Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;The highest nuclearity metal oxime clusters: Ni14 and Ni12Na2 complexes from the use of 2-pyridinealdoximate and azide ligands ; _publ_contact_author_name 'Prof. George Christou' _publ_contact_author_email CHRISTOU@CHEM.UFL.EDU loop_ _publ_author_name 'George Christou' 'Khalil A. Abboud' 'Spyros P. Perlepes' 'Theocharis C. Stamatatos' # Attachment 'MSNo422_Ni_oxime_Charis_NEW_CIF_Ni14__Dalton_.cif' data_st64 _database_code_depnum_ccdc_archive 'CCDC 640087' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C116 H148 Cl2 N56 Ni14 O42' _chemical_formula_weight 3891.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.143(6) _cell_length_b 20.214(7) _cell_length_c 25.715(9) _cell_angle_alpha 83.379(7) _cell_angle_beta 82.208(7) _cell_angle_gamma 65.901(8) _cell_volume 8041(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description yellow _exptl_crystal_colour plates _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3996 _exptl_absorpt_coefficient_mu 1.722 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7645 _exptl_absorpt_correction_T_max 0.9601 _exptl_absorpt_process_details 'based on measured indexed crystal faces, Bruker SHELXTL v6.12 (Bruker 1998)' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 36302 _diffrn_reflns_av_R_equivalents 0.1731 _diffrn_reflns_av_sigmaI/netI 0.6911 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 23.00 _reflns_number_total 22335 _reflns_number_gt 4447 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART v5.624 (Bruker 1998)' _computing_cell_refinement 'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL v6.14 (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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. The asymmetric unit consists of two Ni14 half clusters, two perchlorate anions, four acetone molecules, two ether molecules and six water molecules. All solvents and anions were disordered and could not be modeled properly, thus program SQUEEZE, a part of the PLATON package of crystallographic software, was used to calculate the solvent disorder area and remove its contribution to the overall intensity data. Due to the low quality data, the important perchlorate anions could not be refined thus the charge balance of the crystal could not be ascertained crystallographically. The refinement of the cluster cations provides the molecular connectivity but distances and angles are probably not very reliable. There were a few restraints applied to fix bond distances of certain atoms that did not refine well. ; _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^)+(0.0457P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22335 _refine_ls_number_parameters 793 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.2199 _refine_ls_R_factor_gt 0.0828 _refine_ls_wR_factor_ref 0.2042 _refine_ls_wR_factor_gt 0.1813 _refine_ls_goodness_of_fit_ref 0.603 _refine_ls_restrained_S_all 0.603 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.23560(15) 0.43200(12) -0.09029(8) 0.0435(7) Uani 1 1 d . . . Ni2 Ni 0.06365(14) 0.38750(12) -0.06737(7) 0.0348(6) Uani 1 1 d . . . Ni3 Ni 0.21046(14) 0.33996(12) -0.17365(7) 0.0375(7) Uani 1 1 d . . . Ni4 Ni 0.08611(14) 0.45822(12) 0.03264(8) 0.0395(7) Uani 1 1 d D . . Ni5 Ni 0.27751(14) 0.15912(12) -0.12352(7) 0.0383(7) Uani 1 1 d . . . Ni6 Ni 0.12427(14) 0.21434(12) -0.01520(7) 0.0372(7) Uani 1 1 d . . . Ni7 Ni -0.05540(14) 0.28920(12) -0.06343(8) 0.0414(7) Uani 1 1 d . . . O1 O 0.1895(5) 0.3531(5) -0.0943(3) 0.026(3) Uiso 1 1 d . . . H1B H 0.2241 0.3072 -0.0743 0.032 Uiso 1 1 calc R . . O2 O 0.0659(5) 0.2865(5) -0.0757(3) 0.020(3) Uiso 1 1 d . . . H2B H 0.0945 0.2683 -0.1108 0.025 Uiso 1 1 calc R . . O3 O 0.0471(6) 0.4908(5) -0.0465(3) 0.027(3) Uiso 1 1 d . . . O4 O 0.2166(3) 0.4146(11) 0.0231(8) 0.160(9) Uiso 1 1 d D . . O5 O 0.0240(6) 0.4335(5) -0.1380(3) 0.028(3) Uiso 1 1 d . . . O6 O 0.3393(6) 0.2744(6) -0.1778(4) 0.041(3) Uiso 1 1 d . . . O7 O 0.1451(5) 0.1216(5) -0.0523(3) 0.022(3) Uiso 1 1 d . . . O8 O 0.0832(6) 0.3644(6) 0.0099(3) 0.031(3) Uiso 1 1 d . . . O9 O -0.0611(6) 0.4341(5) -0.0441(3) 0.030(3) Uiso 1 1 d . . . O10 O 0.0085(8) 0.1236(8) -0.0782(5) 0.087(4) Uiso 1 1 d . . . O11 O 0.0947(6) 0.4378(5) 0.1140(3) 0.038(3) Uiso 1 1 d . . . N1 N 0.2507(7) 0.5297(4) -0.1043(3) 0.036(4) Uiso 1 1 d G . . C1 C 0.3251(5) 0.5401(5) -0.1231(4) 0.059(6) Uiso 1 1 d G . . H1A H 0.3789 0.4997 -0.1256 0.071 Uiso 1 1 calc R . . C2 C 0.3209(6) 0.6097(7) -0.1381(4) 0.082(7) Uiso 1 1 d G . . H2A H 0.3717 0.6168 -0.1509 0.099 Uiso 1 1 calc R . . C3 C 0.2423(8) 0.6689(5) -0.1344(4) 0.061(6) Uiso 1 1 d G . . H3A H 0.2394 0.7165 -0.1446 0.073 Uiso 1 1 calc R . . C4 C 0.1678(6) 0.6585(5) -0.1156(4) 0.063(6) Uiso 1 1 d G . . H4A H 0.1141 0.6989 -0.1131 0.075 Uiso 1 1 calc R . . C5 C 0.1721(5) 0.5889(6) -0.1006(3) 0.033(5) Uiso 1 1 d G . . C6 C 0.0942(10) 0.5761(9) -0.0781(5) 0.035(5) Uiso 1 1 d . . . H6A H 0.0387 0.6121 -0.0692 0.043 Uiso 1 1 calc R . . N2 N 0.1175(7) 0.5036(7) -0.0728(4) 0.028(3) Uiso 1 1 d . . . N3 N 0.3637(6) 0.3614(6) -0.0964(5) 0.044(4) Uiso 1 1 d G . . C7 C 0.4209(11) 0.3470(11) -0.1415(4) 0.266(19) Uiso 1 1 d G . . H7A H 0.4009 0.3668 -0.1749 0.319 Uiso 1 1 calc R . . C8 C 0.5073(10) 0.3036(14) -0.1379(8) 0.88(8) Uiso 1 1 d G . . H8A H 0.5464 0.2937 -0.1688 1.053 Uiso 1 1 calc R . . C9 C 0.5366(7) 0.2746(11) -0.0891(11) 0.28(2) Uiso 1 1 d G . . H9A H 0.5957 0.2450 -0.0866 0.334 Uiso 1 1 calc R . . C10 C 0.4794(13) 0.2890(10) -0.0439(8) 0.159(11) Uiso 1 1 d G . . H10A H 0.4995 0.2692 -0.0105 0.191 Uiso 1 1 calc R . . C11 C 0.3930(11) 0.3324(10) -0.0475(4) 0.167(12) Uiso 1 1 d GD . . N4 N 0.2592(15) 0.3991(12) -0.0052(7) 0.110(7) Uiso 1 1 d . . . N5 N 0.2070(8) 0.3493(7) -0.2573(4) 0.035(4) Uiso 1 1 d . . . C13 C 0.2749(10) 0.3118(9) -0.2906(6) 0.044(5) Uiso 1 1 d . . . H13A H 0.3280 0.2789 -0.2784 0.053 Uiso 1 1 calc R . . C14 C 0.2626(12) 0.3244(11) -0.3452(7) 0.076(7) Uiso 1 1 d . . . H14A H 0.3060 0.2986 -0.3712 0.091 Uiso 1 1 calc R . . C15 C 0.1806(13) 0.3786(11) -0.3586(8) 0.086(7) Uiso 1 1 d . . . H15A H 0.1725 0.3939 -0.3945 0.103 Uiso 1 1 calc R . . C16 C 0.1139(12) 0.4088(10) -0.3209(7) 0.069(6) Uiso 1 1 d . . . H16A H 0.0580 0.4383 -0.3307 0.083 Uiso 1 1 calc R . . C17 C 0.1295(9) 0.3952(8) -0.2671(5) 0.022(4) Uiso 1 1 d . . . C18 C 0.0595(9) 0.4281(8) -0.2301(5) 0.020(4) Uiso 1 1 d . . . H18A H 0.0033 0.4598 -0.2383 0.024 Uiso 1 1 calc R . . N6 N 0.0861(7) 0.4067(6) -0.1777(4) 0.026(3) Uiso 1 1 d . . . N7 N 0.3871(8) 0.0883(7) -0.0940(5) 0.041(4) Uiso 1 1 d . . . C19 C 0.4043(11) 0.0191(9) -0.0709(6) 0.050(5) Uiso 1 1 d . . . H19A H 0.3593 0.0023 -0.0653 0.060 Uiso 1 1 calc R . . C20 C 0.4871(9) -0.0284(9) -0.0552(5) 0.033(4) Uiso 1 1 d . . . H20A H 0.4941 -0.0720 -0.0343 0.039 Uiso 1 1 calc R . . C21 C 0.5541(11) -0.0110(10) -0.0700(6) 0.058(6) Uiso 1 1 d . . . H21A H 0.6098 -0.0428 -0.0611 0.070 Uiso 1 1 calc R . . C22 C 0.5401(11) 0.0585(10) -0.1002(6) 0.060(6) Uiso 1 1 d . . . H22A H 0.5836 0.0762 -0.1114 0.072 Uiso 1 1 calc R . . C23 C 0.4575(10) 0.0936(9) -0.1099(6) 0.033(5) Uiso 1 1 d . . . C24 C 0.4422(11) 0.1679(9) -0.1410(6) 0.050(5) Uiso 1 1 d . . . H24A H 0.4871 0.1840 -0.1524 0.060 Uiso 1 1 calc R . . N8 N 0.3629(9) 0.2061(8) -0.1499(5) 0.048(4) Uiso 1 1 d . . . N9 N 0.2949(8) 0.0958(7) -0.1862(5) 0.041(4) Uiso 1 1 d . . . C25 C 0.3460(10) 0.0960(10) -0.2330(7) 0.056(6) Uiso 1 1 d . . . H25A H 0.3755 0.1274 -0.2410 0.067 Uiso 1 1 calc R . . C26 C 0.3499(16) 0.0434(15) -0.2686(10) 0.133(10) Uiso 1 1 d . . . H26A H 0.3848 0.0387 -0.3011 0.159 Uiso 1 1 calc R . . C27 C 0.3046(14) 0.0006(13) -0.2564(9) 0.109(9) Uiso 1 1 d . . . H27A H 0.3108 -0.0335 -0.2808 0.131 Uiso 1 1 calc R . . C28 C 0.2492(12) 0.0037(11) -0.2099(7) 0.080(7) Uiso 1 1 d . . . H28A H 0.2139 -0.0229 -0.2030 0.096 Uiso 1 1 calc R . . C29 C 0.2527(11) 0.0500(11) -0.1758(7) 0.062(6) Uiso 1 1 d . . . C30 C 0.1950(10) 0.0616(9) -0.1268(6) 0.046(5) Uiso 1 1 d . . . H30A H 0.1605 0.0346 -0.1172 0.055 Uiso 1 1 calc R . . N10 N 0.1929(8) 0.1115(7) -0.0962(5) 0.044(4) Uiso 1 1 d . . . N11 N 0.1677(7) 0.1561(7) 0.0545(5) 0.035(4) Uiso 1 1 d . . . C31 C 0.1935(10) 0.0839(10) 0.0666(7) 0.058(6) Uiso 1 1 d . . . H31A H 0.1973 0.0534 0.0400 0.070 Uiso 1 1 calc R . . C32 C 0.2144(9) 0.0529(10) 0.1162(6) 0.049(5) Uiso 1 1 d . . . H32A H 0.2342 0.0018 0.1237 0.059 Uiso 1 1 calc R . . C33 C 0.2053(12) 0.0995(12) 0.1553(8) 0.081(7) Uiso 1 1 d . . . H33A H 0.2185 0.0780 0.1896 0.098 Uiso 1 1 calc R . . C34 C 0.1787(10) 0.1742(10) 0.1478(6) 0.054(6) Uiso 1 1 d . . . H34A H 0.1741 0.2052 0.1742 0.065 Uiso 1 1 calc R . . C35 C 0.1593(11) 0.1979(11) 0.0951(7) 0.060(6) Uiso 1 1 d . . . C36 C 0.1305(9) 0.2775(9) 0.0787(6) 0.044(5) Uiso 1 1 d . . . H36A H 0.1255 0.3114 0.1030 0.053 Uiso 1 1 calc R . . N12 N 0.1123(8) 0.2993(7) 0.0292(5) 0.038(4) Uiso 1 1 d . . . C12 C 0.3416(16) 0.3450(16) 0.0012(7) 0.170(12) Uiso 1 1 d D . . H12A H 0.3602 0.3203 0.0339 0.204 Uiso 1 1 calc R . . N13 N -0.1753(8) 0.3022(7) -0.0362(4) 0.037(4) Uiso 1 1 d . . . C37 C -0.2165(11) 0.2567(10) -0.0297(6) 0.052(5) Uiso 1 1 d . . . H37A H -0.1825 0.2100 -0.0421 0.063 Uiso 1 1 calc R . . C38 C -0.2961(10) 0.2647(10) -0.0090(6) 0.047(5) Uiso 1 1 d . . . H38A H -0.3151 0.2262 -0.0052 0.056 Uiso 1 1 calc R . . C39 C -0.3470(12) 0.3331(11) 0.0060(6) 0.066(6) Uiso 1 1 d . . . H39A H -0.4049 0.3442 0.0199 0.080 Uiso 1 1 calc R . . C40 C -0.3157(11) 0.3839(11) 0.0013(6) 0.059(6) Uiso 1 1 d . . . H40A H -0.3512 0.4319 0.0106 0.071 Uiso 1 1 calc R . . C41 C -0.2318(10) 0.3659(9) -0.0172(5) 0.027(4) Uiso 1 1 d . . . C42 C -0.1913(9) 0.4198(9) -0.0229(5) 0.033(5) Uiso 1 1 d . . . H42A H -0.2234 0.4693 -0.0157 0.040 Uiso 1 1 calc R . . N14 N -0.1100(7) 0.3951(6) -0.0383(4) 0.024(3) Uiso 1 1 d . . . N15 N -0.0909(8) 0.3314(8) -0.1379(5) 0.039(4) Uiso 1 1 d . . . C43 C -0.1213(11) 0.3943(11) -0.1612(7) 0.071(6) Uiso 1 1 d . . . H43A H -0.1250 0.4324 -0.1412 0.085 Uiso 1 1 calc R . . C44 C -0.1522(12) 0.4184(13) -0.2141(8) 0.100(8) Uiso 1 1 d . . . H44A H -0.1751 0.4680 -0.2267 0.120 Uiso 1 1 calc R . . C45 C -0.1447(13) 0.3612(13) -0.2445(8) 0.095(8) Uiso 1 1 d . . . H45A H -0.1602 0.3706 -0.2795 0.114 Uiso 1 1 calc R . . C46 C -0.1133(12) 0.2900(12) -0.2207(8) 0.086(7) Uiso 1 1 d . . . H46A H -0.1119 0.2513 -0.2391 0.103 Uiso 1 1 calc R . . C47 C -0.0843(12) 0.2751(12) -0.1708(8) 0.077(7) Uiso 1 1 d . . . N16 N -0.0249(8) 0.1930(8) -0.0987(5) 0.055(4) Uiso 1 1 d . . . N17 N 0.2362(8) 0.4377(8) -0.1730(6) 0.057(5) Uiso 1 1 d . . . N18 N 0.2468(14) 0.4790(13) -0.2109(9) 0.133(9) Uiso 1 1 d . . . N19 N 0.264(2) 0.5137(18) -0.2385(12) 0.246(17) Uiso 1 1 d . . . N20 N 0.1784(8) 0.2457(7) -0.1623(5) 0.047(4) Uiso 1 1 d . . . N21 N 0.1452(10) 0.2342(9) -0.1970(6) 0.071(5) Uiso 1 1 d . . . N22 N 0.1120(9) 0.2208(9) -0.2260(6) 0.072(5) Uiso 1 1 d . . . N23 N 0.2432(7) 0.2077(6) -0.0474(4) 0.026(3) Uiso 1 1 d . . . N24 N 0.3031(8) 0.1921(7) -0.0224(5) 0.033(4) Uiso 1 1 d . . . N25 N 0.3565(8) 0.1765(7) 0.0091(5) 0.050(4) Uiso 1 1 d . . . N26 N -0.0008(8) 0.2301(7) 0.0075(5) 0.034(4) Uiso 1 1 d . . . N27 N -0.0322(10) 0.2006(9) 0.0351(6) 0.070(5) Uiso 1 1 d . . . N28 N -0.0599(11) 0.1650(10) 0.0680(7) 0.107(7) Uiso 1 1 d . . . C48 C -0.0546(10) 0.2015(10) -0.1481(6) 0.056(6) Uiso 1 1 d . . . H48A H -0.0551 0.1625 -0.1652 0.068 Uiso 1 1 calc R . . Ni8 Ni 0.47622(15) 0.18989(14) 0.40980(8) 0.0509(8) Uani 1 1 d D . . Ni9 Ni 0.46995(15) 0.07416(13) 0.53257(8) 0.0507(8) Uani 1 1 d . . . Ni10 Ni 0.37335(14) 0.07595(13) 0.43351(7) 0.0443(7) Uani 1 1 d . . . Ni11 Ni 0.16855(15) 0.16715(12) 0.48554(8) 0.0438(7) Uani 1 1 d . . . Ni12 Ni 0.21491(15) 0.01659(13) 0.43761(8) 0.0484(7) Uani 1 1 d . . . Ni13 Ni 0.13857(14) 0.29324(12) 0.37727(7) 0.0385(7) Uani 1 1 d . . . Ni14 Ni 0.35088(14) 0.19616(12) 0.32707(7) 0.0396(7) Uani 1 1 d . . . O12 O 0.3640(6) 0.1803(5) 0.4062(3) 0.033(3) Uani 1 1 d . . . H12B H 0.3154 0.2182 0.4262 0.039 Uiso 1 1 calc R . . O13 O 0.2482(6) 0.1034(5) 0.4297(4) 0.034(3) Uiso 1 1 d . . . H13B H 0.2331 0.1294 0.3946 0.041 Uiso 1 1 calc R . . O14 O 0.4977(6) 0.0390(6) 0.4538(4) 0.044(3) Uiso 1 1 d . . . N29 N 0.6060(8) 0.1740(8) 0.3964(5) 0.048(4) Uiso 1 1 d . . . C49 C 0.6446(11) 0.2201(11) 0.3798(6) 0.059(6) Uiso 1 1 d . . . H49A H 0.6092 0.2706 0.3793 0.070 Uiso 1 1 calc R . . C50 C 0.7281(12) 0.2013(11) 0.3639(6) 0.072(6) Uiso 1 1 d . . . H50A H 0.7484 0.2377 0.3504 0.086 Uiso 1 1 calc R . . C51 C 0.7839(13) 0.1304(12) 0.3668(7) 0.089(7) Uiso 1 1 d . . . H51A H 0.8435 0.1162 0.3564 0.107 Uiso 1 1 calc R . . C52 C 0.7493(12) 0.0796(12) 0.3860(7) 0.078(7) Uiso 1 1 d . . . H52A H 0.7858 0.0296 0.3905 0.093 Uiso 1 1 calc R . . C53 C 0.6619(10) 0.1024(9) 0.3982(6) 0.037(5) Uiso 1 1 d . . . C54 C 0.6230(9) 0.0537(8) 0.4185(5) 0.022(4) Uiso 1 1 d . . . H54A H 0.6563 0.0038 0.4269 0.027 Uiso 1 1 calc R . . N30 N 0.5452(9) 0.0785(7) 0.4247(5) 0.044(4) Uiso 1 1 d . . . O15 O 0.4381(13) 0.1914(11) 0.5275(8) 0.170(8) Uiso 1 1 d . . . N31 N 0.4226(7) 0.3058(6) 0.4068(5) 0.054(4) Uiso 1 1 d GD . . C55 C 0.4296(11) 0.3444(11) 0.3593(5) 0.215(15) Uiso 1 1 d G . . H55A H 0.4563 0.3192 0.3284 0.258 Uiso 1 1 calc R . . C56 C 0.3975(14) 0.4198(11) 0.3569(9) 0.30(2) Uiso 1 1 d G . . H56A H 0.4023 0.4461 0.3244 0.359 Uiso 1 1 calc R . . C57 C 0.3584(14) 0.4566(6) 0.4021(12) 0.28(2) Uiso 1 1 d G . . H57A H 0.3364 0.5081 0.4004 0.337 Uiso 1 1 calc R . . C58 C 0.3514(15) 0.4180(10) 0.4496(10) 0.51(4) Uiso 1 1 d G . . H58A H 0.3246 0.4432 0.4804 0.611 Uiso 1 1 calc R . . C59 C 0.3835(12) 0.3426(10) 0.4519(5) 0.32(2) Uiso 1 1 d GD . . C60 C 0.386(2) 0.2979(17) 0.4983(6) 0.29(2) Uiso 1 1 d D . . H60A H 0.3573 0.3167 0.5310 0.348 Uiso 1 1 calc R . . N32 N 0.4355(16) 0.2213(15) 0.4927(4) 0.172(11) Uiso 1 1 d D . . O16 O 0.3491(6) 0.0988(5) 0.5131(3) 0.034(3) Uiso 1 1 d . . . N33 N 0.1060(8) 0.2167(7) 0.5563(4) 0.032(4) Uiso 1 1 d . . . C61 C 0.0273(10) 0.2531(8) 0.5673(6) 0.036(5) Uiso 1 1 d . . . H61A H -0.0080 0.2614 0.5398 0.043 Uiso 1 1 calc R . . C62 C -0.0136(11) 0.2821(9) 0.6130(6) 0.054(5) Uiso 1 1 d . . . H62A H -0.0738 0.3096 0.6182 0.065 Uiso 1 1 calc R . . C63 C 0.0430(11) 0.2672(10) 0.6532(7) 0.060(6) Uiso 1 1 d . . . H63A H 0.0210 0.2842 0.6872 0.072 Uiso 1 1 calc R . . C64 C 0.1267(11) 0.2293(9) 0.6420(6) 0.051(5) Uiso 1 1 d . . . H64A H 0.1645 0.2204 0.6682 0.061 Uiso 1 1 calc R . . C65 C 0.1620(10) 0.2011(9) 0.5902(6) 0.034(5) Uiso 1 1 d . . . C66 C 0.2482(10) 0.1595(9) 0.5764(6) 0.045(5) Uiso 1 1 d . . . H66A H 0.2895 0.1473 0.6010 0.054 Uiso 1 1 calc R . . N34 N 0.2709(8) 0.1374(7) 0.5285(5) 0.030(4) Uiso 1 1 d . . . O17 O 0.4021(7) -0.0334(6) 0.4577(4) 0.049(3) Uiso 1 1 d . . . N35 N 0.2003(10) -0.0809(8) 0.4639(5) 0.064(5) Uiso 1 1 d . . . C67 C 0.1273(11) -0.0909(10) 0.4686(6) 0.052(5) Uiso 1 1 d . . . H67A H 0.0764 -0.0514 0.4591 0.063 Uiso 1 1 calc R . . C68 C 0.1230(12) -0.1585(10) 0.4872(6) 0.065(6) Uiso 1 1 d . . . H68A H 0.0700 -0.1640 0.4911 0.078 Uiso 1 1 calc R . . C69 C 0.1954(13) -0.2140(12) 0.4990(7) 0.080(7) Uiso 1 1 d . . . H69A H 0.1950 -0.2603 0.5106 0.096 Uiso 1 1 calc R . . C70 C 0.2707(11) -0.2036(10) 0.4942(6) 0.059(6) Uiso 1 1 d . . . H70A H 0.3221 -0.2435 0.5025 0.071 Uiso 1 1 calc R . . C71 C 0.2745(11) -0.1332(10) 0.4768(6) 0.042(5) Uiso 1 1 d . . . C72 C 0.3483(11) -0.1170(9) 0.4723(6) 0.044(5) Uiso 1 1 d . . . H72A H 0.4041 -0.1528 0.4772 0.052 Uiso 1 1 calc R . . N36 N 0.3332(8) -0.0509(8) 0.4612(5) 0.040(4) Uiso 1 1 d . . . O18 O 0.0232(8) 0.1016(7) 0.4244(4) 0.074(4) Uiso 1 1 d . . . N37 N 0.2574(8) -0.0207(7) 0.3617(4) 0.033(4) Uiso 1 1 d . . . C73 C 0.3310(12) -0.0605(10) 0.3406(7) 0.059(6) Uiso 1 1 d . . . H73A H 0.3765 -0.0759 0.3625 0.071 Uiso 1 1 calc R . . C74 C 0.3566(14) -0.0873(12) 0.2848(8) 0.096(8) Uiso 1 1 d . . . H74A H 0.4133 -0.1144 0.2701 0.115 Uiso 1 1 calc R . . C75 C 0.2836(12) -0.0654(10) 0.2600(7) 0.066(6) Uiso 1 1 d . . . H75A H 0.2892 -0.0795 0.2252 0.080 Uiso 1 1 calc R . . C76 C 0.1999(13) -0.0230(11) 0.2827(8) 0.086(7) Uiso 1 1 d . . . H76A H 0.1511 -0.0098 0.2639 0.103 Uiso 1 1 calc R . . C77 C 0.1914(13) -0.0009(11) 0.3346(7) 0.068(6) Uiso 1 1 d . . . C78 C 0.1112(12) 0.0434(10) 0.3523(7) 0.065(6) Uiso 1 1 d . . . H78A H 0.0646 0.0611 0.3311 0.078 Uiso 1 1 calc R . . N38 N 0.1023(9) 0.0606(8) 0.4028(5) 0.055(4) Uiso 1 1 d . . . O19 O 0.0550(6) 0.2089(6) 0.4506(4) 0.042(3) Uiso 1 1 d . . . N39 N 0.0611(8) 0.3226(7) 0.3144(5) 0.039(4) Uiso 1 1 d . . . C79 C 0.0761(11) 0.3567(9) 0.2671(6) 0.052(5) Uiso 1 1 d . . . H79A H 0.1241 0.3697 0.2597 0.063 Uiso 1 1 calc R . . C80 C 0.0163(13) 0.3714(12) 0.2305(8) 0.096(8) Uiso 1 1 d . . . H80A H 0.0255 0.3921 0.1963 0.115 Uiso 1 1 calc R . . C81 C -0.0598(12) 0.3551(11) 0.2443(7) 0.078(7) Uiso 1 1 d . . . H81A H -0.1029 0.3706 0.2206 0.094 Uiso 1 1 calc R . . C82 C -0.0699(13) 0.3174(11) 0.2913(8) 0.093(7) Uiso 1 1 d . . . H82A H -0.1157 0.3018 0.2999 0.112 Uiso 1 1 calc R . . C83 C -0.0045(11) 0.3035(10) 0.3268(7) 0.053(5) Uiso 1 1 d . . . C84 C -0.0091(9) 0.2645(8) 0.3753(5) 0.033(5) Uiso 1 1 d . . . H84A H -0.0550 0.2496 0.3865 0.040 Uiso 1 1 calc R . . N40 N 0.0537(8) 0.2504(7) 0.4035(5) 0.045(4) Uiso 1 1 d . . . O20 O 0.2997(6) 0.3097(5) 0.3271(4) 0.037(3) Uiso 1 1 d . . . N41 N 0.0728(8) 0.3970(7) 0.4047(5) 0.037(4) Uiso 1 1 d . . . C85 C -0.0067(10) 0.4235(9) 0.4288(6) 0.042(5) Uiso 1 1 d . . . H85A H -0.0374 0.3930 0.4356 0.050 Uiso 1 1 calc R . . C86 C -0.0471(11) 0.4961(9) 0.4447(6) 0.049(5) Uiso 1 1 d . . . H86A H -0.1027 0.5160 0.4631 0.059 Uiso 1 1 calc R . . C87 C 0.0035(11) 0.5332(11) 0.4304(6) 0.064(6) Uiso 1 1 d . . . H87A H -0.0192 0.5819 0.4402 0.077 Uiso 1 1 calc R . . C88 C 0.0829(10) 0.5089(9) 0.4036(6) 0.042(5) Uiso 1 1 d . . . H88A H 0.1141 0.5387 0.3939 0.051 Uiso 1 1 calc R . . C89 C 0.1140(10) 0.4380(9) 0.3918(6) 0.032(5) Uiso 1 1 d . . . C90 C 0.1942(11) 0.4074(10) 0.3626(6) 0.053(6) Uiso 1 1 d . . . H90A H 0.2283 0.4345 0.3516 0.064 Uiso 1 1 calc R . . N42 N 0.2203(8) 0.3393(8) 0.3512(5) 0.043(4) Uiso 1 1 d . . . O21 O 0.4228(6) 0.0294(5) 0.3633(3) 0.031(3) Uiso 1 1 d . . . N43 N 0.3594(7) 0.1914(7) 0.2476(4) 0.023(3) Uiso 1 1 d . . . C91 C 0.3328(11) 0.2457(11) 0.2108(7) 0.073(6) Uiso 1 1 d . . . H91A H 0.3027 0.2941 0.2210 0.088 Uiso 1 1 calc R . . C92 C 0.3491(10) 0.2322(10) 0.1550(6) 0.052(5) Uiso 1 1 d . . . H92A H 0.3311 0.2721 0.1296 0.062 Uiso 1 1 calc R . . C93 C 0.3908(13) 0.1615(13) 0.1381(9) 0.109(9) Uiso 1 1 d . . . H93A H 0.4059 0.1526 0.1019 0.131 Uiso 1 1 calc R . . C94 C 0.4087(11) 0.1060(12) 0.1765(7) 0.075(7) Uiso 1 1 d . . . H94A H 0.4290 0.0568 0.1682 0.090 Uiso 1 1 calc R . . C95 C 0.3955(10) 0.1254(9) 0.2299(6) 0.039(5) Uiso 1 1 d . . . C96 C 0.4250(10) 0.0642(10) 0.2712(6) 0.059(6) Uiso 1 1 d . . . H96A H 0.4567 0.0148 0.2638 0.070 Uiso 1 1 calc R . . N44 N 0.4019(8) 0.0869(7) 0.3182(5) 0.046(4) Uiso 1 1 d . . . O22 O 0.4497(6) 0.0843(6) 0.6127(4) 0.041(3) Uiso 1 1 d . . . N45 N 0.4754(8) 0.1907(7) 0.3249(4) 0.028(4) Uiso 1 1 d . . . N46 N 0.5335(11) 0.1817(9) 0.2961(6) 0.068(5) Uiso 1 1 d . . . N47 N 0.5903(13) 0.1749(11) 0.2625(8) 0.125(8) Uiso 1 1 d . . . N48 N 0.2242(8) 0.2036(7) 0.3393(5) 0.044(4) Uiso 1 1 d . . . N49 N 0.1989(8) 0.1794(8) 0.3056(5) 0.045(4) Uiso 1 1 d . . . N50 N 0.1748(10) 0.1584(9) 0.2740(6) 0.080(6) Uiso 1 1 d . . . N51 N 0.1932(8) 0.2567(7) 0.4514(5) 0.041(4) Uiso 1 1 d . . . N52 N 0.1894(8) 0.3065(8) 0.4800(5) 0.041(4) Uiso 1 1 d . . . N53 N 0.1882(9) 0.3472(9) 0.5108(6) 0.080(5) Uiso 1 1 d . . . N54 N 0.1544(9) 0.0641(8) 0.5100(5) 0.055(4) Uiso 1 1 d . . . N55 N 0.1038(10) 0.0587(8) 0.5420(6) 0.061(5) Uiso 1 1 d . . . N56 N 0.0643(10) 0.0427(9) 0.5761(6) 0.084(6) 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 0.0800(19) 0.0437(17) 0.0255(13) 0.0123(12) -0.0194(12) -0.0430(16) Ni2 0.0632(17) 0.0296(15) 0.0188(12) 0.0020(11) -0.0089(11) -0.0252(14) Ni3 0.0656(18) 0.0353(16) 0.0176(12) 0.0095(11) -0.0148(11) -0.0260(15) Ni4 0.0627(18) 0.0323(15) 0.0300(13) -0.0040(12) -0.0054(12) -0.0247(15) Ni5 0.0615(17) 0.0341(16) 0.0232(13) 0.0085(12) -0.0141(12) -0.0228(15) Ni6 0.0656(17) 0.0359(16) 0.0193(12) 0.0036(11) -0.0134(11) -0.0281(15) Ni7 0.0688(18) 0.0343(16) 0.0294(13) 0.0001(12) -0.0114(12) -0.0275(15) Ni8 0.0662(19) 0.067(2) 0.0261(14) 0.0011(13) -0.0084(12) -0.0337(17) Ni9 0.0756(19) 0.0477(18) 0.0303(14) 0.0208(13) -0.0238(13) -0.0266(16) Ni10 0.0685(18) 0.0496(18) 0.0183(13) 0.0132(12) -0.0129(12) -0.0284(16) Ni11 0.0676(18) 0.0422(17) 0.0250(13) 0.0050(12) -0.0094(12) -0.0258(15) Ni12 0.0729(19) 0.0492(18) 0.0317(14) 0.0096(13) -0.0137(13) -0.0335(16) Ni13 0.0556(17) 0.0390(17) 0.0216(13) 0.0025(12) -0.0064(11) -0.0199(15) Ni14 0.0656(18) 0.0317(16) 0.0177(12) 0.0070(11) -0.0113(11) -0.0156(15) O12 0.045(7) 0.027(7) 0.017(6) 0.015(5) 0.004(5) -0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.975(12) . ? Ni1 O1 2.065(10) . ? Ni1 N3 2.069(10) . ? Ni1 N1 2.080(8) . ? Ni1 N17 2.116(14) . ? Ni1 N4 2.254(18) . ? Ni2 O9 1.989(9) . ? Ni2 O5 2.014(9) . ? Ni2 O1 2.025(9) . ? Ni2 O8 2.029(9) . ? Ni2 O2 2.061(10) . ? Ni2 O3 2.113(10) . ? Ni3 N6 2.014(11) . ? Ni3 O1 2.053(9) . ? Ni3 O6 2.055(10) . ? Ni3 N5 2.144(12) . ? Ni3 N20 2.169(14) . ? Ni3 N17 2.196(16) . ? Ni4 O4 2.033(5) . ? Ni4 O8 2.068(11) . ? Ni4 O3 2.085(9) 2_565 ? Ni4 O9 2.087(10) 2_565 ? Ni4 O11 2.098(9) . ? Ni4 O3 2.174(9) . ? Ni5 N7 2.023(12) . ? Ni5 N8 2.054(14) . ? Ni5 N10 2.057(13) . ? Ni5 N9 2.088(13) . ? Ni5 N20 2.139(13) . ? Ni5 N23 2.191(12) . ? Ni6 N26 2.045(13) . ? Ni6 N23 2.051(12) . ? Ni6 O2 2.063(8) . ? Ni6 N11 2.077(12) . ? Ni6 O7 2.080(10) . ? Ni6 N12 2.096(13) . ? Ni7 N13 1.999(12) . ? Ni7 O2 2.040(9) . ? Ni7 N15 2.070(12) . ? Ni7 N16 2.080(15) . ? Ni7 N14 2.095(12) . ? Ni7 N26 2.162(12) . ? O1 H1B 1.0000 . ? O2 H2B 1.0000 . ? O3 N2 1.405(13) . ? O3 Ni4 2.085(9) 2_565 ? O4 N4 0.94(2) . ? O5 N6 1.352(12) . ? O6 N8 1.408(15) . ? O7 N10 1.286(13) . ? O8 N12 1.269(14) . ? O9 N14 1.353(13) . ? O9 Ni4 2.087(10) 2_565 ? O10 N16 1.352(16) . ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C1 H1A 0.9500 . ? C2 C3 1.3900 . ? C2 H2A 0.9500 . ? C3 C4 1.3900 . ? C3 H3A 0.9500 . ? C4 C5 1.3900 . ? C4 H4A 0.9500 . ? C5 C6 1.491(16) . ? C6 N2 1.348(17) . ? C6 H6A 0.9500 . ? N3 C7 1.3900 . ? N3 C11 1.3900 . ? C7 C8 1.3900 . ? C7 H7A 0.9500 . ? C8 C9 1.3900 . ? C8 H8A 0.9500 . ? C9 C10 1.3900 . ? C9 H9A 0.9500 . ? C10 C11 1.3900 . ? C10 H10A 0.9500 . ? C11 C12 1.416(5) . ? N4 C12 1.41(3) . ? N5 C17 1.313(15) . ? N5 C13 1.350(16) . ? C13 C14 1.43(2) . ? C13 H13A 0.9500 . ? C14 C15 1.44(2) . ? C14 H14A 0.9500 . ? C15 C16 1.37(2) . ? C15 H15A 0.9500 . ? C16 C17 1.417(19) . ? C16 H16A 0.9500 . ? C17 C18 1.404(16) . ? C18 N6 1.443(15) . ? C18 H18A 0.9500 . ? N7 C23 1.264(17) . ? N7 C19 1.385(18) . ? C19 C20 1.433(18) . ? C19 H19A 0.9500 . ? C20 C21 1.33(2) . ? C20 H20A 0.9500 . ? C21 C22 1.47(2) . ? C21 H21A 0.9500 . ? C22 C23 1.343(19) . ? C22 H22A 0.9500 . ? C23 C24 1.56(2) . ? C24 N8 1.298(17) . ? C24 H24A 0.9500 . ? N9 C29 1.37(2) . ? N9 C25 1.390(17) . ? C25 C26 1.46(3) . ? C25 H25A 0.9500 . ? C26 C27 1.37(3) . ? C26 H26A 0.9500 . ? C27 C28 1.41(2) . ? C27 H27A 0.9500 . ? C28 C29 1.38(2) . ? C28 H28A 0.9500 . ? C29 C30 1.47(2) . ? C30 N10 1.335(18) . ? C30 H30A 0.9500 . ? N11 C31 1.353(19) . ? N11 C35 1.37(2) . ? C31 C32 1.379(19) . ? C31 H31A 0.9500 . ? C32 C33 1.41(2) . ? C32 H32A 0.9500 . ? C33 C34 1.39(2) . ? C33 H33A 0.9500 . ? C34 C35 1.42(2) . ? C34 H34A 0.9500 . ? C35 C36 1.50(2) . ? C36 N12 1.333(16) . ? C36 H36A 0.9500 . ? C12 H12A 0.9500 . ? N13 C37 1.354(19) . ? N13 C41 1.354(16) . ? C37 C38 1.347(19) . ? C37 H37A 0.9500 . ? C38 C39 1.37(2) . ? C38 H38A 0.9500 . ? C39 C40 1.33(2) . ? C39 H39A 0.9500 . ? C40 C41 1.362(18) . ? C40 H40A 0.9500 . ? C41 C42 1.499(19) . ? C42 N14 1.294(15) . ? C42 H42A 0.9500 . ? N15 C43 1.269(19) . ? N15 C47 1.45(2) . ? C43 C44 1.49(2) . ? C43 H43A 0.9500 . ? C44 C45 1.42(3) . ? C44 H44A 0.9500 . ? C45 C46 1.41(2) . ? C45 H45A 0.9500 . ? C46 C47 1.40(2) . ? C46 H46A 0.9500 . ? C47 C48 1.44(2) . ? N16 C48 1.400(18) . ? N17 N18 1.25(2) . ? N18 N19 1.04(4) . ? N20 N21 1.211(18) . ? N21 N22 1.114(19) . ? N23 N24 1.198(14) . ? N24 N25 1.223(15) . ? N26 N27 1.100(17) . ? N27 N28 1.22(2) . ? C48 H48A 0.9500 . ? Ni8 O12 2.025(10) . ? Ni8 N30 2.089(13) . ? Ni8 N29 2.099(13) . ? Ni8 N31 2.136(12) . ? Ni8 N45 2.184(11) . ? Ni8 N32 2.232(5) . ? Ni9 O16 2.043(10) . ? Ni9 O17 2.043(11) 2_656 ? Ni9 O22 2.061(10) . ? Ni9 O14 2.120(11) 2_656 ? Ni9 O14 2.153(10) . ? Ni9 O15 2.20(2) . ? Ni10 O13 1.998(9) . ? Ni10 O21 2.047(9) . ? Ni10 O14 2.070(10) . ? Ni10 O12 2.093(10) . ? Ni10 O17 2.095(11) . ? Ni10 O16 2.099(9) . ? Ni11 O13 2.011(9) . ? Ni11 N34 2.042(12) . ? Ni11 O19 2.065(10) . ? Ni11 N51 2.094(14) . ? Ni11 N33 2.116(12) . ? Ni11 N54 2.205(15) . ? Ni12 O13 2.038(10) . ? Ni12 N38 2.050(13) . ? Ni12 N36 2.055(12) . ? Ni12 N37 2.101(12) . ? Ni12 N35 2.111(16) . ? Ni12 N54 2.131(14) . ? Ni13 N42 1.986(14) . ? Ni13 N40 1.987(13) . ? Ni13 N48 2.058(13) . ? Ni13 N41 2.089(13) . ? Ni13 N39 2.107(12) . ? Ni13 N51 2.157(12) . ? Ni14 N43 2.040(11) . ? Ni14 N44 2.044(14) . ? Ni14 O12 2.052(8) . ? Ni14 N45 2.086(12) . ? Ni14 O20 2.096(10) . ? Ni14 N48 2.097(13) . ? O12 H12B 1.0000 . ? O13 H13B 1.0000 . ? O14 N30 1.446(15) . ? O14 Ni9 2.120(11) 2_656 ? N29 C49 1.35(2) . ? N29 C53 1.370(18) . ? C49 C50 1.34(2) . ? C49 H49A 0.9500 . ? C50 C51 1.36(2) . ? C50 H50A 0.9500 . ? C51 C52 1.40(2) . ? C51 H51A 0.9500 . ? C52 C53 1.38(2) . ? C52 H52A 0.9500 . ? C53 C54 1.420(19) . ? C54 N30 1.212(15) . ? C54 H54A 0.9500 . ? O15 N32 1.02(3) . ? N31 C55 1.3900 . ? N31 C59 1.3900 . ? C55 C56 1.3900 . ? C55 H55A 0.9500 . ? C56 C57 1.3900 . ? C56 H56A 0.9500 . ? C57 C58 1.3900 . ? C57 H57A 0.9500 . ? C58 C59 1.3900 . ? C58 H58A 0.9500 . ? C59 C60 1.405(5) . ? C60 N32 1.44(3) . ? C60 H60A 0.9500 . ? O16 N34 1.279(12) . ? N33 C61 1.255(15) . ? N33 C65 1.302(16) . ? C61 C62 1.349(18) . ? C61 H61A 0.9500 . ? C62 C63 1.43(2) . ? C62 H62A 0.9500 . ? C63 C64 1.330(19) . ? C63 H63A 0.9500 . ? C64 C65 1.462(19) . ? C64 H64A 0.9500 . ? C65 C66 1.390(18) . ? C66 N34 1.314(16) . ? C66 H66A 0.9500 . ? O17 N36 1.355(15) . ? O17 Ni9 2.043(11) 2_656 ? N35 C67 1.333(19) . ? N35 C71 1.334(17) . ? C67 C68 1.42(2) . ? C67 H67A 0.9500 . ? C68 C69 1.33(2) . ? C68 H68A 0.9500 . ? C69 C70 1.38(2) . ? C69 H69A 0.9500 . ? C70 C71 1.47(2) . ? C70 H70A 0.9500 . ? C71 C72 1.42(2) . ? C72 N36 1.257(18) . ? C72 H72A 0.9500 . ? O18 N38 1.349(14) . ? N37 C73 1.272(17) . ? N37 C77 1.307(19) . ? C73 C74 1.54(2) . ? C73 H73A 0.9500 . ? C74 C75 1.37(2) . ? C74 H74A 0.9500 . ? C75 C76 1.42(2) . ? C75 H75A 0.9500 . ? C76 C77 1.43(2) . ? C76 H76A 0.9500 . ? C77 C78 1.35(2) . ? C78 N38 1.356(18) . ? C78 H78A 0.9500 . ? O19 N40 1.387(14) . ? N39 C83 1.321(19) . ? N39 C79 1.374(17) . ? C79 C80 1.41(2) . ? C79 H79A 0.9500 . ? C80 C81 1.46(2) . ? C80 H80A 0.9500 . ? C81 C82 1.38(2) . ? C81 H81A 0.9500 . ? C82 C83 1.46(2) . ? C82 H82A 0.9500 . ? C83 C84 1.407(19) . ? C84 N40 1.298(16) . ? C84 H84A 0.9500 . ? O20 N42 1.337(13) . ? N41 C89 1.284(18) . ? N41 C85 1.334(16) . ? C85 C86 1.43(2) . ? C85 H85A 0.9500 . ? C86 C87 1.35(2) . ? C86 H86A 0.9500 . ? C87 C88 1.360(19) . ? C87 H87A 0.9500 . ? C88 C89 1.36(2) . ? C88 H88A 0.9500 . ? C89 C90 1.403(18) . ? C90 N42 1.318(19) . ? C90 H90A 0.9500 . ? O21 N44 1.513(14) . ? N43 C95 1.327(18) . ? N43 C91 1.333(18) . ? C91 C92 1.46(2) . ? C91 H91A 0.9500 . ? C92 C93 1.40(2) . ? C92 H92A 0.9500 . ? C93 C94 1.37(2) . ? C93 H93A 0.9500 . ? C94 C95 1.43(2) . ? C94 H94A 0.9500 . ? C95 C96 1.50(2) . ? C96 N44 1.295(18) . ? C96 H96A 0.9500 . ? N45 N46 1.121(16) . ? N46 N47 1.18(2) . ? N48 N49 1.246(17) . ? N49 N50 1.151(18) . ? N51 N52 1.288(16) . ? N52 N53 1.198(18) . ? N54 N55 1.144(16) . ? N55 N56 1.133(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 O1 90.3(5) . . ? N2 Ni1 N3 170.0(5) . . ? O1 Ni1 N3 95.1(4) . . ? N2 Ni1 N1 78.1(5) . . ? O1 Ni1 N1 160.3(4) . . ? N3 Ni1 N1 98.9(5) . . ? N2 Ni1 N17 99.1(5) . . ? O1 Ni1 N17 82.1(5) . . ? N3 Ni1 N17 90.0(5) . . ? N1 Ni1 N17 84.1(5) . . ? N2 Ni1 N4 93.3(7) . . ? O1 Ni1 N4 92.0(6) . . ? N3 Ni1 N4 78.1(7) . . ? N1 Ni1 N4 104.3(6) . . ? N17 Ni1 N4 166.3(7) . . ? O9 Ni2 O5 82.8(4) . . ? O9 Ni2 O1 172.6(4) . . ? O5 Ni2 O1 93.4(4) . . ? O9 Ni2 O8 87.1(4) . . ? O5 Ni2 O8 166.3(4) . . ? O1 Ni2 O8 95.6(4) . . ? O9 Ni2 O2 96.1(4) . . ? O5 Ni2 O2 97.5(4) . . ? O1 Ni2 O2 90.6(4) . . ? O8 Ni2 O2 92.8(4) . . ? O9 Ni2 O3 76.4(4) . . ? O5 Ni2 O3 88.5(4) . . ? O1 Ni2 O3 97.3(4) . . ? O8 Ni2 O3 80.2(4) . . ? O2 Ni2 O3 169.9(4) . . ? N6 Ni3 O1 87.1(4) . . ? N6 Ni3 O6 174.0(4) . . ? O1 Ni3 O6 98.5(4) . . ? N6 Ni3 N5 80.8(5) . . ? O1 Ni3 N5 166.9(4) . . ? O6 Ni3 N5 93.5(4) . . ? N6 Ni3 N20 91.0(5) . . ? O1 Ni3 N20 91.3(4) . . ? O6 Ni3 N20 90.9(5) . . ? N5 Ni3 N20 93.9(5) . . ? N6 Ni3 N17 87.3(5) . . ? O1 Ni3 N17 80.5(5) . . ? O6 Ni3 N17 91.6(5) . . ? N5 Ni3 N17 93.9(5) . . ? N20 Ni3 N17 171.7(5) . . ? O4 Ni4 O8 91.0(7) . . ? O4 Ni4 O3 175.1(7) . 2_565 ? O8 Ni4 O3 93.6(4) . 2_565 ? O4 Ni4 O9 100.8(7) . 2_565 ? O8 Ni4 O9 164.8(4) . 2_565 ? O3 Ni4 O9 74.9(4) 2_565 2_565 ? O4 Ni4 O11 87.6(6) . . ? O8 Ni4 O11 103.5(4) . . ? O3 Ni4 O11 89.7(3) 2_565 . ? O9 Ni4 O11 86.7(4) 2_565 . ? O4 Ni4 O3 105.0(6) . . ? O8 Ni4 O3 77.9(4) . . ? O3 Ni4 O3 77.7(4) 2_565 . ? O9 Ni4 O3 89.8(4) 2_565 . ? O11 Ni4 O3 167.4(4) . . ? N7 Ni5 N8 77.2(5) . . ? N7 Ni5 N10 102.1(5) . . ? N8 Ni5 N10 179.2(5) . . ? N7 Ni5 N9 92.9(5) . . ? N8 Ni5 N9 100.2(5) . . ? N10 Ni5 N9 80.2(5) . . ? N7 Ni5 N20 167.8(5) . . ? N8 Ni5 N20 90.7(5) . . ? N10 Ni5 N20 90.0(5) . . ? N9 Ni5 N20 88.5(5) . . ? N7 Ni5 N23 86.4(5) . . ? N8 Ni5 N23 94.0(5) . . ? N10 Ni5 N23 85.5(5) . . ? N9 Ni5 N23 165.2(5) . . ? N20 Ni5 N23 95.2(5) . . ? N26 Ni6 N23 171.8(5) . . ? N26 Ni6 O2 80.3(4) . . ? N23 Ni6 O2 91.5(4) . . ? N26 Ni6 N11 93.7(5) . . ? N23 Ni6 N11 94.5(5) . . ? O2 Ni6 N11 169.6(4) . . ? N26 Ni6 O7 91.2(4) . . ? N23 Ni6 O7 88.9(4) . . ? O2 Ni6 O7 95.4(4) . . ? N11 Ni6 O7 93.3(5) . . ? N26 Ni6 N12 90.9(5) . . ? N23 Ni6 N12 90.0(5) . . ? O2 Ni6 N12 91.5(4) . . ? N11 Ni6 N12 79.9(5) . . ? O7 Ni6 N12 173.0(4) . . ? N13 Ni7 O2 166.8(5) . . ? N13 Ni7 N15 92.2(5) . . ? O2 Ni7 N15 96.8(4) . . ? N13 Ni7 N16 95.7(6) . . ? O2 Ni7 N16 95.2(5) . . ? N15 Ni7 N16 80.6(5) . . ? N13 Ni7 N14 76.7(5) . . ? O2 Ni7 N14 93.9(4) . . ? N15 Ni7 N14 88.9(5) . . ? N16 Ni7 N14 166.9(5) . . ? N13 Ni7 N26 94.2(5) . . ? O2 Ni7 N26 78.1(4) . . ? N15 Ni7 N26 170.2(5) . . ? N16 Ni7 N26 91.4(5) . . ? N14 Ni7 N26 99.8(4) . . ? Ni2 O1 Ni3 112.5(4) . . ? Ni2 O1 Ni1 111.4(4) . . ? Ni3 O1 Ni1 100.8(4) . . ? Ni2 O1 H1B 110.6 . . ? Ni3 O1 H1B 110.6 . . ? Ni1 O1 H1B 110.6 . . ? Ni7 O2 Ni2 110.4(4) . . ? Ni7 O2 Ni6 101.6(4) . . ? Ni2 O2 Ni6 110.3(4) . . ? Ni7 O2 H2B 111.4 . . ? Ni2 O2 H2B 111.4 . . ? Ni6 O2 H2B 111.4 . . ? N2 O3 Ni4 140.8(8) . 2_565 ? N2 O3 Ni2 105.6(7) . . ? Ni4 O3 Ni2 101.7(4) 2_565 . ? N2 O3 Ni4 101.5(7) . . ? Ni4 O3 Ni4 102.3(4) 2_565 . ? Ni2 O3 Ni4 97.4(4) . . ? N4 O4 Ni4 136(2) . . ? N6 O5 Ni2 112.0(7) . . ? N8 O6 Ni3 116.7(9) . . ? N10 O7 Ni6 116.7(9) . . ? N12 O8 Ni2 120.9(9) . . ? N12 O8 Ni4 132.1(9) . . ? Ni2 O8 Ni4 103.6(4) . . ? N14 O9 Ni2 120.2(8) . . ? N14 O9 Ni4 133.8(8) . 2_565 ? Ni2 O9 Ni4 106.0(5) . 2_565 ? C1 N1 C5 120.0 . . ? C1 N1 Ni1 127.8(6) . . ? C5 N1 Ni1 111.5(6) . . ? N1 C1 C2 120.0 . . ? N1 C1 H1A 120.0 . . ? C2 C1 H1A 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 N1 120.0 . . ? C4 C5 C6 121.4(10) . . ? N1 C5 C6 118.5(10) . . ? N2 C6 C5 107.0(13) . . ? N2 C6 H6A 126.5 . . ? C5 C6 H6A 126.5 . . ? C6 N2 O3 107.3(11) . . ? C6 N2 Ni1 124.0(11) . . ? O3 N2 Ni1 128.2(9) . . ? C7 N3 C11 120.0 . . ? C7 N3 Ni1 127.4(10) . . ? C11 N3 Ni1 112.3(10) . . ? N3 C7 C8 120.0 . . ? N3 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 120.0 . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 C11 120.0 . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C10 C11 N3 120.0 . . ? C10 C11 C12 114.8(18) . . ? N3 C11 C12 125.2(18) . . ? O4 N4 C12 123(2) . . ? O4 N4 Ni1 124(2) . . ? C12 N4 Ni1 113.0(15) . . ? C17 N5 C13 129.9(13) . . ? C17 N5 Ni3 107.1(10) . . ? C13 N5 Ni3 123.0(10) . . ? N5 C13 C14 116.2(15) . . ? N5 C13 H13A 121.9 . . ? C14 C13 H13A 121.9 . . ? C13 C14 C15 116.2(17) . . ? C13 C14 H14A 121.9 . . ? C15 C14 H14A 121.9 . . ? C16 C15 C14 121.9(19) . . ? C16 C15 H15A 119.0 . . ? C14 C15 H15A 119.0 . . ? C15 C16 C17 119.2(18) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? N5 C17 C18 126.9(13) . . ? N5 C17 C16 115.9(14) . . ? C18 C17 C16 117.0(14) . . ? C17 C18 N6 109.6(12) . . ? C17 C18 H18A 125.2 . . ? N6 C18 H18A 125.2 . . ? O5 N6 C18 115.7(10) . . ? O5 N6 Ni3 128.8(8) . . ? C18 N6 Ni3 115.5(8) . . ? C23 N7 C19 108.7(14) . . ? C23 N7 Ni5 120.0(12) . . ? C19 N7 Ni5 127.9(12) . . ? N7 C19 C20 122.7(16) . . ? N7 C19 H19A 118.6 . . ? C20 C19 H19A 118.6 . . ? C21 C20 C19 119.6(16) . . ? C21 C20 H20A 120.2 . . ? C19 C20 H20A 120.2 . . ? C20 C21 C22 118.7(17) . . ? C20 C21 H21A 120.7 . . ? C22 C21 H21A 120.7 . . ? C23 C22 C21 110.9(17) . . ? C23 C22 H22A 124.6 . . ? C21 C22 H22A 124.6 . . ? N7 C23 C22 137.0(17) . . ? N7 C23 C24 111.0(15) . . ? C22 C23 C24 110.9(16) . . ? N8 C24 C23 114.1(16) . . ? N8 C24 H24A 122.9 . . ? C23 C24 H24A 122.9 . . ? C24 N8 O6 120.6(14) . . ? C24 N8 Ni5 116.2(12) . . ? O6 N8 Ni5 123.2(10) . . ? C29 N9 C25 122.1(16) . . ? C29 N9 Ni5 112.6(11) . . ? C25 N9 Ni5 125.2(12) . . ? N9 C25 C26 113.3(19) . . ? N9 C25 H25A 123.4 . . ? C26 C25 H25A 123.4 . . ? C27 C26 C25 122(2) . . ? C27 C26 H26A 119.1 . . ? C25 C26 H26A 119.1 . . ? C26 C27 C28 124(3) . . ? C26 C27 H27A 117.9 . . ? C28 C27 H27A 117.9 . . ? C29 C28 C27 112(2) . . ? C29 C28 H28A 124.1 . . ? C27 C28 H28A 124.1 . . ? N9 C29 C28 126.3(18) . . ? N9 C29 C30 115.0(18) . . ? C28 C29 C30 117.9(19) . . ? N10 C30 C29 117.6(17) . . ? N10 C30 H30A 121.2 . . ? C29 C30 H30A 121.2 . . ? O7 N10 C30 119.3(14) . . ? O7 N10 Ni5 126.6(11) . . ? C30 N10 Ni5 113.9(11) . . ? C31 N11 C35 116.3(14) . . ? C31 N11 Ni6 128.4(12) . . ? C35 N11 Ni6 114.9(12) . . ? N11 C31 C32 122.3(17) . . ? N11 C31 H31A 118.8 . . ? C32 C31 H31A 118.8 . . ? C31 C32 C33 117.6(18) . . ? C31 C32 H32A 121.2 . . ? C33 C32 H32A 121.2 . . ? C34 C33 C32 125.3(19) . . ? C34 C33 H33A 117.3 . . ? C32 C33 H33A 117.3 . . ? C33 C34 C35 110.3(18) . . ? C33 C34 H34A 124.8 . . ? C35 C34 H34A 124.8 . . ? N11 C35 C34 128.0(17) . . ? N11 C35 C36 113.2(15) . . ? C34 C35 C36 118.7(17) . . ? N12 C36 C35 118.3(16) . . ? N12 C36 H36A 120.8 . . ? C35 C36 H36A 120.8 . . ? O8 N12 C36 126.2(14) . . ? O8 N12 Ni6 120.4(9) . . ? C36 N12 Ni6 113.1(11) . . ? N4 C12 C11 111(2) . . ? N4 C12 H12A 124.6 . . ? C11 C12 H12A 124.6 . . ? C37 N13 C41 106.5(13) . . ? C37 N13 Ni7 132.8(12) . . ? C41 N13 Ni7 120.6(11) . . ? C38 C37 N13 132.6(18) . . ? C38 C37 H37A 113.7 . . ? N13 C37 H37A 113.7 . . ? C37 C38 C39 114.0(19) . . ? C37 C38 H38A 123.0 . . ? C39 C38 H38A 123.0 . . ? C40 C39 C38 120.0(19) . . ? C40 C39 H39A 120.0 . . ? C38 C39 H39A 120.0 . . ? C39 C40 C41 118.8(19) . . ? C39 C40 H40A 120.6 . . ? C41 C40 H40A 120.6 . . ? N13 C41 C40 127.7(17) . . ? N13 C41 C42 110.1(13) . . ? C40 C41 C42 122.0(16) . . ? N14 C42 C41 116.0(15) . . ? N14 C42 H42A 122.0 . . ? C41 C42 H42A 122.0 . . ? C42 N14 O9 125.2(13) . . ? C42 N14 Ni7 115.9(11) . . ? O9 N14 Ni7 118.5(8) . . ? C43 N15 C47 112.1(16) . . ? C43 N15 Ni7 136.1(14) . . ? C47 N15 Ni7 111.6(12) . . ? N15 C43 C44 131(2) . . ? N15 C43 H43A 114.5 . . ? C44 C43 H43A 114.5 . . ? C45 C44 C43 115(2) . . ? C45 C44 H44A 122.7 . . ? C43 C44 H44A 122.7 . . ? C46 C45 C44 118(2) . . ? C46 C45 H45A 121.2 . . ? C44 C45 H45A 121.2 . . ? C47 C46 C45 122(2) . . ? C47 C46 H46A 119.2 . . ? C45 C46 H46A 119.2 . . ? C46 C47 C48 119(2) . . ? C46 C47 N15 123.1(19) . . ? C48 C47 N15 117.7(18) . . ? O10 N16 C48 114.7(15) . . ? O10 N16 Ni7 129.5(11) . . ? C48 N16 Ni7 115.0(12) . . ? N18 N17 Ni1 136.2(16) . . ? N18 N17 Ni3 129.1(16) . . ? Ni1 N17 Ni3 94.7(6) . . ? N19 N18 N17 169(4) . . ? N21 N20 Ni5 121.0(13) . . ? N21 N20 Ni3 117.7(12) . . ? Ni5 N20 Ni3 108.5(6) . . ? N22 N21 N20 175(2) . . ? N24 N23 Ni6 123.8(10) . . ? N24 N23 Ni5 113.7(10) . . ? Ni6 N23 Ni5 111.1(6) . . ? N23 N24 N25 171.2(15) . . ? N27 N26 Ni6 134.2(12) . . ? N27 N26 Ni7 122.3(13) . . ? Ni6 N26 Ni7 98.2(5) . . ? N26 N27 N28 174(2) . . ? N16 C48 C47 113.7(18) . . ? N16 C48 H48A 123.1 . . ? C47 C48 H48A 123.1 . . ? O12 Ni8 N30 94.1(5) . . ? O12 Ni8 N29 161.7(5) . . ? N30 Ni8 N29 74.7(6) . . ? O12 Ni8 N31 95.8(4) . . ? N30 Ni8 N31 167.3(5) . . ? N29 Ni8 N31 97.6(5) . . ? O12 Ni8 N45 79.2(4) . . ? N30 Ni8 N45 98.2(5) . . ? N29 Ni8 N45 88.0(5) . . ? N31 Ni8 N45 91.5(5) . . ? O12 Ni8 N32 90.3(7) . . ? N30 Ni8 N32 98.8(8) . . ? N29 Ni8 N32 105.5(8) . . ? N31 Ni8 N32 73.3(9) . . ? N45 Ni8 N32 160.6(8) . . ? O16 Ni9 O17 168.6(4) . 2_656 ? O16 Ni9 O22 102.4(4) . . ? O17 Ni9 O22 86.0(4) 2_656 . ? O16 Ni9 O14 95.3(4) . 2_656 ? O17 Ni9 O14 77.0(4) 2_656 2_656 ? O22 Ni9 O14 89.5(4) . 2_656 ? O16 Ni9 O14 79.1(4) . . ? O17 Ni9 O14 91.1(4) 2_656 . ? O22 Ni9 O14 167.5(4) . . ? O14 Ni9 O14 78.0(4) 2_656 . ? O16 Ni9 O15 87.5(6) . . ? O17 Ni9 O15 101.0(7) 2_656 . ? O22 Ni9 O15 84.5(6) . . ? O14 Ni9 O15 173.8(6) 2_656 . ? O14 Ni9 O15 108.0(6) . . ? O13 Ni10 O21 100.4(4) . . ? O13 Ni10 O14 167.6(4) . . ? O21 Ni10 O14 88.3(4) . . ? O13 Ni10 O12 92.2(4) . . ? O21 Ni10 O12 96.3(4) . . ? O14 Ni10 O12 95.6(4) . . ? O13 Ni10 O17 95.8(4) . . ? O21 Ni10 O17 79.8(4) . . ? O14 Ni10 O17 76.9(4) . . ? O12 Ni10 O17 171.6(4) . . ? O13 Ni10 O16 90.2(4) . . ? O21 Ni10 O16 164.7(4) . . ? O14 Ni10 O16 79.7(4) . . ? O12 Ni10 O16 94.3(4) . . ? O17 Ni10 O16 88.3(4) . . ? O13 Ni11 N34 88.2(5) . . ? O13 Ni11 O19 100.5(4) . . ? N34 Ni11 O19 171.2(5) . . ? O13 Ni11 N51 91.7(5) . . ? N34 Ni11 N51 89.7(5) . . ? O19 Ni11 N51 88.6(4) . . ? O13 Ni11 N33 166.3(4) . . ? N34 Ni11 N33 79.6(5) . . ? O19 Ni11 N33 91.9(4) . . ? N51 Ni11 N33 94.5(5) . . ? O13 Ni11 N54 79.2(5) . . ? N34 Ni11 N54 91.3(5) . . ? O19 Ni11 N54 91.8(5) . . ? N51 Ni11 N54 170.8(5) . . ? N33 Ni11 N54 94.7(5) . . ? O13 Ni12 N38 100.4(5) . . ? O13 Ni12 N36 91.1(5) . . ? N38 Ni12 N36 164.5(6) . . ? O13 Ni12 N37 99.6(4) . . ? N38 Ni12 N37 78.9(5) . . ? N36 Ni12 N37 89.0(5) . . ? O13 Ni12 N35 164.1(5) . . ? N38 Ni12 N35 93.8(6) . . ? N36 Ni12 N35 76.4(6) . . ? N37 Ni12 N35 90.1(5) . . ? O13 Ni12 N54 80.4(5) . . ? N38 Ni12 N54 92.8(6) . . ? N36 Ni12 N54 99.4(5) . . ? N37 Ni12 N54 171.6(5) . . ? N35 Ni12 N54 91.8(6) . . ? N42 Ni13 N40 178.1(6) . . ? N42 Ni13 N48 86.3(6) . . ? N40 Ni13 N48 95.4(5) . . ? N42 Ni13 N41 78.6(6) . . ? N40 Ni13 N41 99.7(5) . . ? N48 Ni13 N41 164.7(5) . . ? N42 Ni13 N39 100.9(5) . . ? N40 Ni13 N39 78.3(5) . . ? N48 Ni13 N39 89.8(5) . . ? N41 Ni13 N39 90.4(5) . . ? N42 Ni13 N51 92.4(5) . . ? N40 Ni13 N51 88.2(5) . . ? N48 Ni13 N51 94.4(5) . . ? N41 Ni13 N51 88.9(5) . . ? N39 Ni13 N51 166.2(5) . . ? N43 Ni14 N44 77.3(5) . . ? N43 Ni14 O12 167.9(4) . . ? N44 Ni14 O12 92.1(5) . . ? N43 Ni14 N45 92.9(4) . . ? N44 Ni14 N45 88.6(5) . . ? O12 Ni14 N45 80.9(4) . . ? N43 Ni14 O20 96.4(4) . . ? N44 Ni14 O20 173.7(4) . . ? O12 Ni14 O20 94.1(4) . . ? N45 Ni14 O20 91.2(4) . . ? N43 Ni14 N48 94.2(5) . . ? N44 Ni14 N48 93.7(5) . . ? O12 Ni14 N48 92.2(4) . . ? N45 Ni14 N48 172.8(5) . . ? O20 Ni14 N48 87.3(5) . . ? Ni8 O12 Ni14 102.5(4) . . ? Ni8 O12 Ni10 110.8(4) . . ? Ni14 O12 Ni10 110.0(5) . . ? Ni8 O12 H12B 111.1 . . ? Ni14 O12 H12B 111.1 . . ? Ni10 O12 H12B 111.1 . . ? Ni10 O13 Ni11 115.8(5) . . ? Ni10 O13 Ni12 113.4(5) . . ? Ni11 O13 Ni12 103.0(4) . . ? Ni10 O13 H13B 108.1 . . ? Ni11 O13 H13B 108.1 . . ? Ni12 O13 H13B 108.1 . . ? N30 O14 Ni10 112.6(8) . . ? N30 O14 Ni9 130.9(8) . 2_656 ? Ni10 O14 Ni9 101.7(5) . 2_656 ? N30 O14 Ni9 105.9(8) . . ? Ni10 O14 Ni9 98.9(4) . . ? Ni9 O14 Ni9 102.0(4) 2_656 . ? C49 N29 C53 113.5(14) . . ? C49 N29 Ni8 132.0(12) . . ? C53 N29 Ni8 113.9(12) . . ? C50 C49 N29 126.0(19) . . ? C50 C49 H49A 117.0 . . ? N29 C49 H49A 117.0 . . ? C49 C50 C51 120(2) . . ? C49 C50 H50A 119.8 . . ? C51 C50 H50A 119.8 . . ? C50 C51 C52 117(2) . . ? C50 C51 H51A 121.6 . . ? C52 C51 H51A 121.6 . . ? C53 C52 C51 120(2) . . ? C53 C52 H52A 120.2 . . ? C51 C52 H52A 120.2 . . ? N29 C53 C52 123.5(18) . . ? N29 C53 C54 114.0(14) . . ? C52 C53 C54 122.3(17) . . ? N30 C54 C53 116.9(16) . . ? N30 C54 H54A 121.5 . . ? C53 C54 H54A 121.5 . . ? C54 N30 O14 122.7(14) . . ? C54 N30 Ni8 119.4(13) . . ? O14 N30 Ni8 116.2(9) . . ? N32 O15 Ni9 123(2) . . ? C55 N31 C59 120.0 . . ? C55 N31 Ni8 119.2(9) . . ? C59 N31 Ni8 120.8(9) . . ? C56 C55 N31 120.0 . . ? C56 C55 H55A 120.0 . . ? N31 C55 H55A 120.0 . . ? C57 C56 C55 120.0 . . ? C57 C56 H56A 120.0 . . ? C55 C56 H56A 120.0 . . ? C56 C57 C58 120.0 . . ? C56 C57 H57A 120.0 . . ? C58 C57 H57A 120.0 . . ? C57 C58 C59 120.0 . . ? C57 C58 H58A 120.0 . . ? C59 C58 H58A 120.0 . . ? C58 C59 N31 120.0 . . ? C58 C59 C60 124.9(5) . . ? N31 C59 C60 114.9(5) . . ? C59 C60 N32 115.2(13) . . ? C59 C60 H60A 122.4 . . ? N32 C60 H60A 122.4 . . ? O15 N32 C60 112.5(16) . . ? O15 N32 Ni8 132(2) . . ? C60 N32 Ni8 114.8(14) . . ? N34 O16 Ni9 139.7(9) . . ? N34 O16 Ni10 115.5(8) . . ? Ni9 O16 Ni10 101.6(4) . . ? C61 N33 C65 122.4(14) . . ? C61 N33 Ni11 128.1(11) . . ? C65 N33 Ni11 109.4(11) . . ? N33 C61 C62 128.5(16) . . ? N33 C61 H61A 115.8 . . ? C62 C61 H61A 115.8 . . ? C61 C62 C63 113.1(17) . . ? C61 C62 H62A 123.4 . . ? C63 C62 H62A 123.4 . . ? C64 C63 C62 119.1(17) . . ? C64 C63 H63A 120.5 . . ? C62 C63 H63A 120.5 . . ? C63 C64 C65 121.5(16) . . ? C63 C64 H64A 119.2 . . ? C65 C64 H64A 119.2 . . ? N33 C65 C66 120.3(15) . . ? N33 C65 C64 115.3(15) . . ? C66 C65 C64 124.4(15) . . ? N34 C66 C65 117.9(15) . . ? N34 C66 H66A 121.0 . . ? C65 C66 H66A 121.0 . . ? O16 N34 C66 121.4(13) . . ? O16 N34 Ni11 125.9(9) . . ? C66 N34 Ni11 112.7(11) . . ? N36 O17 Ni9 143.6(10) . 2_656 ? N36 O17 Ni10 113.0(9) . . ? Ni9 O17 Ni10 103.4(5) 2_656 . ? C67 N35 C71 122.8(17) . . ? C67 N35 Ni12 126.0(13) . . ? C71 N35 Ni12 111.2(12) . . ? N35 C67 C68 122.4(17) . . ? N35 C67 H67A 118.8 . . ? C68 C67 H67A 118.8 . . ? C69 C68 C67 118.2(19) . . ? C69 C68 H68A 120.9 . . ? C67 C68 H68A 120.9 . . ? C68 C69 C70 119(2) . . ? C68 C69 H69A 120.4 . . ? C70 C69 H69A 120.4 . . ? C69 C70 C71 122.5(18) . . ? C69 C70 H70A 118.8 . . ? C71 C70 H70A 118.8 . . ? N35 C71 C72 118.9(17) . . ? N35 C71 C70 114.8(16) . . ? C72 C71 C70 126.3(17) . . ? N36 C72 C71 114.0(17) . . ? N36 C72 H72A 123.0 . . ? C71 C72 H72A 123.0 . . ? C72 N36 O17 115.5(14) . . ? C72 N36 Ni12 118.4(13) . . ? O17 N36 Ni12 125.2(10) . . ? C73 N37 C77 118.4(16) . . ? C73 N37 Ni12 132.3(12) . . ? C77 N37 Ni12 109.2(13) . . ? N37 C73 C74 129.2(17) . . ? N37 C73 H73A 115.4 . . ? C74 C73 H73A 115.4 . . ? C75 C74 C73 108.2(19) . . ? C75 C74 H74A 125.9 . . ? C73 C74 H74A 125.9 . . ? C74 C75 C76 124(2) . . ? C74 C75 H75A 117.8 . . ? C76 C75 H75A 117.8 . . ? C75 C76 C77 118.0(19) . . ? C75 C76 H76A 121.0 . . ? C77 C76 H76A 121.0 . . ? N37 C77 C78 123(2) . . ? N37 C77 C76 121.8(19) . . ? C78 C77 C76 114.9(19) . . ? C77 C78 N38 114.7(18) . . ? C77 C78 H78A 122.7 . . ? N38 C78 H78A 122.7 . . ? O18 N38 C78 118.4(14) . . ? O18 N38 Ni12 128.0(10) . . ? C78 N38 Ni12 113.6(12) . . ? N40 O19 Ni11 116.6(8) . . ? C83 N39 C79 124.3(15) . . ? C83 N39 Ni13 110.4(11) . . ? C79 N39 Ni13 125.3(12) . . ? N39 C79 C80 116.1(17) . . ? N39 C79 H79A 121.9 . . ? C80 C79 H79A 121.9 . . ? C79 C80 C81 120.7(19) . . ? C79 C80 H80A 119.6 . . ? C81 C80 H80A 119.6 . . ? C82 C81 C80 121(2) . . ? C82 C81 H81A 119.6 . . ? C80 C81 H81A 119.6 . . ? C81 C82 C83 114(2) . . ? C81 C82 H82A 122.8 . . ? C83 C82 H82A 122.8 . . ? N39 C83 C84 118.5(16) . . ? N39 C83 C82 123.1(17) . . ? C84 C83 C82 118.3(18) . . ? N40 C84 C83 115.1(16) . . ? N40 C84 H84A 122.4 . . ? C83 C84 H84A 122.4 . . ? C84 N40 O19 117.8(13) . . ? C84 N40 Ni13 117.2(11) . . ? O19 N40 Ni13 124.9(9) . . ? N42 O20 Ni14 114.6(9) . . ? C89 N41 C85 120.6(16) . . ? C89 N41 Ni13 112.8(11) . . ? C85 N41 Ni13 126.3(12) . . ? N41 C85 C86 122.1(17) . . ? N41 C85 H85A 118.9 . . ? C86 C85 H85A 118.9 . . ? C87 C86 C85 111.7(17) . . ? C87 C86 H86A 124.1 . . ? C85 C86 H86A 124.1 . . ? C86 C87 C88 128(2) . . ? C86 C87 H87A 116.2 . . ? C88 C87 H87A 116.2 . . ? C87 C88 C89 114.2(18) . . ? C87 C88 H88A 122.9 . . ? C89 C88 H88A 122.9 . . ? N41 C89 C88 123.6(16) . . ? N41 C89 C90 116.8(17) . . ? C88 C89 C90 119.5(18) . . ? N42 C90 C89 117.1(18) . . ? N42 C90 H90A 121.5 . . ? C89 C90 H90A 121.5 . . ? C90 N42 O20 115.8(15) . . ? C90 N42 Ni13 114.8(12) . . ? O20 N42 Ni13 129.3(11) . . ? N44 O21 Ni10 110.3(8) . . ? C95 N43 C91 115.2(14) . . ? C95 N43 Ni14 115.9(10) . . ? C91 N43 Ni14 128.9(12) . . ? N43 C91 C92 121.2(18) . . ? N43 C91 H91A 119.4 . . ? C92 C91 H91A 119.4 . . ? C93 C92 C91 121.4(18) . . ? C93 C92 H92A 119.3 . . ? C91 C92 H92A 119.3 . . ? C94 C93 C92 117(2) . . ? C94 C93 H93A 121.7 . . ? C92 C93 H93A 121.7 . . ? C93 C94 C95 117(2) . . ? C93 C94 H94A 121.5 . . ? C95 C94 H94A 121.5 . . ? N43 C95 C94 127.9(16) . . ? N43 C95 C96 115.3(15) . . ? C94 C95 C96 116.8(17) . . ? N44 C96 C95 111.8(17) . . ? N44 C96 H96A 124.1 . . ? C95 C96 H96A 124.1 . . ? C96 N44 O21 116.6(14) . . ? C96 N44 Ni14 118.9(12) . . ? O21 N44 Ni14 124.3(9) . . ? N46 N45 Ni14 139.3(12) . . ? N46 N45 Ni8 123.8(12) . . ? Ni14 N45 Ni8 96.3(5) . . ? N45 N46 N47 175(2) . . ? N49 N48 Ni13 119.1(10) . . ? N49 N48 Ni14 117.5(10) . . ? Ni13 N48 Ni14 114.7(7) . . ? N50 N49 N48 178.6(19) . . ? N52 N51 Ni11 120.6(10) . . ? N52 N51 Ni13 116.5(10) . . ? Ni11 N51 Ni13 110.4(6) . . ? N53 N52 N51 173.3(17) . . ? N55 N54 Ni12 136.5(14) . . ? N55 N54 Ni11 123.7(13) . . ? Ni12 N54 Ni11 93.9(6) . . ? N56 N55 N54 169(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.070 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.128 data_st82 _database_code_depnum_ccdc_archive 'CCDC 640088' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H144 N48 Na2 Ni12 O34' _chemical_formula_weight 3265.09 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' Na Na 0.0362 0.0249 '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 13.7676(12) _cell_length_b 16.2729(14) _cell_length_c 17.5222(14) _cell_angle_alpha 102.327(2) _cell_angle_beta 108.530(2) _cell_angle_gamma 107.775(2) _cell_volume 3328.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 62 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description orange _exptl_crystal_colour plates _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1686 _exptl_absorpt_coefficient_mu 1.752 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7752 _exptl_absorpt_correction_T_max 0.8659 _exptl_absorpt_process_details 'based on measured indexed crystal faces, Bruker SHELXTL v6.14 (Bruker 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 22866 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.1250 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14940 _reflns_number_gt 8180 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART v5.624 (Bruker 1998)' _computing_cell_refinement 'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL v6.14 (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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. The asymmetric unit consists of a half Ni12Na2 cluster and three ether molecules. The latter molecules were disordered and could not be modeled properly, thus program SQUEEZE, a part of the PLATON package of crystallographic software, was used to calculate the solvent disorder area and remove its contribution to the overall intensity data. ; _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^)+(0.0122P)^2^] 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 14940 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 0.761 _refine_ls_restrained_S_all 0.761 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.25604(3) 0.75251(2) 0.50791(2) 0.02689(10) Uani 1 1 d . . . Ni2 Ni 0.32204(3) 0.65807(2) 0.66875(2) 0.02622(10) Uani 1 1 d . . . Ni3 Ni 0.61487(3) 1.01517(3) 0.78296(2) 0.02900(11) Uani 1 1 d . . . Ni4 Ni 0.36091(3) 0.96456(2) 0.66964(2) 0.02712(10) Uani 1 1 d . . . Ni5 Ni 0.42100(3) 0.86736(2) 0.82345(2) 0.02408(10) Uani 1 1 d . . . Ni6 Ni 0.18807(3) 0.68524(2) 0.77977(2) 0.02686(10) Uani 1 1 d . . . Na Na 0.44004(10) 1.06647(8) 0.95664(7) 0.0360(3) Uani 1 1 d . . . O1 O 0.28486(17) 0.75637(13) 0.73018(13) 0.0246(5) Uani 1 1 d . . . H1' H 0.260(2) 0.7776(18) 0.6997(16) 0.019(9) Uiso 1 1 d . . . O2 O 0.46158(19) 0.91148(16) 0.73217(14) 0.0266(6) Uani 1 1 d . . . H2' H 0.456(3) 0.8739(17) 0.7078(17) 0.010(10) Uiso 1 1 d . . . O3 O 0.04894(19) 0.60947(16) 0.66518(14) 0.0344(6) Uani 1 1 d . . . H3' H 0.067(3) 0.593(2) 0.6217(19) 0.052 Uiso 1 1 d . . . H3" H 0.007(3) 0.628(2) 0.651(2) 0.052 Uiso 1 1 d . . . O4 O 0.13506(17) 0.79168(12) 0.80601(11) 0.0348(5) Uani 1 1 d . . . H4' H 0.1765 0.8349 0.8094 0.052 Uiso 1 1 d R . . H4" H 0.0538 0.7847 0.7896 0.052 Uiso 1 1 d R . . O5 O 0.63145(17) 1.01250(13) 0.66898(12) 0.0415(6) Uani 1 1 d . . . H5' H 0.5801 0.9921 0.6303 0.062 Uiso 1 1 d R . . H5" H 0.6832 0.9604 0.6397 0.062 Uiso 1 1 d R . . O6 O 0.68575(18) 0.91886(13) 0.79336(12) 0.0433(6) Uani 1 1 d . . . H6' H 0.6520 0.8821 0.8058 0.065 Uiso 1 1 d R . . H6" H 0.7654 0.9396 0.8228 0.065 Uiso 1 1 d R . . O7 O 0.16379(16) 0.59437(12) 0.56697(11) 0.0282(5) Uani 1 1 d . . . O8 O 0.41187(16) 0.95460(12) 0.56945(11) 0.0302(5) Uani 1 1 d . . . O9 O 0.52886(16) 0.79753(12) 0.82639(11) 0.0274(5) Uani 1 1 d . . . O10 O 0.54682(16) 0.97847(12) 0.92389(11) 0.0271(5) Uani 1 1 d . . . O11 O 0.31642(16) 0.94120(12) 0.82549(11) 0.0266(5) Uani 1 1 d . . . O12 O 0.39942(16) 0.82896(13) 0.92208(11) 0.0285(5) Uani 1 1 d . . . O13 O 0.3489(2) 1.15797(17) 1.00083(14) 0.0807(10) Uani 1 1 d . . . H13' H 0.3888 1.1946 1.0265 0.121 Uiso 1 1 d R . . H13" H 0.3098 1.1700 0.9566 0.121 Uiso 1 1 d R . . O14 O -0.1044(2) 0.68345(17) 0.61077(16) 0.0823(9) Uiso 1 1 d . . . H101 H -0.0783 0.7148 0.5776 0.123 Uiso 1 1 d R . . N1 N 0.1100(2) 0.73685(16) 0.41226(14) 0.0285(6) Uani 1 1 d . . . N2 N 0.1434(2) 0.63819(15) 0.51030(14) 0.0274(6) Uani 1 1 d . . . N3 N 0.2988(2) 0.69899(17) 0.41079(14) 0.0318(7) Uani 1 1 d . . . N4 N 0.3702(2) 0.86919(15) 0.51129(14) 0.0277(6) Uani 1 1 d . . . N5 N 0.3799(2) 0.56199(16) 0.63051(15) 0.0328(7) Uani 1 1 d . . . N6 N 0.4818(2) 0.71507(16) 0.76278(14) 0.0291(6) Uani 1 1 d . . . N7 N 0.7661(2) 1.12816(16) 0.85528(15) 0.0335(7) Uani 1 1 d . . . N8 N 0.6239(2) 1.03076(15) 0.90344(14) 0.0257(6) Uani 1 1 d . . . N9 N 0.2623(2) 1.03281(16) 0.62907(15) 0.0334(7) Uani 1 1 d . . . N10 N 0.2959(2) 0.97488(15) 0.76069(14) 0.0278(6) Uani 1 1 d . . . N11 N 0.1260(2) 0.60797(16) 0.84697(15) 0.0336(7) Uani 1 1 d . . . N12 N 0.3139(2) 0.75035(16) 0.89921(14) 0.0279(6) Uani 1 1 d . . . N13 N 0.3829(2) 0.73573(16) 0.59890(14) 0.0266(6) Uani 1 1 d . . . N14 N 0.4606(3) 0.73113(17) 0.58333(15) 0.0336(7) Uani 1 1 d . . . N15 N 0.5358(3) 0.7267(2) 0.56947(18) 0.0510(8) Uani 1 1 d . . . N16 N 0.2248(2) 0.83621(15) 0.59821(14) 0.0279(6) Uani 1 1 d . . . N17 N 0.1304(3) 0.82936(17) 0.58216(14) 0.0319(7) Uani 1 1 d . . . N18 N 0.0410(2) 0.82406(19) 0.56769(17) 0.0482(8) Uani 1 1 d . . . N19 N 0.2541(2) 0.58851(16) 0.74064(15) 0.0315(7) Uani 1 1 d . . . N20 N 0.3043(2) 0.55958(18) 0.79015(17) 0.0426(8) Uani 1 1 d . . . N21 N 0.3515(3) 0.5302(2) 0.8360(2) 0.0755(11) Uani 1 1 d . . . N22 N 0.5103(2) 1.08775(16) 0.74890(16) 0.0338(7) Uani 1 1 d . . . N23 N 0.5020(3) 1.1409(2) 0.80162(19) 0.0558(10) Uani 1 1 d . . . N24 N 0.4915(3) 1.1902(3) 0.8525(2) 0.125(2) Uani 1 1 d . . . C1 C 0.0968(3) 0.7871(2) 0.36072(18) 0.0359(8) Uani 1 1 d . . . H1A H 0.1598 0.8394 0.3701 0.043 Uiso 1 1 calc R . . C2 C -0.0046(3) 0.7654(2) 0.29470(19) 0.0417(9) Uani 1 1 d . . . H2A H -0.0116 0.8022 0.2595 0.050 Uiso 1 1 calc R . . C3 C -0.0948(3) 0.6897(2) 0.2814(2) 0.0532(11) Uani 1 1 d . . . H3A H -0.1650 0.6725 0.2357 0.064 Uiso 1 1 calc R . . C4 C -0.0840(3) 0.6383(2) 0.3341(2) 0.0476(10) Uani 1 1 d . . . H4A H -0.1467 0.5867 0.3263 0.057 Uiso 1 1 calc R . . C5 C 0.0210(3) 0.6635(2) 0.39931(18) 0.0309(8) Uani 1 1 d . . . C6 C 0.0411(3) 0.61232(19) 0.45792(18) 0.0308(8) Uani 1 1 d . . . H6A H -0.0181 0.5628 0.4572 0.037 Uiso 1 1 calc R . . C7 C 0.2546(3) 0.6114(2) 0.35706(19) 0.0361(8) Uani 1 1 d . . . H7A H 0.2048 0.5647 0.3675 0.043 Uiso 1 1 calc R . . C8 C 0.2796(3) 0.5874(2) 0.2874(2) 0.0436(10) Uani 1 1 d . . . H8A H 0.2458 0.5255 0.2495 0.052 Uiso 1 1 calc R . . C9 C 0.3537(3) 0.6541(2) 0.2740(2) 0.0535(11) Uani 1 1 d . . . H9A H 0.3723 0.6390 0.2266 0.064 Uiso 1 1 calc R . . C10 C 0.4016(3) 0.7439(2) 0.3296(2) 0.0470(10) Uani 1 1 d . . . H10A H 0.4542 0.7909 0.3214 0.056 Uiso 1 1 calc R . . C11 C 0.3718(3) 0.7641(2) 0.39718(19) 0.0335(8) Uani 1 1 d . . . C12 C 0.4159(3) 0.8579(2) 0.45742(18) 0.0308(8) Uani 1 1 d . . . H12A H 0.4741 0.9074 0.4571 0.037 Uiso 1 1 calc R . . C13 C 0.3262(3) 0.4853(2) 0.5600(2) 0.0456(10) Uani 1 1 d . . . H13A H 0.2510 0.4701 0.5230 0.055 Uiso 1 1 calc R . . C14 C 0.3777(3) 0.4290(3) 0.5407(2) 0.0736(14) Uani 1 1 d . . . H14A H 0.3381 0.3748 0.4913 0.088 Uiso 1 1 calc R . . C15 C 0.4861(4) 0.4510(3) 0.5925(3) 0.0964(18) Uani 1 1 d . . . H15A H 0.5229 0.4131 0.5785 0.116 Uiso 1 1 calc R . . C16 C 0.5427(3) 0.5286(3) 0.6655(2) 0.0732(14) Uani 1 1 d . . . H16A H 0.6178 0.5440 0.7029 0.088 Uiso 1 1 calc R . . C17 C 0.4875(3) 0.5831(2) 0.6829(2) 0.0438(10) Uani 1 1 d . . . C18 C 0.5412(3) 0.6690(2) 0.75516(19) 0.0395(9) Uani 1 1 d . . . H18A H 0.6167 0.6900 0.7948 0.047 Uiso 1 1 calc R . . C19 C 0.8352(3) 1.1798(2) 0.8285(2) 0.0426(9) Uani 1 1 d . . . H19A H 0.8140 1.1671 0.7687 0.051 Uiso 1 1 calc R . . C20 C 0.9364(3) 1.2508(2) 0.8852(2) 0.0496(10) Uani 1 1 d . . . H20A H 0.9840 1.2859 0.8643 0.059 Uiso 1 1 calc R . . C21 C 0.9680(3) 1.2706(2) 0.9721(2) 0.0509(10) Uani 1 1 d . . . H21A H 1.0373 1.3192 1.0117 0.061 Uiso 1 1 calc R . . C22 C 0.8969(3) 1.2183(2) 1.0005(2) 0.0439(9) Uani 1 1 d . . . H22A H 0.9166 1.2305 1.0601 0.053 Uiso 1 1 calc R . . C23 C 0.7966(3) 1.1478(2) 0.9409(2) 0.0331(8) Uani 1 1 d . . . C24 C 0.7156(3) 1.0924(2) 0.96522(19) 0.0312(8) Uani 1 1 d . . . H24A H 0.7292 1.1010 1.0236 0.037 Uiso 1 1 calc R . . C25 C 0.2450(3) 1.0592(2) 0.5608(2) 0.0457(10) Uani 1 1 d . . . H25A H 0.2863 1.0507 0.5277 0.055 Uiso 1 1 calc R . . C26 C 0.1700(4) 1.0982(3) 0.5361(2) 0.0643(13) Uani 1 1 d . . . H26A H 0.1593 1.1162 0.4870 0.077 Uiso 1 1 calc R . . C27 C 0.1108(4) 1.1104(3) 0.5846(2) 0.0803(15) Uani 1 1 d . . . H27A H 0.0589 1.1377 0.5692 0.096 Uiso 1 1 calc R . . C28 C 0.1267(3) 1.0829(3) 0.6562(2) 0.0663(13) Uani 1 1 d . . . H28A H 0.0857 1.0904 0.6898 0.080 Uiso 1 1 calc R . . C29 C 0.2035(3) 1.0448(2) 0.6768(2) 0.0414(9) Uani 1 1 d . . . C30 C 0.2250(3) 1.0123(2) 0.74900(18) 0.0366(9) Uani 1 1 d . . . H30A H 0.1882 1.0185 0.7861 0.044 Uiso 1 1 calc R . . C31 C 0.0311(3) 0.5340(2) 0.8178(2) 0.0458(10) Uani 1 1 d . . . H31A H -0.0234 0.5178 0.7616 0.055 Uiso 1 1 calc R . . C32 C 0.0087(3) 0.4799(2) 0.8661(2) 0.0644(12) Uani 1 1 d . . . H32A H -0.0612 0.4291 0.8445 0.077 Uiso 1 1 calc R . . C33 C 0.0892(3) 0.5009(3) 0.9459(2) 0.0672(13) Uani 1 1 d . . . H33A H 0.0772 0.4629 0.9793 0.081 Uiso 1 1 calc R . . C34 C 0.1860(3) 0.5761(2) 0.9766(2) 0.0523(10) Uani 1 1 d . . . H34A H 0.2416 0.5921 1.0324 0.063 Uiso 1 1 calc R . . C35 C 0.2041(3) 0.6298(2) 0.92692(19) 0.0384(9) Uani 1 1 d . . . C36 C 0.3041(3) 0.7118(2) 0.95435(19) 0.0359(8) Uani 1 1 d . . . H36A H 0.3605 0.7360 1.0111 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0273(3) 0.0271(2) 0.0216(2) 0.00509(17) 0.00846(18) 0.00900(19) Ni2 0.0255(2) 0.0257(2) 0.0233(2) 0.00455(17) 0.00683(18) 0.01095(19) Ni3 0.0280(3) 0.0298(2) 0.0234(2) 0.00425(18) 0.01108(18) 0.00713(19) Ni4 0.0318(3) 0.0264(2) 0.0211(2) 0.00597(17) 0.00993(18) 0.01175(19) Ni5 0.0242(2) 0.0246(2) 0.0192(2) 0.00425(17) 0.00738(17) 0.00831(18) Ni6 0.0243(2) 0.0286(2) 0.0228(2) 0.00794(18) 0.00678(18) 0.00811(19) Na 0.0340(8) 0.0421(8) 0.0231(7) 0.0037(6) 0.0086(6) 0.0128(6) O1 0.0284(13) 0.0234(12) 0.0230(12) 0.0087(10) 0.0094(10) 0.0123(10) O2 0.0329(14) 0.0205(14) 0.0231(13) 0.0029(11) 0.0118(11) 0.0093(12) O3 0.0286(15) 0.0408(15) 0.0245(13) 0.0050(11) 0.0064(11) 0.0113(11) O4 0.0267(13) 0.0325(12) 0.0435(13) 0.0105(10) 0.0159(10) 0.0101(10) O5 0.0383(15) 0.0453(14) 0.0319(13) 0.0097(11) 0.0135(11) 0.0087(12) O6 0.0374(15) 0.0464(14) 0.0514(15) 0.0178(11) 0.0238(12) 0.0170(12) O7 0.0315(13) 0.0289(12) 0.0196(11) 0.0066(9) 0.0077(10) 0.0104(10) O8 0.0369(14) 0.0264(12) 0.0197(11) 0.0037(9) 0.0111(10) 0.0064(10) O9 0.0258(13) 0.0242(11) 0.0226(11) -0.0016(9) 0.0046(9) 0.0097(10) O10 0.0251(13) 0.0292(12) 0.0253(12) 0.0083(9) 0.0126(10) 0.0072(10) O11 0.0303(13) 0.0307(12) 0.0207(11) 0.0105(9) 0.0100(9) 0.0140(10) O12 0.0288(13) 0.0277(12) 0.0205(11) 0.0062(9) 0.0073(9) 0.0050(10) O13 0.101(2) 0.109(2) 0.0384(15) 0.0131(15) 0.0089(15) 0.079(2) N1 0.0340(17) 0.0293(15) 0.0229(14) 0.0071(12) 0.0111(12) 0.0155(13) N2 0.0325(17) 0.0241(14) 0.0219(14) 0.0043(11) 0.0092(12) 0.0112(12) N3 0.0329(17) 0.0312(16) 0.0208(14) -0.0005(12) 0.0058(12) 0.0116(13) N4 0.0321(17) 0.0245(15) 0.0196(14) 0.0051(12) 0.0053(12) 0.0102(12) N5 0.0346(18) 0.0275(15) 0.0314(15) 0.0029(12) 0.0100(13) 0.0151(13) N6 0.0279(16) 0.0309(15) 0.0242(14) 0.0072(12) 0.0059(12) 0.0129(13) N7 0.0306(17) 0.0338(16) 0.0280(16) 0.0042(13) 0.0121(13) 0.0071(13) N8 0.0232(16) 0.0231(14) 0.0262(14) 0.0044(12) 0.0104(12) 0.0059(12) N9 0.0457(19) 0.0316(16) 0.0246(15) 0.0116(12) 0.0118(13) 0.0193(14) N10 0.0328(17) 0.0308(15) 0.0154(13) 0.0049(11) 0.0086(12) 0.0106(13) N11 0.0262(17) 0.0340(16) 0.0307(16) 0.0107(13) 0.0083(13) 0.0035(13) N12 0.0287(16) 0.0286(15) 0.0216(14) 0.0076(12) 0.0074(12) 0.0091(13) N13 0.0274(16) 0.0328(15) 0.0232(14) 0.0073(11) 0.0123(12) 0.0162(13) N14 0.038(2) 0.0309(16) 0.0238(15) 0.0024(12) 0.0094(14) 0.0124(15) N15 0.044(2) 0.065(2) 0.049(2) 0.0113(16) 0.0252(17) 0.0282(18) N16 0.0267(17) 0.0295(15) 0.0252(14) 0.0057(11) 0.0079(12) 0.0138(13) N17 0.039(2) 0.0353(17) 0.0193(14) 0.0057(12) 0.0089(14) 0.0176(15) N18 0.0324(19) 0.065(2) 0.0477(19) 0.0160(15) 0.0129(15) 0.0269(17) N19 0.0327(17) 0.0299(15) 0.0305(15) 0.0127(12) 0.0084(13) 0.0140(13) N20 0.045(2) 0.0385(18) 0.0423(19) 0.0139(15) 0.0151(15) 0.0170(15) N21 0.082(3) 0.087(3) 0.076(2) 0.053(2) 0.020(2) 0.055(2) N22 0.0422(19) 0.0268(15) 0.0283(16) 0.0066(12) 0.0146(14) 0.0105(14) N23 0.051(2) 0.051(2) 0.037(2) -0.0052(16) -0.0100(16) 0.0286(18) N24 0.100(4) 0.126(3) 0.074(3) -0.062(2) -0.025(2) 0.080(3) C1 0.045(2) 0.039(2) 0.0293(19) 0.0106(16) 0.0205(17) 0.0202(18) C2 0.052(3) 0.049(2) 0.0278(19) 0.0130(17) 0.0101(18) 0.031(2) C3 0.050(3) 0.051(2) 0.042(2) 0.0122(19) -0.0009(19) 0.022(2) C4 0.036(2) 0.040(2) 0.044(2) 0.0107(18) -0.0012(17) 0.0063(18) C5 0.031(2) 0.0301(19) 0.0267(18) 0.0050(15) 0.0086(15) 0.0120(16) C6 0.025(2) 0.0245(17) 0.0310(19) 0.0027(14) 0.0064(15) 0.0048(15) C7 0.034(2) 0.033(2) 0.0273(19) 0.0037(16) 0.0022(16) 0.0110(16) C8 0.052(3) 0.043(2) 0.0245(19) -0.0009(17) 0.0058(18) 0.023(2) C9 0.082(3) 0.054(3) 0.034(2) 0.009(2) 0.034(2) 0.033(2) C10 0.066(3) 0.049(2) 0.040(2) 0.0165(19) 0.036(2) 0.026(2) C11 0.040(2) 0.033(2) 0.0285(19) 0.0109(16) 0.0138(16) 0.0163(17) C12 0.036(2) 0.0313(19) 0.0253(18) 0.0111(15) 0.0143(16) 0.0104(16) C13 0.035(2) 0.037(2) 0.044(2) -0.0061(17) 0.0012(17) 0.0186(18) C14 0.056(3) 0.066(3) 0.059(3) -0.024(2) -0.007(2) 0.037(2) C15 0.072(4) 0.089(3) 0.082(3) -0.035(3) -0.014(3) 0.066(3) C16 0.051(3) 0.081(3) 0.051(2) -0.027(2) -0.013(2) 0.050(2) C17 0.042(2) 0.043(2) 0.034(2) -0.0007(17) 0.0033(17) 0.0235(19) C18 0.032(2) 0.042(2) 0.034(2) -0.0001(16) 0.0030(16) 0.0201(18) C19 0.043(2) 0.042(2) 0.035(2) 0.0061(17) 0.0212(18) 0.0060(19) C20 0.048(3) 0.046(2) 0.043(2) 0.0087(18) 0.0283(19) -0.0016(19) C21 0.037(2) 0.046(2) 0.050(2) 0.0072(19) 0.0150(19) -0.0001(19) C22 0.037(2) 0.041(2) 0.035(2) 0.0026(17) 0.0121(17) 0.0024(18) C23 0.030(2) 0.0333(19) 0.0299(19) 0.0063(15) 0.0107(16) 0.0103(16) C24 0.030(2) 0.038(2) 0.0214(17) 0.0056(15) 0.0118(15) 0.0098(16) C25 0.062(3) 0.052(2) 0.032(2) 0.0143(17) 0.0203(19) 0.032(2) C26 0.102(4) 0.096(3) 0.038(2) 0.042(2) 0.035(2) 0.078(3) C27 0.129(4) 0.124(4) 0.058(3) 0.058(3) 0.052(3) 0.109(4) C28 0.100(4) 0.110(3) 0.043(2) 0.045(2) 0.041(2) 0.087(3) C29 0.058(3) 0.047(2) 0.0288(19) 0.0144(17) 0.0148(18) 0.035(2) C30 0.050(2) 0.048(2) 0.0274(18) 0.0133(16) 0.0215(17) 0.0341(19) C31 0.033(2) 0.049(2) 0.045(2) 0.0190(19) 0.0113(17) 0.0052(18) C32 0.044(3) 0.060(3) 0.068(3) 0.034(2) 0.016(2) -0.007(2) C33 0.061(3) 0.074(3) 0.057(3) 0.045(2) 0.018(2) 0.007(2) C34 0.048(3) 0.057(3) 0.042(2) 0.028(2) 0.0131(19) 0.008(2) C35 0.039(2) 0.044(2) 0.029(2) 0.0174(17) 0.0115(17) 0.0135(18) C36 0.037(2) 0.037(2) 0.0229(18) 0.0125(15) 0.0041(15) 0.0087(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N4 2.037(2) . ? Ni1 N2 2.045(2) . ? Ni1 N1 2.069(2) . ? Ni1 N3 2.078(2) . ? Ni1 N13 2.091(2) . ? Ni1 N16 2.101(2) . ? Ni2 O1 2.024(2) . ? Ni2 N5 2.045(2) . ? Ni2 N6 2.053(2) . ? Ni2 O7 2.0890(18) . ? Ni2 N19 2.110(3) . ? Ni2 N13 2.112(2) . ? Ni3 O2 2.021(2) . ? Ni3 N8 2.030(2) . ? Ni3 O5 2.074(2) . ? Ni3 N7 2.077(2) . ? Ni3 O6 2.094(2) . ? Ni3 N22 2.149(3) . ? Ni4 O2 2.009(2) . ? Ni4 N9 2.055(2) . ? Ni4 N10 2.064(2) . ? Ni4 O8 2.0810(19) . ? Ni4 N16 2.108(2) . ? Ni4 N22 2.158(3) . ? Ni5 O12 2.0346(19) . ? Ni5 O10 2.0392(18) . ? Ni5 O1 2.043(2) . ? Ni5 O2 2.049(2) . ? Ni5 O9 2.1226(19) . ? Ni5 O11 2.1422(19) . ? Ni5 Na 3.4464(12) . ? Ni5 Na 3.4572(11) 2_677 ? Ni6 O1 2.023(2) . ? Ni6 N12 2.033(2) . ? Ni6 O3 2.068(2) . ? Ni6 N11 2.077(3) . ? Ni6 O4 2.0950(19) . ? Ni6 N19 2.141(2) . ? Na O10 2.333(2) 2_677 ? Na O12 2.339(2) 2_677 ? Na O13 2.378(3) . ? Na O11 2.394(2) . ? Na O10 2.452(2) . ? Na Na 3.421(2) 2_677 ? Na Ni5 3.4571(11) 2_677 ? Na H13' 2.5885 . ? O1 H1' 0.75(2) . ? O2 H2' 0.63(2) . ? O3 H3' 0.89(3) . ? O3 H3" 0.72(3) . ? O4 H4' 0.7344 . ? O4 H4" 1.0255 . ? O5 H5' 0.7249 . ? O5 H5" 1.3811 . ? O6 H6' 0.7556 . ? O6 H6" 0.9604 . ? O7 N2 1.349(3) . ? O8 N4 1.355(3) . ? O9 N6 1.354(3) . ? O10 N8 1.342(3) . ? O10 Na 2.333(2) 2_677 ? O11 N10 1.351(3) . ? O12 N12 1.321(3) . ? O12 Na 2.339(2) 2_677 ? O13 H13' 0.6223 . ? O13 H13" 0.8899 . ? O14 H101 0.9352 . ? N1 C5 1.338(4) . ? N1 C1 1.348(3) . ? N2 C6 1.286(3) . ? N3 C11 1.342(4) . ? N3 C7 1.350(3) . ? N4 C12 1.301(4) . ? N5 C13 1.352(3) . ? N5 C17 1.359(4) . ? N6 C18 1.283(3) . ? N7 C19 1.339(4) . ? N7 C23 1.357(3) . ? N8 C24 1.291(3) . ? N9 C25 1.331(4) . ? N9 C29 1.360(4) . ? N10 C30 1.286(3) . ? N11 C31 1.330(4) . ? N11 C35 1.357(4) . ? N12 C36 1.279(3) . ? N13 N14 1.205(3) . ? N14 N15 1.154(4) . ? N16 N17 1.203(3) . ? N17 N18 1.146(3) . ? N19 N20 1.201(3) . ? N20 N21 1.148(3) . ? N22 N23 1.184(3) . ? N23 N24 1.143(4) . ? C1 C2 1.383(4) . ? C1 H1A 0.9500 . ? C2 C3 1.369(4) . ? C2 H2A 0.9500 . ? C3 C4 1.376(4) . ? C3 H3A 0.9500 . ? C4 C5 1.397(4) . ? C4 H4A 0.9500 . ? C5 C6 1.467(4) . ? C6 H6A 0.9500 . ? C7 C8 1.380(4) . ? C7 H7A 0.9500 . ? C8 C9 1.364(5) . ? C8 H8A 0.9500 . ? C9 C10 1.384(4) . ? C9 H9A 0.9500 . ? C10 C11 1.379(4) . ? C10 H10A 0.9500 . ? C11 C12 1.467(4) . ? C12 H12A 0.9500 . ? C13 C14 1.370(4) . ? C13 H13A 0.9500 . ? C14 C15 1.361(5) . ? C14 H14A 0.9500 . ? C15 C16 1.384(4) . ? C15 H15A 0.9500 . ? C16 C17 1.377(4) . ? C16 H16A 0.9500 . ? C17 C18 1.457(4) . ? C18 H18A 0.9500 . ? C19 C20 1.383(4) . ? C19 H19A 0.9500 . ? C20 C21 1.376(4) . ? C20 H20A 0.9500 . ? C21 C22 1.383(4) . ? C21 H21A 0.9500 . ? C22 C23 1.384(4) . ? C22 H22A 0.9500 . ? C23 C24 1.445(4) . ? C24 H24A 0.9500 . ? C25 C26 1.375(4) . ? C25 H25A 0.9500 . ? C26 C27 1.374(5) . ? C26 H26A 0.9500 . ? C27 C28 1.396(4) . ? C27 H27A 0.9500 . ? C28 C29 1.374(4) . ? C28 H28A 0.9500 . ? C29 C30 1.453(4) . ? C30 H30A 0.9500 . ? C31 C32 1.380(4) . ? C31 H31A 0.9500 . ? C32 C33 1.371(5) . ? C32 H32A 0.9500 . ? C33 C34 1.354(4) . ? C33 H33A 0.9500 . ? C34 C35 1.384(4) . ? C34 H34A 0.9500 . ? C35 C36 1.445(4) . ? C36 H36A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ni1 N2 177.40(9) . . ? N4 Ni1 N1 102.32(10) . . ? N2 Ni1 N1 79.13(10) . . ? N4 Ni1 N3 79.28(10) . . ? N2 Ni1 N3 103.01(10) . . ? N1 Ni1 N3 87.02(9) . . ? N4 Ni1 N13 90.43(9) . . ? N2 Ni1 N13 88.31(10) . . ? N1 Ni1 N13 166.55(10) . . ? N3 Ni1 N13 91.20(9) . . ? N4 Ni1 N16 87.88(10) . . ? N2 Ni1 N16 89.97(9) . . ? N1 Ni1 N16 89.68(9) . . ? N3 Ni1 N16 165.72(10) . . ? N13 Ni1 N16 95.15(9) . . ? O1 Ni2 N5 168.68(9) . . ? O1 Ni2 N6 90.81(9) . . ? N5 Ni2 N6 79.61(10) . . ? O1 Ni2 O7 93.50(8) . . ? N5 Ni2 O7 96.23(9) . . ? N6 Ni2 O7 175.50(9) . . ? O1 Ni2 N19 81.14(9) . . ? N5 Ni2 N19 93.31(10) . . ? N6 Ni2 N19 93.29(10) . . ? O7 Ni2 N19 88.63(9) . . ? O1 Ni2 N13 93.95(9) . . ? N5 Ni2 N13 91.80(10) . . ? N6 Ni2 N13 88.31(10) . . ? O7 Ni2 N13 90.12(8) . . ? N19 Ni2 N13 174.84(10) . . ? O2 Ni3 N8 91.15(10) . . ? O2 Ni3 O5 97.46(8) . . ? N8 Ni3 O5 171.22(9) . . ? O2 Ni3 N7 169.23(10) . . ? N8 Ni3 N7 78.71(10) . . ? O5 Ni3 N7 92.80(9) . . ? O2 Ni3 O6 88.89(9) . . ? N8 Ni3 O6 88.28(8) . . ? O5 Ni3 O6 90.15(8) . . ? N7 Ni3 O6 94.36(9) . . ? O2 Ni3 N22 79.40(10) . . ? N8 Ni3 N22 97.68(10) . . ? O5 Ni3 N22 85.65(9) . . ? N7 Ni3 N22 98.20(10) . . ? O6 Ni3 N22 166.93(9) . . ? O2 Ni4 N9 168.85(10) . . ? O2 Ni4 N10 91.12(10) . . ? N9 Ni4 N10 79.49(10) . . ? O2 Ni4 O8 94.31(9) . . ? N9 Ni4 O8 95.32(9) . . ? N10 Ni4 O8 174.18(9) . . ? O2 Ni4 N16 94.24(9) . . ? N9 Ni4 N16 91.33(10) . . ? N10 Ni4 N16 87.29(9) . . ? O8 Ni4 N16 90.22(8) . . ? O2 Ni4 N22 79.45(10) . . ? N9 Ni4 N22 94.91(10) . . ? N10 Ni4 N22 92.92(10) . . ? O8 Ni4 N22 90.14(9) . . ? N16 Ni4 N22 173.69(9) . . ? O12 Ni5 O10 80.65(8) . . ? O12 Ni5 O1 94.65(8) . . ? O10 Ni5 O1 173.89(8) . . ? O12 Ni5 O2 173.60(9) . . ? O10 Ni5 O2 94.41(9) . . ? O1 Ni5 O2 90.54(9) . . ? O12 Ni5 O9 87.97(7) . . ? O10 Ni5 O9 90.82(7) . . ? O1 Ni5 O9 92.93(8) . . ? O2 Ni5 O9 88.03(8) . . ? O12 Ni5 O11 90.94(8) . . ? O10 Ni5 O11 87.10(7) . . ? O1 Ni5 O11 89.08(8) . . ? O2 Ni5 O11 92.89(8) . . ? O9 Ni5 O11 177.79(7) . . ? O12 Ni5 Na 77.93(6) . . ? O10 Ni5 Na 44.51(6) . . ? O1 Ni5 Na 130.83(6) . . ? O2 Ni5 Na 101.45(7) . . ? O9 Ni5 Na 134.48(5) . . ? O11 Ni5 Na 43.35(5) . . ? O12 Ni5 Na 40.98(6) . 2_677 ? O10 Ni5 Na 40.84(6) . 2_677 ? O1 Ni5 Na 135.16(6) . 2_677 ? O2 Ni5 Na 133.30(7) . 2_677 ? O9 Ni5 Na 81.66(5) . 2_677 ? O11 Ni5 Na 96.26(5) . 2_677 ? Na Ni5 Na 59.41(3) . 2_677 ? O1 Ni6 N12 90.78(9) . . ? O1 Ni6 O3 96.42(9) . . ? N12 Ni6 O3 172.79(10) . . ? O1 Ni6 N11 165.18(9) . . ? N12 Ni6 N11 78.95(10) . . ? O3 Ni6 N11 93.89(10) . . ? O1 Ni6 O4 90.03(8) . . ? N12 Ni6 O4 87.20(8) . . ? O3 Ni6 O4 93.24(8) . . ? N11 Ni6 O4 100.00(9) . . ? O1 Ni6 N19 80.38(9) . . ? N12 Ni6 N19 94.72(9) . . ? O3 Ni6 N19 86.05(9) . . ? N11 Ni6 N19 89.76(10) . . ? O4 Ni6 N19 170.24(9) . . ? O10 Na O12 68.70(7) 2_677 2_677 ? O10 Na O13 88.06(8) 2_677 . ? O12 Na O13 85.88(8) 2_677 . ? O10 Na O11 111.85(8) 2_677 . ? O12 Na O11 162.23(9) 2_677 . ? O13 Na O11 111.83(9) . . ? O10 Na O10 88.75(8) 2_677 . ? O12 Na O10 89.36(8) 2_677 . ? O13 Na O10 174.99(9) . . ? O11 Na O10 72.98(7) . . ? O10 Na Na 45.77(5) 2_677 2_677 ? O12 Na Na 75.18(6) 2_677 2_677 ? O13 Na Na 133.70(8) . 2_677 ? O11 Na Na 92.53(6) . 2_677 ? O10 Na Na 42.98(5) . 2_677 ? O10 Na Ni5 97.51(6) 2_677 . ? O12 Na Ni5 124.76(7) 2_677 . ? O13 Na Ni5 148.83(8) . . ? O11 Na Ni5 37.90(5) . . ? O10 Na Ni5 35.66(5) . . ? Na Na Ni5 60.45(3) 2_677 . ? O10 Na Ni5 34.86(5) 2_677 2_677 ? O12 Na Ni5 34.78(5) 2_677 2_677 ? O13 Na Ni5 80.25(6) . 2_677 ? O11 Na Ni5 146.12(6) . 2_677 ? O10 Na Ni5 94.94(5) . 2_677 ? Na Na Ni5 60.14(3) 2_677 2_677 ? Ni5 Na Ni5 120.59(3) . 2_677 ? O10 Na H13' 87.2 2_677 . ? O12 Na H13' 73.0 2_677 . ? O13 Na H13' 13.6 . . ? O11 Na H13' 124.6 . . ? O10 Na H13' 162.1 . . ? Na Na H13' 130.4 2_677 . ? Ni5 Na H13' 162.2 . . ? Ni5 Na H13' 72.1 2_677 . ? Ni6 O1 Ni2 101.30(9) . . ? Ni6 O1 Ni5 111.69(9) . . ? Ni2 O1 Ni5 114.40(10) . . ? Ni6 O1 H1' 118(2) . . ? Ni2 O1 H1' 110(2) . . ? Ni5 O1 H1' 102(2) . . ? Ni4 O2 Ni3 103.21(10) . . ? Ni4 O2 Ni5 114.51(11) . . ? Ni3 O2 Ni5 112.30(10) . . ? Ni4 O2 H2' 112(3) . . ? Ni3 O2 H2' 116(3) . . ? Ni5 O2 H2' 99(3) . . ? Ni6 O3 H3' 112(2) . . ? Ni6 O3 H3" 120(3) . . ? H3' O3 H3" 107(3) . . ? Ni6 O4 H4' 109.9 . . ? Ni6 O4 H4" 126.2 . . ? H4' O4 H4" 118.3 . . ? Ni3 O5 H5' 116.5 . . ? Ni3 O5 H5" 119.6 . . ? H5' O5 H5" 96.2 . . ? Ni3 O6 H6' 109.8 . . ? Ni3 O6 H6" 119.6 . . ? H6' O6 H6" 114.5 . . ? N2 O7 Ni2 115.97(15) . . ? N4 O8 Ni4 115.93(16) . . ? N6 O9 Ni5 114.03(15) . . ? N8 O10 Ni5 114.46(15) . . ? N8 O10 Na 132.44(16) . 2_677 ? Ni5 O10 Na 104.30(8) . 2_677 ? N8 O10 Na 107.43(15) . . ? Ni5 O10 Na 99.83(8) . . ? Na O10 Na 91.25(8) 2_677 . ? N10 O11 Ni5 113.21(16) . . ? N10 O11 Na 108.69(14) . . ? Ni5 O11 Na 98.75(8) . . ? N12 O12 Ni5 115.18(15) . . ? N12 O12 Na 139.61(15) . 2_677 ? Ni5 O12 Na 104.24(9) . 2_677 ? Na O13 H13' 102.8 . . ? Na O13 H13" 110.0 . . ? H13' O13 H13" 107.9 . . ? C5 N1 C1 118.6(3) . . ? C5 N1 Ni1 113.0(2) . . ? C1 N1 Ni1 128.2(2) . . ? C6 N2 O7 117.5(3) . . ? C6 N2 Ni1 115.6(2) . . ? O7 N2 Ni1 126.48(17) . . ? C11 N3 C7 118.6(3) . . ? C11 N3 Ni1 112.8(2) . . ? C7 N3 Ni1 128.2(2) . . ? C12 N4 O8 117.1(3) . . ? C12 N4 Ni1 115.8(2) . . ? O8 N4 Ni1 126.71(19) . . ? C13 N5 C17 118.7(3) . . ? C13 N5 Ni2 128.1(2) . . ? C17 N5 Ni2 113.12(19) . . ? C18 N6 O9 119.5(2) . . ? C18 N6 Ni2 114.9(2) . . ? O9 N6 Ni2 125.38(17) . . ? C19 N7 C23 118.4(3) . . ? C19 N7 Ni3 128.9(2) . . ? C23 N7 Ni3 112.7(2) . . ? C24 N8 O10 118.0(2) . . ? C24 N8 Ni3 116.3(2) . . ? O10 N8 Ni3 125.59(17) . . ? C25 N9 C29 118.8(3) . . ? C25 N9 Ni4 128.1(2) . . ? C29 N9 Ni4 112.9(2) . . ? C30 N10 O11 119.6(3) . . ? C30 N10 Ni4 114.5(2) . . ? O11 N10 Ni4 125.70(18) . . ? C31 N11 C35 118.3(3) . . ? C31 N11 Ni6 128.7(2) . . ? C35 N11 Ni6 112.0(2) . . ? C36 N12 O12 120.2(2) . . ? C36 N12 Ni6 115.5(2) . . ? O12 N12 Ni6 124.22(17) . . ? N14 N13 Ni1 118.5(2) . . ? N14 N13 Ni2 120.3(2) . . ? Ni1 N13 Ni2 112.40(12) . . ? N15 N14 N13 179.1(3) . . ? N17 N16 Ni1 118.94(19) . . ? N17 N16 Ni4 120.5(2) . . ? Ni1 N16 Ni4 112.20(12) . . ? N18 N17 N16 179.0(4) . . ? N20 N19 Ni2 123.6(2) . . ? N20 N19 Ni6 121.9(2) . . ? Ni2 N19 Ni6 94.79(9) . . ? N21 N20 N19 178.5(4) . . ? N23 N22 Ni3 121.7(2) . . ? N23 N22 Ni4 115.6(2) . . ? Ni3 N22 Ni4 94.35(10) . . ? N24 N23 N22 178.0(5) . . ? N1 C1 C2 122.6(3) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 118.3(3) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C2 C3 C4 120.2(3) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C3 C4 C5 118.6(3) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 120.7 . . ? N1 C5 C4 121.6(3) . . ? N1 C5 C6 115.7(3) . . ? C4 C5 C6 122.6(3) . . ? N2 C6 C5 116.3(3) . . ? N2 C6 H6A 121.9 . . ? C5 C6 H6A 121.9 . . ? N3 C7 C8 122.1(3) . . ? N3 C7 H7A 118.9 . . ? C8 C7 H7A 118.9 . . ? C9 C8 C7 118.8(3) . . ? C9 C8 H8A 120.6 . . ? C7 C8 H8A 120.6 . . ? C8 C9 C10 119.8(3) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? C11 C10 C9 118.9(3) . . ? C11 C10 H10A 120.6 . . ? C9 C10 H10A 120.6 . . ? N3 C11 C10 121.8(3) . . ? N3 C11 C12 115.9(3) . . ? C10 C11 C12 122.3(3) . . ? N4 C12 C11 115.9(3) . . ? N4 C12 H12A 122.0 . . ? C11 C12 H12A 122.0 . . ? N5 C13 C14 121.6(3) . . ? N5 C13 H13A 119.2 . . ? C14 C13 H13A 119.2 . . ? C15 C14 C13 119.6(3) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C14 C15 C16 120.0(4) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C17 C16 C15 118.5(3) . . ? C17 C16 H16A 120.8 . . ? C15 C16 H16A 120.8 . . ? N5 C17 C16 121.6(3) . . ? N5 C17 C18 115.4(3) . . ? C16 C17 C18 122.9(3) . . ? N6 C18 C17 117.0(3) . . ? N6 C18 H18A 121.5 . . ? C17 C18 H18A 121.5 . . ? N7 C19 C20 122.0(3) . . ? N7 C19 H19A 119.0 . . ? C20 C19 H19A 119.0 . . ? C21 C20 C19 119.8(3) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C20 C21 C22 118.7(3) . . ? C20 C21 H21A 120.6 . . ? C22 C21 H21A 120.6 . . ? C21 C22 C23 119.2(3) . . ? C21 C22 H22A 120.4 . . ? C23 C22 H22A 120.4 . . ? N7 C23 C22 121.9(3) . . ? N7 C23 C24 115.4(3) . . ? C22 C23 C24 122.6(3) . . ? N8 C24 C23 116.5(3) . . ? N8 C24 H24A 121.7 . . ? C23 C24 H24A 121.7 . . ? N9 C25 C26 122.9(3) . . ? N9 C25 H25A 118.5 . . ? C26 C25 H25A 118.5 . . ? C27 C26 C25 118.1(3) . . ? C27 C26 H26A 120.9 . . ? C25 C26 H26A 120.9 . . ? C26 C27 C28 120.2(4) . . ? C26 C27 H27A 119.9 . . ? C28 C27 H27A 119.9 . . ? C29 C28 C27 118.1(4) . . ? C29 C28 H28A 121.0 . . ? C27 C28 H28A 121.0 . . ? N9 C29 C28 121.8(3) . . ? N9 C29 C30 115.7(3) . . ? C28 C29 C30 122.5(3) . . ? N10 C30 C29 117.3(3) . . ? N10 C30 H30A 121.3 . . ? C29 C30 H30A 121.3 . . ? N11 C31 C32 122.6(3) . . ? N11 C31 H31A 118.7 . . ? C32 C31 H31A 118.7 . . ? C33 C32 C31 118.8(4) . . ? C33 C32 H32A 120.6 . . ? C31 C32 H32A 120.6 . . ? C34 C33 C32 119.3(3) . . ? C34 C33 H33A 120.4 . . ? C32 C33 H33A 120.4 . . ? C33 C34 C35 120.1(3) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? N11 C35 C34 120.9(3) . . ? N11 C35 C36 115.0(3) . . ? C34 C35 C36 124.1(3) . . ? N12 C36 C35 117.4(3) . . ? N12 C36 H36A 121.3 . . ? C35 C36 H36A 121.3 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.789 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.068