Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Escuer, A.' 'Font-Bardia, Merce' 'Papaefstathiou, Giannis S.' 'Perlepes, Spyros P.' 'Solans, Xavier' 'Vicente, Ramon' _publ_contact_author_name 'Prof Spyros P Perlepes' _publ_contact_author_address ; Prof Spyros P Perlepes Department of Chemistry University of Patras 265 00 Patras GREECE ; _publ_contact_author_email 'PERLEPES@PATREAS.UPATRAS.GR' _publ_section_title ; Reactivity in polynuclear transition metal chemistry as a means to obtain high-spin molecules:substitution of u4-OH- by n-1, u4-N3- increases nine times the ground-state S value of a nonanuclear nickel (II) cage ; data_complex_2 _database_code_CSD 169286 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C60 H56 N14 NI9 O24 4 (C3 H7 N O) 4.5(H2O)' _chemical_formula_sum 'C72 H93 N18 Ni9 O32.50' _chemical_formula_weight 2258.75 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 'Tetragonal' _symmetry_space_group_name_H-M 'P4/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x, z' '-x+1/2, -y+1/2, z' 'y, -x+1/2, z' '-x, -y, -z' 'y-1/2, -x, -z' 'x-1/2, y-1/2, -z' '-y, x-1/2, -z' _cell_length_a 17.841(8) _cell_length_b 17.841(8) _cell_length_c 14.008(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4459(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23354 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 28.89 _exptl_crystal_description 'prism' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 1.948 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.83 _exptl_absorpt_process_details ; phi-scan, North, Phillips and Mathews, 1968, Acta Cryst, A24, 351-359 ; _diffrn_ambient_temperature 293(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 'mar2400 - image plate detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24451 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 28.89 _reflns_number_total 5241 _reflns_number_gt 3417 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MARXDS' _computing_cell_refinement 'MARXDS' _computing_data_reduction 'MARSCALE' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material 'CIFTAB' _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 w=1/[\s^2^(Fo^2^)+(0.0785P)^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_extinction_expression 'Fc' _refine_ls_number_reflns 5241 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1119 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.215 _refine_ls_shift/su_mean 0.006 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.7500 0.7500 0.39309(5) 0.03751(17) Uani 1 d S . . Ni2 Ni 0.868607(18) 0.720393(19) 0.22307(3) 0.04108(12) Uani 1 d . . . Ni3 Ni 0.754705(19) 0.627417(19) 0.56316(3) 0.04174(13) Uani 1 d . . . O1 O 0.80737(9) 0.65780(10) 0.31463(14) 0.0436(4) Uani 1 d . . . O2 O 0.82850(10) 0.67348(10) 0.47169(14) 0.0450(5) Uani 1 d . . . O3 O 0.88159(12) 0.64143(12) 0.11864(16) 0.0569(6) Uani 1 d . . . O4 O 0.93557(12) 0.78634(12) 0.14379(17) 0.0580(5) Uani 1 d . . . O5 O 0.83195(12) 0.59568(12) 0.66419(17) 0.0583(6) Uani 1 d . . . O6 O 0.67996(11) 0.57728(12) 0.64758(17) 0.0569(5) Uani 1 d . . . N1 N 0.95344(12) 0.67066(12) 0.29815(18) 0.0437(5) Uani 1 d . . . N3 N 0.7500 0.7500 0.1699(3) 0.0330(9) Uani 1 d S . . N2 N 0.77996(12) 0.53384(11) 0.48580(18) 0.0430(5) Uani 1 d . . . N4 N 0.7500 0.7500 0.0858(9) 0.094(3) Uani 1 d S . . N5 N 0.7500 0.7500 -0.0020(8) 0.145(4) Uani 1 d S . . N6 N 0.7500 0.7500 0.6160(3) 0.0390(10) Uani 1 d S . . N7 N 0.7500 0.7500 0.7039(9) 0.096(3) Uani 1 d S . . N8 N 0.7500 0.7500 0.7940(7) 0.136(4) Uani 1 d S . . C1 C 0.84746(14) 0.62833(14) 0.39300(18) 0.0365(6) Uani 1 d . . . C2 C 0.93199(14) 0.63099(13) 0.3735(2) 0.0405(6) Uani 1 d . . . C3 C 0.98139(16) 0.59017(16) 0.4285(2) 0.0501(7) Uani 1 d . . . C4 C 1.05565(19) 0.5878(2) 0.4002(3) 0.0605(9) Uani 1 d . . . C5 C 1.07860(18) 0.62632(19) 0.3211(3) 0.0609(9) Uani 1 d . . . C6 C 1.02621(17) 0.66776(18) 0.2720(3) 0.0552(8) Uani 1 d . . . C7 C 0.82437(14) 0.54645(14) 0.4112(2) 0.0410(6) Uani 1 d . . . C8 C 0.84953(17) 0.48868(16) 0.3526(3) 0.0501(7) Uani 1 d . . . C9 C 0.82847(18) 0.41693(16) 0.3749(3) 0.0594(9) Uani 1 d . . . H9 H 0.8449 0.3773 0.3372 0.071 Uiso 1 calc R . . C10 C 0.78368(19) 0.40318(18) 0.4516(3) 0.0638(9) Uani 1 d . . . C11 C 0.76026(17) 0.46253(16) 0.5065(3) 0.0517(8) Uani 1 d . . . C12 C 0.84957(17) 0.57998(18) 0.1126(2) 0.0529(7) Uani 1 d . . . C13 C 0.8923(3) 0.5173(2) 0.0604(4) 0.0926(14) Uani 1 d . . . H13 H 0.9438 0.5176 0.0803 0.111 Uiso 1 calc R . . H13A H 0.8896 0.5256 -0.0073 0.111 Uiso 1 calc R . . H13B H 0.8702 0.4697 0.0756 0.111 Uiso 1 calc R . . C14 C 0.89646(18) 0.62112(17) 0.6808(2) 0.0510(7) Uani 1 d . . . C15 C 0.9458(2) 0.57603(19) 0.7457(3) 0.0722(11) Uani 1 d . . . H15 H 0.9927 0.6015 0.7541 0.087 Uiso 1 calc R . . H15A H 0.9545 0.5276 0.7180 0.087 Uiso 1 calc R . . H15B H 0.9217 0.5702 0.8065 0.087 Uiso 1 calc R . . N9 N 0.7298(2) 0.4934(3) 0.8878(3) 0.1052(13) Uani 1 d . . . O7 O 0.7370(3) 0.3884(3) 0.7882(5) 0.179(2) Uani 1 d . . . C16 C 0.7406(4) 0.5773(3) 0.8952(4) 0.133(2) Uani 1 d . . . H16 H 0.7467 0.5910 0.9610 0.160 Uiso 1 calc R . . H16A H 0.6976 0.6024 0.8693 0.160 Uiso 1 calc R . . H16B H 0.7845 0.5916 0.8601 0.160 Uiso 1 calc R . . C17 C 0.6947(4) 0.4578(5) 0.9719(5) 0.172(3) Uani 1 d . . . H17 H 0.6857 0.4950 1.0201 0.206 Uiso 1 calc R . . H17A H 0.7275 0.4199 0.9968 0.206 Uiso 1 calc R . . H17B H 0.6479 0.4353 0.9535 0.206 Uiso 1 calc R . . C18 C 0.7504(3) 0.4609(3) 0.8043(5) 0.1151(19) Uani 1 d . . . H18 H 0.7742 0.4895 0.7578 0.138 Uiso 1 calc R . . O1W O 0.7500 0.2500 0.3225(6) 0.170(3) Uani 1 d S . . O2W O 0.7500 0.2500 0.944(2) 0.170 Uiso 0.25 d SP . . O2W' O 0.6679(7) 0.2784(6) 0.8882(7) 0.170 Uiso 0.50 d P . . H3 H 0.9638(19) 0.5577(18) 0.498(2) 0.065(9) Uiso 1 d . . . H4 H 1.093(3) 0.567(3) 0.421(3) 0.098(15) Uiso 1 d . . . H5 H 1.1171(18) 0.6311(17) 0.302(2) 0.044(9) Uiso 1 d . . . H6 H 1.0297(17) 0.6990(19) 0.219(2) 0.052(9) Uiso 1 d . . . H8 H 0.8810(16) 0.5007(16) 0.306(2) 0.040(8) Uiso 1 d . . . H10 H 0.7736(14) 0.3502(16) 0.457(2) 0.037(7) Uiso 1 d . . . H11 H 0.7306(17) 0.4564(16) 0.557(2) 0.042(8) Uiso 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 0.0370(2) 0.0370(2) 0.0385(4) 0.000 0.000 0.000 Ni2 0.0425(2) 0.03980(19) 0.0410(3) -0.00046(14) 0.00459(14) 0.00064(13) Ni3 0.0398(2) 0.0435(2) 0.0419(3) 0.00535(14) 0.00055(14) 0.00024(14) O1 0.0385(9) 0.0462(10) 0.0459(12) 0.0100(8) -0.0042(8) -0.0020(8) O2 0.0442(10) 0.0436(10) 0.0473(13) -0.0045(8) 0.0045(8) -0.0063(8) O3 0.0585(12) 0.0582(13) 0.0540(15) -0.0112(10) 0.0147(10) -0.0017(10) O4 0.0557(12) 0.0548(12) 0.0633(15) 0.0058(10) 0.0191(10) 0.0004(10) O5 0.0560(12) 0.0636(13) 0.0552(15) 0.0189(11) -0.0132(10) 0.0020(10) O6 0.0497(12) 0.0584(12) 0.0627(15) 0.0148(10) 0.0079(10) 0.0024(10) N1 0.0356(11) 0.0431(12) 0.0524(16) -0.0055(10) 0.0056(10) 0.0028(9) N3 0.0423(15) 0.0423(15) 0.014(2) 0.000 0.000 0.000 N2 0.0380(11) 0.0362(11) 0.0547(16) 0.0081(10) -0.0042(10) -0.0002(9) N4 0.057(3) 0.057(3) 0.169(11) 0.000 0.000 0.000 N5 0.173(7) 0.173(7) 0.088(8) 0.000 0.000 0.000 N6 0.0513(17) 0.0513(17) 0.014(2) 0.000 0.000 0.000 N7 0.059(3) 0.059(3) 0.172(11) 0.000 0.000 0.000 N8 0.172(7) 0.172(7) 0.064(6) 0.000 0.000 0.000 C1 0.0367(12) 0.0417(13) 0.0312(16) -0.0002(10) 0.0006(10) 0.0040(10) C2 0.0350(13) 0.0326(12) 0.0540(19) -0.0049(11) 0.0014(11) -0.0048(10) C3 0.0441(15) 0.0416(14) 0.065(2) -0.0002(13) -0.0095(13) -0.0017(12) C4 0.0401(16) 0.0554(18) 0.086(3) -0.0027(17) -0.0141(16) 0.0077(15) C5 0.0337(15) 0.0527(18) 0.096(3) -0.0097(18) 0.0078(16) -0.0008(14) C6 0.0424(15) 0.0476(16) 0.075(3) -0.0032(16) 0.0134(15) -0.0043(13) C7 0.0358(13) 0.0376(13) 0.0494(19) 0.0019(11) -0.0042(11) -0.0005(11) C8 0.0476(15) 0.0428(15) 0.060(2) -0.0062(13) -0.0018(14) -0.0011(12) C9 0.0548(17) 0.0387(15) 0.085(3) -0.0109(15) -0.0153(17) 0.0058(14) C10 0.0539(18) 0.0408(17) 0.097(3) 0.0123(16) -0.0170(18) -0.0051(14) C11 0.0446(15) 0.0434(15) 0.067(2) 0.0127(14) -0.0039(15) -0.0026(12) C12 0.0544(17) 0.0539(17) 0.050(2) -0.0108(14) 0.0058(14) 0.0014(14) C13 0.090(3) 0.075(3) 0.113(4) -0.038(2) 0.028(3) 0.004(2) C14 0.0596(18) 0.0529(16) 0.0406(19) -0.0010(13) -0.0110(14) 0.0100(14) C15 0.082(2) 0.0501(18) 0.084(3) 0.0062(17) -0.035(2) 0.0088(17) N9 0.082(2) 0.124(3) 0.110(4) 0.004(3) -0.001(2) -0.002(2) O7 0.155(5) 0.132(4) 0.251(6) -0.040(4) 0.001(4) 0.016(3) C16 0.140(5) 0.107(4) 0.153(6) -0.014(4) -0.060(4) 0.002(4) C17 0.140(6) 0.280(10) 0.095(5) 0.020(6) 0.006(4) -0.063(6) C18 0.128(5) 0.119(4) 0.099(4) -0.007(3) 0.013(3) 0.040(4) O1W 0.204(7) 0.109(4) 0.196(8) 0.000 0.000 -0.021(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 2.227(2) 4_565 ? Ni1 O1 2.227(2) 2_655 ? Ni1 O1 2.227(2) 3_665 ? Ni1 O1 2.227(2) . ? Ni1 O2 2.244(2) 2_655 ? Ni1 O2 2.244(2) . ? Ni1 O2 2.244(2) 4_565 ? Ni1 O2 2.244(2) 3_665 ? Ni2 O4 2.011(2) . ? Ni2 O1 2.0213(19) . ? Ni2 O3 2.044(2) . ? Ni2 N1 2.046(2) . ? Ni2 O1 2.0676(19) 2_655 ? Ni2 N3 2.3048(18) . ? Ni3 O6 1.994(2) . ? Ni3 O2 2.0127(19) . ? Ni3 N2 2.041(2) . ? Ni3 O5 2.055(2) . ? Ni3 O2 2.0882(19) 4_565 ? Ni3 N6 2.3103(18) . ? O1 C1 1.412(3) . ? O1 Ni2 2.0676(19) 4_565 ? O2 C1 1.406(3) . ? O2 Ni3 2.0882(19) 2_655 ? O3 C12 1.239(4) . ? O4 C12 1.241(4) 2_655 ? O5 C14 1.259(4) . ? O6 C14 1.240(4) 4_565 ? N1 C2 1.327(4) . ? N1 C6 1.350(4) . ? N3 N4 1.178(12) . ? N3 Ni2 2.3048(18) 2_655 ? N3 Ni2 2.3048(18) 4_565 ? N3 Ni2 2.3048(18) 3_665 ? N2 C7 1.330(4) . ? N2 C11 1.351(4) . ? N4 N5 1.230(13) . ? N6 N7 1.231(12) . ? N6 Ni3 2.3103(18) 2_655 ? N6 Ni3 2.3103(18) 4_565 ? N6 Ni3 2.3103(18) 3_665 ? N7 N8 1.262(13) . ? C1 C2 1.533(4) . ? C1 C7 1.539(4) . ? C2 C3 1.379(4) . ? C3 C4 1.383(5) . ? C3 H3 1.17(3) . ? C4 C5 1.367(5) . ? C4 H4 0.81(5) . ? C5 C6 1.376(5) . ? C5 H5 0.74(3) . ? C6 H6 0.92(3) . ? C7 C8 1.392(4) . ? C8 C9 1.370(5) . ? C8 H8 0.89(3) . ? C9 C10 1.362(5) . ? C9 H9 0.9300 . ? C10 C11 1.373(5) . ? C10 H10 0.97(3) . ? C11 H11 0.89(3) . ? C12 O4 1.241(4) 4_565 ? C12 C13 1.538(5) . ? C13 H13 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C14 O6 1.240(4) 2_655 ? C14 C15 1.499(4) . ? C15 H15 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? N9 C18 1.356(7) . ? N9 C17 1.478(7) . ? N9 C16 1.513(7) . ? O7 C18 1.335(7) . ? C16 H16 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C17 H17 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C18 H18 0.9300 . ? O2W O2W 1.56(6) 6_667 ? O2W O2W' 1.739(18) 3_655 ? O2W O2W' 1.739(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O1 120.87(10) 4_565 2_655 ? O1 Ni1 O1 75.91(5) 4_565 3_665 ? O1 Ni1 O1 75.91(5) 2_655 3_665 ? O1 Ni1 O1 75.91(5) 4_565 . ? O1 Ni1 O1 75.91(4) 2_655 . ? O1 Ni1 O1 120.87(10) 3_665 . ? O1 Ni1 O2 167.96(6) 4_565 2_655 ? O1 Ni1 O2 60.40(7) 2_655 2_655 ? O1 Ni1 O2 93.48(7) 3_665 2_655 ? O1 Ni1 O2 115.05(6) . 2_655 ? O1 Ni1 O2 115.05(6) 4_565 . ? O1 Ni1 O2 93.48(7) 2_655 . ? O1 Ni1 O2 167.96(6) 3_665 . ? O1 Ni1 O2 60.40(7) . . ? O2 Ni1 O2 76.08(5) 2_655 . ? O1 Ni1 O2 60.40(7) 4_565 4_565 ? O1 Ni1 O2 167.96(6) 2_655 4_565 ? O1 Ni1 O2 115.05(6) 3_665 4_565 ? O1 Ni1 O2 93.48(7) . 4_565 ? O2 Ni1 O2 121.25(10) 2_655 4_565 ? O2 Ni1 O2 76.08(5) . 4_565 ? O1 Ni1 O2 93.48(7) 4_565 3_665 ? O1 Ni1 O2 115.05(6) 2_655 3_665 ? O1 Ni1 O2 60.40(7) 3_665 3_665 ? O1 Ni1 O2 167.96(6) . 3_665 ? O2 Ni1 O2 76.08(5) 2_655 3_665 ? O2 Ni1 O2 121.25(10) . 3_665 ? O2 Ni1 O2 76.08(5) 4_565 3_665 ? O4 Ni2 O1 174.07(9) . . ? O4 Ni2 O3 86.60(9) . . ? O1 Ni2 O3 97.74(9) . . ? O4 Ni2 N1 95.63(9) . . ? O1 Ni2 N1 80.44(8) . . ? O3 Ni2 N1 89.15(9) . . ? O4 Ni2 O1 92.22(9) . 2_655 ? O1 Ni2 O1 84.14(11) . 2_655 ? O3 Ni2 O1 170.76(8) . 2_655 ? N1 Ni2 O1 100.09(8) . 2_655 ? O4 Ni2 N3 103.46(10) . . ? O1 Ni2 N3 80.53(9) . . ? O3 Ni2 N3 91.76(11) . . ? N1 Ni2 N3 160.90(10) . . ? O1 Ni2 N3 79.59(9) 2_655 . ? O6 Ni3 O2 176.49(9) . . ? O6 Ni3 N2 95.48(9) . . ? O2 Ni3 N2 81.46(8) . . ? O6 Ni3 O5 85.21(9) . . ? O2 Ni3 O5 96.45(9) . . ? N2 Ni3 O5 89.56(9) . . ? O6 Ni3 O2 93.94(9) . 4_565 ? O2 Ni3 O2 84.81(11) . 4_565 ? N2 Ni3 O2 97.78(8) . 4_565 ? O5 Ni3 O2 172.66(9) . 4_565 ? O6 Ni3 N6 102.15(10) . . ? O2 Ni3 N6 80.86(10) . . ? N2 Ni3 N6 162.27(11) . . ? O5 Ni3 N6 93.71(11) . . ? O2 Ni3 N6 79.33(10) 4_565 . ? C1 O1 Ni2 115.18(14) . . ? C1 O1 Ni2 141.05(16) . 4_565 ? Ni2 O1 Ni2 97.93(9) . 4_565 ? C1 O1 Ni1 97.13(14) . . ? Ni2 O1 Ni1 98.83(8) . . ? Ni2 O1 Ni1 97.44(7) 4_565 . ? C1 O2 Ni3 114.98(15) . . ? C1 O2 Ni3 141.98(16) . 2_655 ? Ni3 O2 Ni3 97.99(9) . 2_655 ? C1 O2 Ni1 96.55(14) . . ? Ni3 O2 Ni1 98.77(8) . . ? Ni3 O2 Ni1 96.54(8) 2_655 . ? C12 O3 Ni2 127.3(2) . . ? C12 O4 Ni2 126.39(19) 2_655 . ? C14 O5 Ni3 129.9(2) . . ? C14 O6 Ni3 128.3(2) 4_565 . ? C2 N1 C6 118.2(3) . . ? C2 N1 Ni2 115.27(17) . . ? C6 N1 Ni2 126.1(2) . . ? N4 N3 Ni2 108.86(11) . 2_655 ? N4 N3 Ni2 108.86(11) . . ? Ni2 N3 Ni2 84.00(7) 2_655 . ? N4 N3 Ni2 108.86(11) . 4_565 ? Ni2 N3 Ni2 142.3(2) 2_655 4_565 ? Ni2 N3 Ni2 84.00(7) . 4_565 ? N4 N3 Ni2 108.86(11) . 3_665 ? Ni2 N3 Ni2 84.00(7) 2_655 3_665 ? Ni2 N3 Ni2 142.3(2) . 3_665 ? Ni2 N3 Ni2 84.00(7) 4_565 3_665 ? C7 N2 C11 118.9(3) . . ? C7 N2 Ni3 114.21(17) . . ? C11 N2 Ni3 126.8(2) . . ? N3 N4 N5 180.000(4) . . ? N7 N6 Ni3 108.68(11) . 2_655 ? N7 N6 Ni3 108.68(11) . . ? Ni3 N6 Ni3 84.11(7) 2_655 . ? N7 N6 Ni3 108.68(11) . 4_565 ? Ni3 N6 Ni3 142.6(2) 2_655 4_565 ? Ni3 N6 Ni3 84.11(7) . 4_565 ? N7 N6 Ni3 108.68(11) . 3_665 ? Ni3 N6 Ni3 84.11(7) 2_655 3_665 ? Ni3 N6 Ni3 142.6(2) . 3_665 ? Ni3 N6 Ni3 84.11(7) 4_565 3_665 ? N6 N7 N8 180.000(6) . . ? O2 C1 O1 105.9(2) . . ? O2 C1 C2 111.0(2) . . ? O1 C1 C2 110.4(2) . . ? O2 C1 C7 110.4(2) . . ? O1 C1 C7 110.3(2) . . ? C2 C1 C7 108.8(2) . . ? N1 C2 C3 122.8(2) . . ? N1 C2 C1 116.2(2) . . ? C3 C2 C1 120.8(3) . . ? C4 C3 C2 117.9(3) . . ? C4 C3 H3 118.6(16) . . ? C2 C3 H3 123.5(16) . . ? C5 C4 C3 120.3(3) . . ? C5 C4 H4 106(3) . . ? C3 C4 H4 134(3) . . ? C4 C5 C6 118.1(3) . . ? C4 C5 H5 129(3) . . ? C6 C5 H5 113(3) . . ? N1 C6 C5 122.6(3) . . ? N1 C6 H6 104.9(19) . . ? C5 C6 H6 132.5(19) . . ? N2 C7 C8 122.0(3) . . ? N2 C7 C1 116.8(2) . . ? C8 C7 C1 121.2(3) . . ? C9 C8 C7 118.0(3) . . ? C9 C8 H8 124.6(19) . . ? C7 C8 H8 117.3(19) . . ? C8 C9 C10 120.6(3) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C11 118.8(3) . . ? C9 C10 H10 110.6(17) . . ? C11 C10 H10 130.6(17) . . ? N2 C11 C10 121.8(3) . . ? N2 C11 H11 116.2(19) . . ? C10 C11 H11 122.0(19) . . ? O3 C12 O4 126.4(3) . 4_565 ? O3 C12 C13 116.5(3) . . ? O4 C12 C13 117.1(3) 4_565 . ? C12 C13 H13 109.5 . . ? C12 C13 H13A 109.5 . . ? H13 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O6 C14 O5 125.5(3) 2_655 . ? O6 C14 C15 117.4(3) 2_655 . ? O5 C14 C15 117.1(3) . . ? C14 C15 H15 109.5 . . ? C14 C15 H15A 109.5 . . ? H15 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C18 N9 C17 128.2(6) . . ? C18 N9 C16 116.6(5) . . ? C17 N9 C16 115.2(5) . . ? N9 C16 H16 109.5 . . ? N9 C16 H16A 109.5 . . ? H16 C16 H16A 109.5 . . ? N9 C16 H16B 109.5 . . ? H16 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N9 C17 H17 109.5 . . ? N9 C17 H17A 109.5 . . ? H17 C17 H17A 109.5 . . ? N9 C17 H17B 109.5 . . ? H17 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O7 C18 N9 120.7(6) . . ? O7 C18 H18 119.6 . . ? N9 C18 H18 119.6 . . ? O2W O2W O2W' 117.0(10) 6_667 3_655 ? O2W O2W O2W' 117.0(9) 6_667 . ? O2W' O2W O2W' 126.1(19) 3_655 . ? _diffrn_measured_fraction_theta_max 0.819 _diffrn_reflns_theta_full 28.89 _diffrn_measured_fraction_theta_full 0.819 _refine_diff_density_max 0.458 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.074 #===END data_complex_1 _database_code_CSD 169287 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C60 H58 N8 Ni9 O26 19(H2O)' _chemical_formula_sum 'C60 H96 N8 Ni9 O45' _chemical_formula_weight 2177.67 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 'tetragonal' _symmetry_space_group_name_H-M 'P4/ncc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x, z' '-x+1/2, -y+1/2, z' 'y, -x+1/2, z' 'y, x, z+1/2' '-x+1/2, y, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'x, -y+1/2, z+1/2' '-x, -y, -z' 'y-1/2, -x, -z' 'x-1/2, y-1/2, -z' '-y, x-1/2, -z' '-y, -x, -z-1/2' 'x-1/2, -y, -z-1/2' 'y-1/2, x-1/2, -z-1/2' '-x, y-1/2, -z-1/2' _cell_length_a 17.785(8) _cell_length_b 17.785(8) _cell_length_c 27.313(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8639(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30426 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 28.85 _exptl_crystal_description 'prism' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4424 _exptl_absorpt_coefficient_mu 2.014 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details ; phi-scan, North, Phillips and Mathews, 1968, Acta Cryst, A24, 351-359 ; _diffrn_ambient_temperature 293(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 'mar2400 - image plate detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37752 _diffrn_reflns_av_R_equivalents 0.0822 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.85 _diffrn_measured_fraction_theta_max 0.718 _diffrn_reflns_theta_full 28.85 _diffrn_measured_fraction_theta_full 0.718 _reflns_number_total 7038 _reflns_number_gt 4166 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MARXDS' _computing_cell_refinement 'MARXDS' _computing_data_reduction 'MARSCALE' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material 'CIFTAB' _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 w=1/[\s^2^(Fo^2^)+(0.1201P)^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_extinction_expression 'Fc' _refine_ls_number_reflns 7038 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1146 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1821 _refine_ls_wR_factor_gt 0.1703 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.873 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.118 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.2500 0.2500 0.44772(5) 0.0498(4) Uani 1 d S . . Ni2 Ni 0.28387(4) 0.13373(4) 0.35977(3) 0.0533(3) Uani 1 d . . . Ni3 Ni 0.37085(4) 0.24511(4) 0.53577(3) 0.0536(3) Uani 1 d . . . N1 N 0.3347(2) 0.0491(2) 0.39788(17) 0.0561(11) Uani 1 d . . . N2 N 0.4655(2) 0.2209(2) 0.49637(16) 0.0536(11) Uani 1 d . . . O1 O 0.3273(2) 0.1713(2) 0.48761(12) 0.0563(9) Uani 1 d . . . O2 O 0.34578(19) 0.19521(19) 0.40910(13) 0.0577(9) Uani 1 d . . . O3 O 0.2229(2) 0.0651(2) 0.31772(16) 0.0735(12) Uani 1 d . . . O4 O 0.3669(2) 0.1207(2) 0.30618(13) 0.0669(11) Uani 1 d . . . O21 O 0.2500 0.2500 0.3345(2) 0.0416(15) Uani 1 d S . . O5 O 0.4040(2) 0.1675(2) 0.58716(13) 0.0677(11) Uani 1 d . . . O6 O 0.4223(2) 0.3190(2) 0.57854(14) 0.0720(11) Uani 1 d . . . O31 O 0.2500 0.2500 0.5625(3) 0.0543(17) Uani 1 d S . . C1 C 0.3724(3) 0.1547(3) 0.4490(2) 0.0530(14) Uani 1 d . . . C2 C 0.3728(3) 0.0701(3) 0.4362(2) 0.0561(14) Uani 1 d . . . C3 C 0.4096(3) 0.0203(3) 0.4661(2) 0.0685(16) Uani 1 d . . . H3 H 0.4308 0.0362 0.4955 0.082 Uiso 1 calc R . . C4 C 0.4146(4) -0.0552(3) 0.4516(2) 0.0717(17) Uani 1 d . . . H4 H 0.4432 -0.0890 0.4696 0.086 Uiso 1 calc R . . C5 C 0.3770(4) -0.0782(3) 0.4109(2) 0.0787(19) Uani 1 d . . . H5 H 0.3778 -0.1285 0.4016 0.094 Uiso 1 calc R . . C6 C 0.3366(3) -0.0246(3) 0.3830(2) 0.0739(17) Uani 1 d . . . H6 H 0.3115 -0.0393 0.3546 0.089 Uiso 1 calc R . . C7 C 0.4545(3) 0.1777(3) 0.45861(18) 0.0505(13) Uani 1 d . . . C8 C 0.5143(3) 0.1565(4) 0.4290(2) 0.0752(17) Uani 1 d . . . H8 H 0.5050 0.1264 0.4018 0.090 Uiso 1 calc R . . C9 C 0.5857(3) 0.1780(3) 0.4384(3) 0.0769(18) Uani 1 d . . . H9 H 0.6249 0.1647 0.4176 0.092 Uiso 1 calc R . . C10 C 0.5983(3) 0.2202(4) 0.4795(3) 0.084(2) Uani 1 d . . . H10 H 0.6468 0.2336 0.4888 0.101 Uiso 1 calc R . . C11 C 0.5349(3) 0.2429(3) 0.5075(3) 0.0753(18) Uani 1 d . . . H11 H 0.5422 0.2741 0.5345 0.090 Uiso 1 calc R . . C12 C 0.1602(4) 0.0765(3) 0.30197(19) 0.0637(15) Uani 1 d . . . C13 C 0.1206(4) 0.0101(3) 0.2749(3) 0.096(2) Uani 1 d . . . H13 H 0.1542 -0.0321 0.2733 0.115 Uiso 1 calc R . . H13A H 0.1074 0.0255 0.2424 0.115 Uiso 1 calc R . . H13B H 0.0760 -0.0040 0.2924 0.115 Uiso 1 calc R . . C14 C 0.3811(4) 0.1035(4) 0.5958(2) 0.0691(17) Uani 1 d . . . C15 C 0.4213(4) 0.0510(4) 0.6317(2) 0.0806(19) Uani 1 d . . . H15 H 0.3944 0.0043 0.6338 0.097 Uiso 1 calc R . . H15A H 0.4231 0.0741 0.6634 0.097 Uiso 1 calc R . . H15B H 0.4715 0.0417 0.6204 0.097 Uiso 1 calc R . . O1W O 0.3538(5) -0.0197(5) 0.2468(3) 0.231(2) Uani 1 d . . . O2W O 0.2500 0.2500 0.2112(7) 0.231(2) Uani 1 d S . . O3W O 0.2321(6) -0.0161(5) 0.6572(4) 0.231(2) Uani 1 d . . . O4W O 0.2500 -0.2500 0.4157(5) 0.231(2) Uani 1 d S . . O5W O 0.1589(6) -0.2223(5) 0.3420(4) 0.231(2) Uani 1 d . . . O6W O 0.2595(5) -0.1538(6) 0.2783(4) 0.231(2) Uani 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 0.0519(5) 0.0519(5) 0.0457(8) 0.000 0.000 0.000 Ni2 0.0497(4) 0.0564(4) 0.0538(5) -0.0056(3) -0.0015(3) -0.0005(3) Ni3 0.0575(5) 0.0523(4) 0.0509(5) -0.0020(3) -0.0067(3) -0.0006(3) N1 0.041(2) 0.047(3) 0.080(4) -0.002(2) 0.002(2) 0.008(2) N2 0.045(2) 0.058(3) 0.058(3) 0.000(2) -0.002(2) 0.0009(19) O1 0.063(2) 0.066(2) 0.040(2) -0.0112(17) 0.0096(17) -0.0085(18) O2 0.056(2) 0.056(2) 0.061(3) 0.0144(18) 0.0057(18) -0.0025(17) O3 0.067(3) 0.068(3) 0.085(3) -0.029(2) -0.016(2) -0.002(2) O4 0.082(3) 0.069(3) 0.050(3) -0.0151(19) 0.007(2) 0.001(2) O21 0.047(2) 0.047(2) 0.030(4) 0.000 0.000 0.000 O5 0.079(3) 0.061(2) 0.064(3) 0.0141(19) -0.021(2) 0.006(2) O6 0.076(3) 0.071(3) 0.069(3) -0.018(2) -0.013(2) 0.004(2) O31 0.052(2) 0.052(2) 0.059(5) 0.000 0.000 0.000 C1 0.053(3) 0.042(3) 0.064(4) -0.004(3) -0.004(3) 0.011(2) C2 0.052(3) 0.051(3) 0.064(4) 0.000(3) 0.002(3) -0.002(3) C3 0.046(3) 0.064(4) 0.096(5) 0.005(3) -0.001(3) -0.020(3) C4 0.082(4) 0.040(3) 0.093(5) 0.020(3) -0.009(4) -0.008(3) C5 0.076(4) 0.049(3) 0.112(6) 0.007(3) 0.002(4) -0.008(3) C6 0.068(4) 0.058(4) 0.096(5) -0.019(3) -0.003(3) -0.004(3) C7 0.054(3) 0.049(3) 0.048(3) -0.005(2) 0.001(2) 0.007(2) C8 0.059(4) 0.077(4) 0.089(5) 0.012(4) 0.020(3) -0.010(3) C9 0.048(3) 0.062(4) 0.120(6) 0.022(4) 0.000(3) 0.001(3) C10 0.047(4) 0.072(4) 0.133(7) 0.010(4) -0.015(4) -0.002(3) C11 0.075(4) 0.049(3) 0.101(5) 0.001(3) -0.024(4) -0.007(3) C12 0.090(5) 0.066(4) 0.035(3) -0.004(3) -0.017(3) -0.012(4) C13 0.122(6) 0.063(4) 0.101(6) -0.025(4) -0.012(5) -0.017(4) C14 0.090(5) 0.069(4) 0.048(4) 0.022(3) -0.001(3) 0.017(4) C15 0.072(4) 0.094(5) 0.076(5) 0.013(3) -0.020(3) 0.018(4) O1W 0.258(5) 0.215(5) 0.221(4) 0.032(4) -0.013(4) -0.048(3) O2W 0.258(5) 0.215(5) 0.221(4) 0.032(4) -0.013(4) -0.048(3) O3W 0.258(5) 0.215(5) 0.221(4) 0.032(4) -0.013(4) -0.048(3) O4W 0.258(5) 0.215(5) 0.221(4) 0.032(4) -0.013(4) -0.048(3) O5W 0.258(5) 0.215(5) 0.221(4) 0.032(4) -0.013(4) -0.048(3) O6W 0.258(5) 0.215(5) 0.221(4) 0.032(4) -0.013(4) -0.048(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 2.228(3) 4 ? Ni1 O2 2.228(3) 2 ? Ni1 O2 2.228(3) 3 ? Ni1 O2 2.228(3) . ? Ni1 O1 2.244(4) . ? Ni1 O1 2.244(4) 2 ? Ni1 O1 2.244(4) 3 ? Ni1 O1 2.244(4) 4 ? Ni2 O3 1.995(4) . ? Ni2 N1 2.041(4) . ? Ni2 O2 2.055(4) . ? Ni2 O4 2.092(4) . ? Ni2 O2 2.106(3) 4 ? Ni2 O21 2.262(2) . ? Ni3 O6 1.982(4) . ? Ni3 O1 2.013(3) . ? Ni3 N2 2.044(4) . ? Ni3 O5 2.055(4) . ? Ni3 O1 2.105(3) 2 ? Ni3 O31 2.272(3) . ? N1 C2 1.301(7) . ? N1 C6 1.374(6) . ? N2 C7 1.301(6) . ? N2 C11 1.330(6) . ? O1 C1 1.357(6) . ? O1 Ni3 2.105(3) 4 ? O2 C1 1.390(6) . ? O2 Ni2 2.106(3) 2 ? O3 C12 1.213(7) . ? O4 C12 1.234(7) 2 ? O21 Ni2 2.262(2) 4 ? O21 Ni2 2.262(2) 2 ? O21 Ni2 2.262(2) 3 ? O5 C14 1.232(7) . ? O6 C14 1.287(7) 2 ? O31 Ni3 2.272(3) 3 ? O31 Ni3 2.272(3) 4 ? O31 Ni3 2.272(3) 2 ? C1 C7 1.540(7) . ? C1 C2 1.544(7) . ? C2 C3 1.373(8) . ? C3 C4 1.401(8) . ? C3 H3 0.9300 . ? C4 C5 1.360(8) . ? C4 H4 0.9300 . ? C5 C6 1.417(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.388(7) . ? C8 C9 1.350(8) . ? C8 H8 0.9300 . ? C9 C10 1.369(9) . ? C9 H9 0.9300 . ? C10 C11 1.421(9) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 O4 1.234(7) 4 ? C12 C13 1.561(8) . ? C13 H13 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C14 O6 1.287(7) 4 ? C14 C15 1.530(8) . ? C15 H15 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ni1 O2 123.49(19) 4 2 ? O2 Ni1 O2 77.05(8) 4 3 ? O2 Ni1 O2 77.05(8) 2 3 ? O2 Ni1 O2 77.05(8) 4 . ? O2 Ni1 O2 77.05(8) 2 . ? O2 Ni1 O2 123.49(19) 3 . ? O2 Ni1 O1 91.20(13) 4 . ? O2 Ni1 O1 116.02(12) 2 . ? O2 Ni1 O1 166.17(13) 3 . ? O2 Ni1 O1 59.25(13) . . ? O2 Ni1 O1 166.17(13) 4 2 ? O2 Ni1 O1 59.25(13) 2 2 ? O2 Ni1 O1 116.02(12) 3 2 ? O2 Ni1 O1 91.20(13) . 2 ? O1 Ni1 O1 76.36(8) . 2 ? O2 Ni1 O1 116.02(12) 4 3 ? O2 Ni1 O1 91.20(13) 2 3 ? O2 Ni1 O1 59.25(13) 3 3 ? O2 Ni1 O1 166.17(13) . 3 ? O1 Ni1 O1 121.90(17) . 3 ? O1 Ni1 O1 76.36(8) 2 3 ? O2 Ni1 O1 59.25(13) 4 4 ? O2 Ni1 O1 166.17(13) 2 4 ? O2 Ni1 O1 91.20(13) 3 4 ? O2 Ni1 O1 116.02(12) . 4 ? O1 Ni1 O1 76.36(8) . 4 ? O1 Ni1 O1 121.90(17) 2 4 ? O1 Ni1 O1 76.36(8) 3 4 ? O3 Ni2 N1 94.79(17) . . ? O3 Ni2 O2 173.53(16) . . ? N1 Ni2 O2 79.66(15) . . ? O3 Ni2 O4 84.99(16) . . ? N1 Ni2 O4 87.84(16) . . ? O2 Ni2 O4 98.03(15) . . ? O3 Ni2 O2 93.87(16) . 4 ? N1 Ni2 O2 97.64(16) . 4 ? O2 Ni2 O2 83.66(18) . 4 ? O4 Ni2 O2 174.48(16) . 4 ? O3 Ni2 O21 103.79(16) . . ? N1 Ni2 O21 161.41(17) . . ? O2 Ni2 O21 81.75(14) . . ? O4 Ni2 O21 94.34(16) . . ? O2 Ni2 O21 80.67(14) 4 . ? O6 Ni3 O1 174.22(16) . . ? O6 Ni3 N2 93.96(17) . . ? O1 Ni3 N2 80.56(16) . . ? O6 Ni3 O5 84.83(17) . . ? O1 Ni3 O5 96.83(16) . . ? N2 Ni3 O5 88.99(16) . . ? O6 Ni3 O1 94.17(16) . 2 ? O1 Ni3 O1 84.7(2) . 2 ? N2 Ni3 O1 96.34(15) . 2 ? O5 Ni3 O1 174.64(14) . 2 ? O6 Ni3 O31 102.83(18) . . ? O1 Ni3 O31 82.60(16) . . ? N2 Ni3 O31 163.09(19) . . ? O5 Ni3 O31 94.43(17) . . ? O1 Ni3 O31 80.64(16) 2 . ? C2 N1 C6 120.0(5) . . ? C2 N1 Ni2 115.4(3) . . ? C6 N1 Ni2 124.3(4) . . ? C7 N2 C11 119.7(5) . . ? C7 N2 Ni3 114.7(3) . . ? C11 N2 Ni3 125.6(4) . . ? C1 O1 Ni3 115.0(3) . . ? C1 O1 Ni3 144.9(3) . 4 ? Ni3 O1 Ni3 95.23(14) . 4 ? C1 O1 Ni1 96.9(3) . . ? Ni3 O1 Ni1 98.42(15) . . ? Ni3 O1 Ni1 95.75(14) 4 . ? C1 O2 Ni2 114.9(3) . . ? C1 O2 Ni2 146.2(3) . 2 ? Ni2 O2 Ni2 94.11(15) . 2 ? C1 O2 Ni1 96.7(3) . . ? Ni2 O2 Ni1 97.67(14) . . ? Ni2 O2 Ni1 96.19(13) 2 . ? C12 O3 Ni2 127.0(4) . . ? C12 O4 Ni2 125.3(3) 2 . ? Ni2 O21 Ni2 144.4(3) 4 2 ? Ni2 O21 Ni2 84.64(8) 4 . ? Ni2 O21 Ni2 84.64(8) 2 . ? Ni2 O21 Ni2 84.64(8) 4 3 ? Ni2 O21 Ni2 84.64(8) 2 3 ? Ni2 O21 Ni2 144.4(3) . 3 ? C14 O5 Ni3 131.1(4) . . ? C14 O6 Ni3 128.4(4) 2 . ? Ni3 O31 Ni3 84.06(11) 3 4 ? Ni3 O31 Ni3 142.5(3) 3 . ? Ni3 O31 Ni3 84.06(11) 4 . ? Ni3 O31 Ni3 84.06(11) 3 2 ? Ni3 O31 Ni3 142.5(3) 4 2 ? Ni3 O31 Ni3 84.06(11) . 2 ? O1 C1 O2 107.2(4) . . ? O1 C1 C7 111.7(4) . . ? O2 C1 C7 108.6(4) . . ? O1 C1 C2 113.0(4) . . ? O2 C1 C2 109.2(4) . . ? C7 C1 C2 107.0(4) . . ? N1 C2 C3 122.8(5) . . ? N1 C2 C1 117.4(5) . . ? C3 C2 C1 119.8(5) . . ? C2 C3 C4 118.7(6) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 119.2(6) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 119.1(6) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? N1 C6 C5 119.7(6) . . ? N1 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? N2 C7 C8 120.4(5) . . ? N2 C7 C1 115.8(4) . . ? C8 C7 C1 123.8(5) . . ? C9 C8 C7 122.2(7) . . ? C9 C8 H8 118.9 . . ? C7 C8 H8 118.9 . . ? C8 C9 C10 117.7(6) . . ? C8 C9 H9 121.1 . . ? C10 C9 H9 121.1 . . ? C9 C10 C11 117.9(6) . . ? C9 C10 H10 121.1 . . ? C11 C10 H10 121.1 . . ? N2 C11 C10 121.9(6) . . ? N2 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? O3 C12 O4 128.8(5) . 4 ? O3 C12 C13 117.2(6) . . ? O4 C12 C13 113.9(6) 4 . ? C12 C13 H13 109.5 . . ? C12 C13 H13A 109.5 . . ? H13 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O5 C14 O6 122.8(5) . 4 ? O5 C14 C15 122.2(6) . . ? O6 C14 C15 114.7(5) 4 . ? C14 C15 H15 109.5 . . ? C14 C15 H15A 109.5 . . ? H15 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? #===END