Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Richard Winpenny' 'Guillem Aromi' 'Andrei S. Batsanov' 'Paul Christian' 'Madeleine Helliwell' ; O.Roubeau ; 'Grigore A. Timco' _publ_contact_author_name 'Prof Richard Winpenny' _publ_contact_author_address ; Department of Chemistry University of Manchester Oxford Road Manchester M13 9PL UNITED KINGDOM ; _publ_contact_author_email RICHARD.WINPENNY@MAN.AC.UK _publ_section_title ; Synthesis, Structure and Magnetic Properties of Hydroxyquinaladine Bridged Cobalt and Nickel Heterocubanes ; data_02asb011 _database_code_CSD 216670 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H68 N4 O12 Co4,0.5(C3 H6 O)' _chemical_formula_sum 'C61.5 H71 Co4 N4 O12.5' _chemical_formula_weight 1301.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 15.798(5) _cell_length_b 13.933(4) _cell_length_c 27.648(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.19(1) _cell_angle_gamma 90.00 _cell_volume 6008(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 972 _cell_measurement_theta_min 10.06 _cell_measurement_theta_max 23.62 _exptl_crystal_description shapeless _exptl_crystal_colour red _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 1.150 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5147 _exptl_absorpt_correction_T_max 0.6690 _exptl_absorpt_process_details 'SADABS v.2.03 (Bruker,2001), R(int)=0.132 before correction' _exptl_special_details ;The data collection nominally covered full sphere of reciprocal space, by a combination of 5 sets of \w scans; each set at different \f and/or 2\q angles and each scan (10 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(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 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 72017 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 29.00 _reflns_number_total 15916 _reflns_number_gt 12671 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.060 (Bruker, 1999)' _computing_cell_refinement 'SMART version 5.060 (Bruker, 1999)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 1997)' _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. Methyl groups refined as rotating bodies with optimised C---H distance and refined U (common for three H atoms). Other H atoms - riding. ; _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^)+(0.0191P)^2^+8.2604P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15916 _refine_ls_number_parameters 789 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.003 _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 0.359158(18) 0.35051(2) 0.400406(10) 0.01559(6) Uani 1 1 d . . . Co2 Co 0.191213(18) 0.35270(2) 0.323633(10) 0.01634(6) Uani 1 1 d . . . Co3 Co 0.179979(19) 0.23556(2) 0.417456(11) 0.01864(7) Uani 1 1 d . . . Co4 Co 0.306606(19) 0.15220(2) 0.354042(11) 0.01927(7) Uani 1 1 d . . . O1 O 0.22860(9) 0.37545(10) 0.40024(5) 0.0171(3) Uani 1 1 d . . . O2 O 0.17721(9) 0.20815(11) 0.34019(5) 0.0193(3) Uani 1 1 d . . . O3 O 0.31180(9) 0.21475(10) 0.42489(5) 0.0171(3) Uani 1 1 d . . . O4 O 0.32039(9) 0.29234(11) 0.32824(5) 0.0173(3) Uani 1 1 d . . . O5 O 0.35837(10) 0.48731(11) 0.36920(5) 0.0195(3) Uani 1 1 d . . . O6 O 0.23565(10) 0.48509(11) 0.31442(5) 0.0202(3) Uani 1 1 d . . . O7 O 0.06264(10) 0.36808(11) 0.33314(6) 0.0219(3) Uani 1 1 d . . . O8 O 0.05823(10) 0.27905(12) 0.40099(6) 0.0251(3) Uani 1 1 d . . . O9 O 0.17284(11) 0.08927(12) 0.42792(6) 0.0273(4) Uani 1 1 d . . . O10 O 0.26997(11) 0.03026(12) 0.38407(6) 0.0284(4) Uani 1 1 d . . . O11 O 0.43937(10) 0.14786(11) 0.36707(6) 0.0216(3) Uani 1 1 d . . . O12 O 0.47601(9) 0.29552(11) 0.39675(5) 0.0197(3) Uani 1 1 d . . . N1 N 0.36140(12) 0.41202(13) 0.47192(6) 0.0205(4) Uani 1 1 d . . . N2 N 0.14318(12) 0.29757(13) 0.25212(7) 0.0198(4) Uani 1 1 d . . . N3 N 0.21633(12) 0.25126(14) 0.49537(7) 0.0225(4) Uani 1 1 d . . . N4 N 0.32005(12) 0.12386(14) 0.27960(7) 0.0244(4) Uani 1 1 d . . . C1 C 0.30077(14) 0.52663(15) 0.33837(7) 0.0184(4) Uani 1 1 d . . . C2 C 0.31050(15) 0.63344(15) 0.32658(8) 0.0219(4) Uani 1 1 d . . . C3 C 0.37914(17) 0.68091(18) 0.36428(10) 0.0313(5) Uani 1 1 d . . . H3A H 0.3621(7) 0.6774(12) 0.3967(6) 0.047(5) Uiso 1 1 d R . . H3B H 0.3855(9) 0.7481(12) 0.3554(4) 0.047(5) Uiso 1 1 d R . . H3C H 0.4337(10) 0.6476(10) 0.3648(5) 0.047(5) Uiso 1 1 d R . . C4 C 0.3366(2) 0.6395(2) 0.27548(10) 0.0385(7) Uani 1 1 d . . . H4A H 0.2920(10) 0.6102(14) 0.2516(5) 0.050(6) Uiso 1 1 d R . . H4B H 0.3906(12) 0.6057(14) 0.2754(2) 0.050(6) Uiso 1 1 d R . . H4C H 0.3434(13) 0.7067(12) 0.2669(4) 0.050(6) Uiso 1 1 d R . . C5 C 0.22417(17) 0.68410(18) 0.32649(11) 0.0330(6) Uani 1 1 d . . . H5A H 0.1817(8) 0.6576(10) 0.3006(6) 0.040(5) Uiso 1 1 d R . . H5B H 0.2307(3) 0.7524(12) 0.3209(7) 0.040(5) Uiso 1 1 d R . . H5C H 0.2053(7) 0.6744(11) 0.3580(6) 0.040(5) Uiso 1 1 d R . . C6 C 0.02348(14) 0.32273(16) 0.36264(8) 0.0224(4) Uani 1 1 d . . . C7 C -0.07525(15) 0.3229(2) 0.35215(10) 0.0310(5) Uani 1 1 d . . . C8 C -0.11195(18) 0.2510(3) 0.38499(13) 0.0503(9) Uani 1 1 d . . . H8A H -0.0929(12) 0.2686(10) 0.4201(7) 0.064(6) Uiso 1 1 d R . . H8B H -0.0912(12) 0.1851(13) 0.3789(6) 0.064(6) Uiso 1 1 d R . . H8C H -0.1760(12) 0.2525(12) 0.3776(6) 0.064(6) Uiso 1 1 d R . . C9 C -0.1062(2) 0.4236(2) 0.36184(13) 0.0497(8) Uani 1 1 d . . . H9A H -0.0851(12) 0.4416(7) 0.3959(7) 0.053(6) Uiso 1 1 d R . . H9B H -0.1691(11) 0.4250(4) 0.3560(7) 0.053(6) Uiso 1 1 d R . . H9C H -0.0843(12) 0.4691(9) 0.3398(7) 0.053(6) Uiso 1 1 d R . . C10 C -0.10377(18) 0.2960(3) 0.29795(12) 0.0466(8) Uani 1 1 d . . . H10A H -0.1672(11) 0.2929(14) 0.2908(3) 0.051(6) Uiso 1 1 d R . . H10B H -0.0795(11) 0.2327(13) 0.2915(2) 0.051(6) Uiso 1 1 d R . . H10C H -0.0829(12) 0.3450(11) 0.2767(4) 0.051(6) Uiso 1 1 d R . . C11 C 0.50047(16) 0.35633(19) 0.51324(9) 0.0298(5) Uani 1 1 d . . . H11A H 0.5079(6) 0.3384(11) 0.4801(5) 0.037(5) Uiso 1 1 d R . . H11B H 0.4956(5) 0.2984(11) 0.5324(6) 0.037(5) Uiso 1 1 d R . . H11C H 0.5503(8) 0.3930(8) 0.5284(6) 0.037(5) Uiso 1 1 d R . . C12 C 0.42121(16) 0.41563(17) 0.51150(8) 0.0245(5) Uani 1 1 d . . . C13 C 0.4111(2) 0.4745(2) 0.55226(9) 0.0379(6) Uani 1 1 d . . . H13 H 0.4540 0.4744 0.5806 0.045 Uiso 1 1 d R . . C14 C 0.3405(2) 0.5308(2) 0.55061(10) 0.0412(7) Uani 1 1 d . . . H14 H 0.3347 0.5710 0.5777 0.049 Uiso 1 1 d R . . C15 C 0.1997(2) 0.5868(2) 0.50300(12) 0.0452(8) Uani 1 1 d . . . H15 H 0.1914 0.6311 0.5279 0.054 Uiso 1 1 d R . . C16 C 0.13927(19) 0.5773(2) 0.46164(12) 0.0414(7) Uani 1 1 d . . . H16 H 0.0913 0.6194 0.4569 0.050 Uiso 1 1 d R . . C17 C 0.14726(16) 0.50715(18) 0.42583(10) 0.0289(5) Uani 1 1 d . . . H17 H 0.1032 0.4998 0.3983 0.035 Uiso 1 1 d R . . C18 C 0.21913(15) 0.44880(16) 0.43083(8) 0.0214(4) Uani 1 1 d . . . C19 C 0.28675(15) 0.46430(16) 0.47103(8) 0.0232(5) Uani 1 1 d . . . C20 C 0.27471(19) 0.52920(19) 0.50867(10) 0.0340(6) Uani 1 1 d . . . C21 C 0.18039(17) 0.43006(19) 0.20210(9) 0.0295(5) Uani 1 1 d . . . H21A H 0.1736(12) 0.4738(11) 0.2262(7) 0.061(6) Uiso 1 1 d R . . H21B H 0.1607(10) 0.4568(10) 0.1719(7) 0.061(6) Uiso 1 1 d R . . H21C H 0.2378(12) 0.4161(4) 0.2041(8) 0.061(6) Uiso 1 1 d R . . C22 C 0.13108(15) 0.34042(17) 0.20861(8) 0.0235(5) Uani 1 1 d . . . C23 C 0.07339(16) 0.3015(2) 0.16844(9) 0.0297(5) Uani 1 1 d . . . H23 H 0.0652 0.3332 0.1376 0.036 Uiso 1 1 d R . . C24 C 0.03024(16) 0.2185(2) 0.17413(9) 0.0304(5) Uani 1 1 d . . . H24 H -0.0093 0.1939 0.1475 0.037 Uiso 1 1 d R . . C25 C 0.00394(16) 0.08122(19) 0.22806(10) 0.0312(5) Uani 1 1 d . . . H25 H -0.0349 0.0516 0.2027 0.037 Uiso 1 1 d R . . C26 C 0.02090(16) 0.03937(19) 0.27307(10) 0.0328(6) Uani 1 1 d . . . H26 H -0.0059 -0.0197 0.2786 0.039 Uiso 1 1 d R . . C27 C 0.07770(15) 0.08185(17) 0.31201(9) 0.0275(5) Uani 1 1 d . . . H27 H 0.0873 0.0518 0.3432 0.033 Uiso 1 1 d R . . C28 C 0.11956(14) 0.16643(16) 0.30490(8) 0.0209(4) Uani 1 1 d . . . C29 C 0.10242(14) 0.21214(16) 0.25792(8) 0.0206(4) Uani 1 1 d . . . C30 C 0.04414(14) 0.16902(18) 0.21936(9) 0.0254(5) Uani 1 1 d . . . C31 C 0.09031(18) 0.3329(2) 0.51605(10) 0.0397(7) Uani 1 1 d . . . H31A H 0.0673(10) 0.3175(15) 0.4842(8) 0.076(8) Uiso 1 1 d R . . H31B H 0.0990(4) 0.3984(14) 0.5185(9) 0.076(8) Uiso 1 1 d R . . H31C H 0.0525(10) 0.3146(14) 0.5367(7) 0.076(8) Uiso 1 1 d R . . C32 C 0.17402(16) 0.28153(19) 0.53029(9) 0.0291(5) Uani 1 1 d . . . C33 C 0.20582(18) 0.2649(2) 0.58057(10) 0.0375(6) Uani 1 1 d . . . H33 H 0.1755 0.2894 0.6049 0.045 Uiso 1 1 d R . . C34 C 0.27901(18) 0.2134(2) 0.59416(9) 0.0358(6) Uani 1 1 d . . . H34 H 0.2984 0.1998 0.6278 0.043 Uiso 1 1 d R . . C35 C 0.40288(17) 0.12593(18) 0.56808(9) 0.0301(5) Uani 1 1 d . . . H35 H 0.4251 0.1085 0.6009 0.036 Uiso 1 1 d R . . C36 C 0.44453(17) 0.09850(17) 0.53061(9) 0.0285(5) Uani 1 1 d . . . H36 H 0.4948 0.0603 0.5376 0.034 Uiso 1 1 d R . . C37 C 0.41473(15) 0.12607(16) 0.48150(8) 0.0235(5) Uani 1 1 d . . . H37 H 0.4454 0.1070 0.4562 0.028 Uiso 1 1 d R . . C38 C 0.34115(14) 0.18060(15) 0.47028(8) 0.0186(4) Uani 1 1 d . . . C39 C 0.29366(14) 0.20482(16) 0.50851(8) 0.0208(4) Uani 1 1 d . . . C40 C 0.32632(16) 0.18011(18) 0.55772(8) 0.0262(5) Uani 1 1 d . . . C41 C 0.31620(17) 0.04133(19) 0.25541(10) 0.0325(6) Uani 1 1 d . . . C42 C 0.2767(2) -0.0434(2) 0.27587(13) 0.0486(8) Uani 1 1 d . . . H42A H 0.2957(16) -0.0473(13) 0.3084(8) 0.095(9) Uiso 1 1 d R . . H42B H 0.2904(16) -0.0979(13) 0.2612(9) 0.095(9) Uiso 1 1 d R . . H42C H 0.2191(14) -0.0368(11) 0.2708(10) 0.095(9) Uiso 1 1 d R . . C43 C 0.3501(2) 0.0332(2) 0.21071(11) 0.0449(7) Uani 1 1 d . . . H43 H 0.3445 -0.0257 0.1932 0.054 Uiso 1 1 d R . . C44 C 0.3895(2) 0.1086(2) 0.19293(10) 0.0425(7) Uani 1 1 d . . . H44 H 0.4131 0.1017 0.1636 0.051 Uiso 1 1 d R . . C45 C 0.43867(17) 0.2794(2) 0.20346(9) 0.0327(6) Uani 1 1 d . . . H45 H 0.4647 0.2766 0.1748 0.039 Uiso 1 1 d R . . C46 C 0.44248(16) 0.36200(19) 0.23041(9) 0.0292(5) Uani 1 1 d . . . H46 H 0.4720 0.4162 0.2206 0.035 Uiso 1 1 d R . . C47 C 0.40323(15) 0.36753(17) 0.27313(8) 0.0229(4) Uani 1 1 d . . . H47 H 0.4062 0.4258 0.2912 0.027 Uiso 1 1 d R . . C48 C 0.36029(14) 0.29052(16) 0.28861(7) 0.0191(4) Uani 1 1 d . . . C49 C 0.35813(14) 0.20231(17) 0.26155(8) 0.0226(4) Uani 1 1 d . . . C50 C 0.39599(16) 0.1978(2) 0.21833(9) 0.0295(5) Uani 1 1 d . . . C51 C 0.22079(17) 0.02355(17) 0.41586(9) 0.0286(5) Uani 1 1 d . . . C52 C 0.2150(2) -0.07439(18) 0.44075(10) 0.0395(7) Uani 1 1 d . . . C53 C 0.2044(3) -0.0591(2) 0.49418(12) 0.0616(11) Uani 1 1 d . . . H53A H 0.2541(12) -0.0262(16) 0.5112(4) 0.068(7) Uiso 1 1 d R . . H53B H 0.1985(15) -0.1203(12) 0.5095(4) 0.068(7) Uiso 1 1 d R . . H53C H 0.1539(13) -0.0208(16) 0.49548(13) 0.068(7) Uiso 1 1 d R . . C54 C 0.1355(3) -0.1250(2) 0.41257(13) 0.0574(10) Uani 1 1 d . . . H54A H 0.1295(9) -0.1890(14) 0.4270(6) 0.059(6) Uiso 1 1 d R . . H54B H 0.1421(7) -0.1321(14) 0.3778(7) 0.059(6) Uiso 1 1 d R . . H54C H 0.0838(10) -0.0864(11) 0.4148(7) 0.059(6) Uiso 1 1 d R . . C55 C 0.2946(3) -0.1342(2) 0.43850(14) 0.0622(11) Uani 1 1 d . . . H55A H 0.3434(10) -0.1013(10) 0.4541(8) 0.060(6) Uiso 1 1 d R . . H55B H 0.2996(8) -0.1448(14) 0.4055(7) 0.060(6) Uiso 1 1 d R . . H55C H 0.2901(7) -0.1935(13) 0.4541(8) 0.060(6) Uiso 1 1 d R . . C56 C 0.49215(14) 0.21467(16) 0.37830(7) 0.0186(4) Uani 1 1 d . . . C57 C 0.58539(14) 0.19804(17) 0.37074(8) 0.0229(4) Uani 1 1 d . . . C58 C 0.61240(16) 0.28133(19) 0.34024(9) 0.0283(5) Uani 1 1 d . . . H58A H 0.6719(10) 0.2739(7) 0.3368(5) 0.032(4) Uiso 1 1 d R . . H58B H 0.6048(10) 0.3412(10) 0.3566(4) 0.032(4) Uiso 1 1 d R . . H58C H 0.5775(9) 0.2814(7) 0.3082(5) 0.032(4) Uiso 1 1 d R . . C59 C 0.64123(16) 0.1957(2) 0.42162(10) 0.0377(7) Uani 1 1 d . . . H59A H 0.7003(10) 0.1863(14) 0.41810(11) 0.044(5) Uiso 1 1 d R . . H59B H 0.6229(9) 0.1439(12) 0.4405(4) 0.044(5) Uiso 1 1 d R . . H59C H 0.6354(10) 0.2556(12) 0.4381(4) 0.044(5) Uiso 1 1 d R . . C60 C 0.59407(19) 0.1033(2) 0.34402(11) 0.0394(7) Uani 1 1 d . . . H60A H 0.6553(11) 0.0942(7) 0.3397(7) 0.051(6) Uiso 1 1 d R . . H60B H 0.5568(12) 0.1047(6) 0.3112(7) 0.051(6) Uiso 1 1 d R . . H60C H 0.5761(13) 0.0490(10) 0.3638(5) 0.051(6) Uiso 1 1 d R . . C1S C -0.0049(7) -0.0885(7) 0.5170(4) 0.074(3) Uiso 0.50 1 d P . . C2S C 0.0235(10) 0.0317(12) 0.5272(6) 0.135(5) Uiso 0.50 1 d P . . C3S C 0.0492(12) 0.1002(14) 0.5555(7) 0.075(5) Uiso 0.25 1 d P . . C4S C 0.0516(15) 0.0252(17) 0.5748(9) 0.097(6) Uiso 0.25 1 d P . . C5S C -0.0127(11) 0.0666(13) 0.4650(6) 0.057(4) Uiso 0.25 1 d P . . 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 0.01652(13) 0.01443(13) 0.01555(12) -0.00049(10) 0.00174(10) 0.00017(11) Co2 0.01634(13) 0.01456(13) 0.01755(13) 0.00040(10) 0.00103(10) -0.00013(11) Co3 0.01660(14) 0.01746(14) 0.02135(14) 0.00368(11) 0.00153(11) -0.00046(11) Co4 0.01912(14) 0.01498(14) 0.02223(14) -0.00230(11) -0.00119(11) 0.00097(11) O1 0.0199(7) 0.0145(7) 0.0171(7) -0.0005(5) 0.0039(5) 0.0007(6) O2 0.0182(7) 0.0166(7) 0.0217(7) -0.0006(6) -0.0012(6) -0.0017(6) O3 0.0184(7) 0.0160(7) 0.0161(7) 0.0024(5) 0.0002(5) 0.0012(6) O4 0.0185(7) 0.0175(7) 0.0160(7) -0.0019(5) 0.0029(5) 0.0007(6) O5 0.0219(8) 0.0163(7) 0.0208(7) 0.0004(6) 0.0049(6) -0.0006(6) O6 0.0232(8) 0.0166(7) 0.0203(7) 0.0015(6) 0.0021(6) -0.0023(6) O7 0.0180(7) 0.0221(8) 0.0258(8) 0.0026(6) 0.0039(6) 0.0020(6) O8 0.0176(8) 0.0302(9) 0.0273(8) 0.0074(7) 0.0028(6) 0.0022(7) O9 0.0273(9) 0.0199(8) 0.0323(9) 0.0063(7) -0.0028(7) -0.0046(7) O10 0.0331(9) 0.0179(8) 0.0311(9) 0.0005(7) -0.0039(7) -0.0021(7) O11 0.0195(7) 0.0200(8) 0.0243(7) -0.0018(6) 0.0001(6) 0.0012(6) O12 0.0166(7) 0.0207(8) 0.0213(7) -0.0014(6) 0.0009(6) 0.0011(6) N1 0.0254(10) 0.0185(9) 0.0176(8) -0.0008(7) 0.0038(7) -0.0046(7) N2 0.0179(9) 0.0209(9) 0.0202(8) -0.0024(7) 0.0021(7) 0.0033(7) N3 0.0224(9) 0.0228(10) 0.0226(9) 0.0026(7) 0.0044(7) -0.0014(8) N4 0.0217(9) 0.0236(10) 0.0260(9) -0.0079(8) -0.0017(7) 0.0018(8) C1 0.0232(10) 0.0163(10) 0.0172(9) 0.0005(8) 0.0075(8) -0.0005(8) C2 0.0252(11) 0.0155(10) 0.0248(10) 0.0030(8) 0.0037(9) -0.0016(8) C3 0.0313(13) 0.0196(11) 0.0401(14) 0.0021(10) -0.0032(11) -0.0050(10) C4 0.0582(18) 0.0292(14) 0.0312(13) 0.0078(11) 0.0167(13) -0.0074(13) C5 0.0295(13) 0.0203(12) 0.0475(15) 0.0056(11) 0.0004(11) 0.0019(10) C6 0.0185(10) 0.0217(11) 0.0269(11) 0.0009(9) 0.0035(8) 0.0018(8) C7 0.0164(11) 0.0381(14) 0.0386(13) 0.0113(11) 0.0047(9) 0.0046(10) C8 0.0192(13) 0.069(2) 0.063(2) 0.0292(17) 0.0065(12) -0.0036(13) C9 0.0323(15) 0.055(2) 0.064(2) 0.0063(16) 0.0129(14) 0.0196(14) C10 0.0223(13) 0.063(2) 0.0497(18) 0.0049(15) -0.0070(12) -0.0014(13) C11 0.0323(13) 0.0308(13) 0.0228(11) 0.0038(10) -0.0062(9) -0.0099(11) C12 0.0338(13) 0.0217(11) 0.0174(10) 0.0013(8) 0.0024(9) -0.0112(10) C13 0.0526(17) 0.0386(15) 0.0207(11) -0.0059(11) 0.0005(11) -0.0135(13) C14 0.063(2) 0.0370(15) 0.0267(13) -0.0137(11) 0.0155(13) -0.0137(14) C15 0.0546(19) 0.0381(16) 0.0485(17) -0.0221(13) 0.0252(15) -0.0010(14) C16 0.0381(15) 0.0318(15) 0.0591(19) -0.0117(13) 0.0223(14) 0.0077(12) C17 0.0283(12) 0.0245(12) 0.0362(13) -0.0030(10) 0.0116(10) 0.0022(10) C18 0.0258(11) 0.0178(10) 0.0226(10) 0.0002(8) 0.0102(8) -0.0013(9) C19 0.0299(12) 0.0208(11) 0.0207(10) -0.0030(8) 0.0091(9) -0.0049(9) C20 0.0439(15) 0.0303(13) 0.0307(13) -0.0113(11) 0.0151(11) -0.0061(12) C21 0.0323(13) 0.0335(14) 0.0223(11) 0.0055(10) 0.0027(9) -0.0007(11) C22 0.0229(11) 0.0265(12) 0.0207(10) -0.0013(9) 0.0021(8) 0.0050(9) C23 0.0292(12) 0.0394(14) 0.0195(10) -0.0023(10) 0.0003(9) 0.0049(11) C24 0.0262(12) 0.0398(15) 0.0229(11) -0.0096(10) -0.0036(9) 0.0027(11) C25 0.0233(12) 0.0298(13) 0.0381(13) -0.0121(11) -0.0030(10) -0.0023(10) C26 0.0261(12) 0.0233(12) 0.0461(15) -0.0039(11) -0.0032(11) -0.0074(10) C27 0.0207(11) 0.0235(12) 0.0357(13) 0.0025(10) -0.0037(9) -0.0032(9) C28 0.0169(10) 0.0187(11) 0.0255(10) -0.0029(8) -0.0016(8) -0.0001(8) C29 0.0159(10) 0.0213(11) 0.0237(10) -0.0043(8) 0.0006(8) 0.0018(8) C30 0.0183(10) 0.0279(12) 0.0283(11) -0.0087(9) -0.0019(9) 0.0023(9) C31 0.0358(15) 0.0522(18) 0.0346(14) 0.0030(13) 0.0160(12) 0.0087(13) C32 0.0276(12) 0.0327(13) 0.0290(12) 0.0048(10) 0.0103(10) -0.0014(10) C33 0.0363(14) 0.0521(17) 0.0269(12) 0.0021(12) 0.0138(11) -0.0023(13) C34 0.0402(15) 0.0471(17) 0.0200(11) 0.0071(11) 0.0045(10) -0.0061(13) C35 0.0354(14) 0.0274(13) 0.0239(11) 0.0070(9) -0.0063(10) -0.0029(10) C36 0.0308(13) 0.0210(11) 0.0301(12) 0.0059(9) -0.0059(10) 0.0011(10) C37 0.0256(11) 0.0184(11) 0.0253(11) 0.0027(8) 0.0003(9) 0.0001(9) C38 0.0207(10) 0.0147(9) 0.0193(9) 0.0014(8) 0.0000(8) -0.0040(8) C39 0.0211(10) 0.0191(10) 0.0219(10) 0.0026(8) 0.0026(8) -0.0055(8) C40 0.0301(12) 0.0260(12) 0.0218(11) 0.0052(9) 0.0015(9) -0.0060(10) C41 0.0332(14) 0.0268(13) 0.0357(13) -0.0149(11) 0.0002(10) 0.0017(11) C42 0.059(2) 0.0288(15) 0.059(2) -0.0212(14) 0.0109(16) -0.0082(14) C43 0.0520(18) 0.0400(17) 0.0418(16) -0.0255(13) 0.0053(13) 0.0008(14) C44 0.0498(18) 0.0492(18) 0.0291(13) -0.0170(12) 0.0085(12) 0.0086(14) C45 0.0355(14) 0.0439(16) 0.0198(11) 0.0013(10) 0.0077(10) 0.0113(12) C46 0.0290(12) 0.0344(14) 0.0257(11) 0.0073(10) 0.0091(9) 0.0074(10) C47 0.0253(11) 0.0225(11) 0.0208(10) 0.0020(8) 0.0038(8) 0.0052(9) C48 0.0188(10) 0.0230(11) 0.0146(9) -0.0012(8) 0.0003(7) 0.0044(8) C49 0.0215(11) 0.0251(11) 0.0192(10) -0.0047(8) -0.0024(8) 0.0058(9) C50 0.0299(13) 0.0365(14) 0.0212(11) -0.0063(10) 0.0015(9) 0.0101(11) C51 0.0318(13) 0.0173(11) 0.0315(12) 0.0027(9) -0.0115(10) -0.0074(10) C52 0.0570(18) 0.0182(12) 0.0369(14) 0.0084(10) -0.0117(13) -0.0073(12) C53 0.106(3) 0.0337(17) 0.0384(17) 0.0179(14) -0.0085(18) -0.0032(18) C54 0.077(3) 0.0314(16) 0.057(2) 0.0140(14) -0.0120(18) -0.0275(16) C55 0.086(3) 0.0231(15) 0.069(2) 0.0122(15) -0.014(2) 0.0105(16) C56 0.0197(10) 0.0214(10) 0.0139(9) 0.0041(8) 0.0002(7) 0.0035(8) C57 0.0193(10) 0.0252(11) 0.0246(11) 0.0064(9) 0.0050(8) 0.0053(9) C58 0.0240(12) 0.0330(13) 0.0285(12) 0.0067(10) 0.0058(9) -0.0001(10) C59 0.0202(12) 0.0585(19) 0.0330(13) 0.0172(13) 0.0001(10) 0.0059(12) C60 0.0412(16) 0.0308(14) 0.0519(17) 0.0013(12) 0.0248(13) 0.0098(12) _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 O12 2.0160(16) . ? Co1 O1 2.0909(16) . ? Co1 O5 2.0914(16) . ? Co1 O4 2.1500(15) . ? Co1 N1 2.1500(18) . ? Co1 O3 2.1812(15) . ? Co2 O6 2.0044(16) . ? Co2 O2 2.0849(16) . ? Co2 O7 2.1003(17) . ? Co2 O1 2.1297(15) . ? Co2 N2 2.1438(19) . ? Co2 O4 2.1920(16) . ? Co3 O8 1.9985(17) . ? Co3 O9 2.0644(17) . ? Co3 O3 2.0801(16) . ? Co3 N3 2.150(2) . ? Co3 O2 2.1638(16) . ? Co3 O1 2.1755(16) . ? Co4 O10 2.0161(18) . ? Co4 O11 2.0715(17) . ? Co4 O4 2.1019(16) . ? Co4 O3 2.1333(15) . ? Co4 N4 2.139(2) . ? Co4 O2 2.1641(16) . ? O1 C18 1.350(3) . ? O2 C28 1.355(3) . ? O3 C38 1.353(2) . ? O4 C48 1.349(2) . ? O5 C1 1.268(3) . ? O6 C1 1.271(3) . ? O7 C6 1.268(3) . ? O8 C6 1.269(3) . ? O9 C51 1.266(3) . ? O10 C51 1.266(3) . ? O11 C56 1.255(3) . ? O12 C56 1.279(3) . ? N1 C12 1.328(3) . ? N1 C19 1.383(3) . ? N2 C22 1.329(3) . ? N2 C29 1.375(3) . ? N3 C32 1.328(3) . ? N3 C39 1.379(3) . ? N4 C41 1.327(3) . ? N4 C49 1.379(3) . ? C1 C2 1.536(3) . ? C2 C3 1.529(3) . ? C2 C5 1.535(3) . ? C2 C4 1.536(3) . ? C6 C7 1.540(3) . ? C7 C9 1.523(4) . ? C7 C8 1.527(4) . ? C7 C10 1.541(4) . ? C11 C12 1.494(4) . ? C12 C13 1.423(3) . ? C13 C14 1.359(4) . ? C14 C20 1.428(4) . ? C15 C16 1.374(5) . ? C15 C20 1.418(4) . ? C16 C17 1.411(4) . ? C17 C18 1.385(3) . ? C18 C19 1.430(3) . ? C19 C20 1.414(3) . ? C21 C22 1.498(3) . ? C22 C23 1.427(3) . ? C23 C24 1.364(4) . ? C24 C30 1.414(4) . ? C25 C26 1.362(4) . ? C25 C30 1.417(4) . ? C26 C27 1.416(3) . ? C27 C28 1.381(3) . ? C28 C29 1.433(3) . ? C29 C30 1.425(3) . ? C31 C32 1.500(4) . ? C32 C33 1.420(4) . ? C33 C34 1.362(4) . ? C34 C40 1.424(4) . ? C35 C36 1.368(4) . ? C35 C40 1.416(4) . ? C36 C37 1.417(3) . ? C37 C38 1.382(3) . ? C38 C39 1.431(3) . ? C39 C40 1.418(3) . ? C41 C43 1.428(4) . ? C41 C42 1.489(4) . ? C43 C44 1.354(5) . ? C44 C50 1.423(4) . ? C45 C46 1.367(4) . ? C45 C50 1.416(4) . ? C46 C47 1.421(3) . ? C47 C48 1.374(3) . ? C48 C49 1.437(3) . ? C49 C50 1.420(3) . ? C51 C52 1.538(3) . ? C52 C55 1.518(5) . ? C52 C53 1.528(4) . ? C52 C54 1.540(4) . ? C56 C57 1.538(3) . ? C57 C60 1.529(4) . ? C57 C58 1.535(3) . ? C57 C59 1.537(3) . ? C1S C5S 0.613(18) 3_556 ? C1S C2S 1.447(17) 3_556 ? C1S C2S 1.746(19) . ? C1S C3S 2.02(2) 3_556 ? C2S C3S 1.26(2) . ? C2S C4S 1.32(3) . ? C2S C5S 1.40(2) 3_556 ? C2S C1S 1.447(17) 3_556 ? C2S C5S 1.79(2) . ? C2S C2S 1.80(3) 3_556 ? C3S C4S 1.17(3) . ? C3S C1S 2.02(2) 3_556 ? C4S C5S 1.73(3) 3_556 ? C5S C1S 0.613(18) 3_556 ? C5S C2S 1.40(2) 3_556 ? C5S C4S 1.73(3) 3_556 ? 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 O12 Co1 O1 166.87(6) . . ? O12 Co1 O5 105.72(6) . . ? O1 Co1 O5 84.64(6) . . ? O12 Co1 O4 86.43(6) . . ? O1 Co1 O4 85.75(6) . . ? O5 Co1 O4 88.78(6) . . ? O12 Co1 N1 108.47(7) . . ? O1 Co1 N1 78.88(7) . . ? O5 Co1 N1 90.81(7) . . ? O4 Co1 N1 164.59(7) . . ? O12 Co1 O3 92.76(6) . . ? O1 Co1 O3 75.98(6) . . ? O5 Co1 O3 159.82(6) . . ? O4 Co1 O3 84.26(6) . . ? N1 Co1 O3 90.94(6) . . ? O6 Co2 O2 165.58(6) . . ? O6 Co2 O7 106.70(6) . . ? O2 Co2 O7 86.12(6) . . ? O6 Co2 O1 86.68(6) . . ? O2 Co2 O1 87.01(6) . . ? O7 Co2 O1 88.88(6) . . ? O6 Co2 N2 106.98(7) . . ? O2 Co2 N2 79.75(7) . . ? O7 Co2 N2 86.85(7) . . ? O1 Co2 N2 166.33(7) . . ? O6 Co2 O4 91.08(6) . . ? O2 Co2 O4 75.35(6) . . ? O7 Co2 O4 160.36(6) . . ? O1 Co2 O4 83.77(6) . . ? N2 Co2 O4 96.04(6) . . ? O8 Co3 O9 105.02(7) . . ? O8 Co3 O3 167.61(6) . . ? O9 Co3 O3 85.68(6) . . ? O8 Co3 N3 106.90(7) . . ? O9 Co3 N3 88.39(7) . . ? O3 Co3 N3 79.18(7) . . ? O8 Co3 O2 87.80(6) . . ? O9 Co3 O2 88.35(6) . . ? O3 Co3 O2 86.27(6) . . ? N3 Co3 O2 165.29(7) . . ? O8 Co3 O1 92.24(6) . . ? O9 Co3 O1 160.81(6) . . ? O3 Co3 O1 76.33(6) . . ? N3 Co3 O1 94.65(6) . . ? O2 Co3 O1 83.93(6) . . ? O10 Co4 O11 104.66(7) . . ? O10 Co4 O4 167.08(7) . . ? O11 Co4 O4 85.94(6) . . ? O10 Co4 O3 86.42(7) . . ? O11 Co4 O3 87.87(6) . . ? O4 Co4 O3 86.63(6) . . ? O10 Co4 N4 108.65(8) . . ? O11 Co4 N4 84.75(7) . . ? O4 Co4 N4 79.24(7) . . ? O3 Co4 N4 164.47(7) . . ? O10 Co4 O2 92.94(7) . . ? O11 Co4 O2 160.54(6) . . ? O4 Co4 O2 75.61(6) . . ? O3 Co4 O2 84.96(6) . . ? N4 Co4 O2 97.60(7) . . ? C18 O1 Co1 109.41(13) . . ? C18 O1 Co2 134.02(14) . . ? Co1 O1 Co2 95.41(6) . . ? C18 O1 Co3 117.56(12) . . ? Co1 O1 Co3 103.49(6) . . ? Co2 O1 Co3 91.87(6) . . ? C28 O2 Co2 109.82(13) . . ? C28 O2 Co3 133.79(14) . . ? Co2 O2 Co3 93.45(6) . . ? C28 O2 Co4 118.71(13) . . ? Co2 O2 Co4 104.86(7) . . ? Co3 O2 Co4 91.10(6) . . ? C38 O3 Co3 109.27(13) . . ? C38 O3 Co4 131.70(13) . . ? Co3 O3 Co4 94.31(6) . . ? C38 O3 Co1 120.60(13) . . ? Co3 O3 Co1 103.65(6) . . ? Co4 O3 Co1 91.96(6) . . ? C48 O4 Co4 110.21(13) . . ? C48 O4 Co1 131.31(13) . . ? Co4 O4 Co1 93.72(6) . . ? C48 O4 Co2 120.77(13) . . ? Co4 O4 Co2 103.31(6) . . ? Co1 O4 Co2 91.94(6) . . ? C1 O5 Co1 128.87(14) . . ? C1 O6 Co2 128.60(14) . . ? C6 O7 Co2 127.63(14) . . ? C6 O8 Co3 127.44(15) . . ? C51 O9 Co3 128.94(16) . . ? C51 O10 Co4 126.62(16) . . ? C56 O11 Co4 129.46(14) . . ? C56 O12 Co1 126.67(14) . . ? C12 N1 C19 119.2(2) . . ? C12 N1 Co1 132.70(16) . . ? C19 N1 Co1 107.75(14) . . ? C22 N2 C29 119.47(19) . . ? C22 N2 Co2 130.73(16) . . ? C29 N2 Co2 107.82(14) . . ? C32 N3 C39 119.0(2) . . ? C32 N3 Co3 132.52(17) . . ? C39 N3 Co3 107.45(14) . . ? C41 N4 C49 119.5(2) . . ? C41 N4 Co4 129.89(18) . . ? C49 N4 Co4 108.54(14) . . ? O5 C1 O6 126.0(2) . . ? O5 C1 C2 118.42(19) . . ? O6 C1 C2 115.52(19) . . ? C3 C2 C5 109.6(2) . . ? C3 C2 C4 109.7(2) . . ? C5 C2 C4 110.0(2) . . ? C3 C2 C1 111.00(19) . . ? C5 C2 C1 109.07(19) . . ? C4 C2 C1 107.41(19) . . ? O7 C6 O8 125.9(2) . . ? O7 C6 C7 117.5(2) . . ? O8 C6 C7 116.6(2) . . ? C9 C7 C8 109.6(3) . . ? C9 C7 C6 108.2(2) . . ? C8 C7 C6 110.9(2) . . ? C9 C7 C10 110.0(2) . . ? C8 C7 C10 109.8(3) . . ? C6 C7 C10 108.2(2) . . ? N1 C12 C13 121.3(2) . . ? N1 C12 C11 119.2(2) . . ? C13 C12 C11 119.5(2) . . ? C14 C13 C12 120.1(3) . . ? C13 C14 C20 120.3(2) . . ? C16 C15 C20 119.7(2) . . ? C15 C16 C17 121.5(3) . . ? C18 C17 C16 120.0(3) . . ? O1 C18 C17 123.5(2) . . ? O1 C18 C19 117.2(2) . . ? C17 C18 C19 119.2(2) . . ? N1 C19 C20 122.6(2) . . ? N1 C19 C18 117.60(19) . . ? C20 C19 C18 119.8(2) . . ? C19 C20 C15 119.2(3) . . ? C19 C20 C14 116.2(3) . . ? C15 C20 C14 124.6(2) . . ? N2 C22 C23 121.0(2) . . ? N2 C22 C21 118.7(2) . . ? C23 C22 C21 120.2(2) . . ? C24 C23 C22 120.1(2) . . ? C23 C24 C30 120.4(2) . . ? C26 C25 C30 119.8(2) . . ? C25 C26 C27 121.6(2) . . ? C28 C27 C26 120.5(2) . . ? O2 C28 C27 123.1(2) . . ? O2 C28 C29 118.03(19) . . ? C27 C28 C29 118.9(2) . . ? N2 C29 C30 122.4(2) . . ? N2 C29 C28 117.79(19) . . ? C30 C29 C28 119.8(2) . . ? C24 C30 C25 124.1(2) . . ? C24 C30 C29 116.5(2) . . ? C25 C30 C29 119.4(2) . . ? N3 C32 C33 121.3(2) . . ? N3 C32 C31 119.1(2) . . ? C33 C32 C31 119.6(2) . . ? C34 C33 C32 120.5(2) . . ? C33 C34 C40 119.7(2) . . ? C36 C35 C40 119.6(2) . . ? C35 C36 C37 121.6(2) . . ? C38 C37 C36 120.2(2) . . ? O3 C38 C37 123.6(2) . . ? O3 C38 C39 117.38(19) . . ? C37 C38 C39 119.0(2) . . ? N3 C39 C40 122.5(2) . . ? N3 C39 C38 117.59(19) . . ? C40 C39 C38 119.9(2) . . ? C35 C40 C39 119.5(2) . . ? C35 C40 C34 123.9(2) . . ? C39 C40 C34 116.6(2) . . ? N4 C41 C43 120.8(3) . . ? N4 C41 C42 118.9(2) . . ? C43 C41 C42 120.2(2) . . ? C44 C43 C41 120.7(2) . . ? C43 C44 C50 120.0(3) . . ? C46 C45 C50 120.0(2) . . ? C45 C46 C47 120.8(2) . . ? C48 C47 C46 121.3(2) . . ? O4 C48 C47 123.8(2) . . ? O4 C48 C49 117.6(2) . . ? C47 C48 C49 118.5(2) . . ? N4 C49 C50 122.4(2) . . ? N4 C49 C48 117.71(19) . . ? C50 C49 C48 119.9(2) . . ? C45 C50 C49 119.5(2) . . ? C45 C50 C44 123.9(2) . . ? C49 C50 C44 116.5(3) . . ? O10 C51 O9 126.1(2) . . ? O10 C51 C52 117.6(2) . . ? O9 C51 C52 116.3(2) . . ? C55 C52 C53 109.6(3) . . ? C55 C52 C51 111.1(3) . . ? C53 C52 C51 109.4(2) . . ? C55 C52 C54 110.0(3) . . ? C53 C52 C54 110.3(3) . . ? C51 C52 C54 106.4(2) . . ? O11 C56 O12 125.8(2) . . ? O11 C56 C57 117.87(19) . . ? O12 C56 C57 116.31(19) . . ? C60 C57 C58 109.4(2) . . ? C60 C57 C59 110.0(2) . . ? C58 C57 C59 110.5(2) . . ? C60 C57 C56 110.9(2) . . ? C58 C57 C56 108.49(18) . . ? C59 C57 C56 107.52(18) . . ? C5S C1S C2S 115(2) 3_556 3_556 ? C5S C1S C2S 47(2) 3_556 . ? C2S C1S C2S 67.9(11) 3_556 . ? C5S C1S C3S 153(2) 3_556 3_556 ? C2S C1S C3S 38.2(8) 3_556 3_556 ? C2S C1S C3S 106.1(10) . 3_556 ? C3S C2S C4S 53.9(14) . . ? C3S C2S C5S 132.8(19) . 3_556 ? C4S C2S C5S 79.0(17) . 3_556 ? C3S C2S C1S 96.5(16) . 3_556 ? C4S C2S C1S 150.3(18) . 3_556 ? C5S C2S C1S 130.7(14) 3_556 3_556 ? C3S C2S C1S 151.2(17) . . ? C4S C2S C1S 97.6(16) . . ? C5S C2S C1S 18.6(8) 3_556 . ? C1S C2S C1S 112.1(10) 3_556 . ? C3S C2S C5S 114.4(17) . . ? C4S C2S C5S 168.2(19) . . ? C5S C2S C5S 112.7(12) 3_556 . ? C1S C2S C5S 18.1(7) 3_556 . ? C1S C2S C5S 94.0(9) . . ? C3S C2S C2S 160(2) . 3_556 ? C4S C2S C2S 146(2) . 3_556 ? C5S C2S C2S 66.7(12) 3_556 3_556 ? C1S C2S C2S 64.0(10) 3_556 3_556 ? C1S C2S C2S 48.1(8) . 3_556 ? C5S C2S C2S 45.9(9) . 3_556 ? C4S C3S C2S 65.8(16) . . ? C4S C3S C1S 111.1(18) . 3_556 ? C2S C3S C1S 45.3(11) . 3_556 ? C3S C4S C2S 60.4(16) . . ? C3S C4S C5S 113(2) . 3_556 ? C2S C4S C5S 52.5(12) . 3_556 ? C1S C5S C2S 114(3) 3_556 3_556 ? C1S C5S C4S 162(3) 3_556 3_556 ? C2S C5S C4S 48.5(11) 3_556 3_556 ? C1S C5S C2S 47.1(19) 3_556 . ? C2S C5S C2S 67.3(12) 3_556 . ? C4S C5S C2S 115.8(14) 3_556 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.670 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.081 data_pc1 _database_code_CSD 216671 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit contains the cluster, a water at 0.5 occupancy, and a disordered acetone solvent molecule at 0.25 occupancy. All non-H atoms were refined anisotropically, except those of the acetone. H atoms were included in calculated positions, except those bonded to the water and acetone molecules. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60.75 H69.75 N4 Ni4 O12.75' _chemical_formula_weight 1294.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c 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 15.77400(10) _cell_length_b 13.95460(10) _cell_length_c 27.3512(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.9772(3) _cell_angle_gamma 90.00 _cell_volume 5946.80(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 67320 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 25.028 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2705 _exptl_absorpt_coefficient_mu 1.313 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7792 _exptl_absorpt_correction_T_max 0.7792 _exptl_absorpt_process_details '(SORTAV; Blessing, 1997)' _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 'Nonius KappaCCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48328 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.17 _reflns_number_total 10380 _reflns_number_gt 9207 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _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^)+(0.0396P)^2^+5.8532P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00171(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10380 _refine_ls_number_parameters 759 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0835 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.006 _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 0.354371(18) 0.349662(19) 0.399483(10) 0.01807(9) Uani 1 1 d . . . Ni2 Ni 0.191778(18) 0.350354(19) 0.323917(10) 0.01919(9) Uani 1 1 d . . . Ni3 Ni 0.182284(18) 0.23481(2) 0.415671(10) 0.02040(9) Uani 1 1 d . . . Ni4 Ni 0.306484(18) 0.157598(19) 0.352835(10) 0.02049(9) Uani 1 1 d . . . O1 O 0.22635(10) 0.37300(10) 0.39871(5) 0.0202(3) Uani 1 1 d . . . O2 O 0.17872(10) 0.20827(11) 0.34044(5) 0.0214(3) Uani 1 1 d . . . O3 O 0.31194(9) 0.21502(10) 0.42266(5) 0.0192(3) Uani 1 1 d . . . O4 O 0.31911(9) 0.29572(10) 0.32837(5) 0.0196(3) Uani 1 1 d . . . O5 O 0.35679(10) 0.48517(11) 0.36908(5) 0.0224(3) Uani 1 1 d . . . O6 O 0.23218(10) 0.48465(11) 0.31550(6) 0.0237(3) Uani 1 1 d . . . O7 O 0.06435(10) 0.36734(11) 0.33299(6) 0.0253(4) Uani 1 1 d . . . O8 O 0.05915(10) 0.27171(12) 0.39918(6) 0.0275(4) Uani 1 1 d . . . O9 O 0.17380(10) 0.08979(11) 0.42597(6) 0.0280(4) Uani 1 1 d . . . O10 O 0.27483(11) 0.03371(11) 0.38346(6) 0.0284(4) Uani 1 1 d . . . O11 O 0.43848(10) 0.15083(11) 0.36557(6) 0.0236(3) Uani 1 1 d . . . O12 O 0.47271(10) 0.29930(11) 0.39518(5) 0.0222(3) Uani 1 1 d . . . N1 N 0.35769(13) 0.41010(13) 0.47016(7) 0.0233(4) Uani 1 1 d . . . N2 N 0.14464(12) 0.29893(14) 0.25316(7) 0.0234(4) Uani 1 1 d . . . N3 N 0.21514(12) 0.24968(14) 0.49258(7) 0.0241(4) Uani 1 1 d . . . N4 N 0.31765(13) 0.12950(14) 0.27914(7) 0.0263(4) Uani 1 1 d . . . C1 C 0.29872(15) 0.52449(16) 0.33873(8) 0.0216(5) Uani 1 1 d . . . C2 C 0.30988(16) 0.63097(16) 0.32649(9) 0.0264(5) Uani 1 1 d . . . C3 C 0.37948(18) 0.67696(18) 0.36422(11) 0.0382(6) Uani 1 1 d . . . H3A H 0.3619 0.6754 0.3970 0.057 Uiso 1 1 calc R . . H3B H 0.3880 0.7436 0.3547 0.057 Uiso 1 1 calc R . . H3C H 0.4333 0.6414 0.3651 0.057 Uiso 1 1 calc R . . C4 C 0.3357(2) 0.6370(2) 0.27513(11) 0.0506(8) Uani 1 1 d . . . H4A H 0.3897 0.6025 0.2750 0.076 Uiso 1 1 calc R . . H4B H 0.3432 0.7044 0.2666 0.076 Uiso 1 1 calc R . . H4C H 0.2907 0.6082 0.2508 0.076 Uiso 1 1 calc R . . C5 C 0.22478(17) 0.68331(18) 0.32689(12) 0.0397(7) Uani 1 1 d . . . H5A H 0.1806 0.6551 0.3019 0.060 Uiso 1 1 calc R . . H5B H 0.2318 0.7513 0.3194 0.060 Uiso 1 1 calc R . . H5C H 0.2075 0.6771 0.3596 0.060 Uiso 1 1 calc R . . C6 C 0.02494(15) 0.32036(17) 0.36218(9) 0.0256(5) Uani 1 1 d . . . C7 C -0.07326(16) 0.3237(2) 0.35231(10) 0.0355(6) Uani 1 1 d . . . C8 C -0.11102(18) 0.2531(3) 0.38578(13) 0.0546(9) Uani 1 1 d . . . H8A H -0.0935 0.1878 0.3787 0.082 Uiso 1 1 calc R . . H8B H -0.1738 0.2576 0.3796 0.082 Uiso 1 1 calc R . . H8C H -0.0900 0.2687 0.4205 0.082 Uiso 1 1 calc R . . C9 C -0.10190(19) 0.4252(2) 0.36271(13) 0.0520(8) Uani 1 1 d . . . H9A H -0.0791 0.4427 0.3969 0.078 Uiso 1 1 calc R . . H9B H -0.1647 0.4280 0.3578 0.078 Uiso 1 1 calc R . . H9C H -0.0803 0.4701 0.3400 0.078 Uiso 1 1 calc R . . C10 C -0.10334(18) 0.2978(3) 0.29786(11) 0.0491(8) Uani 1 1 d . . . H10A H -0.0806 0.3446 0.2766 0.074 Uiso 1 1 calc R . . H10B H -0.1662 0.2986 0.2910 0.074 Uiso 1 1 calc R . . H10C H -0.0825 0.2337 0.2912 0.074 Uiso 1 1 calc R . . C11 C 0.49742(17) 0.35570(18) 0.51162(9) 0.0339(6) Uani 1 1 d . . . H11A H 0.4921 0.2977 0.5311 0.051 Uiso 1 1 calc R . . H11B H 0.5473 0.3927 0.5270 0.051 Uiso 1 1 calc R . . H11C H 0.5048 0.3377 0.4779 0.051 Uiso 1 1 calc R . . C12 C 0.41840(17) 0.41494(17) 0.50986(8) 0.0285(5) Uani 1 1 d . . . C13 C 0.4076(2) 0.47368(19) 0.55076(9) 0.0388(7) Uani 1 1 d . . . H13 H 0.4503 0.4740 0.5794 0.047 Uiso 1 1 calc R . . C14 C 0.3372(2) 0.5292(2) 0.54927(10) 0.0427(7) Uani 1 1 d . . . H14 H 0.3315 0.5698 0.5764 0.051 Uiso 1 1 calc R . . C15 C 0.1968(2) 0.5845(2) 0.50154(11) 0.0454(7) Uani 1 1 d . . . H15 H 0.1883 0.6295 0.5264 0.054 Uiso 1 1 calc R . . C16 C 0.1371(2) 0.5751(2) 0.46051(12) 0.0443(7) Uani 1 1 d . . . H16 H 0.0886 0.6165 0.4561 0.053 Uiso 1 1 calc R . . C17 C 0.14510(17) 0.50511(18) 0.42393(10) 0.0331(6) Uani 1 1 d . . . H17 H 0.1015 0.4985 0.3960 0.040 Uiso 1 1 calc R . . C18 C 0.21577(16) 0.44730(16) 0.42901(8) 0.0245(5) Uani 1 1 d . . . C19 C 0.28352(16) 0.46216(16) 0.46952(8) 0.0262(5) Uani 1 1 d . . . C20 C 0.27181(18) 0.52723(18) 0.50743(9) 0.0354(6) Uani 1 1 d . . . C21 C 0.18298(17) 0.43141(19) 0.20321(9) 0.0345(6) Uani 1 1 d . . . H21A H 0.1727 0.4787 0.2281 0.052 Uiso 1 1 calc R . . H21B H 0.1648 0.4579 0.1701 0.052 Uiso 1 1 calc R . . H21C H 0.2443 0.4160 0.2074 0.052 Uiso 1 1 calc R . . C22 C 0.13289(16) 0.34233(17) 0.20937(9) 0.0264(5) Uani 1 1 d . . . C23 C 0.07502(17) 0.3047(2) 0.16906(9) 0.0338(6) Uani 1 1 d . . . H23 H 0.0669 0.3371 0.1382 0.041 Uiso 1 1 calc R . . C24 C 0.03120(17) 0.2225(2) 0.17432(9) 0.0347(6) Uani 1 1 d . . . H24 H -0.0088 0.1990 0.1474 0.042 Uiso 1 1 calc R . . C25 C 0.00335(16) 0.08537(19) 0.22813(10) 0.0358(6) Uani 1 1 d . . . H25 H -0.0360 0.0569 0.2024 0.043 Uiso 1 1 calc R . . C26 C 0.01992(16) 0.04271(19) 0.27341(10) 0.0359(6) Uani 1 1 d . . . H26 H -0.0077 -0.0160 0.2788 0.043 Uiso 1 1 calc R . . C27 C 0.07702(16) 0.08375(18) 0.31243(10) 0.0315(6) Uani 1 1 d . . . H27 H 0.0861 0.0535 0.3439 0.038 Uiso 1 1 calc R . . C28 C 0.11978(14) 0.16735(16) 0.30538(9) 0.0237(5) Uani 1 1 d . . . C29 C 0.10294(15) 0.21365(17) 0.25865(9) 0.0247(5) Uani 1 1 d . . . C30 C 0.04482(16) 0.17201(18) 0.21952(9) 0.0292(5) Uani 1 1 d . . . C31 C 0.08809(19) 0.3305(2) 0.51284(11) 0.0412(7) Uani 1 1 d . . . H31A H 0.0961 0.3993 0.5192 0.062 Uiso 1 1 calc R . . H31B H 0.0458 0.3054 0.5322 0.062 Uiso 1 1 calc R . . H31C H 0.0676 0.3201 0.4775 0.062 Uiso 1 1 calc R . . C32 C 0.17177(16) 0.27968(18) 0.52741(9) 0.0304(6) Uani 1 1 d . . . C33 C 0.20307(18) 0.2635(2) 0.57818(10) 0.0382(6) Uani 1 1 d . . . H33 H 0.1725 0.2883 0.6027 0.046 Uiso 1 1 calc R . . C34 C 0.27593(18) 0.2131(2) 0.59211(9) 0.0363(6) Uani 1 1 d . . . H34 H 0.2948 0.2001 0.6262 0.044 Uiso 1 1 calc R . . C35 C 0.40077(17) 0.12626(18) 0.56674(9) 0.0317(6) Uani 1 1 d . . . H35 H 0.4227 0.1094 0.6000 0.038 Uiso 1 1 calc R . . C36 C 0.44320(16) 0.09872(17) 0.52930(9) 0.0302(6) Uani 1 1 d . . . H36 H 0.4935 0.0606 0.5367 0.036 Uiso 1 1 calc R . . C37 C 0.41407(15) 0.12563(16) 0.47979(9) 0.0250(5) Uani 1 1 d . . . H37 H 0.4450 0.1061 0.4544 0.030 Uiso 1 1 calc R . . C38 C 0.34113(15) 0.18000(15) 0.46827(8) 0.0209(5) Uani 1 1 d . . . C39 C 0.29250(15) 0.20395(16) 0.50640(8) 0.0228(5) Uani 1 1 d . . . C40 C 0.32424(16) 0.17985(17) 0.55609(9) 0.0289(5) Uani 1 1 d . . . C41 C 0.31153(18) 0.04826(19) 0.25374(10) 0.0370(6) Uani 1 1 d . . . C42 C 0.2683(2) -0.0356(2) 0.27323(13) 0.0562(9) Uani 1 1 d . . . H42A H 0.2740 -0.0310 0.3093 0.084 Uiso 1 1 calc R . . H42B H 0.2953 -0.0950 0.2643 0.084 Uiso 1 1 calc R . . H42C H 0.2074 -0.0359 0.2589 0.084 Uiso 1 1 calc R . . C43 C 0.3451(2) 0.0405(2) 0.20889(11) 0.0482(8) Uani 1 1 d . . . H43 H 0.3385 -0.0178 0.1907 0.058 Uiso 1 1 calc R . . C44 C 0.3864(2) 0.1147(2) 0.19151(10) 0.0451(7) Uani 1 1 d . . . H44 H 0.4098 0.1081 0.1617 0.054 Uiso 1 1 calc R . . C45 C 0.43918(17) 0.2832(2) 0.20326(9) 0.0353(6) Uani 1 1 d . . . H45 H 0.4652 0.2807 0.1742 0.042 Uiso 1 1 calc R . . C46 C 0.44435(16) 0.36462(19) 0.23115(9) 0.0321(6) Uani 1 1 d . . . H46 H 0.4750 0.4183 0.2216 0.039 Uiso 1 1 calc R . . C47 C 0.40489(15) 0.37046(18) 0.27392(9) 0.0269(5) Uani 1 1 d . . . H47 H 0.4093 0.4280 0.2927 0.032 Uiso 1 1 calc R . . C48 C 0.36039(14) 0.29436(16) 0.28885(8) 0.0210(5) Uani 1 1 d . . . C49 C 0.35687(15) 0.20709(17) 0.26112(8) 0.0255(5) Uani 1 1 d . . . C50 C 0.39487(16) 0.2025(2) 0.21777(9) 0.0324(6) Uani 1 1 d . . . C51 C 0.22386(16) 0.02574(16) 0.41440(9) 0.0282(6) Uani 1 1 d . . . C52 C 0.21765(19) -0.07270(18) 0.43931(10) 0.0383(6) Uani 1 1 d . . . C53 C 0.2098(2) -0.0579(2) 0.49344(11) 0.0547(9) Uani 1 1 d . . . H53A H 0.2616 -0.0260 0.5103 0.082 Uiso 1 1 calc R . . H53B H 0.2033 -0.1201 0.5090 0.082 Uiso 1 1 calc R . . H53C H 0.1596 -0.0179 0.4959 0.082 Uiso 1 1 calc R . . C54 C 0.1374(2) -0.1220(2) 0.41187(13) 0.0557(9) Uani 1 1 d . . . H54A H 0.1322 -0.1861 0.4258 0.084 Uiso 1 1 calc R . . H54B H 0.1420 -0.1275 0.3767 0.084 Uiso 1 1 calc R . . H54C H 0.0865 -0.0841 0.4156 0.084 Uiso 1 1 calc R . . C55 C 0.2963(2) -0.1337(2) 0.43530(13) 0.0554(9) Uani 1 1 d . . . H55A H 0.3477 -0.1018 0.4526 0.083 Uiso 1 1 calc R . . H55B H 0.3018 -0.1420 0.4004 0.083 Uiso 1 1 calc R . . H55C H 0.2901 -0.1965 0.4503 0.083 Uiso 1 1 calc R . . C56 C 0.49040(14) 0.21863(16) 0.37781(8) 0.0214(5) Uani 1 1 d . . . C57 C 0.58454(15) 0.20278(17) 0.37196(9) 0.0267(5) Uani 1 1 d . . . C58 C 0.61212(16) 0.28493(19) 0.34067(9) 0.0311(6) Uani 1 1 d . . . H58A H 0.6736 0.2793 0.3391 0.047 Uiso 1 1 calc R . . H58B H 0.6009 0.3464 0.3558 0.047 Uiso 1 1 calc R . . H58C H 0.5795 0.2816 0.3071 0.047 Uiso 1 1 calc R . . C59 C 0.63784(17) 0.2038(2) 0.42385(10) 0.0419(7) Uani 1 1 d . . . H59A H 0.6202 0.1505 0.4433 0.063 Uiso 1 1 calc R . . H59B H 0.6286 0.2645 0.4403 0.063 Uiso 1 1 calc R . . H59C H 0.6988 0.1972 0.4212 0.063 Uiso 1 1 calc R . . C60 C 0.59656(19) 0.1075(2) 0.34652(12) 0.0434(7) Uani 1 1 d . . . H60A H 0.5793 0.0549 0.3665 0.065 Uiso 1 1 calc R . . H60B H 0.6570 0.0998 0.3430 0.065 Uiso 1 1 calc R . . H60C H 0.5611 0.1067 0.3137 0.065 Uiso 1 1 calc R . . O1W O 0.5669(3) 0.0503(3) 0.64560(18) 0.0605(12) Uani 0.50 1 d P . . C1S C 0.0220(8) 0.0280(10) 0.5249(5) 0.051(3) Uiso 0.25 1 d P . . C2S C -0.0005(4) 0.0805(5) 0.4760(2) 0.0514(15) Uiso 0.50 1 d P . . O1S O 0.0524(9) 0.0778(10) 0.5567(5) 0.103(4) Uiso 0.25 1 d P . . 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 0.02108(16) 0.01486(15) 0.01804(15) -0.00109(10) 0.00231(11) 0.00034(11) Ni2 0.02060(17) 0.01616(15) 0.02032(15) 0.00040(11) 0.00171(11) 0.00104(11) Ni3 0.02023(17) 0.01741(15) 0.02328(16) 0.00286(11) 0.00255(12) 0.00079(11) Ni4 0.02148(17) 0.01588(15) 0.02312(16) -0.00291(11) 0.00034(12) 0.00101(11) O1 0.0250(8) 0.0159(7) 0.0203(8) -0.0007(6) 0.0054(6) 0.0003(6) O2 0.0212(8) 0.0179(8) 0.0237(8) -0.0009(6) -0.0004(6) -0.0015(6) O3 0.0212(8) 0.0166(7) 0.0192(8) 0.0010(6) 0.0008(6) 0.0009(6) O4 0.0210(8) 0.0183(8) 0.0193(8) -0.0012(6) 0.0022(6) 0.0014(6) O5 0.0260(9) 0.0182(8) 0.0232(8) 0.0012(6) 0.0040(7) 0.0000(6) O6 0.0269(9) 0.0183(8) 0.0254(8) 0.0012(6) 0.0025(7) -0.0001(7) O7 0.0244(9) 0.0233(8) 0.0282(9) 0.0032(7) 0.0044(7) 0.0037(7) O8 0.0219(9) 0.0290(9) 0.0318(9) 0.0072(7) 0.0045(7) 0.0031(7) O9 0.0273(9) 0.0208(8) 0.0342(9) 0.0059(7) -0.0005(7) -0.0040(7) O10 0.0311(9) 0.0191(8) 0.0334(9) -0.0012(7) 0.0002(7) -0.0013(7) O11 0.0230(9) 0.0196(8) 0.0272(9) -0.0027(6) 0.0005(7) 0.0008(6) O12 0.0214(8) 0.0208(8) 0.0236(8) -0.0016(6) 0.0009(6) 0.0002(6) N1 0.0311(11) 0.0184(10) 0.0206(10) -0.0010(8) 0.0049(8) -0.0056(8) N2 0.0220(10) 0.0238(10) 0.0240(10) -0.0020(8) 0.0019(8) 0.0033(8) N3 0.0258(11) 0.0221(10) 0.0250(10) 0.0032(8) 0.0059(8) -0.0013(8) N4 0.0261(11) 0.0257(11) 0.0259(10) -0.0077(8) 0.0000(8) 0.0024(8) C1 0.0271(13) 0.0184(11) 0.0208(11) 0.0005(9) 0.0080(10) 0.0011(10) C2 0.0312(14) 0.0174(11) 0.0303(13) 0.0032(9) 0.0040(10) -0.0013(10) C3 0.0369(16) 0.0219(13) 0.0531(17) 0.0040(12) -0.0016(13) -0.0033(11) C4 0.084(2) 0.0323(15) 0.0403(17) 0.0089(13) 0.0235(16) -0.0098(15) C5 0.0346(15) 0.0201(13) 0.0615(19) 0.0033(12) -0.0017(13) 0.0021(11) C6 0.0244(13) 0.0221(12) 0.0300(13) -0.0007(10) 0.0037(10) 0.0044(10) C7 0.0221(13) 0.0409(15) 0.0435(15) 0.0104(12) 0.0047(11) 0.0071(11) C8 0.0226(15) 0.069(2) 0.072(2) 0.0274(18) 0.0062(14) 0.0006(14) C9 0.0339(17) 0.055(2) 0.069(2) 0.0056(16) 0.0132(15) 0.0198(14) C10 0.0277(15) 0.063(2) 0.0535(19) 0.0032(16) -0.0047(13) 0.0024(14) C11 0.0370(15) 0.0337(14) 0.0276(13) 0.0009(11) -0.0052(11) -0.0097(11) C12 0.0398(15) 0.0238(12) 0.0214(12) 0.0008(10) 0.0030(10) -0.0126(11) C13 0.0574(19) 0.0339(15) 0.0237(13) -0.0050(11) 0.0025(12) -0.0159(14) C14 0.068(2) 0.0340(15) 0.0283(14) -0.0147(12) 0.0152(13) -0.0145(14) C15 0.059(2) 0.0333(15) 0.0492(17) -0.0185(13) 0.0264(15) -0.0008(14) C16 0.0462(18) 0.0303(15) 0.061(2) -0.0092(13) 0.0240(15) 0.0099(13) C17 0.0358(15) 0.0247(13) 0.0406(15) -0.0016(11) 0.0122(11) 0.0048(11) C18 0.0355(14) 0.0168(11) 0.0237(12) -0.0016(9) 0.0125(10) -0.0010(10) C19 0.0362(14) 0.0191(11) 0.0250(12) -0.0019(9) 0.0102(10) -0.0038(10) C20 0.0527(17) 0.0254(13) 0.0318(14) -0.0081(11) 0.0185(12) -0.0072(12) C21 0.0398(15) 0.0360(15) 0.0272(13) 0.0073(11) 0.0038(11) 0.0022(12) C22 0.0266(13) 0.0306(13) 0.0221(12) -0.0004(10) 0.0038(10) 0.0086(10) C23 0.0344(15) 0.0429(16) 0.0224(12) -0.0022(11) -0.0009(10) 0.0082(12) C24 0.0298(14) 0.0435(16) 0.0275(13) -0.0096(11) -0.0054(11) 0.0047(12) C25 0.0278(14) 0.0329(14) 0.0436(15) -0.0127(12) -0.0038(11) -0.0023(11) C26 0.0277(14) 0.0275(13) 0.0497(16) -0.0057(12) -0.0030(12) -0.0070(11) C27 0.0261(13) 0.0262(13) 0.0399(14) 0.0018(11) -0.0015(11) -0.0017(10) C28 0.0183(12) 0.0217(12) 0.0301(12) -0.0045(10) 0.0003(9) 0.0019(9) C29 0.0207(12) 0.0245(12) 0.0284(12) -0.0052(10) 0.0020(9) 0.0041(10) C30 0.0236(13) 0.0323(14) 0.0301(13) -0.0077(11) -0.0013(10) 0.0038(10) C31 0.0411(17) 0.0470(17) 0.0391(15) 0.0019(13) 0.0172(13) 0.0118(13) C32 0.0315(14) 0.0322(14) 0.0295(13) 0.0008(11) 0.0107(11) -0.0028(11) C33 0.0414(17) 0.0476(17) 0.0282(13) -0.0001(12) 0.0139(12) -0.0005(13) C34 0.0419(16) 0.0435(16) 0.0234(13) 0.0039(11) 0.0050(11) -0.0061(13) C35 0.0372(15) 0.0282(13) 0.0263(13) 0.0070(10) -0.0058(11) -0.0033(11) C36 0.0309(14) 0.0225(12) 0.0336(13) 0.0037(10) -0.0062(11) 0.0017(10) C37 0.0268(13) 0.0182(11) 0.0289(12) 0.0009(9) 0.0013(10) 0.0006(10) C38 0.0254(12) 0.0149(10) 0.0212(11) 0.0003(9) -0.0003(9) -0.0050(9) C39 0.0267(13) 0.0165(11) 0.0246(12) 0.0026(9) 0.0019(9) -0.0028(9) C40 0.0347(14) 0.0248(12) 0.0263(12) 0.0028(10) 0.0019(10) -0.0058(11) C41 0.0382(16) 0.0323(14) 0.0395(15) -0.0171(12) 0.0026(12) -0.0007(12) C42 0.068(2) 0.0374(17) 0.066(2) -0.0284(16) 0.0198(17) -0.0149(15) C43 0.0563(19) 0.0457(18) 0.0433(17) -0.0275(14) 0.0096(14) -0.0013(15) C44 0.0509(18) 0.0543(19) 0.0310(14) -0.0179(13) 0.0096(13) 0.0063(15) C45 0.0386(15) 0.0470(16) 0.0219(12) 0.0036(11) 0.0093(11) 0.0120(13) C46 0.0310(14) 0.0365(14) 0.0301(13) 0.0101(11) 0.0087(11) 0.0065(11) C47 0.0289(13) 0.0267(12) 0.0252(12) 0.0025(10) 0.0049(10) 0.0067(10) C48 0.0182(11) 0.0251(12) 0.0186(11) -0.0015(9) -0.0006(9) 0.0057(9) C49 0.0227(12) 0.0293(13) 0.0230(12) -0.0044(10) -0.0011(9) 0.0059(10) C50 0.0324(14) 0.0413(15) 0.0220(12) -0.0064(11) 0.0000(10) 0.0092(12) C51 0.0297(13) 0.0168(12) 0.0326(13) 0.0011(10) -0.0123(11) -0.0038(10) C52 0.0497(17) 0.0192(13) 0.0414(15) 0.0083(11) -0.0076(13) -0.0058(12) C53 0.081(2) 0.0349(16) 0.0448(18) 0.0155(14) -0.0008(16) 0.0034(16) C54 0.067(2) 0.0291(15) 0.065(2) 0.0109(15) -0.0089(17) -0.0221(15) C55 0.071(2) 0.0253(15) 0.067(2) 0.0101(14) 0.0017(18) 0.0117(14) C56 0.0231(12) 0.0232(12) 0.0175(11) 0.0025(9) 0.0014(9) 0.0033(10) C57 0.0229(13) 0.0280(13) 0.0290(12) 0.0056(10) 0.0037(10) 0.0033(10) C58 0.0249(13) 0.0364(14) 0.0320(13) 0.0068(11) 0.0049(10) 0.0003(11) C59 0.0225(14) 0.063(2) 0.0392(15) 0.0198(14) 0.0010(11) 0.0051(13) C60 0.0416(17) 0.0308(15) 0.0631(19) 0.0023(14) 0.0249(14) 0.0088(12) O1W 0.061(3) 0.044(3) 0.072(3) -0.003(2) 0.000(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O12 2.0151(15) . ? Ni1 O1 2.0423(15) . ? Ni1 O5 2.0685(15) . ? Ni1 O4 2.0789(14) . ? Ni1 N1 2.1023(18) . ? Ni1 O3 2.1243(15) . ? Ni2 O6 2.0043(15) . ? Ni2 O2 2.0511(15) . ? Ni2 O1 2.0577(15) . ? Ni2 O7 2.0769(16) . ? Ni2 N2 2.0891(19) . ? Ni2 O4 2.1341(15) . ? Ni3 O8 1.9919(16) . ? Ni3 O3 2.0429(15) . ? Ni3 O9 2.0504(16) . ? Ni3 O2 2.0828(15) . ? Ni3 N3 2.0969(19) . ? Ni3 O1 2.1255(15) . ? Ni4 O10 2.0175(16) . ? Ni4 O11 2.0589(16) . ? Ni4 O4 2.0601(15) . ? Ni4 O3 2.0605(15) . ? Ni4 N4 2.0876(19) . ? Ni4 O2 2.1126(15) . ? O1 C18 1.354(3) . ? O2 C28 1.353(3) . ? O3 C38 1.352(3) . ? O4 C48 1.346(3) . ? O5 C1 1.262(3) . ? O6 C1 1.267(3) . ? O7 C6 1.268(3) . ? O8 C6 1.267(3) . ? O9 C51 1.265(3) . ? O10 C51 1.260(3) . ? O11 C56 1.262(3) . ? O12 C56 1.270(3) . ? N1 C12 1.333(3) . ? N1 C19 1.375(3) . ? N2 C22 1.329(3) . ? N2 C29 1.379(3) . ? N3 C32 1.324(3) . ? N3 C39 1.377(3) . ? N4 C41 1.325(3) . ? N4 C49 1.376(3) . ? C1 C2 1.539(3) . ? C2 C4 1.525(4) . ? C2 C3 1.526(4) . ? C2 C5 1.530(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.531(3) . ? C7 C8 1.527(4) . ? C7 C9 1.528(4) . ? C7 C10 1.534(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.490(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.418(4) . ? C13 C14 1.349(4) . ? C13 H13 0.9500 . ? C14 C20 1.416(4) . ? C14 H14 0.9500 . ? C15 C16 1.354(4) . ? C15 C20 1.416(4) . ? C15 H15 0.9500 . ? C16 C17 1.418(4) . ? C16 H16 0.9500 . ? C17 C18 1.366(3) . ? C17 H17 0.9500 . ? C18 C19 1.429(3) . ? C19 C20 1.412(3) . ? C21 C22 1.497(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.418(3) . ? C23 C24 1.358(4) . ? C23 H23 0.9500 . ? C24 C30 1.410(4) . ? C24 H24 0.9500 . ? C25 C26 1.362(4) . ? C25 C30 1.412(4) . ? C25 H25 0.9500 . ? C26 C27 1.406(4) . ? C26 H26 0.9500 . ? C27 C28 1.376(3) . ? C27 H27 0.9500 . ? C28 C29 1.420(3) . ? C29 C30 1.420(3) . ? C31 C32 1.497(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.417(4) . ? C33 C34 1.350(4) . ? C33 H33 0.9500 . ? C34 C40 1.415(4) . ? C34 H34 0.9500 . ? C35 C36 1.363(4) . ? C35 C40 1.411(4) . ? C35 H35 0.9500 . ? C36 C37 1.411(3) . ? C36 H36 0.9500 . ? C37 C38 1.373(3) . ? C37 H37 0.9500 . ? C38 C39 1.427(3) . ? C39 C40 1.414(3) . ? C41 C43 1.414(4) . ? C41 C42 1.494(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.349(4) . ? C43 H43 0.9500 . ? C44 C50 1.416(4) . ? C44 H44 0.9500 . ? C45 C46 1.364(4) . ? C45 C50 1.415(4) . ? C45 H45 0.9500 . ? C46 C47 1.411(3) . ? C46 H46 0.9500 . ? C47 C48 1.370(3) . ? C47 H47 0.9500 . ? C48 C49 1.431(3) . ? C49 C50 1.411(3) . ? C51 C52 1.543(3) . ? C52 C53 1.519(4) . ? C52 C55 1.522(4) . ? C52 C54 1.531(4) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.534(3) . ? C57 C60 1.526(4) . ? C57 C59 1.533(4) . ? C57 C58 1.534(3) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C1S O1S 1.158(17) . ? C1S C2S 1.516(14) . ? C1S C2S 1.551(15) 3_556 ? C1S C1S 1.63(3) 3_556 ? C2S C1S 1.551(15) 3_556 ? 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 O12 Ni1 O1 168.08(6) . . ? O12 Ni1 O5 102.71(6) . . ? O1 Ni1 O5 86.00(6) . . ? O12 Ni1 O4 86.22(6) . . ? O1 Ni1 O4 85.89(6) . . ? O5 Ni1 O4 88.50(6) . . ? O12 Ni1 N1 107.65(7) . . ? O1 Ni1 N1 80.11(7) . . ? O5 Ni1 N1 90.21(7) . . ? O4 Ni1 N1 165.99(7) . . ? O12 Ni1 O3 92.68(6) . . ? O1 Ni1 O3 77.70(6) . . ? O5 Ni1 O3 162.74(6) . . ? O4 Ni1 O3 84.73(6) . . ? N1 Ni1 O3 92.53(6) . . ? O6 Ni2 O2 166.87(6) . . ? O6 Ni2 O1 86.04(6) . . ? O2 Ni2 O1 87.11(6) . . ? O6 Ni2 O7 103.77(6) . . ? O2 Ni2 O7 87.23(6) . . ? O1 Ni2 O7 88.57(6) . . ? O6 Ni2 N2 106.76(7) . . ? O2 Ni2 N2 80.71(7) . . ? O1 Ni2 N2 167.05(7) . . ? O7 Ni2 N2 86.48(7) . . ? O6 Ni2 O4 91.56(6) . . ? O2 Ni2 O4 76.59(6) . . ? O1 Ni2 O4 84.09(6) . . ? O7 Ni2 O4 162.51(6) . . ? N2 Ni2 O4 97.23(6) . . ? O8 Ni3 O3 169.32(6) . . ? O8 Ni3 O9 101.77(7) . . ? O3 Ni3 O9 86.53(6) . . ? O8 Ni3 O2 86.97(6) . . ? O3 Ni3 O2 86.60(6) . . ? O9 Ni3 O2 88.17(6) . . ? O8 Ni3 N3 106.33(7) . . ? O3 Ni3 N3 80.35(7) . . ? O9 Ni3 N3 88.34(7) . . ? O2 Ni3 N3 166.67(7) . . ? O8 Ni3 O1 93.24(6) . . ? O3 Ni3 O1 77.66(6) . . ? O9 Ni3 O1 162.94(6) . . ? O2 Ni3 O1 84.55(6) . . ? N3 Ni3 O1 95.22(7) . . ? O10 Ni4 O11 101.52(6) . . ? O10 Ni4 O4 168.33(6) . . ? O11 Ni4 O4 87.21(6) . . ? O10 Ni4 O3 85.73(6) . . ? O11 Ni4 O3 88.06(6) . . ? O4 Ni4 O3 86.85(6) . . ? O10 Ni4 N4 107.67(7) . . ? O11 Ni4 N4 85.37(7) . . ? O4 Ni4 N4 80.51(7) . . ? O3 Ni4 N4 166.01(7) . . ? O10 Ni4 O2 93.54(6) . . ? O11 Ni4 O2 163.07(6) . . ? O4 Ni4 O2 76.87(6) . . ? O3 Ni4 O2 85.38(6) . . ? N4 Ni4 O2 97.47(7) . . ? C18 O1 Ni1 109.38(14) . . ? C18 O1 Ni2 133.42(14) . . ? Ni1 O1 Ni2 95.39(6) . . ? C18 O1 Ni3 119.05(13) . . ? Ni1 O1 Ni3 102.10(6) . . ? Ni2 O1 Ni3 91.87(6) . . ? C28 O2 Ni2 109.46(13) . . ? C28 O2 Ni3 133.20(14) . . ? Ni2 O2 Ni3 93.31(6) . . ? C28 O2 Ni4 120.34(13) . . ? Ni2 O2 Ni4 103.47(6) . . ? Ni3 O2 Ni4 91.32(6) . . ? C38 O3 Ni3 109.09(13) . . ? C38 O3 Ni4 132.35(13) . . ? Ni3 O3 Ni4 93.98(6) . . ? C38 O3 Ni1 121.15(13) . . ? Ni3 O3 Ni1 102.12(6) . . ? Ni4 O3 Ni1 92.11(6) . . ? C48 O4 Ni4 109.33(13) . . ? C48 O4 Ni1 131.61(13) . . ? Ni4 O4 Ni1 93.45(6) . . ? C48 O4 Ni2 121.87(13) . . ? Ni4 O4 Ni2 102.41(6) . . ? Ni1 O4 Ni2 92.06(6) . . ? C1 O5 Ni1 127.23(14) . . ? C1 O6 Ni2 127.29(14) . . ? C6 O7 Ni2 126.50(15) . . ? C6 O8 Ni3 126.73(15) . . ? C51 O9 Ni3 127.32(15) . . ? C51 O10 Ni4 125.44(15) . . ? C56 O11 Ni4 127.43(14) . . ? C56 O12 Ni1 126.21(14) . . ? C12 N1 C19 119.0(2) . . ? C12 N1 Ni1 132.92(17) . . ? C19 N1 Ni1 107.53(14) . . ? C22 N2 C29 119.3(2) . . ? C22 N2 Ni2 131.13(16) . . ? C29 N2 Ni2 107.60(14) . . ? C32 N3 C39 119.0(2) . . ? C32 N3 Ni3 132.71(17) . . ? C39 N3 Ni3 107.41(14) . . ? C41 N4 C49 119.0(2) . . ? C41 N4 Ni4 131.04(19) . . ? C49 N4 Ni4 107.97(14) . . ? O5 C1 O6 126.8(2) . . ? O5 C1 C2 117.8(2) . . ? O6 C1 C2 115.4(2) . . ? C4 C2 C3 109.4(2) . . ? C4 C2 C5 109.9(2) . . ? C3 C2 C5 109.5(2) . . ? C4 C2 C1 108.0(2) . . ? C3 C2 C1 110.7(2) . . ? C5 C2 C1 109.2(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O8 C6 O7 126.2(2) . . ? O8 C6 C7 116.7(2) . . ? O7 C6 C7 117.1(2) . . ? C8 C7 C9 109.4(3) . . ? C8 C7 C6 110.7(2) . . ? C9 C7 C6 108.4(2) . . ? C8 C7 C10 109.9(3) . . ? C9 C7 C10 110.1(2) . . ? C6 C7 C10 108.4(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C13 120.8(2) . . ? N1 C12 C11 119.3(2) . . ? C13 C12 C11 119.9(2) . . ? C14 C13 C12 120.5(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C20 120.4(2) . . ? C13 C14 H14 119.8 . . ? C20 C14 H14 119.8 . . ? C16 C15 C20 120.0(2) . . ? C16 C15 H15 120.0 . . ? C20 C15 H15 120.0 . . ? C15 C16 C17 121.6(3) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C18 C17 C16 119.8(3) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? O1 C18 C17 124.5(2) . . ? O1 C18 C19 115.9(2) . . ? C17 C18 C19 119.5(2) . . ? N1 C19 C20 122.6(2) . . ? N1 C19 C18 117.7(2) . . ? C20 C19 C18 119.7(2) . . ? C19 C20 C14 116.3(3) . . ? C19 C20 C15 118.8(3) . . ? C14 C20 C15 124.9(2) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 C23 120.9(2) . . ? N2 C22 C21 118.6(2) . . ? C23 C22 C21 120.5(2) . . ? C24 C23 C22 120.5(2) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C30 120.3(2) . . ? C23 C24 H24 119.9 . . ? C30 C24 H24 119.9 . . ? C26 C25 C30 119.9(2) . . ? C26 C25 H25 120.1 . . ? C30 C25 H25 120.1 . . ? C25 C26 C27 121.4(2) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C28 C27 C26 120.6(2) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? O2 C28 C27 123.8(2) . . ? O2 C28 C29 117.2(2) . . ? C27 C28 C29 119.0(2) . . ? N2 C29 C28 117.7(2) . . ? N2 C29 C30 122.3(2) . . ? C28 C29 C30 120.0(2) . . ? C24 C30 C25 124.3(2) . . ? C24 C30 C29 116.6(2) . . ? C25 C30 C29 119.1(2) . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 C33 120.9(2) . . ? N3 C32 C31 119.4(2) . . ? C33 C32 C31 119.6(2) . . ? C34 C33 C32 120.7(2) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C40 120.1(2) . . ? C33 C34 H34 119.9 . . ? C40 C34 H34 119.9 . . ? C36 C35 C40 119.9(2) . . ? C36 C35 H35 120.0 . . ? C40 C35 H35 120.0 . . ? C35 C36 C37 121.4(2) . . ? C35 C36 H36 119.3 . . ? C37 C36 H36 119.3 . . ? C38 C37 C36 120.2(2) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? O3 C38 C37 124.3(2) . . ? O3 C38 C39 116.42(19) . . ? C37 C38 C39 119.2(2) . . ? N3 C39 C40 122.7(2) . . ? N3 C39 C38 117.5(2) . . ? C40 C39 C38 119.8(2) . . ? C35 C40 C39 119.2(2) . . ? C35 C40 C34 124.5(2) . . ? C39 C40 C34 116.3(2) . . ? N4 C41 C43 120.9(3) . . ? N4 C41 C42 118.9(2) . . ? C43 C41 C42 120.2(2) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C41 120.9(3) . . ? C44 C43 H43 119.6 . . ? C41 C43 H43 119.6 . . ? C43 C44 C50 119.9(3) . . ? C43 C44 H44 120.1 . . ? C50 C44 H44 120.1 . . ? C46 C45 C50 119.7(2) . . ? C46 C45 H45 120.2 . . ? C50 C45 H45 120.2 . . ? C45 C46 C47 121.1(2) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C48 C47 C46 121.0(2) . . ? C48 C47 H47 119.5 . . ? C46 C47 H47 119.5 . . ? O4 C48 C47 124.3(2) . . ? O4 C48 C49 117.0(2) . . ? C47 C48 C49 118.7(2) . . ? N4 C49 C50 122.6(2) . . ? N4 C49 C48 117.5(2) . . ? C50 C49 C48 119.9(2) . . ? C49 C50 C45 119.5(2) . . ? C49 C50 C44 116.6(3) . . ? C45 C50 C44 123.9(2) . . ? O10 C51 O9 126.5(2) . . ? O10 C51 C52 117.8(2) . . ? O9 C51 C52 115.7(2) . . ? C53 C52 C55 109.7(2) . . ? C53 C52 C54 110.6(3) . . ? C55 C52 C54 109.5(3) . . ? C53 C52 C51 109.2(2) . . ? C55 C52 C51 110.9(2) . . ? C54 C52 C51 106.8(2) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O11 C56 O12 126.3(2) . . ? O11 C56 C57 117.6(2) . . ? O12 C56 C57 116.1(2) . . ? C60 C57 C59 110.0(2) . . ? C60 C57 C58 109.3(2) . . ? C59 C57 C58 110.3(2) . . ? C60 C57 C56 111.4(2) . . ? C59 C57 C56 107.58(19) . . ? C58 C57 C56 108.29(19) . . ? 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 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O1S C1S C2S 112.7(13) . . ? O1S C1S C2S 131.4(13) . 3_556 ? C2S C1S C2S 115.9(9) . 3_556 ? O1S C1S C1S 171.7(18) . 3_556 ? C2S C1S C1S 59.0(8) . 3_556 ? C2S C1S C1S 56.9(8) 3_556 3_556 ? C1S C2S C1S 64.1(9) . 3_556 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 Ni1 O1 C18 159.0(3) . . . . ? O5 Ni1 O1 C18 -63.55(13) . . . . ? O4 Ni1 O1 C18 -152.33(14) . . . . ? N1 Ni1 O1 C18 27.36(13) . . . . ? O3 Ni1 O1 C18 122.17(14) . . . . ? O12 Ni1 O1 Ni2 -61.1(3) . . . . ? O5 Ni1 O1 Ni2 76.36(6) . . . . ? O4 Ni1 O1 Ni2 -12.42(6) . . . . ? N1 Ni1 O1 Ni2 167.27(7) . . . . ? O3 Ni1 O1 Ni2 -97.91(6) . . . . ? O12 Ni1 O1 Ni3 32.0(3) . . . . ? O5 Ni1 O1 Ni3 169.45(7) . . . . ? O4 Ni1 O1 Ni3 80.67(6) . . . . ? N1 Ni1 O1 Ni3 -99.64(7) . . . . ? O3 Ni1 O1 Ni3 -4.83(6) . . . . ? O6 Ni2 O1 C18 43.39(19) . . . . ? O2 Ni2 O1 C18 -147.82(19) . . . . ? O7 Ni2 O1 C18 -60.52(19) . . . . ? N2 Ni2 O1 C18 -128.0(3) . . . . ? O4 Ni2 O1 C18 135.38(19) . . . . ? O6 Ni2 O1 Ni1 -79.86(6) . . . . ? O2 Ni2 O1 Ni1 88.93(6) . . . . ? O7 Ni2 O1 Ni1 176.23(6) . . . . ? N2 Ni2 O1 Ni1 108.7(3) . . . . ? O4 Ni2 O1 Ni1 12.13(6) . . . . ? O6 Ni2 O1 Ni3 177.80(6) . . . . ? O2 Ni2 O1 Ni3 -13.41(6) . . . . ? O7 Ni2 O1 Ni3 73.89(6) . . . . ? N2 Ni2 O1 Ni3 6.4(3) . . . . ? O4 Ni2 O1 Ni3 -90.21(6) . . . . ? O8 Ni3 O1 C18 70.19(16) . . . . ? O3 Ni3 O1 C18 -115.46(16) . . . . ? O9 Ni3 O1 C18 -138.0(2) . . . . ? O2 Ni3 O1 C18 156.83(16) . . . . ? N3 Ni3 O1 C18 -36.55(17) . . . . ? O8 Ni3 O1 Ni1 -169.32(7) . . . . ? O3 Ni3 O1 Ni1 5.02(6) . . . . ? O9 Ni3 O1 Ni1 -17.5(2) . . . . ? O2 Ni3 O1 Ni1 -82.68(7) . . . . ? N3 Ni3 O1 Ni1 83.94(7) . . . . ? O8 Ni3 O1 Ni2 -73.40(7) . . . . ? O3 Ni3 O1 Ni2 100.95(6) . . . . ? O9 Ni3 O1 Ni2 78.4(2) . . . . ? O2 Ni3 O1 Ni2 13.25(6) . . . . ? N3 Ni3 O1 Ni2 179.86(7) . . . . ? O6 Ni2 O2 C28 -149.3(3) . . . . ? O1 Ni2 O2 C28 152.10(14) . . . . ? O7 Ni2 O2 C28 63.39(14) . . . . ? N2 Ni2 O2 C28 -23.49(14) . . . . ? O4 Ni2 O2 C28 -123.29(14) . . . . ? O6 Ni2 O2 Ni3 72.3(3) . . . . ? O1 Ni2 O2 Ni3 13.71(6) . . . . ? O7 Ni2 O2 Ni3 -75.00(6) . . . . ? N2 Ni2 O2 Ni3 -161.89(7) . . . . ? O4 Ni2 O2 Ni3 98.32(6) . . . . ? O6 Ni2 O2 Ni4 -19.8(3) . . . . ? O1 Ni2 O2 Ni4 -78.44(7) . . . . ? O7 Ni2 O2 Ni4 -167.15(7) . . . . ? N2 Ni2 O2 Ni4 105.96(8) . . . . ? O4 Ni2 O2 Ni4 6.17(6) . . . . ? O8 Ni3 O2 C28 -40.56(19) . . . . ? O3 Ni3 O2 C28 147.97(19) . . . . ? O9 Ni3 O2 C28 61.34(19) . . . . ? N3 Ni3 O2 C28 136.2(3) . . . . ? O1 Ni3 O2 C28 -134.11(19) . . . . ? O8 Ni3 O2 Ni2 80.25(7) . . . . ? O3 Ni3 O2 Ni2 -91.22(6) . . . . ? O9 Ni3 O2 Ni2 -177.86(6) . . . . ? N3 Ni3 O2 Ni2 -103.0(3) . . . . ? O1 Ni3 O2 Ni2 -13.30(6) . . . . ? O8 Ni3 O2 Ni4 -176.18(6) . . . . ? O3 Ni3 O2 Ni4 12.35(6) . . . . ? O9 Ni3 O2 Ni4 -74.29(6) . . . . ? N3 Ni3 O2 Ni4 0.6(3) . . . . ? O1 Ni3 O2 Ni4 90.27(6) . . . . ? O10 Ni4 O2 C28 -70.63(16) . . . . ? O11 Ni4 O2 C28 136.4(2) . . . . ? O4 Ni4 O2 C28 116.11(16) . . . . ? O3 Ni4 O2 C28 -156.05(16) . . . . ? N4 Ni4 O2 C28 37.72(17) . . . . ? O10 Ni4 O2 Ni2 166.88(7) . . . . ? O11 Ni4 O2 Ni2 13.9(2) . . . . ? O4 Ni4 O2 Ni2 -6.38(6) . . . . ? O3 Ni4 O2 Ni2 81.46(7) . . . . ? N4 Ni4 O2 Ni2 -84.77(8) . . . . ? O10 Ni4 O2 Ni3 73.16(6) . . . . ? O11 Ni4 O2 Ni3 -79.8(2) . . . . ? O4 Ni4 O2 Ni3 -100.10(6) . . . . ? O3 Ni4 O2 Ni3 -12.26(6) . . . . ? N4 Ni4 O2 Ni3 -178.48(7) . . . . ? O8 Ni3 O3 C38 156.6(3) . . . . ? O9 Ni3 O3 C38 -61.95(13) . . . . ? O2 Ni3 O3 C38 -150.31(13) . . . . ? N3 Ni3 O3 C38 26.96(13) . . . . ? O1 Ni3 O3 C38 124.53(13) . . . . ? O8 Ni3 O3 Ni4 -65.8(4) . . . . ? O9 Ni3 O3 Ni4 75.67(6) . . . . ? O2 Ni3 O3 Ni4 -12.69(6) . . . . ? N3 Ni3 O3 Ni4 164.58(7) . . . . ? O1 Ni3 O3 Ni4 -97.85(6) . . . . ? O8 Ni3 O3 Ni1 27.2(4) . . . . ? O9 Ni3 O3 Ni1 168.70(7) . . . . ? O2 Ni3 O3 Ni1 80.33(6) . . . . ? N3 Ni3 O3 Ni1 -102.40(7) . . . . ? O1 Ni3 O3 Ni1 -4.83(6) . . . . ? O10 Ni4 O3 C38 39.09(18) . . . . ? O11 Ni4 O3 C38 -62.62(18) . . . . ? O4 Ni4 O3 C38 -149.93(18) . . . . ? N4 Ni4 O3 C38 -124.6(3) . . . . ? O2 Ni4 O3 C38 133.00(18) . . . . ? O10 Ni4 O3 Ni3 -81.38(6) . . . . ? O11 Ni4 O3 Ni3 176.92(6) . . . . ? O4 Ni4 O3 Ni3 89.60(6) . . . . ? N4 Ni4 O3 Ni3 114.9(3) . . . . ? O2 Ni4 O3 Ni3 12.53(6) . . . . ? O10 Ni4 O3 Ni1 176.32(6) . . . . ? O11 Ni4 O3 Ni1 74.61(6) . . . . ? O4 Ni4 O3 Ni1 -12.71(6) . . . . ? N4 Ni4 O3 Ni1 12.6(3) . . . . ? O2 Ni4 O3 Ni1 -89.78(6) . . . . ? O12 Ni1 O3 C38 70.77(16) . . . . ? O1 Ni1 O3 C38 -116.35(16) . . . . ? O5 Ni1 O3 C38 -135.9(2) . . . . ? O4 Ni1 O3 C38 156.72(16) . . . . ? N1 Ni1 O3 C38 -37.05(16) . . . . ? O12 Ni1 O3 Ni3 -167.86(6) . . . . ? O1 Ni1 O3 Ni3 5.03(6) . . . . ? O5 Ni1 O3 Ni3 -14.6(2) . . . . ? O4 Ni1 O3 Ni3 -81.90(6) . . . . ? N1 Ni1 O3 Ni3 84.33(7) . . . . ? O12 Ni1 O3 Ni4 -73.33(6) . . . . ? O1 Ni1 O3 Ni4 99.55(6) . . . . ? O5 Ni1 O3 Ni4 80.0(2) . . . . ? O4 Ni1 O3 Ni4 12.62(6) . . . . ? N1 Ni1 O3 Ni4 178.85(7) . . . . ? O10 Ni4 O4 C48 -159.8(3) . . . . ? O11 Ni4 O4 C48 61.36(13) . . . . ? O3 Ni4 O4 C48 149.57(13) . . . . ? N4 Ni4 O4 C48 -24.41(13) . . . . ? O2 Ni4 O4 C48 -124.45(14) . . . . ? O10 Ni4 O4 Ni1 63.6(3) . . . . ? O11 Ni4 O4 Ni1 -75.21(6) . . . . ? O3 Ni4 O4 Ni1 13.00(6) . . . . ? N4 Ni4 O4 Ni1 -160.97(7) . . . . ? O2 Ni4 O4 Ni1 98.99(6) . . . . ? O10 Ni4 O4 Ni2 -29.3(3) . . . . ? O11 Ni4 O4 Ni2 -168.09(7) . . . . ? O3 Ni4 O4 Ni2 -79.87(6) . . . . ? N4 Ni4 O4 Ni2 106.15(7) . . . . ? O2 Ni4 O4 Ni2 6.11(6) . . . . ? O12 Ni1 O4 C48 -39.40(18) . . . . ? O1 Ni1 O4 C48 149.54(18) . . . . ? O5 Ni1 O4 C48 63.45(18) . . . . ? N1 Ni1 O4 C48 148.3(3) . . . . ? O3 Ni1 O4 C48 -132.45(18) . . . . ? O12 Ni1 O4 Ni4 80.41(6) . . . . ? O1 Ni1 O4 Ni4 -90.65(6) . . . . ? O5 Ni1 O4 Ni4 -176.75(6) . . . . ? N1 Ni1 O4 Ni4 -91.9(3) . . . . ? O3 Ni1 O4 Ni4 -12.64(6) . . . . ? O12 Ni1 O4 Ni2 -177.02(6) . . . . ? O1 Ni1 O4 Ni2 11.92(6) . . . . ? O5 Ni1 O4 Ni2 -74.18(6) . . . . ? N1 Ni1 O4 Ni2 10.7(3) . . . . ? O3 Ni1 O4 Ni2 89.93(6) . . . . ? O6 Ni2 O4 C48 -69.61(16) . . . . ? O2 Ni2 O4 C48 116.11(16) . . . . ? O1 Ni2 O4 C48 -155.47(16) . . . . ? O7 Ni2 O4 C48 138.9(2) . . . . ? N2 Ni2 O4 C48 37.50(16) . . . . ? O6 Ni2 O4 Ni4 167.98(6) . . . . ? O2 Ni2 O4 Ni4 -6.30(6) . . . . ? O1 Ni2 O4 Ni4 82.13(6) . . . . ? O7 Ni2 O4 Ni4 16.5(2) . . . . ? N2 Ni2 O4 Ni4 -84.91(7) . . . . ? O6 Ni2 O4 Ni1 73.99(6) . . . . ? O2 Ni2 O4 Ni1 -100.29(6) . . . . ? O1 Ni2 O4 Ni1 -11.86(6) . . . . ? O7 Ni2 O4 Ni1 -77.5(2) . . . . ? N2 Ni2 O4 Ni1 -178.90(7) . . . . ? O12 Ni1 O5 C1 136.58(17) . . . . ? O1 Ni1 O5 C1 -35.19(17) . . . . ? O4 Ni1 O5 C1 50.79(17) . . . . ? N1 Ni1 O5 C1 -115.26(18) . . . . ? O3 Ni1 O5 C1 -16.0(3) . . . . ? O2 Ni2 O6 C1 -17.2(4) . . . . ? O1 Ni2 O6 C1 41.52(18) . . . . ? O7 Ni2 O6 C1 129.07(17) . . . . ? N2 Ni2 O6 C1 -140.48(17) . . . . ? O4 Ni2 O6 C1 -42.45(18) . . . . ? O6 Ni2 O7 C6 -141.37(18) . . . . ? O2 Ni2 O7 C6 31.38(19) . . . . ? O1 Ni2 O7 C6 -55.80(19) . . . . ? N2 Ni2 O7 C6 112.23(19) . . . . ? O4 Ni2 O7 C6 9.2(3) . . . . ? O3 Ni3 O8 C6 12.1(5) . . . . ? O9 Ni3 O8 C6 -128.43(19) . . . . ? O2 Ni3 O8 C6 -40.94(19) . . . . ? N3 Ni3 O8 C6 139.83(19) . . . . ? O1 Ni3 O8 C6 43.42(19) . . . . ? O8 Ni3 O9 C51 143.63(18) . . . . ? O3 Ni3 O9 C51 -29.60(19) . . . . ? O2 Ni3 O9 C51 57.10(19) . . . . ? N3 Ni3 O9 C51 -110.03(19) . . . . ? O1 Ni3 O9 C51 -7.5(3) . . . . ? O11 Ni4 O10 C51 128.87(18) . . . . ? O4 Ni4 O10 C51 -9.0(4) . . . . ? O3 Ni4 O10 C51 41.73(18) . . . . ? N4 Ni4 O10 C51 -142.36(18) . . . . ? O2 Ni4 O10 C51 -43.36(18) . . . . ? O10 Ni4 O11 C56 -140.85(18) . . . . ? O4 Ni4 O11 C56 31.34(18) . . . . ? O3 Ni4 O11 C56 -55.60(18) . . . . ? N4 Ni4 O11 C56 112.04(18) . . . . ? O2 Ni4 O11 C56 11.6(3) . . . . ? O1 Ni1 O12 C56 5.8(4) . . . . ? O5 Ni1 O12 C56 -130.49(17) . . . . ? O4 Ni1 O12 C56 -42.89(17) . . . . ? N1 Ni1 O12 C56 135.17(17) . . . . ? O3 Ni1 O12 C56 41.65(17) . . . . ? O12 Ni1 N1 C12 -4.3(2) . . . . ? O1 Ni1 N1 C12 166.4(2) . . . . ? O5 Ni1 N1 C12 -107.7(2) . . . . ? O4 Ni1 N1 C12 167.7(2) . . . . ? O3 Ni1 N1 C12 89.3(2) . . . . ? O12 Ni1 N1 C19 167.27(14) . . . . ? O1 Ni1 N1 C19 -22.05(14) . . . . ? O5 Ni1 N1 C19 63.85(14) . . . . ? O4 Ni1 N1 C19 -20.8(4) . . . . ? O3 Ni1 N1 C19 -99.10(14) . . . . ? O6 Ni2 N2 C22 -6.1(2) . . . . ? O2 Ni2 N2 C22 -175.0(2) . . . . ? O1 Ni2 N2 C22 165.0(3) . . . . ? O7 Ni2 N2 C22 97.2(2) . . . . ? O4 Ni2 N2 C22 -99.9(2) . . . . ? O6 Ni2 N2 C29 -169.60(14) . . . . ? O2 Ni2 N2 C29 21.50(14) . . . . ? O1 Ni2 N2 C29 1.5(4) . . . . ? O7 Ni2 N2 C29 -66.27(15) . . . . ? O4 Ni2 N2 C29 96.56(14) . . . . ? O8 Ni3 N3 C32 -2.4(2) . . . . ? O3 Ni3 N3 C32 169.0(2) . . . . ? O9 Ni3 N3 C32 -104.2(2) . . . . ? O2 Ni3 N3 C32 -179.1(2) . . . . ? O1 Ni3 N3 C32 92.5(2) . . . . ? O8 Ni3 N3 C39 166.15(14) . . . . ? O3 Ni3 N3 C39 -22.40(14) . . . . ? O9 Ni3 N3 C39 64.37(14) . . . . ? O2 Ni3 N3 C39 -10.5(4) . . . . ? O1 Ni3 N3 C39 -98.91(14) . . . . ? O10 Ni4 N4 C41 -3.6(2) . . . . ? O11 Ni4 N4 C41 97.0(2) . . . . ? O4 Ni4 N4 C41 -175.1(2) . . . . ? O3 Ni4 N4 C41 159.2(3) . . . . ? O2 Ni4 N4 C41 -99.8(2) . . . . ? O10 Ni4 N4 C49 -167.15(14) . . . . ? O11 Ni4 N4 C49 -66.52(15) . . . . ? O4 Ni4 N4 C49 21.42(14) . . . . ? O3 Ni4 N4 C49 -4.3(4) . . . . ? O2 Ni4 N4 C49 96.70(15) . . . . ? Ni1 O5 C1 O6 -10.4(3) . . . . ? Ni1 O5 C1 C2 172.04(14) . . . . ? Ni2 O6 C1 O5 6.2(3) . . . . ? Ni2 O6 C1 C2 -176.19(14) . . . . ? O5 C1 C2 C4 104.8(3) . . . . ? O6 C1 C2 C4 -73.0(3) . . . . ? O5 C1 C2 C3 -15.0(3) . . . . ? O6 C1 C2 C3 167.2(2) . . . . ? O5 C1 C2 C5 -135.6(2) . . . . ? O6 C1 C2 C5 46.5(3) . . . . ? Ni3 O8 C6 O7 -11.9(3) . . . . ? Ni3 O8 C6 C7 168.99(16) . . . . ? Ni2 O7 C6 O8 18.3(3) . . . . ? Ni2 O7 C6 C7 -162.60(16) . . . . ? O8 C6 C7 C8 -8.7(3) . . . . ? O7 C6 C7 C8 172.1(2) . . . . ? O8 C6 C7 C9 111.3(3) . . . . ? O7 C6 C7 C9 -67.9(3) . . . . ? O8 C6 C7 C10 -129.2(2) . . . . ? O7 C6 C7 C10 51.5(3) . . . . ? C19 N1 C12 C13 -0.8(3) . . . . ? Ni1 N1 C12 C13 170.03(17) . . . . ? C19 N1 C12 C11 177.6(2) . . . . ? Ni1 N1 C12 C11 -11.6(3) . . . . ? N1 C12 C13 C14 -3.0(4) . . . . ? C11 C12 C13 C14 178.7(2) . . . . ? C12 C13 C14 C20 2.0(4) . . . . ? C20 C15 C16 C17 3.5(4) . . . . ? C15 C16 C17 C18 -2.1(4) . . . . ? Ni1 O1 C18 C17 153.8(2) . . . . ? Ni2 O1 C18 C17 35.8(3) . . . . ? Ni3 O1 C18 C17 -89.5(2) . . . . ? Ni1 O1 C18 C19 -28.1(2) . . . . ? Ni2 O1 C18 C19 -146.17(16) . . . . ? Ni3 O1 C18 C19 88.6(2) . . . . ? C16 C17 C18 O1 174.0(2) . . . . ? C16 C17 C18 C19 -4.0(4) . . . . ? C12 N1 C19 C20 5.6(3) . . . . ? Ni1 N1 C19 C20 -167.33(19) . . . . ? C12 N1 C19 C18 -173.1(2) . . . . ? Ni1 N1 C19 C18 13.9(2) . . . . ? O1 C18 C19 N1 9.3(3) . . . . ? C17 C18 C19 N1 -172.6(2) . . . . ? O1 C18 C19 C20 -169.5(2) . . . . ? C17 C18 C19 C20 8.6(3) . . . . ? N1 C19 C20 C14 -6.4(4) . . . . ? C18 C19 C20 C14 172.3(2) . . . . ? N1 C19 C20 C15 174.1(2) . . . . ? C18 C19 C20 C15 -7.2(4) . . . . ? C13 C14 C20 C19 2.5(4) . . . . ? C13 C14 C20 C15 -178.1(3) . . . . ? C16 C15 C20 C19 1.2(4) . . . . ? C16 C15 C20 C14 -178.2(3) . . . . ? C29 N2 C22 C23 3.1(3) . . . . ? Ni2 N2 C22 C23 -158.79(18) . . . . ? C29 N2 C22 C21 -176.1(2) . . . . ? Ni2 N2 C22 C21 22.0(3) . . . . ? N2 C22 C23 C24 -0.9(4) . . . . ? C21 C22 C23 C24 178.3(2) . . . . ? C22 C23 C24 C30 -2.0(4) . . . . ? C30 C25 C26 C27 0.8(4) . . . . ? C25 C26 C27 C28 -1.9(4) . . . . ? Ni2 O2 C28 C27 -159.4(2) . . . . ? Ni3 O2 C28 C27 -44.8(3) . . . . ? Ni4 O2 C28 C27 81.1(3) . . . . ? Ni2 O2 C28 C29 21.6(2) . . . . ? Ni3 O2 C28 C29 136.20(18) . . . . ? Ni4 O2 C28 C29 -97.9(2) . . . . ? C26 C27 C28 O2 -176.6(2) . . . . ? C26 C27 C28 C29 2.4(4) . . . . ? C22 N2 C29 C28 177.5(2) . . . . ? Ni2 N2 C29 C28 -16.8(2) . . . . ? C22 N2 C29 C30 -2.6(3) . . . . ? Ni2 N2 C29 C30 163.22(18) . . . . ? O2 C28 C29 N2 -3.0(3) . . . . ? C27 C28 C29 N2 177.9(2) . . . . ? O2 C28 C29 C30 177.0(2) . . . . ? C27 C28 C29 C30 -2.0(3) . . . . ? C23 C24 C30 C25 -178.9(2) . . . . ? C23 C24 C30 C29 2.5(4) . . . . ? C26 C25 C30 C24 -179.0(2) . . . . ? C26 C25 C30 C29 -0.5(4) . . . . ? N2 C29 C30 C24 -0.2(3) . . . . ? C28 C29 C30 C24 179.7(2) . . . . ? N2 C29 C30 C25 -178.9(2) . . . . ? C28 C29 C30 C25 1.1(3) . . . . ? C39 N3 C32 C33 -1.3(4) . . . . ? Ni3 N3 C32 C33 166.22(19) . . . . ? C39 N3 C32 C31 179.3(2) . . . . ? Ni3 N3 C32 C31 -13.2(4) . . . . ? N3 C32 C33 C34 -3.1(4) . . . . ? C31 C32 C33 C34 176.3(3) . . . . ? C32 C33 C34 C40 3.1(4) . . . . ? C40 C35 C36 C37 2.4(4) . . . . ? C35 C36 C37 C38 -0.6(4) . . . . ? Ni3 O3 C38 C37 154.18(19) . . . . ? Ni4 O3 C38 C37 39.7(3) . . . . ? Ni1 O3 C38 C37 -87.9(2) . . . . ? Ni3 O3 C38 C39 -27.1(2) . . . . ? Ni4 O3 C38 C39 -141.64(16) . . . . ? Ni1 O3 C38 C39 90.8(2) . . . . ? C36 C37 C38 O3 174.9(2) . . . . ? C36 C37 C38 C39 -3.7(3) . . . . ? C32 N3 C39 C40 5.8(3) . . . . ? Ni3 N3 C39 C40 -164.63(18) . . . . ? C32 N3 C39 C38 -174.7(2) . . . . ? Ni3 N3 C39 C38 14.9(2) . . . . ? O3 C38 C39 N3 8.0(3) . . . . ? C37 C38 C39 N3 -173.2(2) . . . . ? O3 C38 C39 C40 -172.5(2) . . . . ? C37 C38 C39 C40 6.3(3) . . . . ? C36 C35 C40 C39 0.2(4) . . . . ? C36 C35 C40 C34 -179.1(2) . . . . ? N3 C39 C40 C35 175.0(2) . . . . ? C38 C39 C40 C35 -4.5(3) . . . . ? N3 C39 C40 C34 -5.7(3) . . . . ? C38 C39 C40 C34 174.8(2) . . . . ? C33 C34 C40 C35 -179.6(3) . . . . ? C33 C34 C40 C39 1.1(4) . . . . ? C49 N4 C41 C43 0.4(4) . . . . ? Ni4 N4 C41 C43 -161.6(2) . . . . ? C49 N4 C41 C42 -179.6(3) . . . . ? Ni4 N4 C41 C42 18.4(4) . . . . ? N4 C41 C43 C44 1.9(5) . . . . ? C42 C41 C43 C44 -178.1(3) . . . . ? C41 C43 C44 C50 -1.4(5) . . . . ? C50 C45 C46 C47 -1.1(4) . . . . ? C45 C46 C47 C48 0.2(4) . . . . ? Ni4 O4 C48 C47 -156.59(19) . . . . ? Ni1 O4 C48 C47 -43.2(3) . . . . ? Ni2 O4 C48 C47 84.3(2) . . . . ? Ni4 O4 C48 C49 23.4(2) . . . . ? Ni1 O4 C48 C49 136.73(17) . . . . ? Ni2 O4 C48 C49 -95.7(2) . . . . ? C46 C47 C48 O4 -178.0(2) . . . . ? C46 C47 C48 C49 2.1(3) . . . . ? C41 N4 C49 C50 -3.3(3) . . . . ? Ni4 N4 C49 C50 162.57(19) . . . . ? C41 N4 C49 C48 178.4(2) . . . . ? Ni4 N4 C49 C48 -15.7(2) . . . . ? O4 C48 C49 N4 -5.0(3) . . . . ? C47 C48 C49 N4 174.9(2) . . . . ? O4 C48 C49 C50 176.6(2) . . . . ? C47 C48 C49 C50 -3.4(3) . . . . ? N4 C49 C50 C45 -175.7(2) . . . . ? C48 C49 C50 C45 2.6(3) . . . . ? N4 C49 C50 C44 3.6(4) . . . . ? C48 C49 C50 C44 -178.1(2) . . . . ? C46 C45 C50 C49 -0.3(4) . . . . ? C46 C45 C50 C44 -179.6(3) . . . . ? C43 C44 C50 C49 -1.2(4) . . . . ? C43 C44 C50 C45 178.1(3) . . . . ? Ni4 O10 C51 O9 11.8(3) . . . . ? Ni4 O10 C51 C52 -171.35(15) . . . . ? Ni3 O9 C51 O10 -19.8(3) . . . . ? Ni3 O9 C51 C52 163.29(15) . . . . ? O10 C51 C52 C53 140.7(2) . . . . ? O9 C51 C52 C53 -42.1(3) . . . . ? O10 C51 C52 C55 19.7(3) . . . . ? O9 C51 C52 C55 -163.1(2) . . . . ? O10 C51 C52 C54 -99.6(3) . . . . ? O9 C51 C52 C54 77.6(3) . . . . ? Ni4 O11 C56 O12 16.6(3) . . . . ? Ni4 O11 C56 C57 -164.21(14) . . . . ? Ni1 O12 C56 O11 -9.1(3) . . . . ? Ni1 O12 C56 C57 171.71(14) . . . . ? O11 C56 C57 C60 5.9(3) . . . . ? O12 C56 C57 C60 -174.8(2) . . . . ? O11 C56 C57 C59 -114.7(2) . . . . ? O12 C56 C57 C59 64.6(3) . . . . ? O11 C56 C57 C58 126.1(2) . . . . ? O12 C56 C57 C58 -54.6(3) . . . . ? O1S C1S C2S C1S -179.7(19) . . . 3_556 ? C2S C1S C2S C1S 0.000(2) 3_556 . . 3_556 ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.920 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.063