1 99.27(15) . . ? C31 O9 Ni1 122.0(2) . . ? Ni3 O9 Ni1 95.96(10) . . ? Ni2 O9 Ni1 95.54(9) . . ? Co1 O9 Ni1 97.41(14) . . ? C32 O10 Ni1 117.7(2) . . ? C32 O10 Ni2 124.9(2) . 3_656 ? Ni1 O10 Ni2 95.73(9) . 3_656 ? C32 O10 Ni2 118.2(2) . . ? Ni1 O10 Ni2 96.94(10) . . ? Ni2 O10 Ni2 97.67(9) 3_656 . ? C9 O3 Ni1 127.7(2) . . ? C9 O3 Ni3 129.3(2) . . ? Ni1 O3 Ni3 97.92(12) . . ? C9 O3 Co1 128.9(2) . . ? Ni1 O3 Co1 98.31(15) . . ? Ni3 O3 Co1 0.41(18) . . ? C24 O7 Ni2 132.1(2) . 3_656 ? C24 O7 Ni1 130.5(2) . . ? Ni2 O7 Ni1 96.82(10) 3_656 . ? C30 O8 Ni2 127.0(2) . . ? C30 O8 Co1 135.9(2) . . ? Ni2 O8 Co1 96.55(14) . . ? C30 O8 Ni3 136.3(2) . . ? Ni2 O8 Ni3 95.93(11) . . ? Co1 O8 Ni3 1.48(14) . . ? C15 O4 Ni1 120.9(2) . . ? C22 O6 Ni1 123.6(2) . . ? C7 O2 Co1 130.4(3) . . ? C7 O2 Ni3 128.8(2) . . ? Co1 O2 Ni3 1.56(15) . . ? C35 O13 Ni2 121.7(2) . . ? C33 O11 Ni3 127.3(2) . . ? C33 O11 Co1 126.9(3) . . ? Ni3 O11 Co1 1.47(14) . . ? C34 O12 Co1 125.0(3) . . ? C34 O12 Ni3 124.9(3) . . ? Co1 O12 Ni3 0.29(19) . . ? C16 O5 H1 109.5 . . ? C11 C10 C15 117.4(3) . . ? C11 C10 C9 118.6(3) . . ? C15 C10 C9 123.9(3) . . ? C1 O1 H5 109.5 . . ? C28 C29 C30 123.2(4) . . ? C28 C29 H31 118.4 . . ? C30 C29 H31 118.4 . . ? O8 C30 C29 117.2(3) . . ? O8 C30 C25 125.2(3) . . ? C29 C30 C25 117.6(3) . . ? O2 C7 C8 124.9(3) . . ? O2 C7 C6 114.7(3) . . ? C8 C7 C6 120.3(3) . . ? C22 C23 C24 129.5(3) . . ? C22 C23 H9 115.2 . . ? C24 C23 H9 115.2 . . ? O6 C22 C23 127.0(3) . . ? O6 C22 C21 115.5(3) . . ? C23 C22 C21 117.4(3) . . ? C20 C21 C16 118.1(4) . . ? C20 C21 C22 121.3(4) . . ? C16 C21 C22 120.6(3) . . ? C5 C6 C1 117.6(4) . . ? C5 C6 C7 121.5(4) . . ? C1 C6 C7 120.9(3) . . ? C26 C25 C30 116.6(3) . . ? C26 C25 C24 117.7(3) . 3_656 ? C30 C25 C24 125.7(3) . 3_656 ? C7 C8 C9 126.8(4) . . ? C7 C8 H18 116.6 . . ? C9 C8 H18 116.6 . . ? O7 C24 C23 118.6(3) . . ? O7 C24 C25 119.6(3) . 3_656 ? C23 C24 C25 121.8(3) . 3_656 ? C27 C26 C25 123.8(4) . . ? C27 C26 H28 118.1 . . ? C25 C26 H28 118.1 . . ? C3 C2 C1 121.1(4) . . ? C3 C2 H5A 119.5 . . ? C1 C2 H5A 119.5 . . ? C12 C11 C10 122.8(4) . . ? C12 C11 H21 118.6 . . ? C10 C11 H21 118.6 . . ? O1 C1 C6 123.1(3) . . ? O1 C1 C2 116.9(4) . . ? C6 C1 C2 120.0(4) . . ? O4 C15 C14 118.8(3) . . ? O4 C15 C10 123.3(3) . . ? C14 C15 C10 118.0(3) . . ? C13 C14 C15 122.1(4) . . ? C13 C14 H24 119.0 . . ? C15 C14 H24 119.0 . . ? O3 C9 C8 120.2(3) . . ? O3 C9 C10 119.1(3) . . ? C8 C9 C10 120.7(3) . . ? C19 C20 C21 122.0(4) . . ? C19 C20 H12 119.0 . . ? C21 C20 H12 119.0 . . ? C19 C18 C17 121.1(4) . . ? C19 C18 H14 119.4 . . ? C17 C18 H14 119.4 . . ? C26 C27 C28 118.9(4) . . ? C26 C27 H29 120.6 . . ? C28 C27 H29 120.6 . . ? C18 C19 C20 119.1(4) . . ? C18 C19 H13 120.4 . . ? C20 C19 H13 120.4 . . ? C11 C12 C13 119.3(4) . . ? C11 C12 H22 120.4 . . ? C13 C12 H22 120.4 . . ? C29 C28 C27 119.8(4) . . ? C29 C28 H30 120.1 . . ? C27 C28 H30 120.1 . . ? C18 C17 C16 119.9(4) . . ? C18 C17 H15 120.1 . . ? C16 C17 H15 120.1 . . ? C4 C5 C6 121.5(4) . . ? C4 C5 H2 119.2 . . ? C6 C5 H2 119.2 . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H23 119.9 . . ? C12 C13 H23 119.9 . . ? O5 C16 C17 116.9(3) . . ? O5 C16 C21 123.4(3) . . ? C17 C16 C21 119.6(4) . . ? C3 C4 C5 119.5(4) . . ? C3 C4 H3 120.2 . . ? C5 C4 H3 120.2 . . ? C2 C3 C4 120.3(4) . . ? C2 C3 H4 119.9 . . ? C4 C3 H4 119.9 . . ? O10 C32 H35A 109.5 . . ? O10 C32 H35B 109.5 . . ? H35A C32 H35B 109.5 . . ? O10 C32 H35C 109.5 . . ? H35A C32 H35C 109.5 . . ? H35B C32 H35C 109.5 . . ? O9 C31 H36A 109.5 . . ? O9 C31 H36B 109.5 . . ? H36A C31 H36B 109.5 . . ? O9 C31 H36C 109.5 . . ? H36A C31 H36C 109.5 . . ? H36B C31 H36C 109.5 . . ? O13 C35 H37A 109.5 . . ? O13 C35 H37B 109.5 . . ? H37A C35 H37B 109.5 . . ? O13 C35 H37C 109.5 . . ? H37A C35 H37C 109.5 . . ? H37B C35 H37C 109.5 . . ? O12 C34 H34A 109.5 . . ? O12 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O12 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O11 C33 H33A 109.5 . . ? O11 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O11 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C37 O15 H14A 109.5 . . ? C36 O14 H15A 109.5 . . ? O15 C37 H39A 109.5 . . ? O15 C37 H39B 109.5 . . ? H39A C37 H39B 109.5 . . ? O15 C37 H39C 109.5 . . ? H39A C37 H39C 109.5 . . ? H39B C37 H39C 109.5 . . ? O14 C36 H38A 109.5 . . ? O14 C36 H38B 109.5 . . ? H38A C36 H38B 109.5 . . ? O14 C36 H38C 109.5 . . ? H38A C36 H38C 109.5 . . ? H38B C36 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.066 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.101 data_complex3 _database_code_depnum_ccdc_archive 'CCDC 924185' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H76 Co2 Ni4 O26, 4(C H4 O)' _chemical_formula_sum 'C74 H92 Co2 Ni4 O30' _chemical_formula_weight 1814.18 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' O O 0.0106 0.0060 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.4933(11) _cell_length_b 27.255(3) _cell_length_c 16.116(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.750(2) _cell_angle_gamma 90.00 _cell_volume 3717.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5190 _cell_measurement_theta_min 2.5018 _cell_measurement_theta_max 28.49 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 1.516 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5822 _exptl_absorpt_correction_T_max 0.8632 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20037 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_unetI/netI 0.0508 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6917 _reflns_number_gt 5412 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0794P)^2^+2.5672P] 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 6917 _refine_ls_number_parameters 507 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 Ni2 Ni 0.61631(6) 0.039778(17) 0.53540(3) 0.02308(16) Uani 1 1 d . . . Ni1 Ni 0.46318(6) 0.045733(18) 0.35590(3) 0.02581(16) Uani 1 1 d . . . Co1 Co 0.66569(7) 0.132494(19) 0.42897(3) 0.02673(17) Uani 1 1 d . . . O9 O 0.6855(3) 0.05855(10) 0.42163(16) 0.0246(6) Uani 1 1 d . . . O10 O 0.3958(3) 0.03483(9) 0.47290(16) 0.0230(6) Uani 1 1 d . . . O7 O 0.5216(3) 0.02865(10) 0.64474(16) 0.0260(6) Uani 1 1 d . . . O3 O 0.4466(3) 0.11939(10) 0.36365(17) 0.0281(7) Uani 1 1 d . . . O8 O 0.6037(3) 0.11213(9) 0.55255(16) 0.0256(6) Uani 1 1 d . . . O4 O 0.2381(4) 0.04574(10) 0.30957(18) 0.0314(7) Uani 1 1 d . . . O6 O 0.5537(4) 0.04853(10) 0.24421(17) 0.0293(7) Uani 1 1 d . . . O2 O 0.6034(4) 0.20390(10) 0.41768(18) 0.0329(7) Uani 1 1 d . . . O1 O 0.7546(4) 0.28280(11) 0.4396(2) 0.0449(8) Uani 1 1 d . . . H1 H 0.7381 0.2526 0.4444 0.067 Uiso 1 1 calc R . . C10 C 0.2468(5) 0.12737(15) 0.2509(3) 0.0290(9) Uani 1 1 d . . . O5 O 0.4823(4) 0.09419(12) 0.0998(2) 0.0449(9) Uani 1 1 d . . . H5 H 0.4734 0.0889 0.1506 0.067 Uiso 1 1 calc R . . C30 C 0.5495(5) 0.13522(15) 0.6165(3) 0.0275(9) Uani 1 1 d . . . C29 C 0.5490(5) 0.18707(15) 0.6144(3) 0.0330(10) Uani 1 1 d . . . H29 H 0.5861 0.2029 0.5673 0.040 Uiso 1 1 calc R . . C23 C 0.5668(6) -0.03861(15) 0.2238(3) 0.0327(10) Uani 1 1 d . . . H23 H 0.5917 -0.0621 0.1833 0.039 Uiso 1 1 calc R . . C22 C 0.5851(5) 0.00989(15) 0.2011(3) 0.0297(10) Uani 1 1 d . . . C7 C 0.4857(5) 0.22452(15) 0.3749(3) 0.0301(10) Uani 1 1 d . . . C6 C 0.4862(5) 0.27943(16) 0.3769(3) 0.0320(10) Uani 1 1 d . . . C11 C 0.1913(5) 0.15701(16) 0.1827(3) 0.0309(10) Uani 1 1 d . . . H11 H 0.2340 0.1890 0.1783 0.037 Uiso 1 1 calc R . . C8 C 0.3705(5) 0.19937(15) 0.3264(3) 0.0326(10) Uani 1 1 d . . . H8 H 0.2909 0.2186 0.2972 0.039 Uiso 1 1 calc R . . C21 C 0.6390(5) 0.01961(16) 0.1165(3) 0.0315(10) Uani 1 1 d . . . C18 C 0.7200(6) 0.03312(18) -0.0454(3) 0.0425(12) Uani 1 1 d . . . H18 H 0.7448 0.0370 -0.1014 0.051 Uiso 1 1 calc R . . C24 C 0.4833(5) 0.05829(15) 0.7021(3) 0.0275(9) Uani 1 1 d . . . C25 C 0.4938(5) 0.11199(15) 0.6883(3) 0.0280(9) Uani 1 1 d . . . C15 C 0.1862(5) 0.07832(16) 0.2540(3) 0.0311(10) Uani 1 1 d . . . C20 C 0.7403(6) -0.01228(17) 0.0807(3) 0.0380(11) Uani 1 1 d . . . H20 H 0.7821 -0.0395 0.1121 0.046 Uiso 1 1 calc R . . C1 C 0.6201(6) 0.30512(15) 0.4088(3) 0.0323(10) Uani 1 1 d . . . C2 C 0.6194(6) 0.35638(17) 0.4084(3) 0.0420(12) Uani 1 1 d . . . H2 H 0.7110 0.3737 0.4295 0.050 Uiso 1 1 calc R . . C26 C 0.4414(6) 0.14348(16) 0.7511(3) 0.0378(11) Uani 1 1 d . . . H26 H 0.4016 0.1288 0.7985 0.045 Uiso 1 1 calc R . . C14 C 0.0656(6) 0.06462(16) 0.1934(3) 0.0346(10) Uani 1 1 d . . . H14 H 0.0194 0.0330 0.1966 0.042 Uiso 1 1 calc R . . C31 C 0.8273(5) 0.03687(16) 0.3954(3) 0.0343(10) Uani 1 1 d . . . H31A H 0.8876 0.0617 0.3675 0.051 Uiso 1 1 calc R . . H31B H 0.7997 0.0099 0.3568 0.051 Uiso 1 1 calc R . . H31C H 0.8915 0.0242 0.4441 0.051 Uiso 1 1 calc R . . C9 C 0.3589(5) 0.14852(15) 0.3159(3) 0.0292(10) Uani 1 1 d . . . C17 C 0.6214(6) 0.06656(17) -0.0113(3) 0.0396(11) Uani 1 1 d . . . H17 H 0.5809 0.0937 -0.0434 0.047 Uiso 1 1 calc R . . C28 C 0.4981(6) 0.21540(16) 0.6763(3) 0.0380(11) Uani 1 1 d . . . H28 H 0.4986 0.2501 0.6714 0.046 Uiso 1 1 calc R . . C19 C 0.7824(6) -0.00561(18) 0.0005(3) 0.0415(12) Uani 1 1 d . . . H19 H 0.8538 -0.0276 -0.0226 0.050 Uiso 1 1 calc R . . C27 C 0.4451(6) 0.19338(16) 0.7471(3) 0.0432(12) Uani 1 1 d . . . H27 H 0.4124 0.2128 0.7915 0.052 Uiso 1 1 calc R . . C4 C 0.3567(7) 0.35724(18) 0.3470(3) 0.0481(13) Uani 1 1 d . . . H4 H 0.2663 0.3752 0.3258 0.058 Uiso 1 1 calc R . . C12 C 0.0792(6) 0.14168(17) 0.1229(3) 0.0372(11) Uani 1 1 d . . . H12 H 0.0471 0.1624 0.0771 0.045 Uiso 1 1 calc R . . C13 C 0.0122(6) 0.09538(17) 0.1295(3) 0.0377(11) Uani 1 1 d . . . H13 H -0.0703 0.0850 0.0900 0.045 Uiso 1 1 calc R . . C3 C 0.4900(6) 0.38159(18) 0.3782(3) 0.0455(13) Uani 1 1 d . . . H3 H 0.4915 0.4164 0.3786 0.055 Uiso 1 1 calc R . . C5 C 0.3540(6) 0.30648(17) 0.3464(3) 0.0429(12) Uani 1 1 d . . . H5A H 0.2611 0.2898 0.3250 0.051 Uiso 1 1 calc R . . C16 C 0.5815(5) 0.06043(16) 0.0703(3) 0.0328(10) Uani 1 1 d . . . O13 O 0.8418(3) 0.03015(10) 0.60058(17) 0.0288(7) Uani 1 1 d . . . O11 O 0.7484(4) 0.13210(11) 0.30329(19) 0.0388(8) Uani 1 1 d . . . O12 O 0.8869(4) 0.15394(11) 0.47819(19) 0.0363(7) Uani 1 1 d . . . C32 C 0.2731(5) 0.06554(14) 0.4993(3) 0.0288(10) Uani 1 1 d . . . H35A H 0.1727 0.0569 0.4683 0.043 Uiso 1 1 calc R . . H35B H 0.2983 0.0999 0.4887 0.043 Uiso 1 1 calc R . . H35C H 0.2641 0.0608 0.5590 0.043 Uiso 1 1 calc R . . C35 C 0.9185(6) 0.06896(17) 0.6476(3) 0.0435(12) Uani 1 1 d . . . H34A H 0.9499 0.0946 0.6096 0.065 Uiso 1 1 calc R . . H34B H 1.0124 0.0562 0.6798 0.065 Uiso 1 1 calc R . . H34C H 0.8458 0.0828 0.6855 0.065 Uiso 1 1 calc R . . C34 C 1.0141(6) 0.16899(18) 0.4313(3) 0.0448(12) Uani 1 1 d . . . H33A H 1.0285 0.1449 0.3875 0.067 Uiso 1 1 calc R . . H33B H 1.1114 0.1713 0.4683 0.067 Uiso 1 1 calc R . . H33C H 0.9897 0.2011 0.4060 0.067 Uiso 1 1 calc R . . C33 C 0.7531(7) 0.17279(19) 0.2487(3) 0.0525(14) Uani 1 1 d . . . H32A H 0.6454 0.1813 0.2270 0.079 Uiso 1 1 calc R . . H32B H 0.8159 0.1643 0.2024 0.079 Uiso 1 1 calc R . . H32C H 0.8014 0.2009 0.2791 0.079 Uiso 1 1 calc R . . O15 O -0.0649(5) 0.21083(18) 0.6101(3) 0.0758(14) Uani 1 1 d . . . H15 H -0.0927 0.1883 0.5763 0.114 Uiso 1 1 calc R . . O14 O 0.5346(7) 0.19887(18) 0.0760(3) 0.0836(14) Uani 1 1 d . . . H14A H 0.4707 0.1757 0.0656 0.125 Uiso 1 1 calc R . . C37 C 0.0685(9) 0.1956(3) 0.6613(4) 0.082(2) Uani 1 1 d . . . H37A H 0.1199 0.2243 0.6884 0.122 Uiso 1 1 calc R . . H37B H 0.1429 0.1790 0.6273 0.122 Uiso 1 1 calc R . . H37C H 0.0356 0.1729 0.7038 0.122 Uiso 1 1 calc R . . C36 C 0.6455(9) 0.2000(3) 0.0149(5) 0.087(2) Uani 1 1 d . . . H36A H 0.7021 0.2314 0.0181 0.131 Uiso 1 1 calc R . . H36B H 0.5899 0.1964 -0.0405 0.131 Uiso 1 1 calc R . . H36C H 0.7211 0.1731 0.0249 0.131 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 Ni2 0.0256(3) 0.0187(3) 0.0252(3) -0.0028(2) 0.0037(2) 0.0005(2) Ni1 0.0303(3) 0.0208(3) 0.0265(3) -0.0018(2) 0.0033(2) 0.0004(2) Co1 0.0306(4) 0.0198(3) 0.0301(3) -0.0007(2) 0.0042(2) -0.0011(2) O9 0.0235(16) 0.0247(15) 0.0265(15) -0.0016(12) 0.0072(12) 0.0010(11) O10 0.0246(16) 0.0203(14) 0.0243(14) -0.0039(11) 0.0023(12) 0.0031(11) O7 0.0317(17) 0.0202(14) 0.0265(15) -0.0039(12) 0.0047(13) 0.0007(12) O3 0.0314(18) 0.0219(15) 0.0306(15) -0.0008(12) -0.0004(13) -0.0012(12) O8 0.0320(17) 0.0189(14) 0.0263(14) -0.0048(11) 0.0053(12) -0.0008(12) O4 0.0346(18) 0.0275(16) 0.0314(16) 0.0005(12) -0.0010(13) -0.0018(13) O6 0.0375(19) 0.0229(15) 0.0281(15) -0.0018(12) 0.0064(13) -0.0010(12) O2 0.0399(19) 0.0242(16) 0.0342(16) -0.0006(13) 0.0005(14) -0.0006(13) O1 0.045(2) 0.0280(17) 0.061(2) 0.0047(16) -0.0052(17) -0.0022(14) C10 0.027(2) 0.034(2) 0.026(2) -0.0020(18) 0.0031(18) 0.0028(18) O5 0.060(2) 0.0400(19) 0.0364(18) 0.0047(15) 0.0157(17) 0.0124(16) C30 0.023(2) 0.027(2) 0.032(2) -0.0021(18) -0.0008(18) -0.0007(17) C29 0.037(3) 0.026(2) 0.038(2) -0.0016(19) 0.013(2) -0.0015(19) C23 0.042(3) 0.027(2) 0.029(2) -0.0057(18) 0.010(2) 0.0016(19) C22 0.030(3) 0.031(2) 0.028(2) -0.0053(18) 0.0044(19) -0.0032(18) C7 0.035(3) 0.026(2) 0.030(2) 0.0014(18) 0.009(2) 0.0033(18) C6 0.038(3) 0.027(2) 0.032(2) 0.0013(18) 0.010(2) 0.0001(19) C11 0.035(3) 0.027(2) 0.031(2) -0.0002(18) 0.006(2) 0.0046(19) C8 0.036(3) 0.028(2) 0.033(2) 0.0031(19) 0.003(2) 0.0037(19) C21 0.033(3) 0.030(2) 0.032(2) -0.0050(19) 0.004(2) -0.0050(19) C18 0.050(3) 0.048(3) 0.031(2) -0.008(2) 0.012(2) -0.010(2) C24 0.026(2) 0.029(2) 0.027(2) -0.0065(18) -0.0007(18) 0.0005(17) C25 0.028(2) 0.025(2) 0.031(2) -0.0064(18) 0.0012(18) 0.0016(17) C15 0.029(3) 0.032(2) 0.033(2) -0.0009(19) 0.006(2) 0.0044(18) C20 0.042(3) 0.032(3) 0.041(3) -0.003(2) 0.012(2) -0.004(2) C1 0.041(3) 0.028(2) 0.029(2) 0.0023(18) 0.008(2) 0.000(2) C2 0.049(3) 0.029(3) 0.048(3) 0.002(2) 0.004(2) -0.006(2) C26 0.049(3) 0.030(2) 0.037(3) -0.004(2) 0.014(2) -0.001(2) C14 0.037(3) 0.030(2) 0.037(3) -0.007(2) 0.002(2) 0.0027(19) C31 0.036(3) 0.032(2) 0.035(2) -0.0012(19) 0.007(2) 0.002(2) C9 0.031(3) 0.027(2) 0.031(2) 0.0000(18) 0.0105(19) 0.0035(18) C17 0.048(3) 0.038(3) 0.033(2) 0.001(2) 0.003(2) -0.003(2) C28 0.048(3) 0.019(2) 0.048(3) -0.005(2) 0.013(2) -0.0039(19) C19 0.047(3) 0.038(3) 0.042(3) -0.011(2) 0.016(2) -0.005(2) C27 0.060(3) 0.024(2) 0.048(3) -0.012(2) 0.022(3) -0.001(2) C4 0.047(3) 0.033(3) 0.064(3) -0.004(2) -0.001(3) 0.004(2) C12 0.044(3) 0.036(3) 0.032(2) 0.001(2) 0.003(2) 0.010(2) C13 0.040(3) 0.042(3) 0.030(2) -0.008(2) -0.001(2) 0.005(2) C3 0.052(3) 0.027(2) 0.059(3) -0.001(2) 0.012(3) -0.001(2) C5 0.042(3) 0.031(3) 0.056(3) -0.002(2) 0.001(2) 0.004(2) C16 0.033(3) 0.034(3) 0.032(2) -0.0045(19) 0.003(2) -0.0043(19) O13 0.0275(17) 0.0257(15) 0.0328(16) -0.0071(12) -0.0009(13) -0.0012(12) O11 0.049(2) 0.0323(18) 0.0360(17) 0.0050(14) 0.0109(15) -0.0041(14) O12 0.0314(18) 0.0356(18) 0.0425(18) -0.0029(14) 0.0069(14) -0.0071(13) C32 0.032(3) 0.020(2) 0.036(2) -0.0040(17) 0.0062(19) 0.0054(17) C35 0.038(3) 0.036(3) 0.055(3) -0.006(2) -0.008(2) 0.000(2) C34 0.036(3) 0.044(3) 0.055(3) -0.002(2) 0.006(2) 0.002(2) C33 0.073(4) 0.044(3) 0.044(3) 0.009(2) 0.026(3) 0.004(3) O15 0.052(3) 0.103(4) 0.073(3) -0.041(3) 0.013(2) -0.025(2) O14 0.106(4) 0.073(3) 0.074(3) 0.001(2) 0.022(3) -0.014(3) C37 0.093(6) 0.095(5) 0.056(4) -0.010(4) 0.000(4) -0.037(4) C36 0.093(6) 0.069(5) 0.100(6) 0.012(4) 0.012(5) 0.013(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ni2 O8 1.995(3) . ? Ni2 O7 2.020(3) . ? Ni2 O9 2.037(3) . ? Ni2 O10 2.040(3) 3_656 ? Ni2 O10 2.057(3) . ? Ni2 O13 2.123(3) . ? Ni1 O4 1.994(3) . ? Ni1 O6 2.016(3) . ? Ni1 O3 2.017(3) . ? Ni1 O7 2.032(3) 3_656 ? Ni1 O10 2.037(3) . ? Ni1 O9 2.116(3) . ? Co1 O2 2.021(3) . ? Co1 O9 2.027(3) . ? Co1 O12 2.063(3) . ? Co1 O3 2.091(3) . ? Co1 O8 2.174(3) . ? Co1 O11 2.198(3) . ? O9 C31 1.436(5) . ? O10 C32 1.428(5) . ? O10 Ni2 2.040(3) 3_656 ? O7 C24 1.289(5) . ? O7 Ni1 2.032(3) 3_656 ? O3 C9 1.297(5) . ? O8 C30 1.322(5) . ? O4 C15 1.312(5) . ? O6 C22 1.302(5) . ? O2 C7 1.295(5) . ? O1 C1 1.351(5) . ? O1 H1 0.8400 . ? C10 C11 1.413(6) . ? C10 C15 1.435(6) . ? C10 C9 1.473(6) . ? O5 C16 1.360(5) . ? O5 H5 0.8400 . ? C30 C29 1.414(6) . ? C30 C25 1.434(6) . ? C29 C28 1.360(6) . ? C29 H29 0.9500 . ? C23 C22 1.384(6) . ? C23 C24 1.407(6) 3_656 ? C23 H23 0.9500 . ? C22 C21 1.496(6) . ? C7 C8 1.382(6) . ? C7 C6 1.497(6) . ? C6 C1 1.397(6) . ? C6 C5 1.398(6) . ? C11 C12 1.363(6) . ? C11 H11 0.9500 . ? C8 C9 1.399(6) . ? C8 H8 0.9500 . ? C21 C20 1.382(6) . ? C21 C16 1.404(6) . ? C18 C19 1.370(7) . ? C18 C17 1.381(7) . ? C18 H18 0.9500 . ? C24 C23 1.407(6) 3_656 ? C24 C25 1.484(6) . ? C25 C26 1.425(6) . ? C15 C14 1.406(6) . ? C20 C19 1.382(6) . ? C20 H20 0.9500 . ? C1 C2 1.397(6) . ? C2 C3 1.352(7) . ? C2 H2 0.9500 . ? C26 C27 1.362(6) . ? C26 H26 0.9500 . ? C14 C13 1.374(6) . ? C14 H14 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C17 C16 1.395(6) . ? C17 H17 0.9500 . ? C28 C27 1.396(6) . ? C28 H28 0.9500 . ? C19 H19 0.9500 . ? C27 H27 0.9500 . ? C4 C3 1.372(7) . ? C4 C5 1.384(7) . ? C4 H4 0.9500 . ? C12 C13 1.392(6) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C3 H3 0.9500 . ? C5 H5A 0.9500 . ? O13 C35 1.426(5) . ? O11 C33 1.418(5) . ? O12 C34 1.429(6) . ? C32 H35A 0.9800 . ? C32 H35B 0.9800 . ? C32 H35C 0.9800 . ? C35 H34A 0.9800 . ? C35 H34B 0.9800 . ? C35 H34C 0.9800 . ? C34 H33A 0.9800 . ? C34 H33B 0.9800 . ? C34 H33C 0.9800 . ? C33 H32A 0.9800 . ? C33 H32B 0.9800 . ? C33 H32C 0.9800 . ? O15 C37 1.408(8) . ? O15 H15 0.8400 . ? O14 C36 1.418(8) . ? O14 H14A 0.8400 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 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 O8 Ni2 O7 89.87(11) . . ? O8 Ni2 O9 84.22(11) . . ? O7 Ni2 O9 171.40(11) . . ? O8 Ni2 O10 172.42(11) . 3_656 ? O7 Ni2 O10 83.46(10) . 3_656 ? O9 Ni2 O10 102.01(11) . 3_656 ? O8 Ni2 O10 94.33(11) . . ? O7 Ni2 O10 90.29(11) . . ? O9 Ni2 O10 83.95(11) . . ? O10 Ni2 O10 82.16(11) 3_656 . ? O8 Ni2 O13 96.33(11) . . ? O7 Ni2 O13 87.59(11) . . ? O9 Ni2 O13 99.25(11) . . ? O10 Ni2 O13 87.00(11) 3_656 . ? O10 Ni2 O13 169.12(11) . . ? O4 Ni1 O6 95.18(12) . . ? O4 Ni1 O3 87.34(11) . . ? O6 Ni1 O3 92.94(11) . . ? O4 Ni1 O7 93.30(11) . 3_656 ? O6 Ni1 O7 90.23(11) . 3_656 ? O3 Ni1 O7 176.70(11) . 3_656 ? O4 Ni1 O10 90.70(12) . . ? O6 Ni1 O10 171.45(11) . . ? O3 Ni1 O10 93.53(11) . . ? O7 Ni1 O10 83.23(10) 3_656 . ? O4 Ni1 O9 167.30(11) . . ? O6 Ni1 O9 92.88(11) . . ? O3 Ni1 O9 82.45(11) . . ? O7 Ni1 O9 96.47(11) 3_656 . ? O10 Ni1 O9 82.44(11) . . ? O2 Co1 O9 167.10(12) . . ? O2 Co1 O12 89.14(12) . . ? O9 Co1 O12 103.11(12) . . ? O2 Co1 O3 84.49(12) . . ? O9 Co1 O3 82.85(11) . . ? O12 Co1 O3 170.46(12) . . ? O2 Co1 O8 104.30(11) . . ? O9 Co1 O8 80.05(10) . . ? O12 Co1 O8 90.13(11) . . ? O3 Co1 O8 98.31(11) . . ? O2 Co1 O11 91.31(12) . . ? O9 Co1 O11 84.66(11) . . ? O12 Co1 O11 90.30(12) . . ? O3 Co1 O11 82.77(12) . . ? O8 Co1 O11 164.39(11) . . ? C31 O9 Co1 120.1(2) . . ? C31 O9 Ni2 118.2(2) . . ? Co1 O9 Ni2 99.53(11) . . ? C31 O9 Ni1 121.4(2) . . ? Co1 O9 Ni1 96.79(11) . . ? Ni2 O9 Ni1 95.56(11) . . ? C32 O10 Ni1 117.2(2) . . ? C32 O10 Ni2 124.7(2) . 3_656 ? Ni1 O10 Ni2 95.81(10) . 3_656 ? C32 O10 Ni2 118.2(2) . . ? Ni1 O10 Ni2 97.43(12) . . ? Ni2 O10 Ni2 97.84(11) 3_656 . ? C24 O7 Ni2 132.4(3) . . ? C24 O7 Ni1 130.5(3) . 3_656 ? Ni2 O7 Ni1 96.62(11) . 3_656 ? C9 O3 Ni1 127.7(3) . . ? C9 O3 Co1 129.6(3) . . ? Ni1 O3 Co1 97.91(12) . . ? C30 O8 Ni2 127.2(3) . . ? C30 O8 Co1 136.0(2) . . ? Ni2 O8 Co1 96.06(11) . . ? C15 O4 Ni1 120.9(3) . . ? C22 O6 Ni1 123.8(3) . . ? C7 O2 Co1 130.6(3) . . ? C1 O1 H1 109.5 . . ? C11 C10 C15 117.5(4) . . ? C11 C10 C9 118.9(4) . . ? C15 C10 C9 123.6(4) . . ? C16 O5 H5 109.5 . . ? O8 C30 C29 117.2(4) . . ? O8 C30 C25 125.3(4) . . ? C29 C30 C25 117.4(4) . . ? C28 C29 C30 123.4(4) . . ? C28 C29 H29 118.3 . . ? C30 C29 H29 118.3 . . ? C22 C23 C24 129.6(4) . 3_656 ? C22 C23 H23 115.2 . . ? C24 C23 H23 115.2 3_656 . ? O6 C22 C23 126.8(4) . . ? O6 C22 C21 115.8(4) . . ? C23 C22 C21 117.4(4) . . ? O2 C7 C8 124.4(4) . . ? O2 C7 C6 114.9(4) . . ? C8 C7 C6 120.6(4) . . ? C1 C6 C5 118.1(4) . . ? C1 C6 C7 120.7(4) . . ? C5 C6 C7 121.2(4) . . ? C12 C11 C10 122.9(4) . . ? C12 C11 H11 118.5 . . ? C10 C11 H11 118.5 . . ? C7 C8 C9 126.9(4) . . ? C7 C8 H8 116.6 . . ? C9 C8 H8 116.6 . . ? C20 C21 C16 118.5(4) . . ? C20 C21 C22 121.1(4) . . ? C16 C21 C22 120.3(4) . . ? C19 C18 C17 121.0(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? O7 C24 C23 118.8(4) . 3_656 ? O7 C24 C25 119.3(4) . . ? C23 C24 C25 121.9(4) 3_656 . ? C26 C25 C30 116.7(4) . . ? C26 C25 C24 117.5(4) . . ? C30 C25 C24 125.8(4) . . ? O4 C15 C14 118.6(4) . . ? O4 C15 C10 123.6(4) . . ? C14 C15 C10 117.8(4) . . ? C19 C20 C21 121.7(5) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? O1 C1 C6 123.2(4) . . ? O1 C1 C2 117.1(4) . . ? C6 C1 C2 119.7(4) . . ? C3 C2 C1 120.9(5) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C27 C26 C25 123.9(4) . . ? C27 C26 H26 118.0 . . ? C25 C26 H26 118.0 . . ? C13 C14 C15 122.3(4) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? O9 C31 H31A 109.5 . . ? O9 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O9 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O3 C9 C8 120.2(4) . . ? O3 C9 C10 119.2(4) . . ? C8 C9 C10 120.6(4) . . ? C18 C17 C16 119.8(5) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C29 C28 C27 119.9(4) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C18 C19 C20 119.2(5) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C26 C27 C28 118.5(4) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? C3 C4 C5 119.9(5) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C11 C12 C13 119.3(4) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C14 C13 C12 119.9(4) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C2 C3 C4 120.5(5) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C4 C5 C6 120.8(5) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? O5 C16 C17 117.0(4) . . ? O5 C16 C21 123.3(4) . . ? C17 C16 C21 119.6(4) . . ? C35 O13 Ni2 121.6(3) . . ? C33 O11 Co1 126.5(3) . . ? C34 O12 Co1 125.6(3) . . ? O10 C32 H35A 109.5 . . ? O10 C32 H35B 109.5 . . ? H35A C32 H35B 109.5 . . ? O10 C32 H35C 109.5 . . ? H35A C32 H35C 109.5 . . ? H35B C32 H35C 109.5 . . ? O13 C35 H34A 109.5 . . ? O13 C35 H34B 109.5 . . ? H34A C35 H34B 109.5 . . ? O13 C35 H34C 109.5 . . ? H34A C35 H34C 109.5 . . ? H34B C35 H34C 109.5 . . ? O12 C34 H33A 109.5 . . ? O12 C34 H33B 109.5 . . ? H33A C34 H33B 109.5 . . ? O12 C34 H33C 109.5 . . ? H33A C34 H33C 109.5 . . ? H33B C34 H33C 109.5 . . ? O11 C33 H32A 109.5 . . ? O11 C33 H32B 109.5 . . ? H32A C33 H32B 109.5 . . ? O11 C33 H32C 109.5 . . ? H32A C33 H32C 109.5 . . ? H32B C33 H32C 109.5 . . ? C37 O15 H15 109.5 . . ? C36 O14 H14A 109.5 . . ? O15 C37 H37A 109.5 . . ? O15 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O15 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O14 C36 H36A 109.5 . . ? O14 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O14 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.478 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.123