# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_Colacio _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ; Rational Design of Ferromagnetic Coupled Diphenoxocarboxylate Triply Bridged Nickel(II) Complexes: The Role of the Countercomplementarity of the Bridging Ligands ; _publ_contact_author_name 'Antonio Rodriquez-Dieguez' _publ_contact_author_address ; Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias, Universidad de Granada, Av. Fuentenueva s/n, 18071 Granada, Spain ; _publ_contact_author_email antonio5@ugr.es _publ_contact_author_phone '34 958 240442' _publ_contact_author_fax '34 958 248526' loop_ _publ_author_name _publ_author_address J.Ruiz ; Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias, Universidad de Granada, Av. Fuentenueva s/n, 18071 Granada, Spain ; A.J.Mota ; Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias, Universidad de Granada, Av. Fuentenueva s/n, 18071 Granada, Spain ; A.Rodriquez-Dieguez ; Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias, Universidad de Granada, Av. Fuentenueva s/n, 18071 Granada, Spain ; I.Oyartzabal ; Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias, Universidad de Granada, Av. Fuentenueva s/n, 18071 Granada, Spain ; J.M.Seco ; Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias, Universidad de Granada, Av. Fuentenueva s/n, 18071 Granada, Spain ; ; E.Colacio ; ; Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias, Universidad de Granada, Av. Fuentenueva s/n, 18071 Granada, Spain ; data_Compound1 _database_code_depnum_ccdc_archive 'CCDC 892614' #TrackingRef 'Colacio_Ni.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H44 N4 Ni2 O11' _chemical_formula_weight 718.08 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 12.782(5) _cell_length_b 13.864(5) _cell_length_c 20.835(5) _cell_angle_alpha 90.00 _cell_angle_beta 123.340(15) _cell_angle_gamma 90.00 _cell_volume 3084.5(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9033 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.13 _exptl_crystal_description Prismatic _exptl_crystal_colour Blue-green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 1.286 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.635 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Axs APEX automatic diffractometer' _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 34809 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6993 _reflns_number_gt 5871 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker smart' _computing_cell_refinement 'Bruker smart' _computing_data_reduction 'Bruker smart' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 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. 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^)+(0.0481P)^2^+1.8363P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6993 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0938 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.28383(2) 0.239821(19) 0.015445(15) 0.01456(8) Uani 1 1 d . . . Ni2 Ni 0.49798(2) 0.379310(19) 0.103449(15) 0.01465(8) Uani 1 1 d . . . C1A C 0.32776(19) 0.35672(15) 0.14629(11) 0.0152(4) Uani 1 1 d . . . C2A C 0.3709(2) 0.45057(16) 0.17385(12) 0.0165(4) Uani 1 1 d . . . C3A C 0.3083(2) 0.51003(16) 0.19554(12) 0.0195(5) Uani 1 1 d . . . H3A H 0.3366 0.5726 0.2120 0.023 Uiso 1 1 calc R . . C3B C 0.2425(2) 0.44960(16) -0.01555(12) 0.0173(4) Uani 1 1 d . . . C4A C 0.2029(2) 0.47629(16) 0.19269(12) 0.0197(5) Uani 1 1 d . . . C4B C 0.1576(2) 0.53634(17) -0.04384(16) 0.0308(6) Uani 1 1 d . . . H4B1 H 0.1245 0.5465 -0.0973 0.046 Uiso 1 1 d R . . H4B2 H 0.2041 0.5922 -0.0150 0.046 Uiso 1 1 d R . . H4B3 H 0.0898 0.5256 -0.0372 0.046 Uiso 1 1 d R . . C5A C 0.1625(2) 0.38242(16) 0.16801(12) 0.0189(4) Uani 1 1 d . . . H5A H 0.0934 0.3590 0.1670 0.023 Uiso 1 1 calc R . . C6A C 0.2239(2) 0.32245(15) 0.14466(12) 0.0167(4) Uani 1 1 d . . . C7A C 0.1865(2) 0.21930(16) 0.11962(13) 0.0190(4) Uani 1 1 d . . . H7A1 H 0.2584 0.1779 0.1512 0.023 Uiso 1 1 calc R . . H7A2 H 0.1219 0.2010 0.1282 0.023 Uiso 1 1 calc R . . C8A C 0.1209(2) 0.09825(16) 0.01992(14) 0.0239(5) Uani 1 1 d . . . H8A1 H 0.0727 0.0887 -0.0353 0.029 Uiso 1 1 calc R . . H8A2 H 0.0734 0.0715 0.0394 0.029 Uiso 1 1 calc R . . C9A C 0.2452(2) 0.04471(17) 0.05603(14) 0.0251(5) Uani 1 1 d . . . H9A1 H 0.2801 0.0360 0.1104 0.030 Uiso 1 1 calc R . . H9A2 H 0.2295 -0.0188 0.0329 0.030 Uiso 1 1 calc R . . C10A C 0.3466(2) 0.05457(16) -0.01687(13) 0.0208(5) Uani 1 1 d . . . H10A H 0.3493 -0.0153 -0.0134 0.025 Uiso 1 1 calc R . . H10B H 0.4235 0.0761 -0.0112 0.025 Uiso 1 1 calc R . . C11A C 0.2365(2) 0.08443(16) -0.09517(13) 0.0212(5) Uani 1 1 d . . . H11A H 0.2532 0.0672 -0.1339 0.025 Uiso 1 1 calc R . . H11B H 0.1625 0.0494 -0.1064 0.025 Uiso 1 1 calc R . . C12A C 0.2760(2) 0.24643(16) -0.12981(12) 0.0180(4) Uani 1 1 d . . . H12A H 0.2643 0.3145 -0.1248 0.022 Uiso 1 1 calc R . . H12B H 0.2335 0.2328 -0.1843 0.022 Uiso 1 1 calc R . . C13A C 0.4137(2) 0.22917(15) -0.09329(12) 0.0158(4) Uani 1 1 d . . . C14A C 0.4569(2) 0.20367(15) -0.13979(12) 0.0181(4) Uani 1 1 d . . . H14A H 0.3990 0.1906 -0.1915 0.022 Uiso 1 1 calc R . . C15A C 0.5834(2) 0.19726(15) -0.11101(13) 0.0184(4) Uani 1 1 d . . . C16A C 0.6677(2) 0.21137(15) -0.03210(12) 0.0174(4) Uani 1 1 d . . . H16A H 0.7531 0.2063 -0.0112 0.021 Uiso 1 1 calc R . . C17A C 0.6272(2) 0.23269(15) 0.01570(12) 0.0160(4) Uani 1 1 d . . . C18A C 0.4980(2) 0.24665(14) -0.01490(12) 0.0154(4) Uani 1 1 d . . . C19A C 0.1345(2) 0.54389(18) 0.21511(14) 0.0274(5) Uani 1 1 d . . . H19A H 0.0832 0.5874 0.1734 0.041 Uiso 1 1 d R . . H19B H 0.1946 0.5801 0.2598 0.041 Uiso 1 1 d R . . H19C H 0.0827 0.5071 0.2263 0.041 Uiso 1 1 d R . . C20A C 0.6293(2) 0.17883(18) -0.16287(13) 0.0245(5) Uani 1 1 d . . . H20A H 0.6020 0.1162 -0.1858 0.037 Uiso 1 1 d R . . H20B H 0.7191 0.1815 -0.1333 0.037 Uiso 1 1 d R . . H20C H 0.5960 0.2270 -0.2025 0.037 Uiso 1 1 d R . . C21A C 0.5037(2) 0.57692(16) 0.17674(14) 0.0239(5) Uani 1 1 d . . . H21A H 0.4326 0.6057 0.1321 0.036 Uiso 1 1 d R . . H21B H 0.5764 0.5851 0.1747 0.036 Uiso 1 1 d R . . H21C H 0.5175 0.6075 0.2221 0.036 Uiso 1 1 d R . . C31A C 0.0168(2) 0.25245(17) -0.00978(14) 0.0232(5) Uani 1 1 d . . . H31A H -0.0165 0.2428 -0.0633 0.035 Uiso 1 1 d R . . H31B H 0.0276 0.3202 0.0015 0.035 Uiso 1 1 d R . . H31C H -0.0401 0.2263 0.0022 0.035 Uiso 1 1 d R . . C32A C 0.4654(2) 0.08634(17) 0.11889(13) 0.0261(5) Uani 1 1 d . . . H32A H 0.4875 0.0194 0.1297 0.039 Uiso 1 1 d R . . H32B H 0.4641 0.1147 0.1605 0.039 Uiso 1 1 d R . . H32C H 0.5259 0.1191 0.1131 0.039 Uiso 1 1 d R . . C33A C 0.0763(2) 0.20746(18) -0.15563(13) 0.0238(5) Uani 1 1 d . . . H33A H 0.0529 0.1840 -0.2052 0.036 Uiso 1 1 d R . . H33B H 0.0595 0.2754 -0.1588 0.036 Uiso 1 1 d R . . H33C H 0.0288 0.1743 -0.1393 0.036 Uiso 1 1 d R . . C41A C 0.8349(2) 0.21314(18) 0.12764(14) 0.0243(5) Uani 1 1 d . . . H41A H 0.8368 0.1486 0.1116 0.036 Uiso 1 1 d R . . H41B H 0.8791 0.2153 0.1826 0.036 Uiso 1 1 d R . . H41C H 0.8741 0.2561 0.1108 0.036 Uiso 1 1 d R . . N1A N 0.13900(17) 0.20317(13) 0.03673(11) 0.0186(4) Uani 1 1 d . . . N1N N -0.12043(18) 0.49709(15) 0.28565(12) 0.0268(4) Uani 1 1 d . . . N2A N 0.33972(18) 0.09512(13) 0.04685(11) 0.0198(4) Uani 1 1 d . . . N3A N 0.21158(16) 0.19009(13) -0.09941(10) 0.0175(4) Uani 1 1 d . . . O1A O 0.38635(13) 0.30187(10) 0.12282(8) 0.0149(3) Uani 1 1 d . . . O1B O 0.19365(14) 0.36798(11) -0.02897(9) 0.0182(3) Uani 1 1 d . . . O1N O -0.18407(18) 0.44678(14) 0.30167(10) 0.0374(5) Uani 1 1 d . . . O1W O 0.65389(15) 0.31247(13) 0.19511(9) 0.0191(3) Uani 1 1 d . . . O2A O 0.48077(14) 0.47527(10) 0.17869(8) 0.0174(3) Uani 1 1 d . . . O2B O 0.35982(13) 0.46602(11) 0.02045(8) 0.0184(3) Uani 1 1 d . . . O2N O -0.03301(16) 0.54682(13) 0.33605(11) 0.0362(4) Uani 1 1 d . . . O2W O 0.61861(16) 0.46402(13) 0.09444(11) 0.0255(4) Uani 1 1 d . . . O3A O 0.45726(14) 0.27007(11) 0.03009(8) 0.0170(3) Uani 1 1 d . . . O3N O -0.14382(19) 0.4949(2) 0.21925(11) 0.0596(7) Uani 1 1 d . . . O4A O 0.70807(14) 0.24206(12) 0.09442(9) 0.0227(4) Uani 1 1 d . . . H11W H 0.685(3) 0.280(2) 0.1755(19) 0.047(10) Uiso 1 1 d . . . H22W H 0.614(3) 0.481(2) 0.0538(18) 0.035(8) Uiso 1 1 d . . . H12W H 0.704(3) 0.354(3) 0.224(2) 0.057(11) Uiso 1 1 d . . . H21W H 0.694(3) 0.469(2) 0.1316(19) 0.044(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01329(14) 0.01503(14) 0.01540(15) -0.00084(10) 0.00791(12) -0.00041(10) Ni2 0.01363(14) 0.01757(15) 0.01342(14) -0.00004(10) 0.00786(12) -0.00133(10) C1A 0.0148(10) 0.0191(10) 0.0113(9) 0.0016(8) 0.0068(8) 0.0020(8) C2A 0.0156(10) 0.0211(11) 0.0122(10) 0.0020(8) 0.0072(8) -0.0005(8) C3A 0.0215(11) 0.0176(11) 0.0166(10) -0.0022(8) 0.0087(9) 0.0010(9) C3B 0.0200(11) 0.0193(11) 0.0130(10) 0.0010(8) 0.0093(9) 0.0008(9) C4A 0.0184(11) 0.0241(12) 0.0163(10) 0.0005(9) 0.0093(9) 0.0047(9) C4B 0.0244(13) 0.0199(12) 0.0400(15) 0.0024(11) 0.0126(12) 0.0034(10) C5A 0.0156(10) 0.0260(12) 0.0171(10) 0.0007(9) 0.0102(9) 0.0017(9) C6A 0.0172(10) 0.0179(10) 0.0154(10) 0.0020(8) 0.0092(9) 0.0009(8) C7A 0.0180(11) 0.0207(11) 0.0212(11) 0.0016(9) 0.0125(10) -0.0010(9) C8A 0.0270(12) 0.0206(11) 0.0296(13) -0.0066(10) 0.0190(11) -0.0076(10) C9A 0.0340(13) 0.0173(11) 0.0320(13) -0.0010(10) 0.0231(12) -0.0020(10) C10A 0.0237(12) 0.0156(11) 0.0267(12) -0.0019(9) 0.0161(10) 0.0011(9) C11A 0.0204(11) 0.0190(11) 0.0244(12) -0.0055(9) 0.0124(10) -0.0031(9) C12A 0.0166(11) 0.0216(11) 0.0137(10) -0.0005(8) 0.0070(9) 0.0017(8) C13A 0.0170(10) 0.0141(10) 0.0167(10) 0.0002(8) 0.0094(9) 0.0000(8) C14A 0.0221(11) 0.0152(10) 0.0162(10) -0.0013(8) 0.0100(9) -0.0010(9) C15A 0.0261(12) 0.0144(10) 0.0209(11) -0.0017(8) 0.0168(10) 0.0003(9) C16A 0.0153(10) 0.0159(10) 0.0229(11) -0.0010(8) 0.0116(9) -0.0004(8) C17A 0.0154(10) 0.0141(10) 0.0161(10) -0.0013(8) 0.0071(9) -0.0010(8) C18A 0.0182(11) 0.0137(10) 0.0171(10) -0.0016(8) 0.0115(9) -0.0014(8) C19A 0.0254(13) 0.0300(13) 0.0290(13) -0.0052(10) 0.0162(11) 0.0047(10) C20A 0.0290(13) 0.0297(13) 0.0224(12) -0.0035(10) 0.0188(11) -0.0008(10) C21A 0.0303(13) 0.0177(11) 0.0289(12) -0.0041(9) 0.0196(11) -0.0046(9) C31A 0.0150(11) 0.0295(13) 0.0248(12) -0.0034(10) 0.0107(10) -0.0013(9) C32A 0.0251(12) 0.0208(12) 0.0237(12) 0.0012(9) 0.0080(10) 0.0051(10) C33A 0.0154(11) 0.0322(13) 0.0190(11) -0.0050(10) 0.0064(9) -0.0012(9) C41A 0.0148(11) 0.0324(13) 0.0227(12) 0.0030(10) 0.0084(10) 0.0035(9) N1A 0.0165(9) 0.0192(9) 0.0211(9) -0.0018(8) 0.0110(8) -0.0022(7) N1N 0.0154(10) 0.0313(11) 0.0291(11) 0.0004(9) 0.0094(9) 0.0004(8) N2A 0.0210(10) 0.0188(9) 0.0205(9) -0.0004(8) 0.0118(8) -0.0001(8) N3A 0.0151(9) 0.0197(9) 0.0165(9) -0.0019(7) 0.0079(8) -0.0008(7) O1A 0.0144(7) 0.0167(7) 0.0154(7) -0.0006(6) 0.0093(6) 0.0003(6) O1B 0.0162(7) 0.0178(8) 0.0187(8) -0.0005(6) 0.0084(6) 0.0006(6) O1N 0.0383(11) 0.0478(12) 0.0316(10) -0.0095(9) 0.0227(9) -0.0212(9) O1W 0.0169(8) 0.0250(9) 0.0155(8) -0.0015(7) 0.0090(7) 0.0003(7) O2A 0.0190(8) 0.0153(7) 0.0203(8) -0.0015(6) 0.0123(7) -0.0032(6) O2B 0.0158(8) 0.0209(8) 0.0166(7) 0.0036(6) 0.0078(6) -0.0004(6) O2N 0.0206(9) 0.0331(10) 0.0460(11) -0.0114(9) 0.0127(9) -0.0071(8) O2W 0.0191(9) 0.0380(10) 0.0179(8) 0.0046(7) 0.0091(8) -0.0074(7) O3A 0.0156(7) 0.0214(8) 0.0156(7) -0.0042(6) 0.0096(6) -0.0019(6) O3N 0.0304(11) 0.118(2) 0.0238(10) 0.0017(12) 0.0109(9) -0.0287(12) O4A 0.0136(8) 0.0376(10) 0.0154(8) -0.0036(7) 0.0070(7) 0.0031(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1B 2.0419(16) . ? Ni1 O1A 2.0590(15) . ? Ni1 O3A 2.1069(17) . ? Ni1 N2A 2.109(2) . ? Ni1 N3A 2.1507(19) . ? Ni1 N1A 2.1873(19) . ? Ni2 O1A 1.9961(15) . ? Ni2 O3A 2.0066(15) . ? Ni2 O2W 2.0273(17) . ? Ni2 O2B 2.0488(16) . ? Ni2 O1W 2.0722(17) . ? Ni2 O2A 2.1575(15) . ? C1A O1A 1.334(2) . ? C1A C6A 1.392(3) . ? C1A C2A 1.407(3) . ? C2A C3A 1.386(3) . ? C2A O2A 1.394(3) . ? C3A C4A 1.396(3) . ? C3A H3A 0.9300 . ? C3B O1B 1.248(3) . ? C3B O2B 1.275(3) . ? C3B C4B 1.507(3) . ? C4A C5A 1.390(3) . ? C4A C19A 1.520(3) . ? C4B H4B1 0.9600 . ? C4B H4B2 0.9600 . ? C4B H4B3 0.9600 . ? C5A C6A 1.401(3) . ? C5A H5A 0.9300 . ? C6A C7A 1.507(3) . ? C7A N1A 1.500(3) . ? C7A H7A1 0.9700 . ? C7A H7A2 0.9700 . ? C8A N1A 1.484(3) . ? C8A C9A 1.525(3) . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C9A N2A 1.496(3) . ? C9A H9A1 0.9700 . ? C9A H9A2 0.9700 . ? C10A N2A 1.489(3) . ? C10A C11A 1.513(3) . ? C10A H10A 0.9700 . ? C10A H10B 0.9700 . ? C11A N3A 1.491(3) . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C12A N3A 1.504(3) . ? C12A C13A 1.504(3) . ? C12A H12A 0.9700 . ? C12A H12B 0.9700 . ? C13A C18A 1.397(3) . ? C13A C14A 1.399(3) . ? C14A C15A 1.384(3) . ? C14A H14A 0.9300 . ? C15A C16A 1.398(3) . ? C15A C20A 1.508(3) . ? C16A C17A 1.384(3) . ? C16A H16A 0.9300 . ? C17A O4A 1.383(3) . ? C17A C18A 1.418(3) . ? C18A O3A 1.339(2) . ? C19A H19A 0.9600 . ? C19A H19B 0.9600 . ? C19A H19C 0.9601 . ? C20A H20A 0.9600 . ? C20A H20B 0.9600 . ? C20A H20C 0.9600 . ? C21A O2A 1.445(3) . ? C21A H21A 0.9600 . ? C21A H21B 0.9600 . ? C21A H21C 0.9600 . ? C31A N1A 1.477(3) . ? C31A H31A 0.9600 . ? C31A H31B 0.9600 . ? C31A H31C 0.9600 . ? C32A N2A 1.482(3) . ? C32A H32A 0.9600 . ? C32A H32B 0.9600 . ? C32A H32C 0.9600 . ? C33A N3A 1.481(3) . ? C33A H33A 0.9600 . ? C33A H33B 0.9600 . ? C33A H33C 0.9600 . ? C41A O4A 1.427(3) . ? C41A H41A 0.9600 . ? C41A H41B 0.9600 . ? C41A H41C 0.9600 . ? N1N O2N 1.240(3) . ? N1N O3N 1.245(3) . ? N1N O1N 1.248(3) . ? O1W H11W 0.83(4) . ? O1W H12W 0.82(4) . ? O2W H22W 0.85(3) . ? O2W H21W 0.84(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1B Ni1 O1A 89.57(6) . . ? O1B Ni1 O3A 100.33(6) . . ? O1A Ni1 O3A 76.64(6) . . ? O1B Ni1 N2A 168.17(7) . . ? O1A Ni1 N2A 98.94(7) . . ? O3A Ni1 N2A 89.68(7) . . ? O1B Ni1 N3A 89.11(7) . . ? O1A Ni1 N3A 166.06(6) . . ? O3A Ni1 N3A 89.95(6) . . ? N2A Ni1 N3A 84.57(7) . . ? O1B Ni1 N1A 87.95(7) . . ? O1A Ni1 N1A 88.91(7) . . ? O3A Ni1 N1A 163.18(7) . . ? N2A Ni1 N1A 84.04(7) . . ? N3A Ni1 N1A 104.92(7) . . ? O1A Ni2 O3A 80.39(6) . . ? O1A Ni2 O2W 174.18(7) . . ? O3A Ni2 O2W 105.00(7) . . ? O1A Ni2 O2B 96.08(6) . . ? O3A Ni2 O2B 93.30(7) . . ? O2W Ni2 O2B 85.90(7) . . ? O1A Ni2 O1W 90.31(7) . . ? O3A Ni2 O1W 94.59(7) . . ? O2W Ni2 O1W 87.09(8) . . ? O2B Ni2 O1W 170.58(7) . . ? O1A Ni2 O2A 79.35(6) . . ? O3A Ni2 O2A 158.68(6) . . ? O2W Ni2 O2A 95.54(7) . . ? O2B Ni2 O2A 82.34(6) . . ? O1W Ni2 O2A 92.10(7) . . ? O1A C1A C6A 121.07(19) . . ? O1A C1A C2A 120.26(18) . . ? C6A C1A C2A 118.68(19) . . ? C3A C2A O2A 124.71(19) . . ? C3A C2A C1A 121.1(2) . . ? O2A C2A C1A 114.19(18) . . ? C2A C3A C4A 120.2(2) . . ? C2A C3A H3A 119.9 . . ? C4A C3A H3A 119.9 . . ? O1B C3B O2B 125.2(2) . . ? O1B C3B C4B 118.1(2) . . ? O2B C3B C4B 116.7(2) . . ? C5A C4A C3A 118.9(2) . . ? C5A C4A C19A 122.1(2) . . ? C3A C4A C19A 119.0(2) . . ? C3B C4B H4B1 109.5 . . ? C3B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C3B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? C4A C5A C6A 121.2(2) . . ? C4A C5A H5A 119.4 . . ? C6A C5A H5A 119.4 . . ? C1A C6A C5A 119.8(2) . . ? C1A C6A C7A 116.67(19) . . ? C5A C6A C7A 123.47(19) . . ? N1A C7A C6A 113.01(17) . . ? N1A C7A H7A1 109.0 . . ? C6A C7A H7A1 109.0 . . ? N1A C7A H7A2 109.0 . . ? C6A C7A H7A2 109.0 . . ? H7A1 C7A H7A2 107.8 . . ? N1A C8A C9A 112.07(19) . . ? N1A C8A H8A1 109.2 . . ? C9A C8A H8A1 109.2 . . ? N1A C8A H8A2 109.2 . . ? C9A C8A H8A2 109.2 . . ? H8A1 C8A H8A2 107.9 . . ? N2A C9A C8A 113.88(19) . . ? N2A C9A H9A1 108.8 . . ? C8A C9A H9A1 108.8 . . ? N2A C9A H9A2 108.8 . . ? C8A C9A H9A2 108.8 . . ? H9A1 C9A H9A2 107.7 . . ? N2A C10A C11A 112.45(18) . . ? N2A C10A H10A 109.1 . . ? C11A C10A H10A 109.1 . . ? N2A C10A H10B 109.1 . . ? C11A C10A H10B 109.1 . . ? H10A C10A H10B 107.8 . . ? N3A C11A C10A 111.99(18) . . ? N3A C11A H11A 109.2 . . ? C10A C11A H11A 109.2 . . ? N3A C11A H11B 109.2 . . ? C10A C11A H11B 109.2 . . ? H11A C11A H11B 107.9 . . ? N3A C12A C13A 117.63(18) . . ? N3A C12A H12A 107.9 . . ? C13A C12A H12A 107.9 . . ? N3A C12A H12B 107.9 . . ? C13A C12A H12B 107.9 . . ? H12A C12A H12B 107.2 . . ? C18A C13A C14A 120.6(2) . . ? C18A C13A C12A 119.98(19) . . ? C14A C13A C12A 119.18(19) . . ? C15A C14A C13A 121.8(2) . . ? C15A C14A H14A 119.1 . . ? C13A C14A H14A 119.1 . . ? C14A C15A C16A 117.56(19) . . ? C14A C15A C20A 121.5(2) . . ? C16A C15A C20A 120.9(2) . . ? C17A C16A C15A 121.6(2) . . ? C17A C16A H16A 119.2 . . ? C15A C16A H16A 119.2 . . ? O4A C17A C16A 122.82(19) . . ? O4A C17A C18A 116.57(18) . . ? C16A C17A C18A 120.6(2) . . ? O3A C18A C13A 120.90(19) . . ? O3A C18A C17A 121.53(19) . . ? C13A C18A C17A 117.45(19) . . ? C4A C19A H19A 109.4 . . ? C4A C19A H19B 109.4 . . ? H19A C19A H19B 109.5 . . ? C4A C19A H19C 109.6 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C15A C20A H20A 109.4 . . ? C15A C20A H20B 109.4 . . ? H20A C20A H20B 109.5 . . ? C15A C20A H20C 109.6 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? O2A C21A H21A 109.5 . . ? O2A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? O2A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? N1A C31A H31A 109.4 . . ? N1A C31A H31B 109.5 . . ? H31A C31A H31B 109.5 . . ? N1A C31A H31C 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? N2A C32A H32A 109.4 . . ? N2A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? N2A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? N3A C33A H33A 109.5 . . ? N3A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? N3A C33A H33C 109.4 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? O4A C41A H41A 109.4 . . ? O4A C41A H41B 109.7 . . ? H41A C41A H41B 109.5 . . ? O4A C41A H41C 109.3 . . ? H41A C41A H41C 109.5 . . ? H41B C41A H41C 109.5 . . ? C31A N1A C8A 109.10(17) . . ? C31A N1A C7A 107.43(17) . . ? C8A N1A C7A 109.26(17) . . ? C31A N1A Ni1 117.86(14) . . ? C8A N1A Ni1 102.66(13) . . ? C7A N1A Ni1 110.27(13) . . ? O2N N1N O3N 120.6(2) . . ? O2N N1N O1N 120.0(2) . . ? O3N N1N O1N 119.3(2) . . ? C32A N2A C10A 108.03(18) . . ? C32A N2A C9A 109.51(19) . . ? C10A N2A C9A 112.68(18) . . ? C32A N2A Ni1 112.70(14) . . ? C10A N2A Ni1 104.98(13) . . ? C9A N2A Ni1 108.92(14) . . ? C33A N3A C11A 108.95(17) . . ? C33A N3A C12A 104.71(17) . . ? C11A N3A C12A 112.76(17) . . ? C33A N3A Ni1 115.38(13) . . ? C11A N3A Ni1 107.56(13) . . ? C12A N3A Ni1 107.60(13) . . ? C1A O1A Ni2 112.03(13) . . ? C1A O1A Ni1 119.08(13) . . ? Ni2 O1A Ni1 95.96(6) . . ? C3B O1B Ni1 126.81(14) . . ? Ni2 O1W H11W 105(2) . . ? Ni2 O1W H12W 109(2) . . ? H11W O1W H12W 110(3) . . ? C2A O2A C21A 116.73(17) . . ? C2A O2A Ni2 107.27(12) . . ? C21A O2A Ni2 118.53(12) . . ? C3B O2B Ni2 125.52(14) . . ? Ni2 O2W H22W 128(2) . . ? Ni2 O2W H21W 120(2) . . ? H22W O2W H21W 108(3) . . ? C18A O3A Ni2 132.73(13) . . ? C18A O3A Ni1 129.33(13) . . ? Ni2 O3A Ni1 94.15(6) . . ? C17A O4A C41A 117.31(17) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.960 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.083 data_Compound2 _database_code_depnum_ccdc_archive 'CCDC 892615' #TrackingRef '- ColacioNi2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H60 N4 Ni2 O14' _chemical_formula_weight 890.30 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 P21/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 12.2650(5) _cell_length_b 26.7600(11) _cell_length_c 12.3190(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.6020(10) _cell_angle_gamma 90.00 _cell_volume 3808.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4505 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.52 _exptl_crystal_description Prismatic _exptl_crystal_colour Green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.063 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.774 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_special_details ; Several crystals of compound were measured and the structure was solved from the best data we were able to collect. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Axs APEX automatic diffractometer' _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 22799 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.50 _reflns_number_total 7874 _reflns_number_gt 6169 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker smart' _computing_cell_refinement 'Bruker smart' _computing_data_reduction 'Bruker smart' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Attempts to identify the solvent molecules (methanol) failed in this compound. Instead, a new set of F2 (hkl) values with the contribution from solvent molecules was obtained by the Squeeze procedure implemented in Platon-94. We have used 6 DFIX to fix bond distances among oxygen and nitrogen atoms in nitrate anion. We have used 1 FLAT to make the nitrate anion planar. We have used 3 DFIX to fix H11W and H12W to O1W. 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^)+(0.0875P)^2^+0.6739P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7874 _refine_ls_number_parameters 448 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1901 _refine_ls_wR_factor_gt 0.1823 _refine_ls_goodness_of_fit_ref 1.333 _refine_ls_restrained_S_all 1.356 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.56073(4) 0.141268(19) 0.64638(4) 0.01836(17) Uani 1 1 d . . . Ni2 Ni 0.44470(4) 0.093562(18) 0.41080(4) 0.01871(17) Uani 1 1 d . . . C1A C 0.3518(3) 0.07649(15) 0.5870(4) 0.0207(8) Uani 1 1 d . . . C1M C 0.4669(4) 0.14297(16) 0.1980(4) 0.0321(11) Uani 1 1 d . . . H1M1 H 0.4492 0.1728 0.2320 0.048 Uiso 1 1 d R . . H1M2 H 0.4318 0.1447 0.1157 0.048 Uiso 1 1 d R . . H1M3 H 0.5493 0.1399 0.2177 0.048 Uiso 1 1 d R . . C2A C 0.2537(3) 0.06713(15) 0.4906(4) 0.0229(9) Uani 1 1 d . . . C3A C 0.1447(3) 0.06321(16) 0.5027(4) 0.0266(9) Uani 1 1 d . . . H3A H 0.0799 0.0571 0.4384 0.032 Uiso 1 1 calc R . . C3B C 0.3598(3) 0.19024(15) 0.4669(3) 0.0204(8) Uani 1 1 d . . . C4A C 0.1328(4) 0.06836(17) 0.6107(4) 0.0287(10) Uani 1 1 d . . . C4B C 0.2815(3) 0.23480(15) 0.4300(4) 0.0212(9) Uani 1 1 d . . . C5A C 0.2295(4) 0.07690(16) 0.7049(4) 0.0271(9) Uani 1 1 d . . . H5A H 0.2218 0.0801 0.7771 0.032 Uiso 1 1 calc R . . C5B C 0.2176(3) 0.24242(17) 0.3145(4) 0.0267(9) Uani 1 1 d . . . H5B H 0.2223 0.2196 0.2593 0.032 Uiso 1 1 calc R . . C6A C 0.3399(3) 0.08097(15) 0.6947(4) 0.0226(9) Uani 1 1 d . . . C6B C 0.1466(4) 0.28427(18) 0.2815(4) 0.0345(11) Uani 1 1 d . . . H6B H 0.1028 0.2890 0.2043 0.041 Uiso 1 1 calc R . . C7A C 0.4481(4) 0.08629(17) 0.7966(4) 0.0270(9) Uani 1 1 d . . . H7A1 H 0.4287 0.0837 0.8665 0.032 Uiso 1 1 calc R . . H7A2 H 0.5000 0.0590 0.7964 0.032 Uiso 1 1 calc R . . C7B C 0.1409(4) 0.31859(18) 0.3622(5) 0.0377(12) Uani 1 1 d . . . H7B H 0.0941 0.3467 0.3392 0.045 Uiso 1 1 calc R . . C8A C 0.6221(4) 0.13354(18) 0.8949(4) 0.0307(10) Uani 1 1 d . . . H8A1 H 0.6087 0.1231 0.9648 0.037 Uiso 1 1 calc R . . H8A2 H 0.6554 0.1668 0.9075 0.037 Uiso 1 1 calc R . . C8B C 0.2044(4) 0.31175(18) 0.4780(5) 0.0361(11) Uani 1 1 d . . . H8B H 0.2002 0.3351 0.5325 0.043 Uiso 1 1 calc R . . C9A C 0.7063(4) 0.09769(17) 0.8691(4) 0.0269(10) Uani 1 1 d . . . H9A1 H 0.7828 0.1028 0.9252 0.032 Uiso 1 1 calc R . . H9A2 H 0.6831 0.0637 0.8776 0.032 Uiso 1 1 calc R . . C9B C 0.2748(3) 0.26944(16) 0.5120(4) 0.0271(10) Uani 1 1 d . . . H9B H 0.3172 0.2644 0.5894 0.033 Uiso 1 1 calc R . . C10A C 0.8114(3) 0.13652(15) 0.7522(4) 0.0237(9) Uani 1 1 d . . . H10A H 0.8264 0.1323 0.6803 0.028 Uiso 1 1 calc R . . H10B H 0.8802 0.1263 0.8145 0.028 Uiso 1 1 calc R . . C11A C 0.7874(3) 0.19122(16) 0.7672(4) 0.0242(9) Uani 1 1 d . . . H11A H 0.7901 0.1969 0.8459 0.029 Uiso 1 1 calc R . . H11B H 0.8470 0.2115 0.7536 0.029 Uiso 1 1 calc R . . C12A C 0.6777(3) 0.22584(15) 0.5748(3) 0.0212(8) Uani 1 1 d . . . H12A H 0.7169 0.2579 0.5888 0.025 Uiso 1 1 calc R . . H12B H 0.5995 0.2315 0.5230 0.025 Uiso 1 1 calc R . . C13A C 0.7391(3) 0.19203(15) 0.5146(3) 0.0213(8) Uani 1 1 d . . . C14A C 0.8422(3) 0.20835(16) 0.5004(4) 0.0245(9) Uani 1 1 d . . . H14A H 0.8748 0.2385 0.5331 0.029 Uiso 1 1 calc R . . C15A C 0.8962(4) 0.18055(16) 0.4387(4) 0.0274(10) Uani 1 1 d . . . C16A C 0.8447(4) 0.13581(16) 0.3911(4) 0.0278(10) Uani 1 1 d . . . H16A H 0.8782 0.1170 0.3471 0.033 Uiso 1 1 calc R . . C17A C 0.7452(3) 0.11835(15) 0.4071(4) 0.0223(9) Uani 1 1 d . . . C18A C 0.6900(3) 0.14639(15) 0.4709(3) 0.0202(8) Uani 1 1 d . . . C19A C 0.0155(4) 0.0635(2) 0.6251(5) 0.0386(12) Uani 1 1 d . . . H19A H 0.0240 0.0479 0.6976 0.058 Uiso 1 1 d R . . H19B H -0.0342 0.0435 0.5636 0.058 Uiso 1 1 d R . . H19C H -0.0178 0.0961 0.6230 0.058 Uiso 1 1 d R . . C20A C 1.0079(4) 0.1972(2) 0.4258(5) 0.0458(14) Uani 1 1 d . . . H20A H 1.0265 0.2302 0.4568 0.069 Uiso 1 1 d R . . H20B H 1.0002 0.1974 0.3456 0.069 Uiso 1 1 d R . . H20C H 1.0687 0.1746 0.4665 0.069 Uiso 1 1 d R . . C21A C 0.1816(4) 0.07008(18) 0.2836(4) 0.0312(10) Uani 1 1 d . . . H21A H 0.1224 0.0454 0.2746 0.047 Uiso 1 1 d R . . H21B H 0.2088 0.0685 0.2191 0.047 Uiso 1 1 d R . . H21C H 0.1503 0.1027 0.2872 0.047 Uiso 1 1 d R . . C31A C 0.4359(4) 0.17437(17) 0.8185(4) 0.0295(10) Uani 1 1 d . . . H31A H 0.3641 0.1755 0.7553 0.044 Uiso 1 1 d R . . H31B H 0.4747 0.2060 0.8249 0.044 Uiso 1 1 d R . . H31C H 0.4208 0.1675 0.8886 0.044 Uiso 1 1 d R . . C32A C 0.7314(4) 0.05459(16) 0.7060(4) 0.0283(10) Uani 1 1 d . . . H32A H 0.8038 0.0409 0.7543 0.043 Uiso 1 1 d R . . H32B H 0.7328 0.0584 0.6290 0.043 Uiso 1 1 d R . . H32C H 0.6697 0.0325 0.7054 0.043 Uiso 1 1 d R . . C33A C 0.6311(4) 0.24961(16) 0.7376(4) 0.0287(10) Uani 1 1 d . . . H33A H 0.6381 0.2419 0.8157 0.043 Uiso 1 1 d R . . H33B H 0.5515 0.2563 0.6940 0.043 Uiso 1 1 d R . . H33C H 0.6771 0.2785 0.7363 0.043 Uiso 1 1 d R . . C41A C 0.7324(5) 0.05005(19) 0.2773(5) 0.0406(12) Uani 1 1 d . . . H41A H 0.7338 0.0744 0.2206 0.061 Uiso 1 1 d R . . H41B H 0.6797 0.0237 0.2409 0.061 Uiso 1 1 d R . . H41C H 0.8086 0.0365 0.3125 0.061 Uiso 1 1 d R . . N1A N 0.5099(3) 0.13490(13) 0.7980(3) 0.0230(8) Uani 1 1 d . . . N2A N 0.7128(3) 0.10392(13) 0.7516(3) 0.0226(7) Uani 1 1 d . . . N3A N 0.6716(3) 0.20673(13) 0.6862(3) 0.0218(7) Uani 1 1 d . . . O1A O 0.4576(2) 0.07951(10) 0.5751(2) 0.0199(6) Uani 1 1 d . . . O1B O 0.4266(2) 0.18847(10) 0.5708(2) 0.0220(6) Uani 1 1 d . . . O1M O 0.4232(3) 0.10114(11) 0.2411(3) 0.0268(7) Uani 1 1 d . . . H1M H 0.425(4) 0.0782(19) 0.211(4) 0.032 Uiso 1 1 d . . . O1W O 0.5161(2) 0.02491(11) 0.3951(3) 0.0268(7) Uani 1 1 d D . . H11W H 0.581(2) 0.0326(15) 0.388(4) 0.032 Uiso 1 1 d D . . H12W H 0.522(3) -0.0050(9) 0.417(4) 0.032 Uiso 1 1 d D . . O2A O 0.2755(2) 0.06051(10) 0.3879(2) 0.0228(6) Uani 1 1 d . . . O2B O 0.3554(2) 0.15803(10) 0.3908(2) 0.0238(6) Uani 1 1 d . . . O3A O 0.5962(2) 0.12937(10) 0.4934(2) 0.0199(6) Uani 1 1 d . . . O4A O 0.6948(2) 0.07355(11) 0.3636(3) 0.0277(7) Uani 1 1 d . . . O4N O 0.4541(5) 0.0323(2) 0.0951(5) 0.1053(19) Uiso 1 1 d D . . O3N O 0.3585(8) -0.0143(3) -0.0419(7) 0.194(4) Uiso 1 1 d D . . O2N O 0.2698(6) 0.0368(5) 0.0338(12) 0.303(7) Uiso 1 1 d D . . N1N N 0.3612(6) 0.0189(3) 0.0324(7) 0.148(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0163(3) 0.0168(3) 0.0213(3) -0.0004(2) 0.0053(2) 0.00027(19) Ni2 0.0177(3) 0.0149(3) 0.0227(3) -0.0004(2) 0.0056(2) -0.00092(19) C1A 0.019(2) 0.0133(19) 0.030(2) -0.0010(17) 0.0096(17) -0.0013(15) C1M 0.042(3) 0.022(2) 0.033(3) 0.0092(19) 0.014(2) 0.0014(19) C2A 0.023(2) 0.017(2) 0.029(2) -0.0003(17) 0.0081(17) 0.0036(16) C3A 0.017(2) 0.021(2) 0.039(2) -0.0003(19) 0.0055(18) -0.0014(17) C3B 0.020(2) 0.016(2) 0.025(2) 0.0026(17) 0.0079(17) -0.0021(16) C4A 0.020(2) 0.027(2) 0.042(3) 0.003(2) 0.0138(19) 0.0012(17) C4B 0.0163(19) 0.018(2) 0.030(2) 0.0022(17) 0.0082(16) -0.0020(15) C5A 0.028(2) 0.021(2) 0.038(3) 0.0002(19) 0.019(2) -0.0005(18) C5B 0.021(2) 0.028(2) 0.030(2) 0.0071(19) 0.0076(18) -0.0011(17) C6A 0.024(2) 0.016(2) 0.029(2) 0.0006(17) 0.0110(18) 0.0002(16) C6B 0.023(2) 0.033(3) 0.045(3) 0.016(2) 0.008(2) 0.0039(19) C7A 0.026(2) 0.030(2) 0.027(2) 0.0058(19) 0.0113(18) 0.0007(18) C7B 0.021(2) 0.026(3) 0.069(4) 0.011(2) 0.020(2) 0.0092(19) C8A 0.030(2) 0.038(3) 0.021(2) -0.0005(19) 0.0055(19) -0.003(2) C8B 0.027(2) 0.024(2) 0.060(3) 0.001(2) 0.018(2) 0.0047(19) C9A 0.021(2) 0.030(2) 0.025(2) 0.0066(18) 0.0015(17) 0.0018(18) C9B 0.022(2) 0.020(2) 0.039(3) 0.0011(19) 0.0105(19) -0.0008(17) C10A 0.017(2) 0.022(2) 0.028(2) -0.0008(17) 0.0020(17) 0.0005(16) C11A 0.020(2) 0.023(2) 0.025(2) -0.0025(18) 0.0028(17) -0.0034(17) C12A 0.022(2) 0.0128(19) 0.027(2) 0.0004(16) 0.0046(17) -0.0024(15) C13A 0.021(2) 0.022(2) 0.019(2) 0.0026(16) 0.0047(16) -0.0009(16) C14A 0.023(2) 0.021(2) 0.026(2) 0.0031(17) 0.0028(17) -0.0058(17) C15A 0.024(2) 0.024(2) 0.035(2) 0.0062(19) 0.0115(19) -0.0033(18) C16A 0.028(2) 0.025(2) 0.034(2) 0.0039(19) 0.0160(19) 0.0022(18) C17A 0.021(2) 0.019(2) 0.027(2) 0.0028(17) 0.0086(17) -0.0012(16) C18A 0.020(2) 0.020(2) 0.020(2) 0.0052(16) 0.0063(16) -0.0011(16) C19A 0.023(2) 0.044(3) 0.052(3) 0.005(2) 0.017(2) -0.001(2) C20A 0.036(3) 0.037(3) 0.074(4) -0.004(3) 0.031(3) -0.009(2) C21A 0.023(2) 0.030(3) 0.036(3) -0.003(2) 0.0030(19) -0.0005(19) C31A 0.030(2) 0.029(2) 0.034(2) -0.008(2) 0.016(2) -0.0026(19) C32A 0.022(2) 0.019(2) 0.040(3) 0.0000(19) 0.0046(19) 0.0038(17) C33A 0.026(2) 0.020(2) 0.036(3) -0.0054(19) 0.0057(19) 0.0015(18) C41A 0.055(3) 0.028(3) 0.049(3) -0.011(2) 0.030(3) -0.004(2) N1A 0.0223(17) 0.0213(18) 0.0258(19) 0.0002(15) 0.0086(15) 0.0009(14) N2A 0.0192(17) 0.0214(18) 0.0248(18) 0.0009(15) 0.0040(14) 0.0011(14) N3A 0.0218(17) 0.0182(18) 0.0257(18) -0.0030(14) 0.0084(14) -0.0003(14) O1A 0.0153(13) 0.0201(14) 0.0253(15) 0.0012(12) 0.0082(11) 0.0014(11) O1B 0.0203(14) 0.0200(15) 0.0256(15) -0.0011(12) 0.0075(12) 0.0016(11) O1M 0.0345(17) 0.0197(16) 0.0260(17) -0.0034(13) 0.0097(14) -0.0034(14) O1W 0.0235(16) 0.0159(15) 0.0444(18) 0.0027(14) 0.0161(14) 0.0008(12) O2A 0.0178(13) 0.0204(15) 0.0270(15) -0.0022(12) 0.0035(12) -0.0016(11) O2B 0.0246(15) 0.0188(15) 0.0254(15) -0.0029(12) 0.0053(12) 0.0015(12) O3A 0.0168(13) 0.0189(14) 0.0227(14) -0.0003(12) 0.0048(11) -0.0029(11) O4A 0.0275(16) 0.0208(16) 0.0393(18) -0.0039(13) 0.0170(14) -0.0031(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 Ni1 O1B 2.035(3) . ? Ni1 O1A 2.087(3) . ? Ni1 O3A 2.096(3) . ? Ni1 N2A 2.130(3) . ? Ni1 N1A 2.165(3) . ? Ni1 N3A 2.170(3) . ? Ni2 O1A 2.012(3) . ? Ni2 O2B 2.014(3) . ? Ni2 O1M 2.028(3) . ? Ni2 O3A 2.034(3) . ? Ni2 O1W 2.072(3) . ? Ni2 O2A 2.185(3) . ? C1A O1A 1.357(4) . ? C1A C6A 1.388(6) . ? C1A C2A 1.400(6) . ? C1M O1M 1.419(5) . ? C2A C3A 1.397(6) . ? C2A O2A 1.390(5) . ? C3A C4A 1.393(6) . ? C3B O2B 1.261(5) . ? C3B O1B 1.268(5) . ? C3B C4B 1.503(5) . ? C4A C5A 1.372(6) . ? C4A C19A 1.512(6) . ? C4B C5B 1.390(6) . ? C4B C9B 1.393(6) . ? C5A C6A 1.405(6) . ? C5B C6B 1.393(6) . ? C6A C7A 1.497(6) . ? C6B C7B 1.373(7) . ? C7A N1A 1.502(5) . ? C7B C8B 1.390(7) . ? C8A N1A 1.489(5) . ? C8A C9A 1.520(6) . ? C8B C9B 1.400(6) . ? C9A N2A 1.485(5) . ? C10A N2A 1.489(5) . ? C10A C11A 1.517(6) . ? C11A N3A 1.495(5) . ? C12A N3A 1.490(5) . ? C12A C13A 1.520(5) . ? C13A C18A 1.388(6) . ? C13A C14A 1.403(5) . ? C14A C15A 1.381(6) . ? C15A C16A 1.389(6) . ? C15A C20A 1.499(6) . ? C16A C17A 1.381(5) . ? C17A O4A 1.373(5) . ? C17A C18A 1.413(6) . ? C18A O3A 1.349(4) . ? C21A O2A 1.432(5) . ? C31A N1A 1.468(5) . ? C32A N2A 1.482(5) . ? C33A N3A 1.475(5) . ? C41A O4A 1.438(5) . ? O4N N1N 1.197(4) . ? O3N N1N 1.267(4) . ? O2N N1N 1.225(4) . ? 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 O1B Ni1 O1A 90.93(11) . . ? O1B Ni1 O3A 93.59(11) . . ? O1A Ni1 O3A 77.33(10) . . ? O1B Ni1 N2A 168.03(12) . . ? O1A Ni1 N2A 99.66(12) . . ? O3A Ni1 N2A 94.16(12) . . ? O1B Ni1 N1A 91.20(12) . . ? O1A Ni1 N1A 89.51(12) . . ? O3A Ni1 N1A 166.05(12) . . ? N2A Ni1 N1A 83.39(13) . . ? O1B Ni1 N3A 87.21(12) . . ? O1A Ni1 N3A 168.33(12) . . ? O3A Ni1 N3A 91.28(11) . . ? N2A Ni1 N3A 83.51(13) . . ? N1A Ni1 N3A 102.04(13) . . ? O1A Ni2 O2B 97.99(11) . . ? O1A Ni2 O1M 174.28(12) . . ? O2B Ni2 O1M 84.91(12) . . ? O1A Ni2 O3A 80.48(11) . . ? O2B Ni2 O3A 91.46(11) . . ? O1M Ni2 O3A 104.44(12) . . ? O1A Ni2 O1W 91.99(12) . . ? O2B Ni2 O1W 167.91(12) . . ? O1M Ni2 O1W 84.58(13) . . ? O3A Ni2 O1W 96.93(11) . . ? O1A Ni2 O2A 78.77(11) . . ? O2B Ni2 O2A 82.94(11) . . ? O1M Ni2 O2A 96.77(12) . . ? O3A Ni2 O2A 157.51(11) . . ? O1W Ni2 O2A 92.39(11) . . ? O1A C1A C6A 120.6(4) . . ? O1A C1A C2A 120.0(4) . . ? C6A C1A C2A 119.3(4) . . ? C3A C2A O2A 124.8(4) . . ? C3A C2A C1A 120.2(4) . . ? O2A C2A C1A 114.9(3) . . ? C2A C3A C4A 120.4(4) . . ? O2B C3B O1B 125.2(4) . . ? O2B C3B C4B 117.0(4) . . ? O1B C3B C4B 117.8(4) . . ? C5A C4A C3A 119.1(4) . . ? C5A C4A C19A 120.1(4) . . ? C3A C4A C19A 120.8(4) . . ? C5B C4B C9B 119.6(4) . . ? C5B C4B C3B 120.7(4) . . ? C9B C4B C3B 119.7(4) . . ? C4A C5A C6A 121.6(4) . . ? C4B C5B C6B 120.0(4) . . ? C1A C6A C5A 119.5(4) . . ? C1A C6A C7A 117.5(3) . . ? C5A C6A C7A 122.9(4) . . ? C7B C6B C5B 120.3(5) . . ? N1A C7A C6A 113.2(3) . . ? C6B C7B C8B 120.6(4) . . ? N1A C8A C9A 111.0(3) . . ? C7B C8B C9B 119.4(5) . . ? N2A C9A C8A 113.3(3) . . ? C8B C9B C4B 120.1(4) . . ? N2A C10A C11A 112.0(3) . . ? N3A C11A C10A 111.5(3) . . ? N3A C12A C13A 115.6(3) . . ? C18A C13A C14A 121.2(4) . . ? C18A C13A C12A 119.4(3) . . ? C14A C13A C12A 119.4(4) . . ? C15A C14A C13A 121.3(4) . . ? C14A C15A C16A 117.6(4) . . ? C14A C15A C20A 121.5(4) . . ? C16A C15A C20A 120.9(4) . . ? C17A C16A C15A 122.0(4) . . ? O4A C17A C16A 122.9(4) . . ? O4A C17A C18A 116.3(3) . . ? C16A C17A C18A 120.7(4) . . ? O3A C18A C13A 120.4(4) . . ? O3A C18A C17A 122.4(4) . . ? C13A C18A C17A 117.1(4) . . ? C31A N1A C7A 106.6(3) . . ? C31A N1A C8A 109.8(3) . . ? C7A N1A C8A 108.3(3) . . ? C31A N1A Ni1 117.7(3) . . ? C7A N1A Ni1 110.4(2) . . ? C8A N1A Ni1 103.7(2) . . ? C32A N2A C10A 107.2(3) . . ? C32A N2A C9A 109.6(3) . . ? C10A N2A C9A 111.7(3) . . ? C32A N2A Ni1 113.7(2) . . ? C10A N2A Ni1 105.8(2) . . ? C9A N2A Ni1 108.9(2) . . ? C33A N3A C12A 104.9(3) . . ? C33A N3A C11A 108.1(3) . . ? C12A N3A C11A 112.4(3) . . ? C33A N3A Ni1 116.7(2) . . ? C12A N3A Ni1 106.9(2) . . ? C11A N3A Ni1 108.0(2) . . ? C1A O1A Ni2 111.4(2) . . ? C1A O1A Ni1 117.9(2) . . ? Ni2 O1A Ni1 96.16(11) . . ? C3B O1B Ni1 129.4(3) . . ? C1M O1M Ni2 122.0(3) . . ? C2A O2A C21A 116.8(3) . . ? C2A O2A Ni2 107.2(2) . . ? C21A O2A Ni2 119.2(2) . . ? C3B O2B Ni2 127.5(3) . . ? C18A O3A Ni2 139.0(3) . . ? C18A O3A Ni1 125.6(2) . . ? Ni2 O3A Ni1 95.21(11) . . ? C17A O4A C41A 117.2(3) . . ? O4N N1N O2N 123.4(5) . . ? O4N N1N O3N 117.7(5) . . ? O2N N1N O3N 118.9(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.168 _refine_diff_density_min -1.766 _refine_diff_density_rms 0.125 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 303 65 ' ' 2 0.000 0.500 0.500 303 65 ' ' _platon_squeeze_details ; ; data_Compound3 _database_code_depnum_ccdc_archive 'CCDC 892616' #TrackingRef 'Colacio_Ni.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H52 N4 Ni2 O11' _chemical_formula_weight 894.29 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.564(2) _cell_length_b 16.014(3) _cell_length_c 19.338(3) _cell_angle_alpha 79.755(3) _cell_angle_beta 71.845(2) _cell_angle_gamma 81.492(3) _cell_volume 3908.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11480 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.55 _exptl_crystal_description Prismatic _exptl_crystal_colour Green _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 1.032 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.643 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _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 'Bruker Axs APEX automatic diffractometer' _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 44593 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.00 _reflns_number_total 16791 _reflns_number_gt 13145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker smart' _computing_cell_refinement 'Bruker smart' _computing_data_reduction 'Bruker smart' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; We have used 7 DFIX to fix the hydrogen atoms pertaining to the water molecules, O1W and O2W. There are two peaks too large near to Ni ions, Q1 and Q2. Q1 is located to 0.747 A from Ni4, while Q2 is located to 0.713 A from Ni2. 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^)+(0.1216P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16791 _refine_ls_number_parameters 1076 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1869 _refine_ls_wR_factor_gt 0.1746 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.015 _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 0.86966(3) -0.24847(2) 0.36030(2) 0.01302(11) Uani 1 1 d . . . Ni2 Ni 0.96733(3) -0.12097(2) 0.22927(2) 0.01504(12) Uani 1 1 d . . . Ni3 Ni 0.64623(3) 0.25278(2) 0.12837(2) 0.01237(11) Uani 1 1 d . . . Ni4 Ni 0.57467(3) 0.11164(2) 0.25492(2) 0.01529(12) Uani 1 1 d D . . C1A C 0.8167(2) -0.21837(19) 0.22053(17) 0.0156(6) Uani 1 1 d . . . C1B C 0.7080(2) 0.22017(19) 0.26777(17) 0.0144(6) Uani 1 1 d . . . C1M C 1.1941(3) -0.0873(2) 0.20907(19) 0.0259(8) Uani 1 1 d . . . H1M1 H 1.1785 -0.1076 0.2607 0.039 Uiso 1 1 d R . . H1M2 H 1.2381 -0.0418 0.1969 0.039 Uiso 1 1 d R . . H1M3 H 1.2294 -0.1330 0.1817 0.039 Uiso 1 1 d R . . C2A C 0.8654(3) -0.1956(2) 0.14444(18) 0.0177(7) Uani 1 1 d . . . C2B C 0.6646(2) 0.1889(2) 0.34241(17) 0.0170(6) Uani 1 1 d . . . C3A C 0.8461(3) -0.2341(2) 0.09210(18) 0.0186(7) Uani 1 1 d . . . H3A H 0.8793 -0.2183 0.0425 0.022 Uiso 1 1 calc R . . C3B C 0.6733(2) 0.2284(2) 0.39811(17) 0.0170(6) Uani 1 1 d . . . H3B H 0.6415 0.2077 0.4469 0.020 Uiso 1 1 calc R . . C3E C 1.0557(2) -0.30045(19) 0.23755(16) 0.0138(6) Uani 1 1 d . . . C3D C 0.4627(2) 0.28558(19) 0.26116(16) 0.0137(6) Uani 1 1 d . . . C4A C 0.7770(2) -0.2964(2) 0.11326(18) 0.0171(7) Uani 1 1 d . . . C4B C 0.7296(2) 0.2993(2) 0.38127(17) 0.0171(7) Uani 1 1 d . . . C4E C 1.1373(2) -0.36890(19) 0.20452(16) 0.0140(6) Uani 1 1 d . . . C4D C 0.3745(2) 0.34757(19) 0.29829(16) 0.0147(6) Uani 1 1 d . . . C2M C 0.3502(3) 0.0566(2) 0.29781(19) 0.0262(8) Uani 1 1 d . . . H2M1 H 0.3165 0.0945 0.3334 0.039 Uiso 1 1 d R . . H2M2 H 0.3154 0.0056 0.3105 0.039 Uiso 1 1 d R . . H2M3 H 0.3474 0.0841 0.2500 0.039 Uiso 1 1 d R . . C5A C 0.7290(2) -0.3197(2) 0.18822(18) 0.0176(7) Uani 1 1 d . . . H5A H 0.6839 -0.3623 0.2028 0.021 Uiso 1 1 calc R . . C5B C 0.7741(2) 0.3299(2) 0.30799(17) 0.0163(6) Uani 1 1 d . . . H5B H 0.8110 0.3775 0.2960 0.020 Uiso 1 1 calc R . . C5E C 1.2397(2) -0.3730(2) 0.21000(16) 0.0160(6) Uani 1 1 d . . . C5D C 0.2746(2) 0.3457(2) 0.29222(16) 0.0168(6) Uani 1 1 d . . . C6A C 0.7469(2) -0.2807(2) 0.24158(17) 0.0167(6) Uani 1 1 d . . . C6B C 0.7643(2) 0.2902(2) 0.25146(17) 0.0156(6) Uani 1 1 d . . . C6E C 1.2703(3) -0.3143(2) 0.24533(17) 0.0204(7) Uani 1 1 d . . . H6E H 1.2217 -0.2712 0.2657 0.024 Uiso 1 1 calc R . . C6D C 0.2505(3) 0.2840(2) 0.25638(17) 0.0193(7) Uani 1 1 d . . . H6D H 0.3024 0.2424 0.2370 0.023 Uiso 1 1 calc R . . C7A C 0.6880(2) -0.2969(2) 0.32171(17) 0.0201(7) Uani 1 1 d . . . H7A1 H 0.6521 -0.2434 0.3375 0.024 Uiso 1 1 calc R . . H7A2 H 0.6356 -0.3350 0.3281 0.024 Uiso 1 1 calc R . . C7B C 0.8214(2) 0.3165(2) 0.17215(17) 0.0183(7) Uani 1 1 d . . . H7B1 H 0.8646 0.3608 0.1694 0.022 Uiso 1 1 calc R . . H7B2 H 0.8675 0.2680 0.1534 0.022 Uiso 1 1 calc R . . C7E C 1.3698(3) -0.3204(2) 0.24965(19) 0.0257(8) Uani 1 1 d . . . H7E H 1.3887 -0.2811 0.2721 0.031 Uiso 1 1 calc R . . C7D C 0.1527(3) 0.2848(2) 0.24995(18) 0.0245(8) Uani 1 1 d . . . H7D H 0.1386 0.2441 0.2265 0.029 Uiso 1 1 calc R . . C8A C 0.6906(3) -0.3384(2) 0.44806(17) 0.0217(7) Uani 1 1 d . . . H8A1 H 0.7292 -0.3736 0.4791 0.026 Uiso 1 1 calc R . . H8A2 H 0.6278 -0.3649 0.4546 0.026 Uiso 1 1 calc R . . C8B C 0.8236(2) 0.3580(2) 0.04659(17) 0.0187(7) Uani 1 1 d . . . H8B1 H 0.8835 0.3861 0.0443 0.022 Uiso 1 1 calc R . . H8B2 H 0.7870 0.3932 0.0142 0.022 Uiso 1 1 calc R . . C8E C 1.4442(3) -0.3863(2) 0.22003(19) 0.0285(8) Uani 1 1 d . . . H8E H 1.5117 -0.3898 0.2231 0.034 Uiso 1 1 calc R . . C8D C 0.0729(3) 0.3481(2) 0.2791(2) 0.0276(8) Uani 1 1 d . . . H8D H 0.0066 0.3484 0.2744 0.033 Uiso 1 1 calc R . . C9A C 0.6604(3) -0.2497(2) 0.47202(18) 0.0226(7) Uani 1 1 d . . . H9A1 H 0.6027 -0.2219 0.4542 0.027 Uiso 1 1 calc R . . H9A2 H 0.6369 -0.2557 0.5253 0.027 Uiso 1 1 calc R . . C9B C 0.8601(2) 0.2712(2) 0.02129(18) 0.0205(7) Uani 1 1 d . . . H9B1 H 0.9026 0.2780 -0.0297 0.025 Uiso 1 1 calc R . . H9B2 H 0.9023 0.2378 0.0507 0.025 Uiso 1 1 calc R . . C9E C 1.4183(3) -0.4447(2) 0.18700(18) 0.0246(8) Uani 1 1 d . . . H9E H 1.4679 -0.4883 0.1688 0.029 Uiso 1 1 calc R . . C9D C 0.0917(3) 0.4082(2) 0.31375(18) 0.0241(8) Uani 1 1 d . . . H9D H 0.0382 0.4491 0.3324 0.029 Uiso 1 1 calc R . . C10A C 0.8000(3) -0.1885(2) 0.50019(17) 0.0241(7) Uani 1 1 d . . . H10A H 0.7467 -0.1768 0.5452 0.029 Uiso 1 1 calc R . . H10B H 0.8429 -0.1413 0.4835 0.029 Uiso 1 1 calc R . . C10B C 0.7301(3) 0.2599(2) -0.03659(17) 0.0224(7) Uani 1 1 d . . . H10C H 0.7451 0.3187 -0.0535 0.027 Uiso 1 1 calc R . . H10D H 0.7663 0.2268 -0.0762 0.027 Uiso 1 1 calc R . . C10E C 1.3157(2) -0.4396(2) 0.18009(16) 0.0171(7) Uani 1 1 d . . . C10D C 0.1932(2) 0.4095(2) 0.32193(17) 0.0183(7) Uani 1 1 d . . . C11A C 0.8671(3) -0.2697(2) 0.51619(17) 0.0233(8) Uani 1 1 d . . . H11A H 0.9082 -0.2594 0.5463 0.028 Uiso 1 1 calc R . . H11B H 0.8224 -0.3137 0.5439 0.028 Uiso 1 1 calc R . . C11B C 0.6152(2) 0.2548(2) -0.01728(17) 0.0179(7) Uani 1 1 d . . . H11C H 0.5901 0.2828 -0.0582 0.021 Uiso 1 1 calc R . . H11G H 0.6012 0.1955 -0.0079 0.021 Uiso 1 1 calc R . . C11E C 1.2881(2) -0.4980(2) 0.14552(16) 0.0176(7) Uani 1 1 d . . . H11E H 1.3375 -0.5416 0.1270 0.021 Uiso 1 1 calc R . . C11D C 0.2144(2) 0.4701(2) 0.35686(16) 0.0187(7) Uani 1 1 d . . . H11D H 0.1617 0.5118 0.3749 0.022 Uiso 1 1 calc R . . C12A C 1.0459(2) -0.27152(19) 0.42561(17) 0.0174(7) Uani 1 1 d . . . H12A H 1.0839 -0.2897 0.3784 0.021 Uiso 1 1 calc R . . H12B H 1.0809 -0.3017 0.4609 0.021 Uiso 1 1 calc R . . C12B C 0.4510(2) 0.27088(19) 0.08081(17) 0.0154(6) Uani 1 1 d . . . H12C H 0.4093 0.3005 0.0496 0.019 Uiso 1 1 calc R . . H12D H 0.4214 0.2899 0.1286 0.019 Uiso 1 1 calc R . . C12E C 1.1884(2) -0.4929(2) 0.13806(16) 0.0158(6) Uani 1 1 d . . . C12D C 0.3126(3) 0.4704(2) 0.36568(17) 0.0179(7) Uani 1 1 d . . . C13A C 1.0556(2) -0.1779(2) 0.41945(17) 0.0172(7) Uani 1 1 d . . . C13B C 0.4419(2) 0.1764(2) 0.08966(17) 0.0160(6) Uani 1 1 d . . . C13E C 1.1607(3) -0.5519(2) 0.10212(17) 0.0197(7) Uani 1 1 d . . . H13E H 1.2098 -0.5959 0.0840 0.024 Uiso 1 1 calc R . . C13D C 0.3347(3) 0.5323(2) 0.40239(18) 0.0233(7) Uani 1 1 d . . . H13D H 0.2819 0.5733 0.4217 0.028 Uiso 1 1 calc R . . C14A C 1.1197(3) -0.1534(2) 0.45424(17) 0.0199(7) Uani 1 1 d . . . H14A H 1.1519 -0.1947 0.4826 0.024 Uiso 1 1 calc R . . C14B C 0.3692(2) 0.1500(2) 0.06224(17) 0.0189(7) Uani 1 1 d . . . H14B H 0.3256 0.1909 0.0423 0.023 Uiso 1 1 calc R . . C14E C 1.0642(3) -0.5453(2) 0.09382(18) 0.0217(7) Uani 1 1 d . . . H14E H 1.0475 -0.5844 0.0700 0.026 Uiso 1 1 calc R . . C14D C 0.4308(3) 0.5323(2) 0.40951(19) 0.0244(8) Uani 1 1 d . . . H14D H 0.4439 0.5735 0.4329 0.029 Uiso 1 1 calc R . . C15A C 1.1370(3) -0.0686(2) 0.44773(17) 0.0189(7) Uani 1 1 d . . . C15B C 0.3607(2) 0.0645(2) 0.06404(17) 0.0190(7) Uani 1 1 d . . . C15E C 0.9884(3) -0.4787(2) 0.12144(18) 0.0203(7) Uani 1 1 d . . . H15E H 0.9228 -0.4741 0.1146 0.024 Uiso 1 1 calc R . . C15D C 0.5116(3) 0.4691(2) 0.3813(2) 0.0257(8) Uani 1 1 d . . . H15D H 0.5769 0.4686 0.3875 0.031 Uiso 1 1 calc R . . C16A C 1.0821(2) -0.0074(2) 0.40933(17) 0.0172(6) Uani 1 1 d . . . H16A H 1.0897 0.0500 0.4066 0.021 Uiso 1 1 calc R . . C16B C 0.4298(2) 0.0046(2) 0.09198(16) 0.0172(7) Uani 1 1 d . . . H16B H 0.4268 -0.0531 0.0922 0.021 Uiso 1 1 calc R . . C16E C 1.0099(2) -0.4217(2) 0.15756(17) 0.0176(7) Uani 1 1 d . . . H16E H 0.9587 -0.3790 0.1756 0.021 Uiso 1 1 calc R . . C16D C 0.4949(3) 0.4092(2) 0.34506(17) 0.0189(7) Uani 1 1 d . . . H16D H 0.5493 0.3692 0.3262 0.023 Uiso 1 1 calc R . . C17A C 1.0172(2) -0.0301(2) 0.37553(16) 0.0154(6) Uani 1 1 d . . . C17B C 0.5024(2) 0.0291(2) 0.11927(16) 0.0156(6) Uani 1 1 d . . . C17E C 1.1109(2) -0.42664(19) 0.16835(16) 0.0150(6) Uani 1 1 d . . . C17D C 0.3949(2) 0.4074(2) 0.33574(16) 0.0161(6) Uani 1 1 d . . . C18A C 1.0066(2) -0.11731(19) 0.37600(16) 0.0143(6) Uani 1 1 d . . . C18B C 0.5086(2) 0.11644(19) 0.12064(16) 0.0139(6) Uani 1 1 d . . . C19A C 0.7552(3) -0.3380(2) 0.05644(18) 0.0228(7) Uani 1 1 d . . . H19A H 0.7845 -0.3075 0.0086 0.034 Uiso 1 1 d R . . H19B H 0.6812 -0.3369 0.0660 0.034 Uiso 1 1 d R . . H19C H 0.7860 -0.3960 0.0584 0.034 Uiso 1 1 d R . . C19B C 0.7422(3) 0.3417(2) 0.44170(18) 0.0234(7) Uani 1 1 d . . . H19D H 0.8150 0.3416 0.4363 0.035 Uiso 1 1 d R . . H19E H 0.7091 0.3109 0.4886 0.035 Uiso 1 1 d R . . H19F H 0.7104 0.3994 0.4386 0.035 Uiso 1 1 d R . . C20A C 1.2120(3) -0.0441(2) 0.48300(19) 0.0250(8) Uani 1 1 d . . . H20A H 1.2646 -0.0135 0.4461 0.038 Uiso 1 1 d R . . H20B H 1.2442 -0.0947 0.5053 0.038 Uiso 1 1 d R . . H20C H 1.1747 -0.0086 0.5199 0.038 Uiso 1 1 d R . . C20B C 0.2830(3) 0.0375(2) 0.03325(19) 0.0239(7) Uani 1 1 d . . . H20D H 0.2410 0.0868 0.0182 0.036 Uiso 1 1 d R . . H20E H 0.2391 -0.0003 0.0704 0.036 Uiso 1 1 d R . . H20F H 0.3193 0.0085 -0.0083 0.036 Uiso 1 1 d R . . C21A C 0.9225(3) -0.0657(2) 0.07145(19) 0.0265(8) Uani 1 1 d . . . H21A H 0.9448 -0.0864 0.0248 0.040 Uiso 1 1 d R . . H21B H 0.9637 -0.0211 0.0698 0.040 Uiso 1 1 d R . . H21C H 0.8504 -0.0438 0.0821 0.040 Uiso 1 1 d R . . C21B C 0.5446(3) 0.0917(2) 0.42441(18) 0.0258(8) Uani 1 1 d . . . H21D H 0.5814 0.0804 0.4607 0.039 Uiso 1 1 d R . . H21E H 0.5140 0.0414 0.4241 0.039 Uiso 1 1 d R . . H21F H 0.4907 0.1375 0.4360 0.039 Uiso 1 1 d R . . C31A C 0.7953(3) -0.4223(2) 0.35315(18) 0.0198(7) Uani 1 1 d . . . H31A H 0.8356 -0.4493 0.3854 0.030 Uiso 1 1 d R . . H31B H 0.8384 -0.4199 0.3031 0.030 Uiso 1 1 d R . . H31C H 0.7377 -0.4545 0.3602 0.030 Uiso 1 1 d R . . C31B C 0.7006(3) 0.4324(2) 0.14209(18) 0.0194(7) Uani 1 1 d . . . H31D H 0.7518 0.4697 0.1386 0.029 Uiso 1 1 d R . . H31E H 0.6547 0.4256 0.1914 0.029 Uiso 1 1 d R . . H31F H 0.6611 0.4567 0.1086 0.029 Uiso 1 1 d R . . C32A C 0.7110(3) -0.1059(2) 0.41756(19) 0.0240(7) Uani 1 1 d . . . H32A H 0.6586 -0.0828 0.4575 0.036 Uiso 1 1 d R . . H32B H 0.6817 -0.1071 0.3786 0.036 Uiso 1 1 d R . . H32C H 0.7679 -0.0709 0.3998 0.036 Uiso 1 1 d R . . C32B C 0.7988(3) 0.1340(2) 0.03284(19) 0.0265(8) Uani 1 1 d . . . H32D H 0.8571 0.1230 -0.0090 0.040 Uiso 1 1 d R . . H32E H 0.7413 0.1055 0.0328 0.040 Uiso 1 1 d R . . H32F H 0.8178 0.1132 0.0771 0.040 Uiso 1 1 d R . . C33A C 0.9546(3) -0.39444(19) 0.46075(18) 0.0198(7) Uani 1 1 d . . . H33A H 0.9896 -0.4122 0.4978 0.030 Uiso 1 1 d R . . H33B H 0.9962 -0.4151 0.4159 0.030 Uiso 1 1 d R . . H33C H 0.8882 -0.4172 0.4768 0.030 Uiso 1 1 d R . . C33B C 0.5495(3) 0.39002(19) 0.02937(18) 0.0191(7) Uani 1 1 d . . . H33D H 0.6175 0.4090 0.0055 0.029 Uiso 1 1 d R . . H33E H 0.5179 0.4158 0.0733 0.029 Uiso 1 1 d R . . H33F H 0.5069 0.4062 -0.0032 0.029 Uiso 1 1 d R . . C41A C 0.9604(3) 0.11644(19) 0.34082(18) 0.0213(7) Uani 1 1 d . . . H41A H 0.9424 0.1267 0.3909 0.032 Uiso 1 1 d R . . H41B H 0.9117 0.1500 0.3176 0.032 Uiso 1 1 d R . . H41C H 1.0295 0.1320 0.3151 0.032 Uiso 1 1 d R . . C41B C 0.5639(3) -0.1170(2) 0.1525(2) 0.0272(8) Uani 1 1 d . . . H41D H 0.4972 -0.1293 0.1861 0.041 Uiso 1 1 d R . . H41E H 0.6181 -0.1494 0.1709 0.041 Uiso 1 1 d R . . H41F H 0.5695 -0.1320 0.1054 0.041 Uiso 1 1 d R . . N1A N 0.7551(2) -0.33486(17) 0.37010(14) 0.0173(6) Uani 1 1 d . . . N1B N 0.7533(2) 0.34855(16) 0.12314(14) 0.0150(5) Uani 1 1 d . . . N1N N 1.4365(2) -0.17043(19) 0.37571(16) 0.0251(7) Uani 1 1 d . . . N2A N 0.7495(2) -0.19436(17) 0.44372(15) 0.0201(6) Uani 1 1 d . . . N2B N 0.7683(2) 0.22634(17) 0.02900(14) 0.0195(6) Uani 1 1 d . . . N3A N 0.9383(2) -0.30041(16) 0.44778(14) 0.0156(6) Uani 1 1 d . . . N3B N 0.55929(19) 0.29641(16) 0.04896(13) 0.0137(5) Uani 1 1 d . . . N5N N 1.0546(2) 0.15190(18) 0.13145(14) 0.0195(6) Uani 1 1 d . . . O1A O 0.83664(17) -0.17923(13) 0.26895(11) 0.0158(5) Uani 1 1 d . . . O1B O 0.69626(17) 0.18235(13) 0.21509(11) 0.0151(4) Uani 1 1 d . . . O1E O 1.06576(17) -0.22572(13) 0.20493(11) 0.0160(5) Uani 1 1 d . . . O1D O 0.52728(16) 0.31644(13) 0.20215(11) 0.0139(4) Uani 1 1 d . . . O1M O 1.09903(18) -0.05653(15) 0.19100(13) 0.0218(5) Uani 1 1 d . . . H1M H 1.080(3) 0.002(2) 0.1886(19) 0.026 Uiso 1 1 d . . . O1W O 0.88234(19) -0.00011(14) 0.23156(13) 0.0196(5) Uani 1 1 d D . . H11W H 0.880(3) 0.014(2) 0.2701(11) 0.023 Uiso 1 1 d D . . H12W H 0.905(3) 0.0420(17) 0.1978(12) 0.023 Uiso 1 1 d D . . O2A O 0.93542(18) -0.13348(14) 0.12731(12) 0.0205(5) Uani 1 1 d . . . O2B O 0.61559(17) 0.11517(13) 0.35311(11) 0.0183(5) Uani 1 1 d . . . O2E O 0.98524(16) -0.32396(13) 0.29526(11) 0.0149(5) Uani 1 1 d . . . O2D O 0.46521(17) 0.20890(13) 0.29028(12) 0.0171(5) Uani 1 1 d . . . O2N O 1.4800(3) -0.11471(19) 0.3879(2) 0.0543(9) Uani 1 1 d . . . O2W O 0.66962(19) -0.00087(14) 0.24340(13) 0.0203(5) Uani 1 1 d D . . H21W H 0.673(3) -0.011(2) 0.1993(10) 0.024 Uiso 1 1 d D . . H22W H 0.644(2) -0.0394(11) 0.2713(13) 0.024 Uiso 1 1 d D . . O3A O 0.94976(17) -0.14021(13) 0.33879(11) 0.0158(5) Uani 1 1 d . . . O3B O 0.57762(17) 0.13978(13) 0.14858(11) 0.0148(4) Uani 1 1 d . . . O2M O 0.45733(18) 0.03478(14) 0.29694(13) 0.0243(5) Uani 1 1 d . . . H2M H 0.4746 -0.0202 0.3178 0.029 Uiso 1 1 calc R . . O3N O 1.3929(3) -0.1522(2) 0.32672(18) 0.0739(12) Uani 1 1 d . . . O4A O 0.95644(18) 0.02816(13) 0.33941(12) 0.0182(5) Uani 1 1 d . . . O4B O 0.57403(18) -0.02755(13) 0.14516(12) 0.0192(5) Uani 1 1 d . . . O4N O 1.4347(2) -0.24189(17) 0.41126(17) 0.0463(8) Uani 1 1 d . . . O6N O 1.09909(19) 0.11388(15) 0.17825(13) 0.0250(5) Uani 1 1 d . . . O7N O 1.0759(2) 0.22320(15) 0.09894(14) 0.0282(6) Uani 1 1 d . . . O8N O 0.9871(2) 0.11518(15) 0.11851(14) 0.0274(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0140(2) 0.0103(2) 0.0134(2) -0.00142(15) -0.00291(16) 0.00045(15) Ni2 0.0202(2) 0.0115(2) 0.0144(2) 0.00113(16) -0.00697(17) -0.00388(16) Ni3 0.0128(2) 0.0105(2) 0.0133(2) -0.00109(15) -0.00419(16) 0.00043(15) Ni4 0.0198(2) 0.0107(2) 0.0155(2) 0.00081(16) -0.00629(17) -0.00251(16) C1A 0.0140(15) 0.0129(15) 0.0211(16) -0.0040(13) -0.0083(13) 0.0036(12) C1B 0.0121(15) 0.0148(15) 0.0163(15) -0.0030(12) -0.0063(12) 0.0040(12) C1M 0.0222(18) 0.0258(19) 0.0285(18) -0.0026(15) -0.0034(15) -0.0088(15) C2A 0.0193(17) 0.0143(15) 0.0216(16) 0.0018(13) -0.0105(13) -0.0034(12) C2B 0.0167(16) 0.0146(15) 0.0182(16) 0.0013(12) -0.0061(13) 0.0009(12) C3A 0.0235(17) 0.0155(16) 0.0183(16) -0.0008(13) -0.0094(14) -0.0012(13) C3B 0.0188(16) 0.0160(16) 0.0157(15) -0.0002(12) -0.0066(13) 0.0015(12) C3E 0.0126(15) 0.0164(15) 0.0142(15) -0.0028(12) -0.0048(12) -0.0044(12) C3D 0.0169(16) 0.0132(15) 0.0132(14) -0.0030(12) -0.0052(12) -0.0047(12) C4A 0.0171(16) 0.0156(15) 0.0224(16) -0.0050(13) -0.0118(13) 0.0027(12) C4B 0.0164(16) 0.0165(16) 0.0202(16) -0.0036(13) -0.0099(13) 0.0038(12) C4E 0.0163(16) 0.0137(15) 0.0111(14) 0.0012(12) -0.0037(12) -0.0032(12) C4D 0.0145(15) 0.0163(15) 0.0105(14) 0.0026(12) -0.0021(12) -0.0019(12) C2M 0.0216(18) 0.0255(19) 0.0256(18) -0.0029(15) 0.0024(15) -0.0053(14) C5A 0.0139(16) 0.0153(16) 0.0254(17) -0.0030(13) -0.0073(13) -0.0039(12) C5B 0.0129(15) 0.0148(15) 0.0218(16) -0.0003(13) -0.0080(13) -0.0001(12) C5E 0.0185(16) 0.0191(16) 0.0095(14) 0.0018(12) -0.0032(12) -0.0056(13) C5D 0.0169(16) 0.0198(16) 0.0122(14) 0.0032(12) -0.0033(12) -0.0055(13) C6A 0.0138(15) 0.0171(16) 0.0180(16) -0.0015(13) -0.0043(13) 0.0001(12) C6B 0.0137(15) 0.0161(15) 0.0166(15) -0.0020(12) -0.0056(12) 0.0024(12) C6E 0.0236(18) 0.0209(17) 0.0173(16) -0.0015(13) -0.0068(14) -0.0035(14) C6D 0.0180(17) 0.0221(17) 0.0157(15) 0.0006(13) -0.0024(13) -0.0050(13) C7A 0.0161(16) 0.0219(17) 0.0208(17) -0.0023(13) -0.0037(13) -0.0018(13) C7B 0.0112(15) 0.0247(17) 0.0192(16) -0.0011(13) -0.0057(13) -0.0019(13) C7E 0.0232(18) 0.033(2) 0.0238(18) 0.0008(15) -0.0103(15) -0.0117(15) C7D 0.0248(19) 0.0288(19) 0.0209(17) 0.0015(14) -0.0069(14) -0.0113(15) C8A 0.0185(17) 0.0237(18) 0.0159(16) 0.0001(13) 0.0037(13) -0.0029(14) C8B 0.0147(16) 0.0223(17) 0.0171(16) -0.0014(13) -0.0020(13) -0.0027(13) C8E 0.0180(18) 0.042(2) 0.0269(19) -0.0022(16) -0.0078(15) -0.0066(16) C8D 0.0150(17) 0.039(2) 0.0299(19) 0.0056(16) -0.0118(15) -0.0070(15) C9A 0.0198(17) 0.0232(18) 0.0190(16) -0.0026(14) 0.0009(14) 0.0014(14) C9B 0.0135(16) 0.0256(18) 0.0181(16) -0.0011(14) -0.0018(13) 0.0030(13) C9E 0.0154(17) 0.034(2) 0.0219(17) -0.0006(15) -0.0048(14) -0.0016(14) C9D 0.0149(17) 0.033(2) 0.0196(17) 0.0013(15) -0.0022(13) 0.0001(14) C10A 0.0261(19) 0.0231(18) 0.0190(16) -0.0040(14) -0.0008(14) -0.0005(14) C10B 0.0231(18) 0.0234(18) 0.0167(16) -0.0029(14) -0.0005(14) -0.0014(14) C10E 0.0114(15) 0.0261(18) 0.0105(14) 0.0026(13) -0.0007(12) -0.0036(13) C10D 0.0146(16) 0.0251(17) 0.0124(15) 0.0046(13) -0.0035(12) -0.0032(13) C11A 0.031(2) 0.0225(18) 0.0122(15) -0.0015(13) -0.0045(14) 0.0068(15) C11B 0.0187(17) 0.0191(16) 0.0130(15) -0.0024(13) -0.0012(13) -0.0001(13) C11E 0.0177(16) 0.0185(16) 0.0110(14) -0.0004(12) 0.0007(12) 0.0033(13) C11D 0.0185(17) 0.0200(17) 0.0111(14) -0.0007(12) 0.0028(12) 0.0008(13) C12A 0.0182(16) 0.0160(16) 0.0181(16) -0.0020(13) -0.0079(13) 0.0029(12) C12B 0.0124(15) 0.0158(15) 0.0170(15) -0.0006(12) -0.0047(12) 0.0008(12) C12E 0.0182(16) 0.0190(16) 0.0085(14) -0.0006(12) -0.0025(12) -0.0014(13) C12D 0.0180(16) 0.0191(16) 0.0131(15) -0.0017(13) -0.0010(13) 0.0010(13) C13A 0.0165(16) 0.0160(16) 0.0184(16) -0.0017(13) -0.0053(13) -0.0003(12) C13B 0.0124(15) 0.0182(16) 0.0155(15) -0.0017(13) -0.0011(12) -0.0027(12) C13E 0.0215(17) 0.0180(16) 0.0167(15) -0.0053(13) -0.0024(13) 0.0032(13) C13D 0.0282(19) 0.0200(17) 0.0196(17) -0.0065(14) -0.0038(14) 0.0019(14) C14A 0.0194(17) 0.0220(17) 0.0174(16) -0.0026(13) -0.0062(13) 0.0026(13) C14B 0.0144(16) 0.0210(17) 0.0208(16) -0.0021(13) -0.0057(13) -0.0001(13) C14E 0.0235(18) 0.0211(17) 0.0233(17) -0.0074(14) -0.0074(14) -0.0047(14) C14D 0.031(2) 0.0199(18) 0.0259(18) -0.0084(14) -0.0105(15) -0.0024(15) C15A 0.0182(16) 0.0214(17) 0.0187(16) -0.0066(13) -0.0063(13) -0.0005(13) C15B 0.0153(16) 0.0249(18) 0.0170(15) -0.0062(13) -0.0029(13) -0.0025(13) C15E 0.0149(16) 0.0207(17) 0.0274(18) -0.0049(14) -0.0083(14) -0.0016(13) C15D 0.0264(19) 0.0247(19) 0.0310(19) -0.0074(15) -0.0131(16) -0.0033(15) C16A 0.0185(16) 0.0166(16) 0.0157(15) -0.0035(12) -0.0021(13) -0.0042(13) C16B 0.0175(16) 0.0192(16) 0.0143(15) -0.0041(13) -0.0007(12) -0.0064(13) C16E 0.0173(16) 0.0162(16) 0.0186(16) -0.0019(13) -0.0047(13) -0.0018(12) C16D 0.0183(17) 0.0163(16) 0.0216(16) -0.0023(13) -0.0062(13) 0.0003(13) C17A 0.0155(16) 0.0155(15) 0.0137(15) -0.0018(12) -0.0028(12) -0.0002(12) C17B 0.0160(16) 0.0155(15) 0.0131(14) -0.0024(12) -0.0013(12) 0.0000(12) C17E 0.0147(15) 0.0157(15) 0.0129(14) 0.0020(12) -0.0029(12) -0.0037(12) C17D 0.0165(16) 0.0194(16) 0.0125(14) -0.0003(12) -0.0047(12) -0.0034(13) C18A 0.0122(15) 0.0145(15) 0.0147(15) -0.0031(12) -0.0013(12) -0.0013(12) C18B 0.0121(15) 0.0165(16) 0.0124(14) -0.0018(12) -0.0017(12) -0.0038(12) C19A 0.0301(19) 0.0217(18) 0.0220(17) -0.0028(14) -0.0141(15) -0.0053(14) C19B 0.031(2) 0.0209(17) 0.0219(17) -0.0044(14) -0.0125(15) -0.0036(15) C20A 0.0233(18) 0.0262(19) 0.0289(19) -0.0051(15) -0.0118(15) -0.0024(14) C20B 0.0219(18) 0.0279(19) 0.0259(18) -0.0070(15) -0.0084(15) -0.0080(15) C21A 0.032(2) 0.0250(19) 0.0230(18) 0.0062(15) -0.0107(15) -0.0114(15) C21B 0.027(2) 0.0252(19) 0.0188(17) -0.0030(14) 0.0051(14) -0.0097(15) C31A 0.0216(17) 0.0152(16) 0.0208(16) -0.0038(13) -0.0015(14) -0.0052(13) C31B 0.0197(17) 0.0145(16) 0.0239(17) -0.0040(13) -0.0049(14) -0.0026(13) C32A 0.0187(17) 0.0190(17) 0.0294(18) -0.0077(14) 0.0005(14) 0.0021(13) C32B 0.0232(18) 0.0219(18) 0.0308(19) -0.0101(15) -0.0023(15) 0.0045(14) C33A 0.0226(17) 0.0111(15) 0.0227(17) 0.0030(13) -0.0061(14) 0.0001(13) C33B 0.0180(16) 0.0147(16) 0.0235(17) 0.0020(13) -0.0077(14) -0.0001(13) C41A 0.0289(19) 0.0119(16) 0.0244(17) -0.0032(13) -0.0103(15) -0.0005(13) C41B 0.035(2) 0.0126(16) 0.034(2) -0.0006(15) -0.0129(17) 0.0007(14) N1A 0.0169(14) 0.0148(13) 0.0162(13) 0.0004(11) -0.0003(11) -0.0027(11) N1B 0.0137(13) 0.0154(13) 0.0141(13) -0.0011(10) -0.0030(11) 0.0002(10) N1N 0.0248(16) 0.0219(16) 0.0253(16) -0.0062(13) -0.0025(13) 0.0014(12) N2A 0.0169(14) 0.0203(14) 0.0212(14) -0.0040(12) -0.0046(11) 0.0028(11) N2B 0.0169(14) 0.0209(14) 0.0208(14) -0.0073(11) -0.0043(11) 0.0007(11) N3A 0.0197(14) 0.0115(13) 0.0129(13) 0.0018(10) -0.0044(11) 0.0023(10) N3B 0.0126(13) 0.0117(13) 0.0136(13) 0.0001(10) -0.0007(10) 0.0001(10) N5N 0.0195(14) 0.0205(15) 0.0151(13) -0.0028(11) -0.0011(11) -0.0003(11) O1A 0.0185(12) 0.0139(11) 0.0161(11) -0.0024(9) -0.0069(9) 0.0000(9) O1B 0.0172(11) 0.0137(11) 0.0148(11) -0.0025(9) -0.0065(9) 0.0012(9) O1E 0.0176(11) 0.0132(11) 0.0157(11) 0.0003(9) -0.0036(9) -0.0027(9) O1D 0.0113(10) 0.0145(11) 0.0148(10) -0.0012(9) -0.0025(8) -0.0021(8) O1M 0.0222(13) 0.0163(12) 0.0261(13) 0.0000(10) -0.0058(10) -0.0062(10) O1W 0.0264(13) 0.0138(11) 0.0212(12) -0.0014(9) -0.0117(11) -0.0017(9) O2A 0.0265(13) 0.0179(12) 0.0195(12) 0.0046(9) -0.0113(10) -0.0087(10) O2B 0.0235(12) 0.0169(11) 0.0141(11) 0.0010(9) -0.0045(9) -0.0064(9) O2E 0.0147(11) 0.0124(11) 0.0151(11) -0.0010(9) -0.0012(9) -0.0020(8) O2D 0.0179(12) 0.0152(11) 0.0161(11) 0.0013(9) -0.0037(9) -0.0024(9) O2N 0.050(2) 0.0328(17) 0.094(3) -0.0124(17) -0.0385(19) -0.0050(15) O2W 0.0269(13) 0.0130(11) 0.0211(12) 0.0004(9) -0.0095(10) 0.0002(9) O3A 0.0225(12) 0.0129(11) 0.0143(11) -0.0020(9) -0.0085(9) -0.0018(9) O3B 0.0164(11) 0.0144(11) 0.0153(11) -0.0018(9) -0.0073(9) -0.0017(9) O2M 0.0206(13) 0.0179(12) 0.0321(13) 0.0024(10) -0.0066(11) -0.0044(10) O3N 0.121(4) 0.067(2) 0.044(2) -0.0200(18) -0.045(2) 0.019(2) O4A 0.0254(13) 0.0114(11) 0.0207(11) -0.0017(9) -0.0115(10) -0.0011(9) O4B 0.0254(13) 0.0108(11) 0.0244(12) -0.0036(9) -0.0120(10) 0.0002(9) O4N 0.0391(17) 0.0253(15) 0.0567(19) 0.0120(14) 0.0032(15) -0.0073(13) O6N 0.0310(14) 0.0213(13) 0.0246(13) 0.0002(10) -0.0130(11) -0.0017(10) O7N 0.0290(14) 0.0220(13) 0.0302(14) 0.0042(11) -0.0053(11) -0.0091(11) O8N 0.0347(15) 0.0219(13) 0.0319(14) 0.0009(11) -0.0191(12) -0.0083(11) _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 O1A 2.049(2) . ? Ni1 O2E 2.062(2) . ? Ni1 O3A 2.092(2) . ? Ni1 N2A 2.110(3) . ? Ni1 N3A 2.162(3) . ? Ni1 N1A 2.173(3) . ? Ni2 O1A 1.997(2) . ? Ni2 O1E 2.011(2) . ? Ni2 O3A 2.028(2) . ? Ni2 O1M 2.063(2) . ? Ni2 O1W 2.101(2) . ? Ni2 O2A 2.194(2) . ? Ni3 O1D 2.067(2) . ? Ni3 O3B 2.077(2) . ? Ni3 O1B 2.087(2) . ? Ni3 N2B 2.171(3) . ? Ni3 N3B 2.177(3) . ? Ni3 N1B 2.232(3) . ? Ni4 O1B 2.012(2) . ? Ni4 O3B 2.014(2) . ? Ni4 O2M 2.031(2) . ? Ni4 O2D 2.039(2) . ? Ni4 O2W 2.057(2) . ? Ni4 O2B 2.150(2) . ? C1A O1A 1.327(4) . ? C1A C6A 1.398(4) . ? C1A C2A 1.418(4) . ? C1B O1B 1.334(4) . ? C1B C6B 1.385(4) . ? C1B C2B 1.408(4) . ? C1M O1M 1.435(4) . ? C2A C3A 1.382(4) . ? C2A O2A 1.403(4) . ? C2B C3B 1.385(4) . ? C2B O2B 1.393(4) . ? C3A C4A 1.389(4) . ? C3B C4B 1.395(4) . ? C3E O1E 1.255(4) . ? C3E O2E 1.262(4) . ? C3E C4E 1.512(4) . ? C3D O2D 1.257(4) . ? C3D O1D 1.272(4) . ? C3D C4D 1.516(4) . ? C4A C5A 1.399(5) . ? C4A C19A 1.504(4) . ? C4B C5B 1.385(4) . ? C4B C19B 1.516(4) . ? C4E C17E 1.399(4) . ? C4E C5E 1.417(4) . ? C4D C5D 1.401(4) . ? C4D C17D 1.403(4) . ? C2M O2M 1.439(4) . ? C5A C6A 1.394(4) . ? C5B C6B 1.406(4) . ? C5E C6E 1.430(4) . ? C5E C10E 1.434(4) . ? C5D C6D 1.430(4) . ? C5D C10D 1.439(4) . ? C6A C7A 1.501(4) . ? C6B C7B 1.502(4) . ? C6E C7E 1.367(5) . ? C6D C7D 1.368(5) . ? C7A N1A 1.496(4) . ? C7B N1B 1.499(4) . ? C7E C8E 1.414(5) . ? C7D C8D 1.419(5) . ? C8A N1A 1.484(4) . ? C8A C9A 1.530(4) . ? C8B N1B 1.486(4) . ? C8B C9B 1.518(4) . ? C8E C9E 1.362(5) . ? C8D C9D 1.360(5) . ? C9A N2A 1.509(4) . ? C9B N2B 1.483(4) . ? C9E C10E 1.429(4) . ? C9D C10D 1.436(5) . ? C10A N2A 1.481(4) . ? C10A C11A 1.516(4) . ? C10B C11B 1.496(4) . ? C10B N2B 1.500(4) . ? C10E C11E 1.395(4) . ? C10D C11D 1.385(5) . ? C11A N3A 1.490(4) . ? C11B N3B 1.486(4) . ? C11E C12E 1.393(4) . ? C11D C12D 1.395(5) . ? C12A N3A 1.505(4) . ? C12A C13A 1.504(4) . ? C12B N3B 1.493(4) . ? C12B C13B 1.511(4) . ? C12E C13E 1.420(4) . ? C12E C17E 1.442(4) . ? C12D C13D 1.430(5) . ? C12D C17D 1.439(4) . ? C13A C14A 1.387(4) . ? C13A C18A 1.399(4) . ? C13B C14B 1.400(4) . ? C13B C18B 1.406(4) . ? C13E C14E 1.355(5) . ? C13D C14D 1.353(5) . ? C14A C15A 1.389(5) . ? C14B C15B 1.384(5) . ? C14E C15E 1.419(5) . ? C14D C15D 1.420(5) . ? C15A C16A 1.392(4) . ? C15A C20A 1.516(4) . ? C15B C16B 1.398(5) . ? C15B C20B 1.507(4) . ? C15E C16E 1.355(4) . ? C15D C16D 1.365(5) . ? C16A C17A 1.368(4) . ? C16B C17B 1.384(4) . ? C16E C17E 1.438(4) . ? C16D C17D 1.428(4) . ? C17A O4A 1.392(4) . ? C17A C18A 1.423(4) . ? C17B O4B 1.378(4) . ? C17B C18B 1.419(4) . ? C18A O3A 1.330(4) . ? C18B O3B 1.341(4) . ? C21A O2A 1.421(4) . ? C21B O2B 1.437(4) . ? C31A N1A 1.481(4) . ? C31B N1B 1.476(4) . ? C32A N2A 1.492(4) . ? C32B N2B 1.470(4) . ? C33A N3A 1.477(4) . ? C33B N3B 1.476(4) . ? C41A O4A 1.428(4) . ? C41B O4B 1.437(4) . ? N1N O4N 1.225(4) . ? N1N O2N 1.232(4) . ? N1N O3N 1.238(4) . ? N5N O7N 1.229(3) . ? N5N O6N 1.261(4) . ? N5N O8N 1.265(4) . ? 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 O1A Ni1 O2E 90.53(8) . . ? O1A Ni1 O3A 75.59(8) . . ? O2E Ni1 O3A 97.85(8) . . ? O1A Ni1 N2A 100.19(10) . . ? O2E Ni1 N2A 167.87(9) . . ? O3A Ni1 N2A 90.37(10) . . ? O1A Ni1 N3A 164.72(9) . . ? O2E Ni1 N3A 86.63(9) . . ? O3A Ni1 N3A 89.92(9) . . ? N2A Ni1 N3A 84.46(10) . . ? O1A Ni1 N1A 90.45(9) . . ? O2E Ni1 N1A 90.95(9) . . ? O3A Ni1 N1A 163.49(9) . . ? N2A Ni1 N1A 83.37(10) . . ? N3A Ni1 N1A 104.59(10) . . ? O1A Ni2 O1E 96.85(9) . . ? O1A Ni2 O3A 78.19(9) . . ? O1E Ni2 O3A 96.90(9) . . ? O1A Ni2 O1M 177.46(9) . . ? O1E Ni2 O1M 85.47(9) . . ? O3A Ni2 O1M 100.55(9) . . ? O1A Ni2 O1W 91.64(9) . . ? O1E Ni2 O1W 167.52(9) . . ? O3A Ni2 O1W 93.78(9) . . ? O1M Ni2 O1W 86.23(9) . . ? O1A Ni2 O2A 78.97(8) . . ? O1E Ni2 O2A 82.16(9) . . ? O3A Ni2 O2A 156.86(9) . . ? O1M Ni2 O2A 102.42(9) . . ? O1W Ni2 O2A 90.54(9) . . ? O1D Ni3 O3B 96.58(8) . . ? O1D Ni3 O1B 90.05(8) . . ? O3B Ni3 O1B 76.43(8) . . ? O1D Ni3 N2B 161.17(9) . . ? O3B Ni3 N2B 97.17(9) . . ? O1B Ni3 N2B 105.65(9) . . ? O1D Ni3 N3B 87.12(9) . . ? O3B Ni3 N3B 86.23(9) . . ? O1B Ni3 N3B 162.00(9) . . ? N2B Ni3 N3B 81.02(10) . . ? O1D Ni3 N1B 90.05(9) . . ? O3B Ni3 N1B 162.46(9) . . ? O1B Ni3 N1B 87.38(9) . . ? N2B Ni3 N1B 80.54(10) . . ? N3B Ni3 N1B 110.38(9) . . ? O1B Ni4 O3B 79.55(8) . . ? O1B Ni4 O2M 176.79(9) . . ? O3B Ni4 O2M 102.10(9) . . ? O1B Ni4 O2D 96.27(9) . . ? O3B Ni4 O2D 95.71(9) . . ? O2M Ni4 O2D 86.32(9) . . ? O1B Ni4 O2W 92.63(9) . . ? O3B Ni4 O2W 95.73(9) . . ? O2M Ni4 O2W 84.49(9) . . ? O2D Ni4 O2W 166.61(9) . . ? O1B Ni4 O2B 78.79(8) . . ? O3B Ni4 O2B 158.18(8) . . ? O2M Ni4 O2B 99.66(9) . . ? O2D Ni4 O2B 84.10(9) . . ? O2W Ni4 O2B 87.86(9) . . ? O1A C1A C6A 122.3(3) . . ? O1A C1A C2A 119.6(3) . . ? C6A C1A C2A 118.1(3) . . ? O1B C1B C6B 121.7(3) . . ? O1B C1B C2B 120.7(3) . . ? C6B C1B C2B 117.6(3) . . ? C3A C2A O2A 123.5(3) . . ? C3A C2A C1A 121.5(3) . . ? O2A C2A C1A 115.0(3) . . ? C3B C2B O2B 124.9(3) . . ? C3B C2B C1B 121.8(3) . . ? O2B C2B C1B 113.3(3) . . ? C2A C3A C4A 120.3(3) . . ? C2B C3B C4B 120.3(3) . . ? O1E C3E O2E 126.7(3) . . ? O1E C3E C4E 116.3(3) . . ? O2E C3E C4E 116.9(3) . . ? O2D C3D O1D 125.9(3) . . ? O2D C3D C4D 117.9(3) . . ? O1D C3D C4D 116.2(3) . . ? C3A C4A C5A 118.7(3) . . ? C3A C4A C19A 120.4(3) . . ? C5A C4A C19A 120.9(3) . . ? C5B C4B C3B 118.5(3) . . ? C5B C4B C19B 120.7(3) . . ? C3B C4B C19B 120.8(3) . . ? C17E C4E C5E 121.0(3) . . ? C17E C4E C3E 119.5(3) . . ? C5E C4E C3E 119.5(3) . . ? C5D C4D C17D 121.3(3) . . ? C5D C4D C3D 119.0(3) . . ? C17D C4D C3D 119.7(3) . . ? C6A C5A C4A 121.6(3) . . ? C4B C5B C6B 121.2(3) . . ? C4E C5E C6E 122.7(3) . . ? C4E C5E C10E 118.9(3) . . ? C6E C5E C10E 118.4(3) . . ? C4D C5D C6D 122.7(3) . . ? C4D C5D C10D 118.8(3) . . ? C6D C5D C10D 118.4(3) . . ? C5A C6A C1A 119.8(3) . . ? C5A C6A C7A 123.2(3) . . ? C1A C6A C7A 116.8(3) . . ? C1B C6B C5B 120.6(3) . . ? C1B C6B C7B 117.3(3) . . ? C5B C6B C7B 121.9(3) . . ? C7E C6E C5E 121.0(3) . . ? C7D C6D C5D 121.4(3) . . ? N1A C7A C6A 114.0(3) . . ? N1B C7B C6B 115.1(3) . . ? C6E C7E C8E 120.2(3) . . ? C6D C7D C8D 119.9(3) . . ? N1A C8A C9A 112.1(3) . . ? N1B C8B C9B 110.2(3) . . ? C9E C8E C7E 121.0(3) . . ? C9D C8D C7D 121.1(3) . . ? N2A C9A C8A 112.6(3) . . ? N2B C9B C8B 109.5(3) . . ? C8E C9E C10E 120.6(3) . . ? C8D C9D C10D 120.9(3) . . ? N2A C10A C11A 112.2(3) . . ? C11B C10B N2B 110.4(3) . . ? C11E C10E C9E 121.5(3) . . ? C11E C10E C5E 119.7(3) . . ? C9E C10E C5E 118.8(3) . . ? C11D C10D C9D 122.0(3) . . ? C11D C10D C5D 119.7(3) . . ? C9D C10D C5D 118.3(3) . . ? N3A C11A C10A 112.2(3) . . ? N3B C11B C10B 110.5(3) . . ? C10E C11E C12E 121.7(3) . . ? C10D C11D C12D 121.9(3) . . ? N3A C12A C13A 118.3(3) . . ? N3B C12B C13B 115.2(2) . . ? C11E C12E C13E 121.6(3) . . ? C11E C12E C17E 119.2(3) . . ? C13E C12E C17E 119.2(3) . . ? C11D C12D C13D 122.1(3) . . ? C11D C12D C17D 119.0(3) . . ? C13D C12D C17D 118.9(3) . . ? C14A C13A C18A 120.5(3) . . ? C14A C13A C12A 118.3(3) . . ? C18A C13A C12A 121.0(3) . . ? C14B C13B C18B 120.8(3) . . ? C14B C13B C12B 118.1(3) . . ? C18B C13B C12B 121.0(3) . . ? C14E C13E C12E 121.1(3) . . ? C14D C13D C12D 121.3(3) . . ? C13A C14A C15A 121.6(3) . . ? C15B C14B C13B 121.6(3) . . ? C13E C14E C15E 120.1(3) . . ? C13D C14D C15D 119.9(3) . . ? C14A C15A C16A 118.0(3) . . ? C14A C15A C20A 120.6(3) . . ? C16A C15A C20A 121.4(3) . . ? C14B C15B C16B 117.9(3) . . ? C14B C15B C20B 120.8(3) . . ? C16B C15B C20B 121.3(3) . . ? C16E C15E C14E 121.2(3) . . ? C16D C15D C14D 121.1(3) . . ? C17A C16A C15A 121.2(3) . . ? C17B C16B C15B 121.5(3) . . ? C15E C16E C17E 120.8(3) . . ? C15D C16D C17D 120.8(3) . . ? C16A C17A O4A 123.9(3) . . ? C16A C17A C18A 121.1(3) . . ? O4A C17A C18A 114.9(3) . . ? O4B C17B C16B 123.5(3) . . ? O4B C17B C18B 115.5(3) . . ? C16B C17B C18B 121.0(3) . . ? C4E C17E C16E 122.9(3) . . ? C4E C17E C12E 119.5(3) . . ? C16E C17E C12E 117.6(3) . . ? C4D C17D C16D 122.7(3) . . ? C4D C17D C12D 119.3(3) . . ? C16D C17D C12D 118.0(3) . . ? O3A C18A C13A 121.3(3) . . ? O3A C18A C17A 121.6(3) . . ? C13A C18A C17A 117.0(3) . . ? O3B C18B C13B 122.2(3) . . ? O3B C18B C17B 120.7(3) . . ? C13B C18B C17B 117.1(3) . . ? C31A N1A C8A 109.7(2) . . ? C31A N1A C7A 107.6(3) . . ? C8A N1A C7A 108.9(2) . . ? C31A N1A Ni1 117.1(2) . . ? C8A N1A Ni1 103.65(19) . . ? C7A N1A Ni1 109.63(19) . . ? C31B N1B C8B 110.1(2) . . ? C31B N1B C7B 107.8(2) . . ? C8B N1B C7B 106.6(2) . . ? C31B N1B Ni3 114.69(19) . . ? C8B N1B Ni3 105.94(18) . . ? C7B N1B Ni3 111.48(19) . . ? O4N N1N O2N 121.6(3) . . ? O4N N1N O3N 120.2(4) . . ? O2N N1N O3N 118.2(3) . . ? C10A N2A C32A 107.3(2) . . ? C10A N2A C9A 113.1(3) . . ? C32A N2A C9A 110.0(2) . . ? C10A N2A Ni1 104.37(19) . . ? C32A N2A Ni1 111.95(19) . . ? C9A N2A Ni1 109.97(19) . . ? C32B N2B C9B 109.5(3) . . ? C32B N2B C10B 111.0(3) . . ? C9B N2B C10B 107.5(2) . . ? C32B N2B Ni3 109.6(2) . . ? C9B N2B Ni3 109.70(19) . . ? C10B N2B Ni3 109.43(19) . . ? C33A N3A C11A 108.8(2) . . ? C33A N3A C12A 104.9(2) . . ? C11A N3A C12A 113.8(3) . . ? C33A N3A Ni1 114.9(2) . . ? C11A N3A Ni1 107.02(19) . . ? C12A N3A Ni1 107.53(18) . . ? C33B N3B C11B 110.4(2) . . ? C33B N3B C12B 106.6(2) . . ? C11B N3B C12B 110.6(2) . . ? C33B N3B Ni3 113.01(19) . . ? C11B N3B Ni3 106.75(19) . . ? C12B N3B Ni3 109.51(18) . . ? O7N N5N O6N 121.0(3) . . ? O7N N5N O8N 120.4(3) . . ? O6N N5N O8N 118.6(3) . . ? C1A O1A Ni2 113.82(19) . . ? C1A O1A Ni1 120.25(19) . . ? Ni2 O1A Ni1 97.19(9) . . ? C1B O1B Ni4 110.64(18) . . ? C1B O1B Ni3 121.22(18) . . ? Ni4 O1B Ni3 95.74(9) . . ? C3E O1E Ni2 127.0(2) . . ? C3D O1D Ni3 128.63(19) . . ? C1M O1M Ni2 123.4(2) . . ? C2A O2A C21A 115.0(2) . . ? C2A O2A Ni2 107.49(17) . . ? C21A O2A Ni2 126.1(2) . . ? C2B O2B C21B 117.5(2) . . ? C2B O2B Ni4 107.49(17) . . ? C21B O2B Ni4 120.7(2) . . ? C3E O2E Ni1 127.9(2) . . ? C3D O2D Ni4 127.1(2) . . ? C18A O3A Ni2 129.99(19) . . ? C18A O3A Ni1 129.46(19) . . ? Ni2 O3A Ni1 94.88(8) . . ? C18B O3B Ni4 124.41(18) . . ? C18B O3B Ni3 131.05(19) . . ? Ni4 O3B Ni3 95.96(9) . . ? C2M O2M Ni4 126.7(2) . . ? C17A O4A C41A 116.9(2) . . ? C17B O4B C41B 117.7(3) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 4.660 _refine_diff_density_min -1.037 _refine_diff_density_rms 0.173 data_Compound4 _database_code_depnum_ccdc_archive 'CCDC 892617' #TrackingRef 'Colacio_Ni.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H46 N6 Ni2 O8' _chemical_formula_weight 712.13 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2625(6) _cell_length_b 9.9065(8) _cell_length_c 20.2078(16) _cell_angle_alpha 80.7740(10) _cell_angle_beta 88.7840(10) _cell_angle_gamma 76.4930(10) _cell_volume 1587.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6105 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.58 _exptl_crystal_description Prismatic _exptl_crystal_colour Green _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 1.243 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.639 _exptl_absorpt_correction_T_max 0.767 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _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 'Bruker Axs APEX automatic diffractometer' _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 15715 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5576 _reflns_number_gt 4888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker smart' _computing_cell_refinement 'Bruker smart' _computing_data_reduction 'Bruker smart' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; We have used 3 DFIX to fix the hydrogen atoms pertaining to the water molecule, O1W. 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^)+(0.0412P)^2^+1.0401P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5576 _refine_ls_number_parameters 415 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0844 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Ni1 Ni 1.15189(4) 1.05577(3) 0.760074(15) 0.01507(9) Uani 1 1 d . . . Ni2 Ni 0.98425(4) 0.81202(3) 0.761561(15) 0.01599(10) Uani 1 1 d . . . C21A C 0.9293(3) 0.5880(3) 0.88598(13) 0.0248(6) Uani 1 1 d . . . H21A H 0.9767 0.4946 0.9086 0.037 Uiso 1 1 d R . . H21B H 0.8433 0.5852 0.8554 0.037 Uiso 1 1 d R . . H21C H 0.8828 0.6469 0.9183 0.037 Uiso 1 1 d R . . C2A C 1.1711(3) 0.6834(2) 0.88770(12) 0.0179(5) Uani 1 1 d . . . C1A C 1.2487(3) 0.7848(2) 0.85220(12) 0.0166(5) Uani 1 1 d . . . C6A C 1.3736(3) 0.8233(2) 0.88501(12) 0.0181(5) Uani 1 1 d . . . C5A C 1.4124(3) 0.7673(3) 0.95204(12) 0.0206(5) Uani 1 1 d . . . H5A H 1.4948 0.7950 0.9735 0.025 Uiso 1 1 calc R . . C4A C 1.3316(3) 0.6713(3) 0.98784(12) 0.0212(5) Uani 1 1 d . . . C19A C 1.3711(3) 0.6140(3) 1.06102(13) 0.0268(6) Uani 1 1 d . . . H19A H 1.4695 0.6397 1.0740 0.040 Uiso 1 1 d R . . H19B H 1.3895 0.5134 1.0680 0.040 Uiso 1 1 d R . . H19C H 1.2795 0.6525 1.0876 0.040 Uiso 1 1 d R . . C3A C 1.2109(3) 0.6288(3) 0.95434(12) 0.0207(5) Uani 1 1 d . . . H3A H 1.1566 0.5632 0.9770 0.025 Uiso 1 1 calc R . . C7A C 1.4641(3) 0.9225(2) 0.84434(12) 0.0187(5) Uani 1 1 d . . . H7A1 H 1.5579 0.9295 0.8705 0.022 Uiso 1 1 calc R . . H7A2 H 1.5076 0.8838 0.8046 0.022 Uiso 1 1 calc R . . C31A C 1.3142(3) 1.1314(3) 0.88436(12) 0.0227(6) Uani 1 1 d . . . H31A H 1.4146 1.1352 0.9063 0.034 Uiso 1 1 d R . . H31B H 1.2537 1.0763 0.9142 0.034 Uiso 1 1 d R . . H31C H 1.2467 1.2250 0.8722 0.034 Uiso 1 1 d R . . C8A C 1.4518(3) 1.1516(3) 0.77786(13) 0.0214(5) Uani 1 1 d . . . H8A1 H 1.5583 1.1460 0.7988 0.026 Uiso 1 1 calc R . . H8A2 H 1.3912 1.2493 0.7708 0.026 Uiso 1 1 calc R . . C9A C 1.4807(3) 1.1009(3) 0.71075(12) 0.0208(5) Uani 1 1 d . . . H9A1 H 1.5192 1.1709 0.6792 0.025 Uiso 1 1 calc R . . H9A2 H 1.5676 1.0149 0.7160 0.025 Uiso 1 1 calc R . . C32A C 1.3735(3) 0.9464(3) 0.65026(13) 0.0234(6) Uani 1 1 d . . . H32A H 1.2756 0.9299 0.6313 0.035 Uiso 1 1 d R . . H32B H 1.4234 0.8666 0.6829 0.035 Uiso 1 1 d R . . H32C H 1.4514 0.9603 0.6154 0.035 Uiso 1 1 d R . . C10A C 1.2405(3) 1.1934(3) 0.63231(12) 0.0210(5) Uani 1 1 d . . . H10A H 1.1620 1.1622 0.6068 0.025 Uiso 1 1 calc R . . H10B H 1.3215 1.2231 0.6014 0.025 Uiso 1 1 calc R . . C11A C 1.1483(3) 1.3176(3) 0.66394(13) 0.0210(5) Uani 1 1 d . . . H11A H 1.2280 1.3633 0.6802 0.025 Uiso 1 1 calc R . . H11B H 1.0773 1.3853 0.6304 0.025 Uiso 1 1 calc R . . C33A C 1.0285(3) 1.3712(3) 0.76956(13) 0.0227(6) Uani 1 1 d . . . H33A H 1.1372 1.3769 0.7830 0.034 Uiso 1 1 d R . . H33B H 0.9705 1.3382 0.8082 0.034 Uiso 1 1 d R . . H33C H 0.9672 1.4626 0.7492 0.034 Uiso 1 1 d R . . C12A C 0.8700(3) 1.2810(3) 0.69956(12) 0.0198(5) Uani 1 1 d . . . H12A H 0.8144 1.3798 0.6889 0.024 Uiso 1 1 calc R . . H12B H 0.8142 1.2407 0.7378 0.024 Uiso 1 1 calc R . . C13A C 0.8440(3) 1.2110(3) 0.64071(12) 0.0175(5) Uani 1 1 d . . . C18A C 0.9026(3) 1.0644(2) 0.64518(12) 0.0172(5) Uani 1 1 d . . . C17A C 0.8660(3) 1.0036(3) 0.59057(12) 0.0192(5) Uani 1 1 d . . . C41A C 0.8941(3) 0.7929(3) 0.54191(13) 0.0258(6) Uani 1 1 d . . . H41A H 0.7755 0.8068 0.5383 0.039 Uiso 1 1 d R . . H41B H 0.9443 0.6941 0.5517 0.039 Uiso 1 1 d R . . H41C H 0.9359 0.8323 0.5004 0.039 Uiso 1 1 d R . . C16A C 0.7692(3) 1.0833(3) 0.53677(13) 0.0233(6) Uani 1 1 d . . . H16A H 0.7425 1.0393 0.5025 0.028 Uiso 1 1 calc R . . C15A C 0.7107(3) 1.2288(3) 0.53287(13) 0.0252(6) Uani 1 1 d . . . C20A C 0.6105(4) 1.3142(3) 0.47232(14) 0.0363(7) Uani 1 1 d . . . H20A H 0.5316 1.2652 0.4595 0.054 Uiso 1 1 d R . . H20B H 0.6843 1.3282 0.4358 0.054 Uiso 1 1 d R . . H20C H 0.5522 1.4038 0.4829 0.054 Uiso 1 1 d R . . C14A C 0.7507(3) 1.2902(3) 0.58538(13) 0.0221(6) Uani 1 1 d . . . H14A H 0.7141 1.3869 0.5836 0.027 Uiso 1 1 calc R . . N1A N 1.3566(2) 1.0668(2) 0.82325(10) 0.0180(4) Uani 1 1 d . . . N2A N 1.3270(2) 1.0739(2) 0.68267(10) 0.0186(4) Uani 1 1 d . . . N3A N 1.0451(2) 1.2719(2) 0.72069(10) 0.0183(4) Uani 1 1 d . . . O2A O 1.0569(2) 0.64343(17) 0.84969(8) 0.0192(4) Uani 1 1 d . . . O1A O 1.20593(19) 0.83902(16) 0.78851(8) 0.0164(4) Uani 1 1 d . . . O3A O 0.9957(2) 0.98955(17) 0.69773(8) 0.0181(4) Uani 1 1 d . . . O4A O 0.9336(2) 0.86065(17) 0.59474(8) 0.0224(4) Uani 1 1 d . . . C4B C 0.8387(3) 1.0150(3) 0.93302(13) 0.0296(6) Uani 1 1 d . . . H4B1 H 0.7193 1.0372 0.9316 0.044 Uiso 1 1 d R . . H4B2 H 0.8764 1.0890 0.9488 0.044 Uiso 1 1 d R . . H4B3 H 0.8791 0.9282 0.9628 0.044 Uiso 1 1 d R . . C3B C 0.9035(3) 1.0005(2) 0.86418(12) 0.0181(5) Uani 1 1 d . . . O2B O 0.8616(2) 0.90995(18) 0.83573(8) 0.0208(4) Uani 1 1 d . . . O1B O 0.9976(2) 1.07940(17) 0.83981(8) 0.0204(4) Uani 1 1 d . . . N1C N 0.7658(2) 0.7688(2) 0.73800(11) 0.0209(5) Uani 1 1 d . . . N2C N 0.7338(2) 0.7062(2) 0.69640(11) 0.0216(5) Uani 1 1 d . . . N3C N 0.6948(3) 0.6455(2) 0.65631(11) 0.0265(5) Uani 1 1 d . . . C1M C 0.4835(4) 0.5180(3) 0.77766(13) 0.0292(6) Uani 1 1 d . . . H1M1 H 0.5089 0.6040 0.7853 0.044 Uiso 1 1 d R . . H1M2 H 0.5812 0.4427 0.7861 0.044 Uiso 1 1 d R . . H1M3 H 0.3968 0.4975 0.8073 0.044 Uiso 1 1 d R . . O1M O 0.4285(2) 0.5319(2) 0.71040(10) 0.0280(4) Uani 1 1 d . . . H1M H 0.512(4) 0.575(3) 0.6903(15) 0.034 Uiso 1 1 d . . . O1W O 1.1021(2) 0.67728(18) 0.69703(9) 0.0192(4) Uani 1 1 d D . . H11W H 1.080(3) 0.730(2) 0.6609(10) 0.023 Uiso 1 1 d D . . H12W H 1.207(2) 0.650(3) 0.7000(12) 0.023 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01453(17) 0.01532(17) 0.01599(17) -0.00276(12) 0.00025(12) -0.00454(12) Ni2 0.01607(17) 0.01605(17) 0.01666(18) -0.00318(13) -0.00017(12) -0.00491(13) C21A 0.0269(14) 0.0291(15) 0.0226(14) -0.0025(11) 0.0016(11) -0.0162(12) C2A 0.0185(12) 0.0167(12) 0.0193(13) -0.0062(10) 0.0004(10) -0.0033(10) C1A 0.0177(12) 0.0145(12) 0.0157(12) -0.0025(10) 0.0008(10) 0.0001(10) C6A 0.0161(12) 0.0164(12) 0.0207(13) -0.0048(10) -0.0002(10) -0.0006(10) C5A 0.0193(13) 0.0205(13) 0.0215(13) -0.0048(10) -0.0037(10) -0.0021(10) C4A 0.0249(13) 0.0192(13) 0.0186(13) -0.0026(10) -0.0005(10) -0.0036(10) C19A 0.0309(15) 0.0298(15) 0.0195(14) 0.0012(11) -0.0037(11) -0.0103(12) C3A 0.0246(13) 0.0176(13) 0.0198(13) -0.0020(10) 0.0034(10) -0.0057(11) C7A 0.0168(12) 0.0205(13) 0.0200(13) -0.0047(10) -0.0009(10) -0.0056(10) C31A 0.0230(13) 0.0248(14) 0.0220(14) -0.0066(11) -0.0031(11) -0.0068(11) C8A 0.0176(13) 0.0235(14) 0.0247(14) 0.0004(11) -0.0030(10) -0.0108(11) C9A 0.0147(12) 0.0224(13) 0.0244(14) 0.0013(11) 0.0011(10) -0.0059(10) C32A 0.0214(13) 0.0243(14) 0.0255(14) -0.0093(11) 0.0045(11) -0.0041(11) C10A 0.0191(13) 0.0261(14) 0.0179(13) 0.0006(11) -0.0005(10) -0.0082(11) C11A 0.0211(13) 0.0188(13) 0.0221(14) 0.0024(10) -0.0018(10) -0.0059(10) C33A 0.0259(14) 0.0170(13) 0.0251(14) -0.0048(11) -0.0031(11) -0.0034(11) C12A 0.0158(12) 0.0184(13) 0.0226(13) -0.0007(10) -0.0007(10) -0.0007(10) C13A 0.0137(12) 0.0207(13) 0.0191(13) -0.0034(10) 0.0006(10) -0.0054(10) C18A 0.0122(12) 0.0186(13) 0.0203(13) 0.0000(10) 0.0014(10) -0.0050(10) C17A 0.0177(12) 0.0193(13) 0.0208(13) -0.0010(10) 0.0010(10) -0.0061(10) C41A 0.0354(15) 0.0243(14) 0.0205(14) -0.0073(11) -0.0035(11) -0.0099(12) C16A 0.0236(14) 0.0276(15) 0.0197(13) -0.0054(11) -0.0031(11) -0.0068(11) C15A 0.0226(14) 0.0286(15) 0.0217(14) -0.0023(11) -0.0029(11) -0.0017(11) C20A 0.0432(18) 0.0304(16) 0.0292(16) -0.0062(13) -0.0140(14) 0.0057(13) C14A 0.0185(13) 0.0205(13) 0.0245(14) 0.0000(11) 0.0007(11) -0.0012(10) N1A 0.0199(11) 0.0169(11) 0.0187(11) -0.0041(8) -0.0004(9) -0.0069(9) N2A 0.0171(10) 0.0190(11) 0.0206(11) -0.0044(9) 0.0006(8) -0.0054(8) N3A 0.0195(11) 0.0169(11) 0.0190(11) -0.0038(8) -0.0004(8) -0.0046(8) O2A 0.0217(9) 0.0216(9) 0.0172(9) -0.0015(7) 0.0004(7) -0.0117(7) O1A 0.0178(8) 0.0158(8) 0.0160(9) -0.0021(7) -0.0006(7) -0.0047(7) O3A 0.0198(9) 0.0164(9) 0.0174(9) 0.0014(7) -0.0039(7) -0.0056(7) O4A 0.0298(10) 0.0184(9) 0.0201(9) -0.0042(7) -0.0058(8) -0.0063(8) C4B 0.0293(15) 0.0401(17) 0.0248(15) -0.0114(13) 0.0049(12) -0.0148(13) C3B 0.0155(12) 0.0176(13) 0.0205(13) -0.0026(10) -0.0032(10) -0.0024(10) O2B 0.0188(9) 0.0244(10) 0.0219(9) -0.0077(8) 0.0036(7) -0.0077(7) O1B 0.0205(9) 0.0192(9) 0.0220(9) -0.0048(7) 0.0030(7) -0.0047(7) N1C 0.0179(11) 0.0238(12) 0.0234(12) -0.0093(10) 0.0001(9) -0.0058(9) N2C 0.0162(11) 0.0206(11) 0.0248(12) 0.0019(10) 0.0000(9) -0.0017(9) N3C 0.0274(12) 0.0268(12) 0.0269(13) -0.0077(10) -0.0028(10) -0.0071(10) C1M 0.0327(15) 0.0285(15) 0.0262(15) -0.0051(12) 0.0037(12) -0.0065(12) O1M 0.0222(10) 0.0316(11) 0.0312(11) -0.0059(9) -0.0024(8) -0.0076(8) O1W 0.0185(9) 0.0197(9) 0.0184(9) -0.0033(7) -0.0016(7) -0.0018(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1B 2.0422(17) . ? Ni1 O1A 2.0755(16) . ? Ni1 O3A 2.1005(16) . ? Ni1 N2A 2.123(2) . ? Ni1 N3A 2.144(2) . ? Ni1 N1A 2.173(2) . ? Ni2 O1A 2.0102(16) . ? Ni2 O3A 2.0276(16) . ? Ni2 N1C 2.032(2) . ? Ni2 O2B 2.0389(17) . ? Ni2 O1W 2.0803(17) . ? Ni2 O2A 2.2236(16) . ? C21A O2A 1.435(3) . ? C2A C3A 1.384(3) . ? C2A O2A 1.393(3) . ? C2A C1A 1.409(3) . ? C1A O1A 1.334(3) . ? C1A C6A 1.394(3) . ? C6A C5A 1.393(3) . ? C6A C7A 1.503(3) . ? C5A C4A 1.389(4) . ? C4A C3A 1.395(4) . ? C4A C19A 1.510(3) . ? C7A N1A 1.497(3) . ? C31A N1A 1.479(3) . ? C8A N1A 1.483(3) . ? C8A C9A 1.516(4) . ? C9A N2A 1.498(3) . ? C32A N2A 1.484(3) . ? C10A N2A 1.482(3) . ? C10A C11A 1.516(3) . ? C11A N3A 1.490(3) . ? C33A N3A 1.484(3) . ? C12A N3A 1.495(3) . ? C12A C13A 1.512(3) . ? C13A C14A 1.390(3) . ? C13A C18A 1.408(3) . ? C18A O3A 1.336(3) . ? C18A C17A 1.408(3) . ? C17A C16A 1.382(3) . ? C17A O4A 1.386(3) . ? C41A O4A 1.429(3) . ? C16A C15A 1.399(4) . ? C15A C14A 1.386(4) . ? C15A C20A 1.511(4) . ? C4B C3B 1.496(4) . ? C3B O2B 1.254(3) . ? C3B O1B 1.266(3) . ? N1C N2C 1.190(3) . ? N2C N3C 1.174(3) . ? C1M O1M 1.418(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1B Ni1 O1A 90.21(6) . . ? O1B Ni1 O3A 98.59(7) . . ? O1A Ni1 O3A 76.29(6) . . ? O1B Ni1 N2A 166.59(7) . . ? O1A Ni1 N2A 100.30(7) . . ? O3A Ni1 N2A 92.03(7) . . ? O1B Ni1 N3A 87.73(7) . . ? O1A Ni1 N3A 166.66(7) . . ? O3A Ni1 N3A 90.98(7) . . ? N2A Ni1 N3A 83.89(8) . . ? O1B Ni1 N1A 88.89(7) . . ? O1A Ni1 N1A 89.73(7) . . ? O3A Ni1 N1A 164.09(7) . . ? N2A Ni1 N1A 82.91(8) . . ? N3A Ni1 N1A 103.40(7) . . ? O1A Ni2 O3A 79.41(6) . . ? O1A Ni2 N1C 175.49(8) . . ? O3A Ni2 N1C 104.88(8) . . ? O1A Ni2 O2B 93.26(7) . . ? O3A Ni2 O2B 96.46(7) . . ? N1C Ni2 O2B 87.68(8) . . ? O1A Ni2 O1W 90.07(7) . . ? O3A Ni2 O1W 94.40(7) . . ? N1C Ni2 O1W 88.22(8) . . ? O2B Ni2 O1W 169.05(7) . . ? O1A Ni2 O2A 77.71(6) . . ? O3A Ni2 O2A 156.46(6) . . ? N1C Ni2 O2A 98.15(7) . . ? O2B Ni2 O2A 79.47(7) . . ? O1W Ni2 O2A 91.08(7) . . ? C3A C2A O2A 124.5(2) . . ? C3A C2A C1A 121.2(2) . . ? O2A C2A C1A 114.3(2) . . ? O1A C1A C6A 121.4(2) . . ? O1A C1A C2A 120.5(2) . . ? C6A C1A C2A 118.1(2) . . ? C5A C6A C1A 120.0(2) . . ? C5A C6A C7A 123.0(2) . . ? C1A C6A C7A 117.0(2) . . ? C4A C5A C6A 121.9(2) . . ? C5A C4A C3A 118.1(2) . . ? C5A C4A C19A 121.6(2) . . ? C3A C4A C19A 120.3(2) . . ? C2A C3A C4A 120.6(2) . . ? N1A C7A C6A 113.29(19) . . ? N1A C8A C9A 111.61(19) . . ? N2A C9A C8A 112.57(19) . . ? N2A C10A C11A 112.5(2) . . ? N3A C11A C10A 111.0(2) . . ? N3A C12A C13A 117.8(2) . . ? C14A C13A C18A 120.9(2) . . ? C14A C13A C12A 119.5(2) . . ? C18A C13A C12A 119.4(2) . . ? O3A C18A C17A 122.5(2) . . ? O3A C18A C13A 120.5(2) . . ? C17A C18A C13A 116.9(2) . . ? C16A C17A O4A 123.1(2) . . ? C16A C17A C18A 121.4(2) . . ? O4A C17A C18A 115.5(2) . . ? C17A C16A C15A 121.2(2) . . ? C14A C15A C16A 117.7(2) . . ? C14A C15A C20A 122.1(2) . . ? C16A C15A C20A 120.2(2) . . ? C15A C14A C13A 121.7(2) . . ? C31A N1A C8A 109.19(19) . . ? C31A N1A C7A 107.61(19) . . ? C8A N1A C7A 109.04(19) . . ? C31A N1A Ni1 117.52(15) . . ? C8A N1A Ni1 103.42(14) . . ? C7A N1A Ni1 109.81(14) . . ? C10A N2A C32A 108.63(19) . . ? C10A N2A C9A 112.10(18) . . ? C32A N2A C9A 109.11(19) . . ? C10A N2A Ni1 104.86(14) . . ? C32A N2A Ni1 112.53(15) . . ? C9A N2A Ni1 109.59(14) . . ? C33A N3A C11A 108.74(19) . . ? C33A N3A C12A 104.41(18) . . ? C11A N3A C12A 112.67(19) . . ? C33A N3A Ni1 115.42(15) . . ? C11A N3A Ni1 108.57(14) . . ? C12A N3A Ni1 107.09(14) . . ? C2A O2A C21A 116.48(18) . . ? C2A O2A Ni2 107.14(13) . . ? C21A O2A Ni2 118.88(14) . . ? C1A O1A Ni2 113.27(14) . . ? C1A O1A Ni1 118.99(14) . . ? Ni2 O1A Ni1 96.46(7) . . ? C18A O3A Ni2 133.56(14) . . ? C18A O3A Ni1 128.60(14) . . ? Ni2 O3A Ni1 95.15(7) . . ? C17A O4A C41A 117.65(19) . . ? O2B C3B O1B 125.4(2) . . ? O2B C3B C4B 117.3(2) . . ? O1B C3B C4B 117.3(2) . . ? C3B O2B Ni2 127.32(15) . . ? C3B O1B Ni1 127.35(16) . . ? N2C N1C Ni2 130.55(18) . . ? N3C N2C N1C 176.9(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.602 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.068