# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Beata Nowicka' _publ_contact_author_email beata.nowicka@uj.edu.pl loop_ _publ_author_name 'Beata Nowicka' 'Katarzyna Stadnicka' 'Wojciech Nitek' 'Michal Rams' 'Barbara Sieklucka' data_1a _database_code_depnum_ccdc_archive 'CCDC 876827' #TrackingRef '- clusters1-4_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; {Ni[Ni(bpy)(H2O)]8[W(CN)8]6}. 11.8 H2O ; _chemical_name_common '(Ni(Ni(bpy)(H2O))8(W(CN)8)6). 11.8 H2O' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C128 H103.60 N64 Ni9 O19.80 W6' _chemical_formula_weight 4486.64 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' W W -0.8490 6.8722 '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 18.6069(11) _cell_length_b 19.1286(9) _cell_length_c 24.0604(14) _cell_angle_alpha 91.308(2) _cell_angle_beta 91.075(3) _cell_angle_gamma 94.282(4) _cell_volume 8535.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 19914 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.028 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4348 _exptl_absorpt_coefficient_mu 5.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4160 _exptl_absorpt_correction_T_max 0.5589 _exptl_absorpt_process_details 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \o scans to fill Ewald sphere' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 35941 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_sigmaI/netI 0.062 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.00 _reflns_number_total 33833 _reflns_number_gt 24712 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (ALTOMARE et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+74.3669P] 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 33833 _refine_ls_number_parameters 2031 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.005 _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 W1 W 0.466498(16) 0.450214(17) 0.280903(12) 0.02019(7) Uani 1 1 d . . . C11 C 0.4867(4) 0.4751(4) 0.3686(3) 0.0222(17) Uani 1 1 d . . . N11 N 0.4948(3) 0.4867(3) 0.4150(3) 0.0254(15) Uani 1 1 d . . . C12 C 0.3711(4) 0.4133(4) 0.3263(3) 0.0254(18) Uani 1 1 d . . . N12 N 0.3222(4) 0.3919(4) 0.3499(3) 0.0307(16) Uani 1 1 d . . . C13 C 0.4188(4) 0.5485(5) 0.2967(3) 0.0277(19) Uani 1 1 d . . . N13 N 0.3963(4) 0.6020(4) 0.3050(3) 0.0335(17) Uani 1 1 d . . . C14 C 0.5082(4) 0.3577(5) 0.3168(3) 0.0288(19) Uani 1 1 d . . . N14 N 0.5331(4) 0.3114(4) 0.3360(3) 0.0325(17) Uani 1 1 d . . . C15 C 0.5690(4) 0.5109(4) 0.2891(3) 0.0248(17) Uani 1 1 d . . . N15 N 0.6238(4) 0.5403(4) 0.2956(3) 0.0301(16) Uani 1 1 d . . . C16 C 0.5374(5) 0.4061(5) 0.2202(4) 0.034(2) Uani 1 1 d . . . N16 N 0.5751(5) 0.3843(5) 0.1885(3) 0.054(2) Uani 1 1 d . . . C17 C 0.3978(7) 0.3836(8) 0.2274(5) 0.083(5) Uani 1 1 d . . . N17 N 0.3564(8) 0.3496(10) 0.1997(5) 0.160(8) Uani 1 1 d . . . C18 C 0.4643(7) 0.5115(7) 0.2055(4) 0.070(4) Uani 1 1 d . . . N18 N 0.4633(9) 0.5425(8) 0.1669(5) 0.130(6) Uani 1 1 d . . . W2 W 0.765817(15) 0.413883(17) 0.490732(12) 0.01965(7) Uani 1 1 d . . . C21 C 0.6575(4) 0.4432(4) 0.4980(3) 0.0242(17) Uani 1 1 d . . . N21 N 0.6003(3) 0.4623(3) 0.5017(3) 0.0252(15) Uani 1 1 d . . . C22 C 0.7738(4) 0.5146(4) 0.5348(3) 0.0244(18) Uani 1 1 d . . . N22 N 0.7764(4) 0.5643(4) 0.5618(3) 0.0302(16) Uani 1 1 d . . . C23 C 0.7217(4) 0.3735(4) 0.5672(3) 0.0249(18) Uani 1 1 d . . . N23 N 0.3028(4) 0.6494(4) 0.3935(3) 0.0305(16) Uani 1 1 d . . . C24 C 0.6999(4) 0.3417(4) 0.4357(3) 0.0271(18) Uani 1 1 d . . . N24 N 0.6633(4) 0.3029(4) 0.4090(3) 0.0304(16) Uani 1 1 d . . . C25 C 0.7429(4) 0.4849(4) 0.4236(3) 0.0265(18) Uani 1 1 d . . . N25 N 0.7281(4) 0.5200(4) 0.3893(3) 0.0335(17) Uani 1 1 d . . . C26 C 0.8072(4) 0.3108(5) 0.4984(3) 0.031(2) Uani 1 1 d . . . N26 N 0.8294(5) 0.2571(5) 0.5044(4) 0.053(2) Uani 1 1 d . . . C27 C 0.8594(5) 0.4236(5) 0.5452(4) 0.039(2) Uani 1 1 d . . . N27 N 0.9067(5) 0.4292(5) 0.5756(5) 0.071(3) Uani 1 1 d . . . C28 C 0.8532(4) 0.4146(5) 0.4334(4) 0.039(2) Uani 1 1 d . . . N28 N 0.9006(5) 0.4158(5) 0.4026(4) 0.064(3) Uani 1 1 d . . . W3 W 0.596273(16) 0.763713(16) 0.462055(13) 0.01982(7) Uani 1 1 d . . . C31 C 0.5605(4) 0.6576(4) 0.4809(3) 0.0194(16) Uani 1 1 d . . . N31 N 0.5433(3) 0.6003(4) 0.4914(3) 0.0245(15) Uani 1 1 d . . . C32 C 0.6736(4) 0.7223(4) 0.5180(4) 0.0276(18) Uani 1 1 d . . . N32 N 0.7107(4) 0.6968(4) 0.5491(3) 0.0315(16) Uani 1 1 d . . . C33 C 0.5019(4) 0.7314(4) 0.4107(3) 0.0245(17) Uani 1 1 d . . . N33 N 0.4517(4) 0.7141(4) 0.3847(3) 0.0352(17) Uani 1 1 d . . . C34 C 0.5148(4) 0.7676(4) 0.5241(3) 0.0269(18) Uani 1 1 d . . . N34 N 0.4740(4) 0.7683(4) 0.5594(3) 0.0346(17) Uani 1 1 d . . . C35 C 0.6399(4) 0.6961(4) 0.4005(3) 0.0238(17) Uani 1 1 d . . . N35 N 0.6669(4) 0.6589(4) 0.3715(3) 0.0307(16) Uani 1 1 d . . . C36 C 0.5550(5) 0.8545(5) 0.4266(5) 0.045(3) Uani 1 1 d . . . N36 N 0.5316(6) 0.9045(6) 0.4086(5) 0.086(4) Uani 1 1 d . . . C37 C 0.6927(5) 0.8141(4) 0.4292(4) 0.039(2) Uani 1 1 d . . . N37 N 0.7469(5) 0.8387(5) 0.4128(4) 0.066(3) Uani 1 1 d . . . C38 C 0.6296(5) 0.8505(5) 0.5184(4) 0.039(2) Uani 1 1 d . . . N38 N 0.6486(6) 0.8963(5) 0.5481(4) 0.066(3) Uani 1 1 d . . . W4 W 1.162558(16) 0.946812(17) 0.175912(12) 0.02151(8) Uani 1 1 d . . . C41 C 1.1006(4) 0.9553(4) 0.0997(3) 0.0229(17) Uani 1 1 d . . . N41 N 1.0665(4) 0.9651(4) 0.0612(3) 0.0281(16) Uani 1 1 d . . . C42 C 1.0739(5) 1.0110(5) 0.1926(3) 0.032(2) Uani 1 1 d . . . N42 N 1.0263(4) 1.0437(4) 0.2012(3) 0.0387(19) Uani 1 1 d . . . C43 C 1.0745(4) 0.8669(4) 0.1773(3) 0.0246(17) Uani 1 1 d . . . N43 N 1.0278(4) 0.8249(4) 0.1772(3) 0.0357(17) Uani 1 1 d . . . C44 C 1.2261(4) 0.9080(5) 0.1089(4) 0.032(2) Uani 1 1 d . . . N44 N 0.7457(4) 1.1152(4) -0.0716(3) 0.0383(18) Uani 1 1 d . . . C45 C 1.1979(4) 1.0483(5) 0.1420(3) 0.031(2) Uani 1 1 d . . . N45 N 0.7831(4) 0.8998(4) -0.1229(3) 0.0349(17) Uani 1 1 d . . . C46 C 1.2676(4) 0.9801(5) 0.2092(4) 0.034(2) Uani 1 1 d . . . N46 N 1.3242(5) 0.9979(5) 0.2268(4) 0.054(2) Uani 1 1 d . . . C47 C 1.2063(5) 0.8515(5) 0.2056(4) 0.035(2) Uani 1 1 d . . . N47 N 0.2286(5) 0.8026(5) 0.2202(4) 0.064(3) Uani 1 1 d . . . C48 C 1.1464(5) 0.9509(5) 0.2643(4) 0.037(2) Uani 1 1 d . . . N48 N 1.1344(5) 0.9523(5) 0.3107(3) 0.061(3) Uani 1 1 d . . . W5 W 1.002573(19) 0.733256(18) -0.057849(14) 0.02770(8) Uani 1 1 d . . . C51 C 1.0253(5) 0.7904(5) -0.1328(4) 0.036(2) Uani 1 1 d . . . N51 N 1.0357(4) 0.8224(4) -0.1712(3) 0.0398(19) Uani 1 1 d . . . C52 C 0.9950(4) 0.8430(5) -0.0412(3) 0.0278(19) Uani 1 1 d . . . N52 N 0.9918(4) 0.9020(4) -0.0336(3) 0.0301(16) Uani 1 1 d . . . C53 C 0.9796(4) 0.7443(5) 0.0298(4) 0.0309(19) Uani 1 1 d . . . N53 N 0.9679(4) 0.7498(4) 0.0757(3) 0.0370(18) Uani 1 1 d . . . C54 C 0.8949(5) 1.2250(5) 0.0232(4) 0.035(2) Uani 1 1 d . . . N54 N 0.8388(4) 1.2035(4) 0.0075(3) 0.0403(19) Uani 1 1 d . . . C55 C 0.8905(5) 0.7543(5) -0.0656(4) 0.037(2) Uani 1 1 d . . . N55 N 0.8327(4) 0.7716(4) -0.0700(3) 0.0412(19) Uani 1 1 d . . . C56 C 0.9593(7) 0.6661(6) -0.1249(5) 0.071(4) Uani 1 1 d . . . N56 N 0.9353(9) 0.6316(7) -0.1616(6) 0.128(6) Uani 1 1 d . . . C57A C 1.0816(14) 0.6633(14) -0.0781(11) 0.073(7) Uiso 0.55 1 d P . . C57B C 1.0916(13) 0.6873(14) -0.1002(11) 0.047(6) Uiso 0.45 1 d P . . N57A N 1.1332(12) 0.6380(12) -0.0977(9) 0.081(6) Uiso 0.55 1 d P . . N57B N 1.1478(14) 0.6768(14) -0.1250(11) 0.082(7) Uiso 0.45 1 d P . . C58A C 0.9614(14) 0.6319(14) -0.0270(10) 0.067(7) Uiso 0.50 1 d P . . C58B C 1.0246(18) 0.6401(18) -0.0153(14) 0.097(9) Uiso 0.50 1 d P . . N58A N 0.927(2) 0.584(2) -0.0127(15) 0.148(12) Uiso 0.50 1 d P . . N58B N 1.018(2) 0.579(2) 0.0056(18) 0.189(16) Uiso 0.50 1 d P . . W6 W 0.758965(16) 0.939572(17) 0.113857(13) 0.02241(8) Uani 1 1 d . . . C61 C 0.8576(4) 0.9614(4) 0.0682(3) 0.0246(18) Uani 1 1 d . . . N61 N 0.9091(4) 0.9743(4) 0.0456(3) 0.0284(16) Uani 1 1 d . . . C62 C 0.8259(5) 1.0160(5) 0.1630(3) 0.0286(19) Uani 1 1 d . . . N62 N 0.8654(4) 1.0534(4) 0.1888(3) 0.0367(18) Uani 1 1 d . . . C63 C 0.8330(4) 0.8650(5) 0.1385(3) 0.0276(19) Uani 1 1 d . . . N63 N 0.8726(4) 0.8230(4) 0.1508(3) 0.0359(18) Uani 1 1 d . . . C64 C 0.7482(4) 1.0368(5) 0.0694(3) 0.0257(18) Uani 1 1 d . . . N64 N 0.7405(4) 1.0862(4) 0.0465(3) 0.0341(17) Uani 1 1 d . . . C65 C 0.7393(4) 0.8924(5) 0.0317(4) 0.0304(19) Uani 1 1 d . . . N65 N 0.7332(4) 0.8647(4) -0.0110(3) 0.0371(18) Uani 1 1 d . . . C66 C 0.6928(5) 0.8401(5) 0.1211(4) 0.037(2) Uani 1 1 d . . . N66 N 0.6597(5) 0.7888(5) 0.1233(4) 0.056(2) Uani 1 1 d . . . C67 C 0.7353(5) 0.9281(5) 0.2014(4) 0.038(2) Uani 1 1 d . . . N67 N 0.7252(6) 0.9225(5) 0.2471(4) 0.074(3) Uani 1 1 d . . . C68 C 0.6502(5) 0.9697(6) 0.1199(5) 0.056(3) Uani 1 1 d . . . N68 N 0.5941(5) 0.9858(7) 0.1238(6) 0.103(5) Uani 1 1 d . . . Ni1 Ni 0.5000 0.5000 0.5000 0.0158(3) Uani 1 2 d S . . Ni2 Ni 0.76868(5) 0.65248(5) 0.61127(4) 0.0253(2) Uani 1 1 d . . . O213 O 0.8314(3) 0.6109(3) 0.6767(3) 0.0433(16) Uani 1 1 d . . . N201 N 0.8633(4) 0.7040(4) 0.5852(3) 0.0373(18) Uani 1 1 d . . . C202 C 0.9146(5) 0.6761(6) 0.5554(4) 0.047(3) Uani 1 1 d . . . H202 H 0.9078 0.6292 0.5441 0.056 Uiso 1 1 calc R . . C203 C 0.9774(6) 0.7142(8) 0.5407(5) 0.072(4) Uani 1 1 d . . . H203 H 1.0137 0.6934 0.5218 0.087 Uiso 1 1 calc R . . C204 C 0.9833(7) 0.7849(9) 0.5556(6) 0.083(4) Uani 1 1 d . . . H204 H 1.0236 0.8126 0.5448 0.100 Uiso 1 1 calc R . . C205 C 0.9339(7) 0.8138(7) 0.5846(5) 0.069(4) Uani 1 1 d . . . H205 H 0.9402 0.8611 0.5949 0.083 Uiso 1 1 calc R . . C206 C 0.8714(5) 0.7737(5) 0.6001(4) 0.044(2) Uani 1 1 d . . . C207 C 0.8144(5) 0.7989(5) 0.6348(4) 0.040(2) Uani 1 1 d . . . C208 C 0.8098(7) 0.8690(6) 0.6493(5) 0.065(3) Uani 1 1 d . . . H208 H 0.8438 0.9029 0.6369 0.078 Uiso 1 1 calc R . . C209 C 0.7533(8) 0.8884(6) 0.6827(5) 0.069(4) Uani 1 1 d . . . H209 H 0.7482 0.9354 0.6915 0.083 Uiso 1 1 calc R . . C210 C 0.7071(7) 0.8384(6) 0.7017(5) 0.067(3) Uani 1 1 d . . . H210 H 0.6710 0.8496 0.7258 0.081 Uiso 1 1 calc R . . C211 C 0.7135(6) 0.7700(6) 0.6852(4) 0.054(3) Uani 1 1 d . . . H211 H 0.6796 0.7358 0.6974 0.065 Uiso 1 1 calc R . . N212 N 0.7658(4) 0.7497(4) 0.6524(3) 0.0346(17) Uani 1 1 d . . . Ni3 Ni 0.36175(5) 0.69796(5) 0.33209(4) 0.0235(2) Uani 1 1 d . . . O313 O 0.2718(3) 0.6817(3) 0.2769(2) 0.0356(14) Uani 1 1 d . . . N301 N 0.3299(4) 0.7967(4) 0.3552(3) 0.0336(17) Uani 1 1 d . . . C302 C 0.2840(5) 0.8094(5) 0.3956(4) 0.045(2) Uani 1 1 d . . . H302 H 0.2614 0.7718 0.4140 0.054 Uiso 1 1 calc R . . C303 C 0.2691(6) 0.8777(6) 0.4109(5) 0.060(3) Uani 1 1 d . . . H303 H 0.2368 0.8858 0.4390 0.072 Uiso 1 1 calc R . . C304 C 0.3036(7) 0.9329(6) 0.3832(5) 0.063(3) Uani 1 1 d . . . H304 H 0.2954 0.9790 0.3925 0.076 Uiso 1 1 calc R . . C305 C 0.3500(6) 0.9184(5) 0.3419(4) 0.049(3) Uani 1 1 d . . . H305 H 0.3736 0.9549 0.3230 0.059 Uiso 1 1 calc R . . C306 C 0.3621(5) 0.8507(5) 0.3280(4) 0.034(2) Uani 1 1 d . . . C307 C 0.4113(5) 0.8304(5) 0.2839(4) 0.043(2) Uani 1 1 d . . . C308 C 0.4500(8) 0.8793(7) 0.2521(6) 0.094(5) Uani 1 1 d . . . H308 H 0.4440 0.9270 0.2563 0.113 Uiso 1 1 calc R . . C309 C 0.4976(12) 0.8551(10) 0.2141(9) 0.171(11) Uani 1 1 d . . . H309 H 0.5252 0.8870 0.1933 0.205 Uiso 1 1 calc R . . C310 C 0.5046(11) 0.7872(10) 0.2071(9) 0.162(10) Uani 1 1 d . . . H310 H 0.5382 0.7717 0.1824 0.195 Uiso 1 1 calc R . . C311 C 0.4610(8) 0.7379(7) 0.2370(6) 0.097(5) Uani 1 1 d . . . H311 H 0.4627 0.6901 0.2300 0.116 Uiso 1 1 calc R . . N312 N 0.4175(4) 0.7612(4) 0.2754(3) 0.044(2) Uani 1 1 d . . . Ni4 Ni 0.58712(5) 0.23131(5) 0.37105(4) 0.0252(2) Uani 1 1 d . . . O413 O 0.5039(4) 0.1577(4) 0.3336(3) 0.0532(18) Uani 1 1 d . . . N401 N 0.6461(4) 0.2127(4) 0.3003(3) 0.0331(17) Uani 1 1 d . . . C402 C 0.6518(5) 0.2538(6) 0.2557(4) 0.045(2) Uani 1 1 d . . . H402 H 0.6343 0.2981 0.2575 0.054 Uiso 1 1 calc R . . C403 C 0.6821(6) 0.2326(6) 0.2087(4) 0.057(3) Uani 1 1 d . . . H403 H 0.6848 0.2619 0.1784 0.069 Uiso 1 1 calc R . . C404 C 0.7091(6) 0.1681(7) 0.2051(4) 0.062(3) Uani 1 1 d . . . H404 H 0.7309 0.1537 0.1728 0.075 Uiso 1 1 calc R . . C405 C 0.7035(6) 0.1243(6) 0.2506(4) 0.057(3) Uani 1 1 d . . . H405 H 0.7200 0.0796 0.2488 0.068 Uiso 1 1 calc R . . C406 C 0.6730(5) 0.1488(5) 0.2981(4) 0.038(2) Uani 1 1 d . . . C407 C 0.6680(5) 0.1094(4) 0.3503(4) 0.034(2) Uani 1 1 d . . . C408 C 0.6915(6) 0.0426(6) 0.3568(5) 0.059(3) Uani 1 1 d . . . H408 H 0.7100 0.0191 0.3266 0.071 Uiso 1 1 calc R . . C409 C 0.6874(6) 0.0116(6) 0.4071(5) 0.063(3) Uani 1 1 d . . . H409 H 0.7039 -0.0327 0.4118 0.076 Uiso 1 1 calc R . . C410 C 0.6591(6) 0.0463(6) 0.4501(5) 0.059(3) Uani 1 1 d . . . H410 H 0.6551 0.0257 0.4847 0.071 Uiso 1 1 calc R . . C411 C 0.6363(5) 0.1121(5) 0.4423(4) 0.044(2) Uani 1 1 d . . . H411 H 0.6186 0.1362 0.4725 0.053 Uiso 1 1 calc R . . N412 N 0.6385(4) 0.1427(4) 0.3932(3) 0.0301(16) Uani 1 1 d . . . Ni5 Ni 0.72051(5) 0.58939(5) 0.32366(4) 0.0236(2) Uani 1 1 d . . . O513 O 0.7218(4) 0.6603(4) 0.2571(3) 0.0468(17) Uani 1 1 d . . . N501 N 0.8224(3) 0.6316(4) 0.3480(3) 0.0290(16) Uani 1 1 d . . . C502 C 0.8380(5) 0.6848(5) 0.3842(4) 0.044(2) Uani 1 1 d . . . H502 H 0.8004 0.7092 0.3977 0.053 Uiso 1 1 calc R . . C503 C 0.9067(6) 0.7050(6) 0.4022(5) 0.053(3) Uani 1 1 d . . . H503 H 0.9159 0.7437 0.4262 0.064 Uiso 1 1 calc R . . C504 C 0.9615(6) 0.6673(7) 0.3844(5) 0.062(3) Uani 1 1 d . . . H504 H 1.0085 0.6788 0.3972 0.074 Uiso 1 1 calc R . . C505 C 0.9469(5) 0.6120(6) 0.3472(5) 0.053(3) Uani 1 1 d . . . H505 H 0.9839 0.5863 0.3343 0.064 Uiso 1 1 calc R . . C506 C 0.8767(4) 0.5952(5) 0.3294(4) 0.034(2) Uani 1 1 d . . . C507 C 0.8548(5) 0.5351(5) 0.2904(4) 0.038(2) Uani 1 1 d . . . C508 C 0.9033(6) 0.4916(6) 0.2656(4) 0.055(3) Uani 1 1 d . . . H508 H 0.9525 0.4982 0.2737 0.066 Uiso 1 1 calc R . . C509 C 0.8771(7) 0.4393(6) 0.2293(5) 0.064(3) Uani 1 1 d . . . H509 H 0.9087 0.4103 0.2124 0.077 Uiso 1 1 calc R . . C510 C 0.8065(7) 0.4297(7) 0.2181(5) 0.068(3) Uani 1 1 d . . . H510 H 0.7888 0.3940 0.1935 0.082 Uiso 1 1 calc R . . C511 C 0.7596(5) 0.4735(5) 0.2435(4) 0.047(3) Uani 1 1 d . . . H511 H 0.7103 0.4665 0.2361 0.056 Uiso 1 1 calc R . . N512 N 0.7845(4) 0.5255(4) 0.2784(3) 0.0350(17) Uani 1 1 d . . . Ni6 Ni 1.0000 1.0000 0.0000 0.0173(3) Uani 1 2 d S . . Ni7 Ni 0.95112(6) 1.10550(6) 0.23280(4) 0.0281(2) Uani 1 1 d . . . O713 O 1.0421(4) 1.1591(4) 0.2768(3) 0.064(2) Uani 1 1 d . . . N701 N 0.8901(4) 1.1662(4) 0.2829(3) 0.042(2) Uani 1 1 d . . . C702 C 0.8722(7) 1.2293(6) 0.2723(5) 0.067(4) Uani 1 1 d . . . H702 H 0.8824 1.2478 0.2377 0.080 Uiso 1 1 calc R . . C703 C 0.8382(8) 1.2698(8) 0.3112(6) 0.083(4) Uani 1 1 d . . . H703 H 0.8250 1.3142 0.3023 0.099 Uiso 1 1 calc R . . C704 C 0.8248(7) 1.2440(8) 0.3612(5) 0.076(4) Uani 1 1 d . . . H704 H 0.8033 1.2708 0.3880 0.092 Uiso 1 1 calc R . . C705 C 0.8427(6) 1.1782(7) 0.3727(4) 0.063(3) Uani 1 1 d . . . H705 H 0.8323 1.1599 0.4073 0.076 Uiso 1 1 calc R . . C706 C 0.8765(5) 1.1377(6) 0.3333(4) 0.046(3) Uani 1 1 d . . . C707 C 0.8969(5) 1.0667(6) 0.3415(4) 0.044(2) Uani 1 1 d . . . C708 C 0.8830(7) 1.0286(8) 0.3876(5) 0.083(4) Uani 1 1 d . . . H708 H 0.8613 1.0486 0.4179 0.099 Uiso 1 1 calc R . . C709 C 0.9013(8) 0.9604(9) 0.3889(6) 0.100(6) Uani 1 1 d . . . H709 H 0.8899 0.9339 0.4199 0.120 Uiso 1 1 calc R . . C710 C 0.9346(7) 0.9314(7) 0.3472(6) 0.081(4) Uani 1 1 d . . . H710 H 0.9472 0.8853 0.3482 0.098 Uiso 1 1 calc R . . C711 C 0.9499(6) 0.9733(7) 0.3018(5) 0.061(3) Uani 1 1 d . . . H711 H 0.9737 0.9545 0.2719 0.074 Uiso 1 1 calc R . . N712 N 0.9322(4) 1.0381(4) 0.2994(3) 0.0413(19) Uani 1 1 d . . . Ni8 Ni 0.94488(5) 0.74832(6) 0.16051(4) 0.0276(2) Uani 1 1 d . . . O813 O 0.9231(4) 0.7453(4) 0.2478(3) 0.0476(17) Uani 1 1 d . . . N801 N 0.8703(4) 0.6650(4) 0.1416(3) 0.0396(19) Uani 1 1 d . . . C802 C 0.8005(5) 0.6678(6) 0.1286(5) 0.054(3) Uani 1 1 d . . . H802 H 0.7799 0.7102 0.1334 0.065 Uiso 1 1 calc R . . C803 C 0.7576(7) 0.6107(8) 0.1083(6) 0.079(4) Uani 1 1 d . . . H803 H 0.7091 0.6143 0.0993 0.095 Uiso 1 1 calc R . . C804 C 0.7889(9) 0.5488(8) 0.1017(6) 0.092(5) Uani 1 1 d . . . H804 H 0.7609 0.5090 0.0893 0.111 Uiso 1 1 calc R . . C805 C 0.8600(7) 0.5442(6) 0.1129(6) 0.073(4) Uani 1 1 d . . . H805 H 0.8816 0.5025 0.1066 0.087 Uiso 1 1 calc R . . C806 C 0.8994(6) 0.6030(5) 0.1340(4) 0.046(2) Uani 1 1 d . . . C807 C 0.9762(6) 0.6027(5) 0.1508(4) 0.047(3) Uani 1 1 d . . . C808 C 1.0137(7) 0.5431(6) 0.1518(6) 0.076(4) Uani 1 1 d . . . H808 H 0.9923 0.5006 0.1378 0.092 Uiso 1 1 calc R . . C809 C 1.0817(8) 0.5466(8) 0.1734(8) 0.102(6) Uani 1 1 d . . . H809 H 1.1072 0.5066 0.1743 0.122 Uiso 1 1 calc R . . C810 C 1.1122(7) 0.6083(7) 0.1935(7) 0.087(5) Uani 1 1 d . . . H810 H 1.1577 0.6104 0.2103 0.104 Uiso 1 1 calc R . . C811 C 1.0764(6) 0.6682(6) 0.1894(5) 0.060(3) Uani 1 1 d . . . H811 H 1.0996 0.7111 0.2004 0.073 Uiso 1 1 calc R . . N812 N 1.0076(4) 0.6655(4) 0.1694(3) 0.0404(19) Uani 1 1 d . . . Ni9 Ni 0.72940(6) 1.17360(6) -0.00121(4) 0.0289(2) Uani 1 1 d . . . O913 O 0.7226(4) 1.2387(4) 0.0724(3) 0.0555(19) Uani 1 1 d . . . N901 N 0.7055(5) 1.2570(5) -0.0502(4) 0.057(2) Uani 1 1 d . . . C902 C 0.7524(8) 1.3014(8) -0.0725(7) 0.097(5) Uani 1 1 d . . . H902 H 0.8011 1.2995 -0.0635 0.117 Uiso 1 1 calc R . . C903 C 0.7313(12) 1.3523(11) -0.1100(10) 0.177(11) Uani 1 1 d . . . H903 H 0.7650 1.3827 -0.1271 0.212 Uiso 1 1 calc R . . C904 C 0.6591(13) 1.3548(14) -0.1199(13) 0.236(18) Uani 1 1 d . . . H904 H 0.6430 1.3880 -0.1438 0.283 Uiso 1 1 calc R . . C905 C 0.6132(9) 1.3121(11) -0.0968(10) 0.154(10) Uani 1 1 d . . . H905 H 0.5644 1.3162 -0.1036 0.184 Uiso 1 1 calc R . . C906 C 0.6336(7) 1.2596(8) -0.0616(6) 0.078(4) Uani 1 1 d . . . C907 C 0.5852(6) 1.2056(7) -0.0376(4) 0.058(3) Uani 1 1 d . . . C908 C 0.5107(7) 1.1999(9) -0.0448(6) 0.093(5) Uani 1 1 d . . . H908 H 0.4891 1.2329 -0.0661 0.112 Uiso 1 1 calc R . . C909 C 0.4691(6) 1.1486(9) -0.0222(7) 0.092(5) Uani 1 1 d . . . H909 H 0.4191 1.1464 -0.0261 0.111 Uiso 1 1 calc R . . C910 C 0.5026(6) 1.1000(8) 0.0065(7) 0.087(5) Uani 1 1 d . . . H910 H 0.4758 1.0617 0.0207 0.105 Uiso 1 1 calc R . . C911 C 0.5766(6) 1.1074(7) 0.0149(5) 0.069(4) Uani 1 1 d . . . H911 H 0.5984 1.0751 0.0366 0.082 Uiso 1 1 calc R . . N912 N 0.6176(4) 1.1593(4) -0.0073(3) 0.044(2) Uani 1 1 d . . . Ni10 Ni 0.73455(6) 0.81214(6) -0.08811(5) 0.0316(3) Uani 1 1 d . . . O113 O 0.7392(4) 0.7611(4) -0.1682(3) 0.060(2) Uani 1 1 d . . . N101 N 0.6309(4) 0.8359(5) -0.1112(4) 0.049(2) Uani 1 1 d . . . C102 C 0.6139(6) 0.8961(7) -0.1348(6) 0.075(4) Uani 1 1 d . . . H102 H 0.6491 0.9329 -0.1376 0.090 Uiso 1 1 calc R . . C103 C 0.5450(8) 0.9037(8) -0.1547(8) 0.113(6) Uani 1 1 d . . . H103 H 0.5335 0.9452 -0.1709 0.136 Uiso 1 1 calc R . . C104 C 0.4939(8) 0.8488(10) -0.1502(8) 0.116(6) Uani 1 1 d . . . H104 H 0.4472 0.8531 -0.1634 0.139 Uiso 1 1 calc R . . C105 C 0.5106(6) 0.7888(9) -0.1268(7) 0.091(5) Uani 1 1 d . . . H105 H 0.4759 0.7513 -0.1247 0.109 Uiso 1 1 calc R . . C106 C 0.5797(5) 0.7831(6) -0.1060(5) 0.055(3) Uani 1 1 d . . . C107 C 0.6027(5) 0.7209(6) -0.0777(5) 0.054(3) Uani 1 1 d . . . C108 C 0.5591(7) 0.6600(8) -0.0681(7) 0.095(5) Uani 1 1 d . . . H108 H 0.5109 0.6570 -0.0796 0.114 Uiso 1 1 calc R . . C109 C 0.5852(10) 0.6073(9) -0.0432(8) 0.123(7) Uani 1 1 d . . . H109 H 0.5553 0.5671 -0.0374 0.147 Uiso 1 1 calc R . . C110 C 0.6551(10) 0.6102(9) -0.0258(8) 0.124(7) Uani 1 1 d . . . H110 H 0.6733 0.5732 -0.0070 0.149 Uiso 1 1 calc R . . C111 C 0.6985(7) 0.6699(7) -0.0370(6) 0.077(4) Uani 1 1 d . . . H111 H 0.7469 0.6723 -0.0263 0.093 Uiso 1 1 calc R . . N112 N 0.6728(5) 0.7236(4) -0.0624(3) 0.048(2) Uani 1 1 d . . . O1W O 1.0989(5) 0.9676(5) 0.4284(4) 0.079(3) Uiso 0.85 1 d P . . O2W O 0.4755(6) 0.0407(6) 0.3897(4) 0.079(3) Uiso 0.85 1 d P . . O3W O 0.9580(4) 0.5514(4) 0.6443(3) 0.0586(19) Uiso 1 1 d . . . O4W O 0.8000(7) 0.9400(7) 0.5157(5) 0.077(3) Uiso 0.70 1 d P . . O5W O 1.0546(5) 0.7890(5) 0.3147(4) 0.073(3) Uiso 0.90 1 d P . . O6W O 0.7893(4) 0.7969(4) 0.2905(3) 0.072(2) Uiso 1 1 d . . . O7W O 0.6100(8) 0.6550(8) 0.1739(6) 0.071(4) Uiso 0.55 1 d P . . O8W O 0.0662(5) 0.8191(5) 0.4285(4) 0.071(3) Uiso 0.90 1 d P . . O9W O 0.6369(5) 0.3439(5) 0.0843(4) 0.080(3) Uiso 0.95 1 d P . . O10W O 0.1373(9) 0.6543(10) 0.3214(7) 0.087(5) Uiso 0.60 1 d P . . O11W O 0.1323(6) 0.2743(6) 0.2372(5) 0.072(3) Uiso 0.70 1 d P . . O12W O 0.2347(13) 0.4964(13) 0.2578(10) 0.093(9) Uiso 0.50 1 d P . . O13W O 0.2436(14) 0.4586(15) 0.1515(11) 0.071(8) Uiso 0.30 1 d P . . O14W O 0.605(3) 0.445(3) 0.016(2) 0.074(16) Uiso 0.15 1 d P . . O15W O 0.2267(19) 0.514(2) 0.2754(19) 0.047(9) Uiso 0.25 1 d P . . O16W O 0.681(3) 0.440(3) 0.007(2) 0.060(13) Uiso 0.15 1 d P . . O17W O 0.832(5) 0.507(5) -0.043(4) 0.07(3) Uiso 0.10 1 d P . . O18W O 0.811(5) 0.475(5) -0.036(3) 0.06(2) Uiso 0.10 1 d P . . O19W O 0.585(2) 0.508(2) 0.0859(17) 0.074(12) Uiso 0.20 1 d P . . O20W O 0.519(3) 0.554(3) 0.066(2) 0.064(14) Uiso 0.15 1 d P . . O21W O 0.1474(11) 0.6867(12) 0.3362(9) 0.059(6) Uiso 0.40 1 d P . . O22W O 0.225(3) 0.529(3) 0.300(3) 0.08(2) Uiso 0.15 1 d P . . O23W O 0.014(2) 0.309(2) 0.2901(19) 0.084(13) Uiso 0.20 1 d P . . O24W O 0.857(4) 0.454(3) -0.024(3) 0.083(18) Uiso 0.15 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01947(15) 0.02290(19) 0.01854(15) -0.00217(12) 0.00298(12) 0.00411(12) C11 0.016(4) 0.021(5) 0.030(5) 0.002(3) 0.005(3) 0.004(3) N11 0.031(4) 0.026(4) 0.020(4) -0.001(3) 0.005(3) 0.009(3) C12 0.021(4) 0.019(5) 0.036(5) 0.007(3) -0.001(4) -0.003(3) N12 0.024(4) 0.025(4) 0.043(4) 0.004(3) 0.007(3) 0.003(3) C13 0.031(4) 0.026(5) 0.026(4) -0.001(3) 0.009(4) -0.001(4) N13 0.036(4) 0.029(5) 0.036(4) 0.001(3) 0.008(3) 0.006(3) C14 0.033(5) 0.025(5) 0.030(4) -0.002(4) 0.006(4) 0.009(4) N14 0.037(4) 0.025(4) 0.038(4) 0.001(3) 0.010(3) 0.009(3) C15 0.026(4) 0.022(5) 0.026(4) -0.004(3) 0.002(3) 0.001(3) N15 0.022(4) 0.030(4) 0.038(4) -0.002(3) 0.009(3) -0.002(3) C16 0.035(5) 0.032(6) 0.034(5) 0.001(4) 0.008(4) 0.004(4) N16 0.056(6) 0.069(7) 0.040(5) -0.007(4) 0.016(4) 0.020(5) C17 0.068(8) 0.115(12) 0.059(8) -0.049(8) 0.035(7) -0.038(8) N17 0.110(11) 0.26(2) 0.090(9) -0.105(11) 0.041(8) -0.112(12) C18 0.114(10) 0.078(9) 0.026(5) 0.010(5) 0.005(6) 0.064(8) N18 0.225(17) 0.129(12) 0.057(7) 0.043(8) 0.044(9) 0.119(12) W2 0.01499(15) 0.02206(19) 0.02282(16) 0.00236(12) 0.00626(12) 0.00556(12) C21 0.023(4) 0.026(5) 0.023(4) -0.002(3) 0.004(3) 0.001(3) N21 0.019(3) 0.028(4) 0.029(4) 0.003(3) 0.001(3) 0.005(3) C22 0.016(4) 0.031(5) 0.026(4) 0.000(4) -0.003(3) 0.000(3) N22 0.032(4) 0.027(5) 0.032(4) 0.002(3) -0.003(3) 0.006(3) C23 0.024(4) 0.024(5) 0.028(4) 0.002(3) 0.009(3) 0.006(3) N23 0.029(4) 0.033(4) 0.031(4) 0.009(3) 0.011(3) 0.010(3) C24 0.025(4) 0.025(5) 0.033(5) 0.006(4) 0.013(4) 0.005(4) N24 0.030(4) 0.029(4) 0.032(4) -0.004(3) 0.010(3) -0.002(3) C25 0.028(4) 0.028(5) 0.025(4) 0.003(4) 0.008(3) 0.009(4) N25 0.036(4) 0.032(5) 0.034(4) 0.014(3) 0.009(3) 0.007(3) C26 0.028(4) 0.029(5) 0.038(5) 0.007(4) 0.014(4) 0.016(4) N26 0.060(6) 0.044(6) 0.060(6) 0.007(4) 0.023(4) 0.026(5) C27 0.021(4) 0.044(6) 0.055(6) 0.004(5) -0.014(4) 0.015(4) N27 0.053(6) 0.066(7) 0.096(8) -0.004(6) -0.024(6) 0.019(5) C28 0.023(4) 0.050(6) 0.046(5) 0.011(4) 0.019(4) 0.014(4) N28 0.043(5) 0.078(7) 0.074(6) 0.022(5) 0.036(5) 0.023(5) W3 0.01833(15) 0.01629(18) 0.02519(16) 0.00245(12) 0.00516(12) 0.00178(12) C31 0.020(4) 0.010(5) 0.028(4) -0.002(3) 0.004(3) 0.003(3) N31 0.019(3) 0.021(4) 0.033(4) 0.000(3) 0.004(3) 0.003(3) C32 0.027(4) 0.019(5) 0.036(5) 0.003(4) -0.003(4) -0.002(3) N32 0.028(4) 0.022(4) 0.045(4) 0.001(3) -0.004(3) 0.000(3) C33 0.026(4) 0.015(5) 0.033(5) 0.005(3) 0.003(4) 0.003(3) N33 0.029(4) 0.030(5) 0.046(5) 0.002(3) 0.004(4) 0.002(3) C34 0.030(4) 0.017(5) 0.034(5) -0.003(3) 0.014(4) 0.004(3) N34 0.039(4) 0.032(5) 0.033(4) 0.001(3) 0.014(3) 0.003(3) C35 0.021(4) 0.023(5) 0.028(4) 0.004(3) 0.007(3) -0.005(3) N35 0.030(4) 0.031(4) 0.032(4) -0.003(3) 0.009(3) 0.004(3) C36 0.037(5) 0.024(6) 0.074(7) 0.019(5) -0.014(5) 0.003(4) N36 0.069(7) 0.053(7) 0.138(11) 0.030(7) -0.025(7) 0.012(5) C37 0.031(5) 0.014(5) 0.071(7) -0.002(4) 0.020(5) -0.003(4) N37 0.051(6) 0.035(6) 0.113(8) 0.001(5) 0.042(6) -0.002(4) C38 0.049(6) 0.022(6) 0.046(6) -0.004(4) -0.002(5) -0.001(4) N38 0.089(7) 0.037(6) 0.071(7) -0.018(5) 0.000(6) 0.002(5) W4 0.02086(16) 0.02374(19) 0.02054(16) 0.00179(12) 0.00090(12) 0.00526(13) C41 0.025(4) 0.023(5) 0.022(4) 0.003(3) 0.004(3) 0.005(3) N41 0.031(4) 0.032(4) 0.022(4) 0.005(3) -0.001(3) 0.004(3) C42 0.035(5) 0.040(6) 0.023(4) 0.007(4) 0.010(4) 0.009(4) N42 0.032(4) 0.043(5) 0.045(5) 0.008(4) 0.018(3) 0.017(4) C43 0.026(4) 0.023(5) 0.024(4) 0.002(3) -0.004(3) 0.001(4) N43 0.038(4) 0.033(5) 0.036(4) 0.002(3) 0.000(3) 0.002(4) C44 0.025(4) 0.042(6) 0.032(5) 0.004(4) -0.002(4) 0.014(4) N44 0.035(4) 0.047(5) 0.035(4) -0.002(4) 0.004(3) 0.017(4) C45 0.016(4) 0.042(6) 0.034(5) -0.005(4) 0.007(3) 0.003(4) N45 0.032(4) 0.031(5) 0.041(4) 0.002(3) 0.006(3) -0.001(3) C46 0.022(4) 0.044(6) 0.034(5) 0.004(4) -0.006(4) -0.005(4) N46 0.050(5) 0.056(6) 0.055(6) 0.015(4) -0.010(4) -0.004(4) C47 0.035(5) 0.029(6) 0.045(5) 0.017(4) -0.002(4) 0.016(4) N47 0.068(6) 0.046(6) 0.078(7) 0.013(5) -0.021(5) 0.015(5) C48 0.040(5) 0.046(6) 0.025(5) -0.002(4) 0.002(4) 0.003(4) N48 0.054(6) 0.093(8) 0.035(5) 0.004(5) 0.009(4) 0.004(5) W5 0.03623(19) 0.0203(2) 0.02734(18) -0.00115(13) 0.00385(14) 0.00696(14) C51 0.045(5) 0.040(6) 0.023(5) -0.006(4) 0.004(4) 0.004(4) N51 0.065(5) 0.026(5) 0.029(4) 0.000(3) 0.008(4) 0.005(4) C52 0.031(5) 0.031(6) 0.023(4) 0.002(4) 0.001(3) 0.009(4) N52 0.027(4) 0.029(5) 0.034(4) -0.003(3) 0.005(3) 0.002(3) C53 0.030(5) 0.032(5) 0.031(5) 0.001(4) 0.001(4) 0.003(4) N53 0.036(4) 0.041(5) 0.034(4) 0.006(3) 0.009(3) -0.002(3) C54 0.037(5) 0.032(6) 0.037(5) -0.001(4) 0.016(4) 0.011(4) N54 0.032(4) 0.040(5) 0.049(5) -0.003(4) 0.005(4) 0.009(4) C55 0.030(5) 0.038(6) 0.042(5) -0.001(4) -0.002(4) -0.001(4) N55 0.040(5) 0.036(5) 0.046(5) 0.002(4) -0.005(4) -0.005(4) C56 0.087(9) 0.048(8) 0.074(8) -0.027(6) -0.014(7) 0.001(6) N56 0.174(14) 0.071(9) 0.133(12) -0.067(8) -0.068(11) 0.020(9) W6 0.01802(15) 0.0254(2) 0.02466(16) 0.00419(13) 0.00829(13) 0.00438(13) C61 0.014(4) 0.036(5) 0.025(4) 0.001(3) 0.009(3) 0.007(3) N61 0.025(4) 0.033(4) 0.028(4) 0.002(3) 0.008(3) 0.005(3) C62 0.033(5) 0.028(5) 0.025(4) 0.002(4) 0.009(4) 0.007(4) N62 0.040(4) 0.040(5) 0.031(4) -0.005(3) 0.006(3) 0.006(4) C63 0.018(4) 0.037(6) 0.028(4) 0.006(4) 0.008(3) 0.005(4) N63 0.033(4) 0.035(5) 0.041(4) 0.010(3) 0.008(3) 0.005(3) C64 0.022(4) 0.029(5) 0.028(4) 0.006(4) 0.005(3) 0.014(3) N64 0.032(4) 0.031(5) 0.041(4) 0.014(4) 0.002(3) 0.011(3) C65 0.026(4) 0.033(5) 0.032(5) 0.007(4) 0.010(4) -0.003(4) N65 0.035(4) 0.037(5) 0.039(5) -0.002(4) 0.005(3) 0.000(3) C66 0.026(5) 0.039(6) 0.045(5) 0.010(4) 0.009(4) -0.005(4) N66 0.042(5) 0.045(6) 0.081(7) 0.016(5) 0.016(5) -0.009(4) C67 0.054(6) 0.029(6) 0.032(5) 0.005(4) 0.017(4) 0.002(4) N67 0.126(9) 0.058(7) 0.040(5) 0.015(4) 0.036(6) 0.015(6) C68 0.029(5) 0.068(8) 0.076(8) 0.040(6) 0.026(5) 0.018(5) N68 0.047(6) 0.115(10) 0.155(12) 0.072(9) 0.053(7) 0.040(6) Ni1 0.0135(6) 0.0171(8) 0.0173(6) 0.0009(5) 0.0045(5) 0.0027(5) Ni2 0.0204(5) 0.0259(6) 0.0294(5) -0.0005(4) 0.0006(4) 0.0001(4) O213 0.038(4) 0.050(4) 0.042(4) 0.012(3) -0.005(3) 0.006(3) N201 0.028(4) 0.049(6) 0.034(4) 0.010(4) 0.002(3) -0.003(4) C202 0.033(5) 0.061(7) 0.047(6) 0.002(5) 0.009(5) 0.003(5) C203 0.038(6) 0.125(13) 0.051(7) 0.014(7) 0.015(5) -0.013(7) C204 0.062(9) 0.104(12) 0.077(9) 0.000(8) 0.021(7) -0.042(8) C205 0.073(8) 0.056(8) 0.070(8) -0.002(6) 0.017(7) -0.044(7) C206 0.045(6) 0.045(7) 0.037(5) 0.005(4) -0.007(4) -0.017(5) C207 0.048(6) 0.031(6) 0.039(5) -0.007(4) -0.008(4) -0.007(4) C208 0.091(9) 0.045(8) 0.055(7) -0.005(5) -0.009(7) -0.019(6) C209 0.114(11) 0.018(7) 0.076(8) -0.016(5) -0.013(8) 0.016(7) C210 0.080(9) 0.041(8) 0.083(9) -0.024(6) 0.012(7) 0.018(6) C211 0.054(7) 0.063(8) 0.045(6) -0.009(5) 0.010(5) 0.002(5) N212 0.042(4) 0.027(4) 0.035(4) -0.003(3) -0.002(3) 0.002(3) Ni3 0.0246(5) 0.0229(6) 0.0243(5) 0.0059(4) 0.0048(4) 0.0069(4) O313 0.033(3) 0.038(4) 0.036(3) 0.006(3) -0.009(3) 0.006(3) N301 0.034(4) 0.029(5) 0.039(4) 0.012(3) 0.006(3) 0.012(3) C302 0.048(6) 0.038(6) 0.050(6) -0.003(4) 0.020(5) 0.010(5) C303 0.076(8) 0.041(7) 0.065(7) -0.005(5) 0.025(6) 0.019(6) C304 0.091(9) 0.039(7) 0.063(7) -0.012(6) -0.009(7) 0.031(6) C305 0.065(7) 0.028(6) 0.053(6) 0.005(5) -0.005(5) 0.000(5) C306 0.042(5) 0.024(6) 0.036(5) 0.008(4) -0.001(4) 0.007(4) C307 0.050(6) 0.030(6) 0.050(6) 0.015(4) 0.013(5) 0.003(4) C308 0.106(11) 0.051(9) 0.133(13) 0.056(8) 0.066(10) 0.020(8) C309 0.21(2) 0.093(14) 0.22(2) 0.090(15) 0.18(2) 0.044(14) C310 0.20(2) 0.096(14) 0.21(2) 0.073(14) 0.173(18) 0.059(14) C311 0.133(13) 0.062(9) 0.103(11) 0.023(8) 0.083(10) 0.034(9) N312 0.045(5) 0.048(6) 0.040(4) 0.015(4) 0.019(4) 0.013(4) Ni4 0.0288(5) 0.0206(6) 0.0270(5) -0.0014(4) 0.0075(4) 0.0071(4) O413 0.055(4) 0.041(4) 0.062(5) -0.005(3) -0.010(4) -0.005(3) N401 0.041(4) 0.031(5) 0.030(4) 0.000(3) 0.010(3) 0.017(3) C402 0.052(6) 0.054(7) 0.034(5) 0.005(5) 0.009(4) 0.023(5) C403 0.063(7) 0.078(9) 0.035(6) 0.013(5) 0.020(5) 0.030(6) C404 0.072(8) 0.083(9) 0.035(6) -0.012(6) 0.021(5) 0.023(7) C405 0.061(7) 0.056(8) 0.057(7) -0.017(6) 0.018(6) 0.026(6) C406 0.037(5) 0.041(6) 0.037(5) -0.004(4) 0.008(4) 0.016(4) C407 0.041(5) 0.015(5) 0.046(5) -0.004(4) 0.010(4) 0.007(4) C408 0.067(8) 0.040(7) 0.073(8) -0.004(6) 0.014(6) 0.021(6) C409 0.074(8) 0.036(7) 0.082(9) 0.019(6) 0.003(7) 0.016(6) C410 0.059(7) 0.051(8) 0.071(8) 0.028(6) 0.013(6) 0.015(6) C411 0.060(7) 0.032(6) 0.042(6) 0.010(4) 0.011(5) 0.009(5) N412 0.032(4) 0.027(4) 0.032(4) 0.001(3) 0.000(3) 0.006(3) Ni5 0.0208(5) 0.0259(6) 0.0247(5) 0.0023(4) 0.0084(4) 0.0022(4) O513 0.052(4) 0.051(5) 0.039(4) 0.016(3) 0.013(3) 0.004(3) N501 0.019(3) 0.037(5) 0.031(4) 0.004(3) 0.007(3) 0.002(3) C502 0.034(5) 0.051(7) 0.047(6) -0.003(5) 0.004(4) 0.001(5) C503 0.052(7) 0.042(7) 0.065(7) 0.006(5) -0.014(6) 0.001(5) C504 0.032(6) 0.074(9) 0.078(8) 0.007(7) -0.009(6) -0.003(6) C505 0.029(5) 0.059(8) 0.074(8) 0.013(6) 0.003(5) 0.013(5) C506 0.023(4) 0.043(6) 0.036(5) 0.014(4) 0.008(4) 0.000(4) C507 0.032(5) 0.049(6) 0.036(5) 0.007(4) 0.004(4) 0.011(4) C508 0.049(6) 0.069(8) 0.050(6) 0.000(6) 0.016(5) 0.026(6) C509 0.069(8) 0.063(8) 0.064(7) -0.009(6) 0.030(6) 0.027(6) C510 0.071(9) 0.064(9) 0.071(8) -0.019(6) 0.025(7) 0.009(6) C511 0.041(6) 0.049(7) 0.049(6) -0.014(5) 0.015(5) 0.003(5) N512 0.033(4) 0.035(5) 0.038(4) -0.003(3) 0.010(3) 0.005(3) Ni6 0.0152(6) 0.0194(8) 0.0179(7) 0.0015(5) 0.0045(5) 0.0034(5) Ni7 0.0305(6) 0.0322(7) 0.0228(5) -0.0025(4) 0.0067(4) 0.0089(5) O713 0.061(5) 0.086(6) 0.041(4) -0.013(4) -0.007(4) -0.012(4) N701 0.041(5) 0.053(6) 0.034(4) -0.004(4) 0.007(4) 0.014(4) C702 0.089(9) 0.060(8) 0.059(7) -0.005(6) 0.015(6) 0.048(7) C703 0.105(11) 0.081(10) 0.067(9) -0.028(7) 0.009(8) 0.051(8) C704 0.076(9) 0.089(11) 0.067(9) -0.037(7) 0.018(7) 0.034(8) C705 0.056(7) 0.102(11) 0.033(6) -0.021(6) 0.013(5) 0.022(7) C706 0.027(5) 0.085(9) 0.025(5) -0.014(5) 0.006(4) 0.013(5) C707 0.039(5) 0.062(7) 0.029(5) 0.015(5) 0.007(4) 0.000(5) C708 0.070(9) 0.112(13) 0.071(9) 0.027(8) 0.040(7) 0.024(8) C709 0.110(12) 0.100(13) 0.098(11) 0.069(10) 0.056(10) 0.032(10) C710 0.085(9) 0.057(9) 0.109(11) 0.041(8) 0.041(9) 0.028(7) C711 0.043(6) 0.073(9) 0.072(8) 0.026(7) 0.019(6) 0.014(6) N712 0.040(4) 0.045(6) 0.041(5) 0.018(4) 0.007(4) 0.010(4) Ni8 0.0276(5) 0.0246(6) 0.0314(6) 0.0066(4) 0.0054(4) 0.0036(4) O813 0.059(4) 0.049(4) 0.037(4) 0.012(3) 0.011(3) 0.006(3) N801 0.044(5) 0.032(5) 0.042(4) 0.007(3) 0.008(4) -0.007(4) C802 0.030(5) 0.063(8) 0.067(7) 0.010(6) -0.006(5) -0.009(5) C803 0.049(7) 0.084(11) 0.101(11) -0.001(8) -0.015(7) -0.015(7) C804 0.092(11) 0.067(11) 0.110(12) -0.016(8) -0.021(9) -0.039(9) C805 0.079(9) 0.041(8) 0.095(10) -0.010(6) -0.016(8) -0.009(6) C806 0.055(6) 0.036(7) 0.044(6) 0.002(4) 0.005(5) -0.009(5) C807 0.054(6) 0.031(6) 0.059(7) 0.012(5) 0.016(5) 0.008(5) C808 0.076(9) 0.035(8) 0.118(12) -0.004(7) 0.000(8) 0.009(6) C809 0.071(10) 0.044(9) 0.194(18) 0.003(10) 0.000(11) 0.031(7) C810 0.058(8) 0.060(10) 0.144(14) 0.004(9) -0.014(8) 0.029(7) C811 0.041(6) 0.047(7) 0.093(9) -0.001(6) -0.018(6) 0.010(5) N812 0.041(5) 0.032(5) 0.049(5) 0.009(4) 0.001(4) 0.010(4) Ni9 0.0269(5) 0.0322(7) 0.0295(6) 0.0046(5) 0.0084(4) 0.0121(5) O913 0.060(5) 0.071(5) 0.040(4) -0.005(3) 0.014(3) 0.029(4) N901 0.058(6) 0.053(6) 0.065(6) 0.028(5) 0.016(5) 0.024(5) C902 0.068(9) 0.088(11) 0.141(14) 0.070(10) 0.021(9) 0.019(8) C903 0.134(18) 0.16(2) 0.25(3) 0.17(2) 0.056(17) 0.034(15) C904 0.120(18) 0.22(3) 0.38(4) 0.26(3) 0.02(2) 0.074(18) C905 0.079(11) 0.144(18) 0.25(2) 0.144(18) 0.008(13) 0.035(11) C906 0.063(8) 0.098(11) 0.081(9) 0.048(8) 0.003(7) 0.039(7) C907 0.040(6) 0.088(9) 0.049(6) 0.012(6) -0.002(5) 0.031(6) C908 0.045(8) 0.136(14) 0.104(11) 0.030(10) -0.019(8) 0.037(8) C909 0.023(6) 0.130(14) 0.123(13) -0.003(11) 0.009(7) 0.003(8) C910 0.035(7) 0.077(10) 0.148(14) 0.002(9) 0.014(8) -0.004(6) C911 0.038(6) 0.081(10) 0.088(9) 0.014(7) 0.021(6) 0.003(6) N912 0.028(4) 0.055(6) 0.053(5) 0.001(4) 0.010(4) 0.017(4) Ni10 0.0285(6) 0.0298(7) 0.0354(6) -0.0003(5) -0.0003(5) -0.0040(5) O113 0.068(5) 0.059(5) 0.050(4) -0.014(4) 0.000(4) -0.008(4) N101 0.035(5) 0.049(6) 0.062(6) 0.011(4) 0.002(4) -0.005(4) C102 0.047(7) 0.066(9) 0.113(11) 0.023(8) 0.000(7) 0.012(6) C103 0.062(9) 0.075(11) 0.20(2) 0.044(12) -0.032(11) 0.000(8) C104 0.046(8) 0.118(15) 0.183(19) 0.029(13) -0.034(10) 0.010(9) C105 0.029(6) 0.103(12) 0.138(14) 0.025(10) -0.018(7) -0.011(7) C106 0.035(6) 0.070(8) 0.057(7) -0.006(6) 0.000(5) -0.010(5) C107 0.031(5) 0.067(8) 0.062(7) 0.002(6) 0.004(5) -0.020(5) C108 0.058(8) 0.094(12) 0.126(13) 0.024(10) -0.009(8) -0.042(8) C109 0.107(14) 0.097(14) 0.159(17) 0.077(13) -0.013(12) -0.051(11) C110 0.114(14) 0.090(13) 0.165(18) 0.078(12) -0.031(13) -0.035(11) C111 0.075(9) 0.062(9) 0.091(10) 0.030(8) -0.017(7) -0.025(7) N112 0.055(5) 0.039(5) 0.049(5) 0.006(4) -0.003(4) -0.008(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C17 2.130(12) . ? W1 C15 2.160(8) . ? W1 C13 2.167(9) . ? W1 C11 2.173(8) . ? W1 C14 2.175(9) . ? W1 C12 2.183(8) . ? W1 C18 2.183(11) . ? W1 C16 2.184(8) . ? C11 N11 1.137(9) . ? N11 Ni1 2.055(6) . ? C12 N12 1.136(9) . ? N12 Ni2 2.082(7) 2_666 ? C13 N13 1.150(10) . ? N13 Ni3 2.084(7) . ? C14 N14 1.133(10) . ? N14 Ni4 2.080(8) . ? C15 N15 1.134(10) . ? N15 Ni5 2.062(7) . ? C16 N16 1.137(11) . ? C17 N17 1.160(14) . ? C18 N18 1.114(14) . ? W2 C21 2.142(8) . ? W2 C28 2.151(8) . ? W2 C27 2.153(9) . ? W2 C23 2.163(8) . ? W2 C22 2.172(9) . ? W2 C26 2.181(9) . ? W2 C24 2.183(9) . ? W2 C25 2.190(8) . ? C21 N21 1.154(9) . ? N21 Ni1 2.051(6) . ? C22 N22 1.137(10) . ? N22 Ni2 2.057(7) . ? C23 N23 1.140(9) 2_666 ? N23 C23 1.140(9) 2_666 ? N23 Ni3 2.055(7) . ? C24 N24 1.146(10) . ? N24 Ni4 2.080(7) . ? C25 N25 1.119(10) . ? N25 Ni5 2.095(7) . ? C26 N26 1.146(11) . ? C27 N27 1.131(11) . ? C28 N28 1.162(11) . ? W3 C36 2.140(9) . ? W3 C37 2.145(8) . ? W3 C31 2.149(8) . ? W3 C34 2.151(8) . ? W3 C35 2.154(8) . ? W3 C32 2.157(9) . ? W3 C38 2.166(9) . ? W3 C33 2.171(9) . ? C31 N31 1.153(9) . ? N31 Ni1 2.042(7) . ? C32 N32 1.150(10) . ? N32 Ni2 2.063(7) . ? C33 N33 1.139(10) . ? N33 Ni3 2.079(8) . ? C34 N34 1.149(9) . ? N34 Ni4 2.042(7) 2_666 ? C35 N35 1.136(10) . ? N35 Ni5 2.064(7) . ? C36 N36 1.167(12) . ? C37 N37 1.161(11) . ? C38 N38 1.148(11) . ? W4 C46 2.145(8) . ? W4 C48 2.154(8) . ? W4 C43 2.158(8) . ? W4 C41 2.163(8) . ? W4 C42 2.166(9) . ? W4 C44 2.168(9) . ? W4 C47 2.180(9) . ? W4 C45 2.184(10) . ? C41 N41 1.140(9) . ? N41 Ni6 2.061(7) . ? C42 N42 1.142(10) . ? N42 Ni7 2.045(7) . ? C43 N43 1.138(10) . ? N43 Ni8 2.074(8) . ? C44 N44 1.144(10) 2_775 ? N44 C44 1.144(10) 2_775 ? N44 Ni9 2.047(7) . ? C45 N45 1.138(11) 2_775 ? N45 C45 1.138(11) 2_775 ? N45 Ni10 2.049(8) . ? C46 N46 1.151(11) . ? C47 N47 1.113(11) 1_655 ? N47 C47 1.113(11) 1_455 ? C48 N48 1.144(11) . ? W5 C57A 2.12(3) . ? W5 C58B 2.14(4) . ? W5 C52 2.144(9) . ? W5 C56 2.147(11) . ? W5 C54 2.157(10) 2_775 ? W5 C55 2.158(9) . ? W5 C51 2.163(9) . ? W5 C53 2.169(9) . ? W5 C58A 2.18(3) . ? W5 C57B 2.19(3) . ? C51 N51 1.132(11) . ? N51 Ni7 2.052(8) 2_775 ? C52 N52 1.145(10) . ? N52 Ni6 2.019(7) . ? C53 N53 1.132(10) . ? N53 Ni8 2.094(7) . ? C54 N54 1.147(11) . ? C54 W5 2.157(10) 2_775 ? N54 Ni9 2.078(8) . ? C55 N55 1.153(11) . ? N55 Ni10 2.079(8) . ? C56 N56 1.152(14) . ? C57A N57A 1.21(3) . ? C57B N57B 1.24(3) . ? C58A N58A 1.15(4) . ? C58B N58B 1.28(5) . ? W6 C63 2.141(8) . ? W6 C68 2.151(9) . ? W6 C62 2.163(9) . ? W6 C65 2.166(9) . ? W6 C67 2.174(9) . ? W6 C61 2.174(7) . ? W6 C64 2.187(9) . ? W6 C66 2.200(9) . ? C61 N61 1.125(9) . ? N61 Ni6 2.068(6) . ? C62 N62 1.150(10) . ? N62 Ni7 2.076(8) . ? C63 N63 1.170(10) . ? N63 Ni8 2.048(8) . ? C64 N64 1.122(10) . ? N64 Ni9 2.069(7) . ? C65 N65 1.146(10) . ? N65 Ni10 2.092(8) . ? C66 N66 1.121(11) . ? C67 N67 1.124(11) . ? C68 N68 1.116(12) . ? Ni1 N31 2.042(7) 2_666 ? Ni1 N21 2.051(6) 2_666 ? Ni1 N11 2.055(6) 2_666 ? Ni2 N201 2.068(7) . ? Ni2 N12 2.082(7) 2_666 ? Ni2 N212 2.091(7) . ? Ni2 O213 2.145(6) . ? N201 C202 1.340(12) . ? N201 C206 1.370(12) . ? C202 C203 1.385(14) . ? C202 H202 0.9300 . ? C203 C204 1.387(19) . ? C203 H203 0.9300 . ? C204 C205 1.311(18) . ? C204 H204 0.9300 . ? C205 C206 1.406(13) . ? C205 H205 0.9300 . ? C206 C207 1.464(14) . ? C207 N212 1.339(11) . ? C207 C208 1.387(15) . ? C208 C209 1.402(17) . ? C208 H208 0.9300 . ? C209 C210 1.333(17) . ? C209 H209 0.9300 . ? C210 C211 1.373(15) . ? C210 H210 0.9300 . ? C211 N212 1.338(12) . ? C211 H211 0.9300 . ? Ni3 N312 2.083(7) . ? Ni3 N301 2.088(7) . ? Ni3 O313 2.116(6) . ? N301 C302 1.335(11) . ? N301 C306 1.344(11) . ? C302 C303 1.398(14) . ? C302 H302 0.9300 . ? C303 C304 1.387(16) . ? C303 H303 0.9300 . ? C304 C305 1.366(15) . ? C304 H304 0.9300 . ? C305 C306 1.365(13) . ? C305 H305 0.9300 . ? C306 C307 1.480(13) . ? C307 N312 1.349(12) . ? C307 C308 1.390(14) . ? C308 C309 1.38(2) . ? C308 H308 0.9300 . ? C309 C310 1.32(2) . ? C309 H309 0.9300 . ? C310 C311 1.416(19) . ? C310 H310 0.9300 . ? C311 N312 1.330(13) . ? C311 H311 0.9300 . ? Ni4 N34 2.042(7) 2_666 ? Ni4 N401 2.080(7) . ? Ni4 N412 2.081(7) . ? Ni4 O413 2.181(7) . ? N401 C402 1.347(11) . ? N401 C406 1.354(11) . ? C402 C403 1.340(13) . ? C402 H402 0.9300 . ? C403 C404 1.367(15) . ? C403 H403 0.9300 . ? C404 C405 1.393(15) . ? C404 H404 0.9300 . ? C405 C406 1.374(12) . ? C405 H405 0.9300 . ? C406 C407 1.480(13) . ? C407 N412 1.349(10) . ? C407 C408 1.392(13) . ? C408 C409 1.361(15) . ? C408 H408 0.9300 . ? C409 C410 1.353(16) . ? C409 H409 0.9300 . ? C410 C411 1.375(14) . ? C410 H410 0.9300 . ? C411 N412 1.328(11) . ? C411 H411 0.9300 . ? Ni5 N501 2.072(7) . ? Ni5 N512 2.074(7) . ? Ni5 O513 2.122(6) . ? N501 C502 1.337(11) . ? N501 C506 1.346(11) . ? C502 C503 1.368(13) . ? C502 H502 0.9300 . ? C503 C504 1.363(15) . ? C503 H503 0.9300 . ? C504 C505 1.376(15) . ? C504 H504 0.9300 . ? C505 C506 1.380(13) . ? C505 H505 0.9300 . ? C506 C507 1.496(13) . ? C507 N512 1.333(11) . ? C507 C508 1.406(13) . ? C508 C509 1.367(15) . ? C508 H508 0.9300 . ? C509 C510 1.335(16) . ? C509 H509 0.9300 . ? C510 C511 1.396(14) . ? C510 H510 0.9300 . ? C511 N512 1.337(11) . ? C511 H511 0.9300 . ? Ni6 N52 2.019(7) 2_775 ? Ni6 N41 2.061(7) 2_775 ? Ni6 N61 2.068(6) 2_775 ? Ni7 N51 2.052(8) 2_775 ? Ni7 N701 2.067(7) . ? Ni7 N712 2.098(7) . ? Ni7 O713 2.158(7) . ? N701 C702 1.306(13) . ? N701 C706 1.362(12) . ? C702 C703 1.392(14) . ? C702 H702 0.9300 . ? C703 C704 1.331(18) . ? C703 H703 0.9300 . ? C704 C705 1.358(17) . ? C704 H704 0.9300 . ? C705 C706 1.398(13) . ? C705 H705 0.9300 . ? C706 C707 1.453(15) . ? C707 N712 1.346(12) . ? C707 C708 1.359(15) . ? C708 C709 1.374(19) . ? C708 H708 0.9300 . ? C709 C710 1.322(19) . ? C709 H709 0.9300 . ? C710 C711 1.391(15) . ? C710 H710 0.9300 . ? C711 N712 1.308(13) . ? C711 H711 0.9300 . ? Ni8 N812 2.049(7) . ? Ni8 N801 2.069(7) . ? Ni8 O813 2.148(6) . ? N801 C802 1.336(12) . ? N801 C806 1.351(13) . ? C802 C803 1.377(16) . ? C802 H802 0.9300 . ? C803 C804 1.367(19) . ? C803 H803 0.9300 . ? C804 C805 1.354(18) . ? C804 H804 0.9300 . ? C805 C806 1.377(15) . ? C805 H805 0.9300 . ? C806 C807 1.479(14) . ? C807 N812 1.359(13) . ? C807 C808 1.381(15) . ? C808 C809 1.355(18) . ? C808 H808 0.9300 . ? C809 C810 1.347(19) . ? C809 H809 0.9300 . ? C810 C811 1.370(16) . ? C810 H810 0.9300 . ? C811 N812 1.356(12) . ? C811 H811 0.9300 . ? Ni9 N901 2.075(8) . ? Ni9 N912 2.079(7) . ? Ni9 O913 2.153(7) . ? N901 C902 1.302(15) . ? N901 C906 1.366(14) . ? C902 C903 1.42(2) . ? C902 H902 0.9300 . ? C903 C904 1.36(3) . ? C903 H903 0.9300 . ? C904 C905 1.28(2) . ? C904 H904 0.9300 . ? C905 C906 1.397(18) . ? C905 H905 0.9300 . ? C906 C907 1.456(17) . ? C907 N912 1.331(12) . ? C907 C908 1.391(16) . ? C908 C909 1.337(19) . ? C908 H908 0.9300 . ? C909 C910 1.35(2) . ? C909 H909 0.9300 . ? C910 C911 1.384(16) . ? C910 H910 0.9300 . ? C911 N912 1.334(13) . ? C911 H911 0.9300 . ? Ni10 N101 2.082(8) . ? Ni10 N112 2.087(8) . ? Ni10 O113 2.147(7) . ? N101 C106 1.345(13) . ? N101 C102 1.352(14) . ? C102 C103 1.379(17) . ? C102 H102 0.9300 . ? C103 C104 1.37(2) . ? C103 H103 0.9300 . ? C104 C105 1.34(2) . ? C104 H104 0.9300 . ? C105 C106 1.384(15) . ? C105 H105 0.9300 . ? C106 C107 1.471(16) . ? C107 N112 1.345(12) . ? C107 C108 1.395(16) . ? C108 C109 1.30(2) . ? C108 H108 0.9300 . ? C109 C110 1.36(2) . ? C109 H109 0.9300 . ? C110 C111 1.383(17) . ? C110 H110 0.9300 . ? C111 N112 1.323(14) . ? C111 H111 0.9300 . ? O10W O21W 0.72(2) . ? O12W O15W 0.56(5) . ? O12W O22W 1.22(7) . ? O14W O16W 1.45(7) . ? O15W O22W 0.67(6) . ? O17W O18W 0.71(10) . ? O17W O24W 1.24(11) . ? O18W O24W 1.02(9) . ? O19W O20W 1.63(6) . ? 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 C17 W1 C15 145.4(3) . . ? C17 W1 C13 110.3(5) . . ? C15 W1 C13 85.8(3) . . ? C17 W1 C11 140.9(4) . . ? C15 W1 C11 72.0(3) . . ? C13 W1 C11 74.2(3) . . ? C17 W1 C14 89.2(5) . . ? C15 W1 C14 93.2(3) . . ? C13 W1 C14 146.4(3) . . ? C11 W1 C14 73.6(3) . . ? C17 W1 C12 71.0(4) . . ? C15 W1 C12 143.5(3) . . ? C13 W1 C12 79.6(3) . . ? C11 W1 C12 71.9(3) . . ? C14 W1 C12 81.6(3) . . ? C17 W1 C18 78.3(6) . . ? C15 W1 C18 79.4(4) . . ? C13 W1 C18 69.3(3) . . ? C11 W1 C18 134.8(4) . . ? C14 W1 C18 143.5(3) . . ? C12 W1 C18 124.5(4) . . ? C17 W1 C16 74.5(4) . . ? C15 W1 C16 73.4(3) . . ? C13 W1 C16 138.0(3) . . ? C11 W1 C16 129.2(3) . . ? C14 W1 C16 72.4(3) . . ? C12 W1 C16 136.6(3) . . ? C18 W1 C16 71.2(4) . . ? N11 C11 W1 177.3(7) . . ? C11 N11 Ni1 173.8(7) . . ? N12 C12 W1 177.6(7) . . ? C12 N12 Ni2 176.0(7) . 2_666 ? N13 C13 W1 177.2(7) . . ? C13 N13 Ni3 171.3(7) . . ? N14 C14 W1 176.6(8) . . ? C14 N14 Ni4 175.1(7) . . ? N15 C15 W1 176.3(7) . . ? C15 N15 Ni5 168.7(7) . . ? N16 C16 W1 178.7(9) . . ? N17 C17 W1 175.3(13) . . ? N18 C18 W1 179.7(12) . . ? C21 W2 C28 141.7(3) . . ? C21 W2 C27 133.8(3) . . ? C28 W2 C27 77.4(4) . . ? C21 W2 C23 70.9(3) . . ? C28 W2 C23 146.7(3) . . ? C27 W2 C23 78.5(3) . . ? C21 W2 C22 74.2(3) . . ? C28 W2 C22 107.4(3) . . ? C27 W2 C22 69.3(3) . . ? C23 W2 C22 84.9(3) . . ? C21 W2 C26 129.1(3) . . ? C28 W2 C26 75.7(3) . . ? C27 W2 C26 71.4(3) . . ? C23 W2 C26 75.0(3) . . ? C22 W2 C26 138.6(3) . . ? C21 W2 C24 74.0(3) . . ? C28 W2 C24 90.7(3) . . ? C27 W2 C24 144.1(3) . . ? C23 W2 C24 95.6(3) . . ? C22 W2 C24 146.1(3) . . ? C26 W2 C24 72.9(3) . . ? C21 W2 C25 71.2(3) . . ? C28 W2 C25 71.8(3) . . ? C27 W2 C25 125.7(3) . . ? C23 W2 C25 141.5(3) . . ? C22 W2 C25 78.6(3) . . ? C26 W2 C25 137.1(3) . . ? C24 W2 C25 80.3(3) . . ? N21 C21 W2 176.7(7) . . ? C21 N21 Ni1 174.0(6) . . ? N22 C22 W2 174.2(7) . . ? C22 N22 Ni2 173.5(7) . . ? N23 C23 W2 177.9(8) 2_666 . ? C23 N23 Ni3 169.6(7) 2_666 . ? N24 C24 W2 176.8(7) . . ? C24 N24 Ni4 171.2(6) . . ? N25 C25 W2 177.0(7) . . ? C25 N25 Ni5 169.8(7) . . ? N26 C26 W2 177.6(8) . . ? N27 C27 W2 177.2(9) . . ? N28 C28 W2 179.3(10) . . ? C36 W3 C37 79.2(4) . . ? C36 W3 C31 139.4(3) . . ? C37 W3 C31 135.0(3) . . ? C36 W3 C34 88.0(4) . . ? C37 W3 C34 146.1(3) . . ? C31 W3 C34 72.3(3) . . ? C36 W3 C35 112.4(4) . . ? C37 W3 C35 70.2(3) . . ? C31 W3 C35 72.5(3) . . ? C34 W3 C35 143.1(3) . . ? C36 W3 C32 147.4(3) . . ? C37 W3 C32 81.5(3) . . ? C31 W3 C32 70.9(3) . . ? C34 W3 C32 93.7(3) . . ? C35 W3 C32 84.8(3) . . ? C36 W3 C38 74.1(4) . . ? C37 W3 C38 73.2(4) . . ? C31 W3 C38 129.1(3) . . ? C34 W3 C38 73.1(3) . . ? C35 W3 C38 140.5(3) . . ? C32 W3 C38 75.4(3) . . ? C36 W3 C33 71.0(3) . . ? C37 W3 C33 122.9(3) . . ? C31 W3 C33 71.1(3) . . ? C34 W3 C33 80.8(3) . . ? C35 W3 C33 77.9(3) . . ? C32 W3 C33 141.4(3) . . ? C38 W3 C33 136.6(3) . . ? N31 C31 W3 178.0(6) . . ? C31 N31 Ni1 170.5(6) . . ? N32 C32 W3 174.9(7) . . ? C32 N32 Ni2 173.7(7) . . ? N33 C33 W3 178.7(7) . . ? C33 N33 Ni3 171.2(7) . . ? N34 C34 W3 176.2(8) . . ? C34 N34 Ni4 172.5(7) . 2_666 ? N35 C35 W3 174.2(7) . . ? C35 N35 Ni5 175.8(7) . . ? N36 C36 W3 178.1(11) . . ? N37 C37 W3 176.3(9) . . ? N38 C38 W3 178.8(9) . . ? C46 W4 C48 76.7(3) . . ? C46 W4 C43 145.2(3) . . ? C48 W4 C43 83.1(3) . . ? C46 W4 C41 138.6(3) . . ? C48 W4 C41 138.6(3) . . ? C43 W4 C41 73.2(3) . . ? C46 W4 C42 118.8(3) . . ? C48 W4 C42 71.3(3) . . ? C43 W4 C42 79.8(3) . . ? C41 W4 C42 71.4(3) . . ? C46 W4 C44 81.6(3) . . ? C48 W4 C44 146.3(3) . . ? C43 W4 C44 101.3(3) . . ? C41 W4 C44 72.9(3) . . ? C42 W4 C44 142.3(3) . . ? C46 W4 C47 75.0(3) . . ? C48 W4 C47 75.9(3) . . ? C43 W4 C47 72.7(3) . . ? C41 W4 C47 125.6(3) . . ? C42 W4 C47 139.2(3) . . ? C44 W4 C47 73.7(3) . . ? C46 W4 C45 70.7(3) . . ? C48 W4 C45 113.4(3) . . ? C43 W4 C45 144.1(3) . . ? C41 W4 C45 74.0(3) . . ? C42 W4 C45 76.3(3) . . ? C44 W4 C45 82.5(3) . . ? C47 W4 C45 140.6(3) . . ? N41 C41 W4 174.3(7) . . ? C41 N41 Ni6 168.8(7) . . ? N42 C42 W4 178.7(9) . . ? C42 N42 Ni7 167.8(8) . . ? N43 C43 W4 179.1(7) . . ? C43 N43 Ni8 168.8(7) . . ? N44 C44 W4 174.1(8) 2_775 . ? C44 N44 Ni9 160.5(8) 2_775 . ? N45 C45 W4 178.0(7) 2_775 . ? C45 N45 Ni10 171.7(7) 2_775 . ? N46 C46 W4 179.6(9) . . ? N47 C47 W4 179.3(9) 1_655 . ? N48 C48 W4 176.8(9) . . ? C57A W5 C52 139.1(8) . . ? C58B W5 C52 139.9(9) . . ? C57A W5 C56 72.6(8) . . ? C58B W5 C56 87.1(9) . . ? C52 W5 C56 131.2(4) . . ? C57A W5 C54 71.3(7) . 2_775 ? C58B W5 C54 84.9(9) . 2_775 ? C52 W5 C54 72.5(3) . 2_775 ? C56 W5 C54 140.1(4) . 2_775 ? C57A W5 C55 145.9(7) . . ? C58B W5 C55 116.1(9) . . ? C52 W5 C55 72.2(3) . . ? C56 W5 C55 74.6(4) . . ? C54 W5 C55 142.8(3) 2_775 . ? C57A W5 C51 90.3(8) . . ? C58B W5 C51 143.0(9) . . ? C52 W5 C51 70.8(3) . . ? C56 W5 C51 74.4(4) . . ? C54 W5 C51 89.2(3) 2_775 . ? C55 W5 C51 89.9(3) . . ? C57A W5 C53 115.8(8) . . ? C58B W5 C53 69.6(9) . . ? C52 W5 C53 73.4(3) . . ? C56 W5 C53 134.6(4) . . ? C54 W5 C53 77.7(3) 2_775 . ? C55 W5 C53 81.5(3) . . ? C51 W5 C53 144.2(3) . . ? C57A W5 C58A 74.8(10) . . ? C52 W5 C58A 139.8(7) . . ? C56 W5 C58A 69.3(8) . . ? C54 W5 C58A 115.9(7) 2_775 . ? C55 W5 C58A 85.0(7) . . ? C51 W5 C58A 143.4(7) . . ? C53 W5 C58A 70.7(7) . . ? C58B W5 C57B 72.5(11) . . ? C52 W5 C57B 125.3(7) . . ? C56 W5 C57B 71.1(7) . . ? C54 W5 C57B 69.1(7) 2_775 . ? C55 W5 C57B 144.2(7) . . ? C51 W5 C57B 71.2(7) . . ? C53 W5 C57B 131.1(7) . . ? N51 C51 W5 177.2(8) . . ? C51 N51 Ni7 170.3(7) . 2_775 ? N52 C52 W5 178.1(7) . . ? C52 N52 Ni6 163.8(7) . . ? N53 C53 W5 179.6(9) . . ? C53 N53 Ni8 173.9(7) . . ? N54 C54 W5 176.4(8) . 2_775 ? C54 N54 Ni9 165.3(7) . . ? N55 C55 W5 174.0(8) . . ? C55 N55 Ni10 171.1(8) . . ? N56 C56 W5 178.0(13) . . ? N57A C57A W5 163(2) . . ? N57B C57B W5 166(2) . . ? N58A C58A W5 166(3) . . ? C63 W6 C68 145.2(3) . . ? C63 W6 C62 86.5(3) . . ? C68 W6 C62 106.4(4) . . ? C63 W6 C65 94.1(3) . . ? C68 W6 C65 92.9(4) . . ? C62 W6 C65 145.0(3) . . ? C63 W6 C67 78.2(3) . . ? C68 W6 C67 76.3(4) . . ? C62 W6 C67 70.3(3) . . ? C65 W6 C67 144.0(3) . . ? C63 W6 C61 72.5(3) . . ? C68 W6 C61 141.9(3) . . ? C62 W6 C61 73.1(3) . . ? C65 W6 C61 73.8(3) . . ? C67 W6 C61 133.9(3) . . ? C63 W6 C64 144.4(3) . . ? C68 W6 C64 70.4(3) . . ? C62 W6 C64 76.9(3) . . ? C65 W6 C64 82.8(3) . . ? C67 W6 C64 123.3(3) . . ? C61 W6 C64 72.6(3) . . ? C63 W6 C66 74.9(3) . . ? C68 W6 C66 75.3(4) . . ? C62 W6 C66 141.6(3) . . ? C65 W6 C66 70.9(3) . . ? C67 W6 C66 73.2(3) . . ? C61 W6 C66 129.2(3) . . ? C64 W6 C66 135.2(3) . . ? N61 C61 W6 178.0(7) . . ? C61 N61 Ni6 176.4(7) . . ? N62 C62 W6 175.0(7) . . ? C62 N62 Ni7 168.5(7) . . ? N63 C63 W6 178.1(8) . . ? C63 N63 Ni8 171.8(7) . . ? N64 C64 W6 178.0(7) . . ? C64 N64 Ni9 175.6(7) . . ? N65 C65 W6 175.0(8) . . ? C65 N65 Ni10 173.4(7) . . ? N66 C66 W6 178.0(9) . . ? N67 C67 W6 177.9(10) . . ? N68 C68 W6 178.9(14) . . ? N31 Ni1 N31 180.000(1) 2_666 . ? N31 Ni1 N21 88.5(3) 2_666 . ? N31 Ni1 N21 91.5(3) . . ? N31 Ni1 N21 91.5(3) 2_666 2_666 ? N31 Ni1 N21 88.5(3) . 2_666 ? N21 Ni1 N21 180.000(1) . 2_666 ? N31 Ni1 N11 90.1(3) 2_666 . ? N31 Ni1 N11 89.9(3) . . ? N21 Ni1 N11 90.2(3) . . ? N21 Ni1 N11 89.8(3) 2_666 . ? N31 Ni1 N11 89.9(3) 2_666 2_666 ? N31 Ni1 N11 90.1(3) . 2_666 ? N21 Ni1 N11 89.8(3) . 2_666 ? N21 Ni1 N11 90.2(3) 2_666 2_666 ? N11 Ni1 N11 180.000(1) . 2_666 ? N22 Ni2 N32 90.0(3) . . ? N22 Ni2 N201 95.5(3) . . ? N32 Ni2 N201 91.0(3) . . ? N22 Ni2 N12 92.1(3) . 2_666 ? N32 Ni2 N12 94.4(3) . 2_666 ? N201 Ni2 N12 170.7(3) . 2_666 ? N22 Ni2 N212 172.3(3) . . ? N32 Ni2 N212 85.1(3) . . ? N201 Ni2 N212 78.7(3) . . ? N12 Ni2 N212 94.2(3) 2_666 . ? N22 Ni2 O213 91.9(3) . . ? N32 Ni2 O213 177.4(3) . . ? N201 Ni2 O213 87.2(3) . . ? N12 Ni2 O213 87.2(3) 2_666 . ? N212 Ni2 O213 92.8(3) . . ? C202 N201 C206 119.2(8) . . ? C202 N201 Ni2 126.5(7) . . ? C206 N201 Ni2 114.4(6) . . ? N201 C202 C203 122.6(11) . . ? N201 C202 H202 118.7 . . ? C203 C202 H202 118.7 . . ? C202 C203 C204 116.7(12) . . ? C202 C203 H203 121.6 . . ? C204 C203 H203 121.6 . . ? C205 C204 C203 122.0(11) . . ? C205 C204 H204 119.0 . . ? C203 C204 H204 119.0 . . ? C204 C205 C206 120.3(12) . . ? C204 C205 H205 119.8 . . ? C206 C205 H205 119.8 . . ? N201 C206 C205 119.1(10) . . ? N201 C206 C207 115.4(8) . . ? C205 C206 C207 125.4(10) . . ? N212 C207 C208 120.8(10) . . ? N212 C207 C206 115.8(8) . . ? C208 C207 C206 123.4(10) . . ? C207 C208 C209 119.5(11) . . ? C207 C208 H208 120.2 . . ? C209 C208 H208 120.2 . . ? C210 C209 C208 118.8(10) . . ? C210 C209 H209 120.6 . . ? C208 C209 H209 120.6 . . ? C209 C210 C211 119.2(11) . . ? C209 C210 H210 120.4 . . ? C211 C210 H210 120.4 . . ? N212 C211 C210 123.6(11) . . ? N212 C211 H211 118.2 . . ? C210 C211 H211 118.2 . . ? C207 N212 C211 118.0(8) . . ? C207 N212 Ni2 114.0(6) . . ? C211 N212 Ni2 126.6(7) . . ? N23 Ni3 N33 91.6(3) . . ? N23 Ni3 N312 171.4(3) . . ? N33 Ni3 N312 87.3(3) . . ? N23 Ni3 N13 90.7(3) . . ? N33 Ni3 N13 90.5(3) . . ? N312 Ni3 N13 97.8(3) . . ? N23 Ni3 N301 92.6(3) . . ? N33 Ni3 N301 89.8(3) . . ? N312 Ni3 N301 78.9(3) . . ? N13 Ni3 N301 176.7(3) . . ? N23 Ni3 O313 89.7(3) . . ? N33 Ni3 O313 178.7(3) . . ? N312 Ni3 O313 91.5(3) . . ? N13 Ni3 O313 88.9(3) . . ? N301 Ni3 O313 90.6(3) . . ? C302 N301 C306 119.4(8) . . ? C302 N301 Ni3 125.3(6) . . ? C306 N301 Ni3 115.2(6) . . ? N301 C302 C303 121.7(9) . . ? N301 C302 H302 119.2 . . ? C303 C302 H302 119.2 . . ? C304 C303 C302 118.3(10) . . ? C304 C303 H303 120.9 . . ? C302 C303 H303 120.9 . . ? C305 C304 C303 118.8(10) . . ? C305 C304 H304 120.6 . . ? C303 C304 H304 120.6 . . ? C306 C305 C304 120.7(10) . . ? C306 C305 H305 119.7 . . ? C304 C305 H305 119.7 . . ? N301 C306 C305 121.2(9) . . ? N301 C306 C307 114.7(8) . . ? C305 C306 C307 124.1(9) . . ? N312 C307 C308 120.5(10) . . ? N312 C307 C306 116.8(8) . . ? C308 C307 C306 122.6(10) . . ? C309 C308 C307 118.0(13) . . ? C309 C308 H308 121.0 . . ? C307 C308 H308 121.0 . . ? C310 C309 C308 120.9(13) . . ? C310 C309 H309 119.5 . . ? C308 C309 H309 119.5 . . ? C309 C310 C311 120.1(14) . . ? C309 C310 H310 119.9 . . ? C311 C310 H310 119.9 . . ? N312 C311 C310 118.9(13) . . ? N312 C311 H311 120.5 . . ? C310 C311 H311 120.5 . . ? C311 N312 C307 121.2(9) . . ? C311 N312 Ni3 124.6(8) . . ? C307 N312 Ni3 114.0(6) . . ? N34 Ni4 N24 90.5(3) 2_666 . ? N34 Ni4 N401 170.4(3) 2_666 . ? N24 Ni4 N401 96.3(3) . . ? N34 Ni4 N14 92.3(3) 2_666 . ? N24 Ni4 N14 91.6(3) . . ? N401 Ni4 N14 94.3(3) . . ? N34 Ni4 N412 94.1(3) 2_666 . ? N24 Ni4 N412 95.4(3) . . ? N401 Ni4 N412 78.5(3) . . ? N14 Ni4 N412 170.4(3) . . ? N34 Ni4 O413 87.3(3) 2_666 . ? N24 Ni4 O413 177.6(3) . . ? N401 Ni4 O413 86.0(3) . . ? N14 Ni4 O413 87.5(3) . . ? N412 Ni4 O413 85.7(3) . . ? C402 N401 C406 119.1(7) . . ? C402 N401 Ni4 126.1(6) . . ? C406 N401 Ni4 114.3(6) . . ? C403 C402 N401 121.7(10) . . ? C403 C402 H402 119.2 . . ? N401 C402 H402 119.2 . . ? C402 C403 C404 120.4(10) . . ? C402 C403 H403 119.8 . . ? C404 C403 H403 119.8 . . ? C403 C404 C405 119.1(9) . . ? C403 C404 H404 120.4 . . ? C405 C404 H404 120.4 . . ? C406 C405 C404 118.3(10) . . ? C406 C405 H405 120.9 . . ? C404 C405 H405 120.9 . . ? N401 C406 C405 121.3(9) . . ? N401 C406 C407 115.0(7) . . ? C405 C406 C407 123.6(9) . . ? N412 C407 C408 120.2(9) . . ? N412 C407 C406 115.4(7) . . ? C408 C407 C406 124.4(8) . . ? C409 C408 C407 120.3(10) . . ? C409 C408 H408 119.9 . . ? C407 C408 H408 119.9 . . ? C410 C409 C408 118.8(11) . . ? C410 C409 H409 120.6 . . ? C408 C409 H409 120.6 . . ? C409 C410 C411 119.4(10) . . ? C409 C410 H410 120.3 . . ? C411 C410 H410 120.3 . . ? N412 C411 C410 122.6(10) . . ? N412 C411 H411 118.7 . . ? C410 C411 H411 118.7 . . ? C411 N412 C407 118.5(8) . . ? C411 N412 Ni4 126.7(6) . . ? C407 N412 Ni4 114.1(6) . . ? N15 Ni5 N35 90.7(3) . . ? N15 Ni5 N501 174.7(3) . . ? N35 Ni5 N501 94.6(3) . . ? N15 Ni5 N512 95.4(3) . . ? N35 Ni5 N512 173.9(3) . . ? N501 Ni5 N512 79.3(3) . . ? N15 Ni5 N25 92.3(3) . . ? N35 Ni5 N25 92.5(3) . . ? N501 Ni5 N25 86.9(3) . . ? N512 Ni5 N25 87.6(3) . . ? N15 Ni5 O513 91.5(3) . . ? N35 Ni5 O513 89.8(3) . . ? N501 Ni5 O513 89.0(3) . . ? N512 Ni5 O513 89.7(3) . . ? N25 Ni5 O513 175.5(3) . . ? C502 N501 C506 118.3(7) . . ? C502 N501 Ni5 126.8(6) . . ? C506 N501 Ni5 114.5(6) . . ? N501 C502 C503 123.1(9) . . ? N501 C502 H502 118.4 . . ? C503 C502 H502 118.4 . . ? C504 C503 C502 118.5(11) . . ? C504 C503 H503 120.8 . . ? C502 C503 H503 120.8 . . ? C503 C504 C505 119.6(10) . . ? C503 C504 H504 120.2 . . ? C505 C504 H504 120.2 . . ? C504 C505 C506 119.2(10) . . ? C504 C505 H505 120.4 . . ? C506 C505 H505 120.4 . . ? N501 C506 C505 121.2(9) . . ? N501 C506 C507 115.3(7) . . ? C505 C506 C507 123.5(9) . . ? N512 C507 C508 120.2(9) . . ? N512 C507 C506 115.6(8) . . ? C508 C507 C506 124.2(9) . . ? C509 C508 C507 118.9(10) . . ? C509 C508 H508 120.5 . . ? C507 C508 H508 120.5 . . ? C510 C509 C508 120.3(10) . . ? C510 C509 H509 119.8 . . ? C508 C509 H509 119.8 . . ? C509 C510 C511 119.5(11) . . ? C509 C510 H510 120.2 . . ? C511 C510 H510 120.2 . . ? N512 C511 C510 120.9(10) . . ? N512 C511 H511 119.6 . . ? C510 C511 H511 119.6 . . ? C507 N512 C511 120.1(8) . . ? C507 N512 Ni5 114.7(6) . . ? C511 N512 Ni5 124.9(6) . . ? N52 Ni6 N52 180.0(4) 2_775 . ? N52 Ni6 N41 91.5(3) 2_775 . ? N52 Ni6 N41 88.5(3) . . ? N52 Ni6 N41 88.5(3) 2_775 2_775 ? N52 Ni6 N41 91.5(3) . 2_775 ? N41 Ni6 N41 180.000(1) . 2_775 ? N52 Ni6 N61 90.9(3) 2_775 . ? N52 Ni6 N61 89.1(3) . . ? N41 Ni6 N61 91.8(3) . . ? N41 Ni6 N61 88.2(3) 2_775 . ? N52 Ni6 N61 89.1(3) 2_775 2_775 ? N52 Ni6 N61 90.9(3) . 2_775 ? N41 Ni6 N61 88.2(3) . 2_775 ? N41 Ni6 N61 91.8(3) 2_775 2_775 ? N61 Ni6 N61 180.0(4) . 2_775 ? N42 Ni7 N51 93.5(3) . 2_775 ? N42 Ni7 N701 165.7(3) . . ? N51 Ni7 N701 95.5(3) 2_775 . ? N42 Ni7 N62 94.4(3) . . ? N51 Ni7 N62 90.7(3) 2_775 . ? N701 Ni7 N62 96.7(3) . . ? N42 Ni7 N712 91.5(3) . . ? N51 Ni7 N712 175.0(3) 2_775 . ? N701 Ni7 N712 79.5(3) . . ? N62 Ni7 N712 89.8(3) . . ? N42 Ni7 O713 84.3(3) . . ? N51 Ni7 O713 88.6(3) 2_775 . ? N701 Ni7 O713 84.7(3) . . ? N62 Ni7 O713 178.5(3) . . ? N712 Ni7 O713 91.1(3) . . ? C702 N701 C706 120.5(9) . . ? C702 N701 Ni7 125.8(7) . . ? C706 N701 Ni7 113.2(6) . . ? N701 C702 C703 122.1(12) . . ? N701 C702 H702 119.0 . . ? C703 C702 H702 119.0 . . ? C704 C703 C702 119.1(13) . . ? C704 C703 H703 120.5 . . ? C702 C703 H703 120.5 . . ? C703 C704 C705 119.5(10) . . ? C703 C704 H704 120.2 . . ? C705 C704 H704 120.2 . . ? C704 C705 C706 121.1(11) . . ? C704 C705 H705 119.4 . . ? C706 C705 H705 119.4 . . ? N701 C706 C705 117.6(10) . . ? N701 C706 C707 117.2(8) . . ? C705 C706 C707 125.2(10) . . ? N712 C707 C708 119.1(11) . . ? N712 C707 C706 115.8(8) . . ? C708 C707 C706 125.1(10) . . ? C707 C708 C709 119.5(12) . . ? C707 C708 H708 120.3 . . ? C709 C708 H708 120.3 . . ? C710 C709 C708 121.6(12) . . ? C710 C709 H709 119.2 . . ? C708 C709 H709 119.2 . . ? C709 C710 C711 116.7(12) . . ? C709 C710 H710 121.6 . . ? C711 C710 H710 121.6 . . ? N712 C711 C710 122.6(11) . . ? N712 C711 H711 118.7 . . ? C710 C711 H711 118.7 . . ? C711 N712 C707 120.3(9) . . ? C711 N712 Ni7 126.0(7) . . ? C707 N712 Ni7 113.7(6) . . ? N63 Ni8 N812 173.7(3) . . ? N63 Ni8 N801 94.4(3) . . ? N812 Ni8 N801 79.3(3) . . ? N63 Ni8 N43 91.1(3) . . ? N812 Ni8 N43 95.2(3) . . ? N801 Ni8 N43 174.0(3) . . ? N63 Ni8 N53 91.2(3) . . ? N812 Ni8 N53 89.5(3) . . ? N801 Ni8 N53 87.1(3) . . ? N43 Ni8 N53 90.6(3) . . ? N63 Ni8 O813 90.1(3) . . ? N812 Ni8 O813 89.3(3) . . ? N801 Ni8 O813 93.0(3) . . ? N43 Ni8 O813 89.2(3) . . ? N53 Ni8 O813 178.8(3) . . ? C802 N801 C806 117.5(9) . . ? C802 N801 Ni8 127.5(7) . . ? C806 N801 Ni8 114.2(6) . . ? N801 C802 C803 123.2(12) . . ? N801 C802 H802 118.4 . . ? C803 C802 H802 118.4 . . ? C804 C803 C802 117.4(12) . . ? C804 C803 H803 121.3 . . ? C802 C803 H803 121.3 . . ? C805 C804 C803 121.3(12) . . ? C805 C804 H804 119.4 . . ? C803 C804 H804 119.4 . . ? C804 C805 C806 118.1(13) . . ? C804 C805 H805 120.9 . . ? C806 C805 H805 120.9 . . ? N801 C806 C805 122.4(11) . . ? N801 C806 C807 115.0(8) . . ? C805 C806 C807 122.6(11) . . ? N812 C807 C808 120.7(10) . . ? N812 C807 C806 115.2(9) . . ? C808 C807 C806 123.9(10) . . ? C809 C808 C807 119.7(12) . . ? C809 C808 H808 120.1 . . ? C807 C808 H808 120.1 . . ? C810 C809 C808 119.7(12) . . ? C810 C809 H809 120.2 . . ? C808 C809 H809 120.2 . . ? C809 C810 C811 120.4(12) . . ? C809 C810 H810 119.8 . . ? C811 C810 H810 119.8 . . ? N812 C811 C810 120.8(11) . . ? N812 C811 H811 119.6 . . ? C810 C811 H811 119.6 . . ? C811 N812 C807 118.5(9) . . ? C811 N812 Ni8 126.8(7) . . ? C807 N812 Ni8 114.6(6) . . ? N44 Ni9 N64 89.9(3) . . ? N44 Ni9 N901 89.7(3) . . ? N64 Ni9 N901 173.2(3) . . ? N44 Ni9 N54 91.7(3) . . ? N64 Ni9 N54 91.3(3) . . ? N901 Ni9 N54 95.4(3) . . ? N44 Ni9 N912 94.4(3) . . ? N64 Ni9 N912 94.7(3) . . ? N901 Ni9 N912 78.7(4) . . ? N54 Ni9 N912 171.5(3) . . ? N44 Ni9 O913 174.6(3) . . ? N64 Ni9 O913 91.0(3) . . ? N901 Ni9 O913 90.0(3) . . ? N54 Ni9 O913 83.0(3) . . ? N912 Ni9 O913 90.8(3) . . ? C902 N901 C906 120.4(10) . . ? C902 N901 Ni9 125.8(8) . . ? C906 N901 Ni9 113.7(8) . . ? N901 C902 C903 121.7(14) . . ? N901 C902 H902 119.1 . . ? C903 C902 H902 119.1 . . ? C904 C903 C902 116.7(16) . . ? C904 C903 H903 121.6 . . ? C902 C903 H903 121.6 . . ? C905 C904 C903 121.1(16) . . ? C905 C904 H904 119.4 . . ? C903 C904 H904 119.4 . . ? C904 C905 C906 122.6(16) . . ? C904 C905 H905 118.7 . . ? C906 C905 H905 118.7 . . ? N901 C906 C905 117.3(13) . . ? N901 C906 C907 116.8(9) . . ? C905 C906 C907 125.8(12) . . ? N912 C907 C908 120.3(12) . . ? N912 C907 C906 114.9(9) . . ? C908 C907 C906 124.8(11) . . ? C909 C908 C907 122.1(13) . . ? C909 C908 H908 119.0 . . ? C907 C908 H908 119.0 . . ? C908 C909 C910 117.3(12) . . ? C908 C909 H909 121.3 . . ? C910 C909 H909 121.3 . . ? C909 C910 C911 120.0(13) . . ? C909 C910 H910 120.0 . . ? C911 C910 H910 120.0 . . ? N912 C911 C910 122.1(12) . . ? N912 C911 H911 118.9 . . ? C910 C911 H911 118.9 . . ? C907 N912 C911 118.0(9) . . ? C907 N912 Ni9 115.9(7) . . ? C911 N912 Ni9 126.0(7) . . ? N45 Ni10 N55 92.7(3) . . ? N45 Ni10 N101 94.0(3) . . ? N55 Ni10 N101 170.4(3) . . ? N45 Ni10 N112 171.0(3) . . ? N55 Ni10 N112 94.5(3) . . ? N101 Ni10 N112 78.3(3) . . ? N45 Ni10 N65 90.5(3) . . ? N55 Ni10 N65 92.6(3) . . ? N101 Ni10 N65 94.2(3) . . ? N112 Ni10 N65 94.5(3) . . ? N45 Ni10 O113 87.4(3) . . ? N55 Ni10 O113 86.7(3) . . ? N101 Ni10 O113 86.7(3) . . ? N112 Ni10 O113 87.6(3) . . ? N65 Ni10 O113 177.8(3) . . ? C106 N101 C102 119.7(10) . . ? C106 N101 Ni10 114.9(7) . . ? C102 N101 Ni10 125.2(7) . . ? N101 C102 C103 120.9(12) . . ? N101 C102 H102 119.6 . . ? C103 C102 H102 119.6 . . ? C104 C103 C102 118.7(14) . . ? C104 C103 H103 120.7 . . ? C102 C103 H103 120.7 . . ? C105 C104 C103 120.7(13) . . ? C105 C104 H104 119.7 . . ? C103 C104 H104 119.7 . . ? C104 C105 C106 119.5(13) . . ? C104 C105 H105 120.3 . . ? C106 C105 H105 120.3 . . ? N101 C106 C105 120.5(12) . . ? N101 C106 C107 115.7(9) . . ? C105 C106 C107 123.8(11) . . ? N112 C107 C108 118.9(12) . . ? N112 C107 C106 115.5(9) . . ? C108 C107 C106 125.5(11) . . ? C109 C108 C107 120.6(13) . . ? C109 C108 H108 119.7 . . ? C107 C108 H108 119.7 . . ? C108 C109 C110 121.2(14) . . ? C108 C109 H109 119.4 . . ? C110 C109 H109 119.4 . . ? C109 C110 C111 117.8(15) . . ? C109 C110 H110 121.1 . . ? C111 C110 H110 121.1 . . ? N112 C111 C110 121.6(13) . . ? N112 C111 H111 119.2 . . ? C110 C111 H111 119.2 . . ? C111 N112 C107 119.8(9) . . ? C111 N112 Ni10 125.1(8) . . ? C107 N112 Ni10 114.9(7) . . ? O15W O12W O22W 10(6) . . ? O12W O15W O22W 162(10) . . ? O18W O17W O24W 55(10) . . ? O17W O18W O24W 90(10) . . ? O15W O22W O12W 8(6) . . ? O18W O24W O17W 35(6) . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 1.799 _refine_diff_density_min -1.454 _refine_diff_density_rms 0.179 #===END data_1b _database_code_depnum_ccdc_archive 'CCDC 876828' #TrackingRef '- clusters1-4_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; {Ni[Ni(bpy)(solv)]8[W(CN)8]6}.11H2O ; _chemical_name_common (Ni(Ni(bpy)(solv))8(W(CN)8)6).11H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C134.40 H114.80 N64 Ni9 O19 W6' _chemical_formula_weight 4561.99 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' W W -0.8490 6.8722 '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 18.4747(11) _cell_length_b 18.5055(12) _cell_length_c 27.732(2) _cell_angle_alpha 84.222(3) _cell_angle_beta 85.211(4) _cell_angle_gamma 87.182(3) _cell_volume 9392.1(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13041 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.028 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4436 _exptl_absorpt_coefficient_mu 4.604 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2603 _exptl_absorpt_correction_T_max 0.3388 _exptl_absorpt_process_details 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\f and \o scans to fill Ewald sphere' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 28440 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_av_sigmaI/netI 0.045 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.50 _reflns_number_total 22957 _reflns_number_gt 17992 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (ALTOMARE et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+1121.0753P] 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 22957 _refine_ls_number_parameters 1073 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1432 _refine_ls_R_factor_gt 0.1125 _refine_ls_wR_factor_ref 0.3040 _refine_ls_wR_factor_gt 0.2804 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.10175(6) 0.26555(6) -0.01864(4) 0.0235(3) Uani 1 1 d . . . C11 C 0.0207(14) 0.2550(14) -0.0679(8) 0.021(5) Uiso 1 1 d . . . N11 N -0.0243(12) 0.2475(12) -0.0940(7) 0.027(5) Uiso 1 1 d . . . C12 C 0.0711(15) 0.1530(15) -0.0110(9) 0.026(6) Uiso 1 1 d . . . N12 N 0.0485(12) 0.0957(12) -0.0064(7) 0.021(5) Uiso 1 1 d . . . C13 C 0.0003(15) 0.2631(15) 0.0283(9) 0.025(6) Uiso 1 1 d . . . N13 N -0.0476(13) 0.2622(13) 0.0550(8) 0.029(5) Uiso 1 1 d . . . C14 C 0.0944(17) 0.3532(17) 0.0276(10) 0.035(7) Uiso 1 1 d . . . N14 N 0.0919(16) 0.4012(16) 0.0503(10) 0.050(7) Uiso 1 1 d . . . C15 C 0.1522(14) 0.2084(14) 0.0431(9) 0.022(6) Uiso 1 1 d . . . N15 N 0.1821(13) 0.1773(13) 0.0741(8) 0.032(6) Uiso 1 1 d . . . C16 C 0.1702(14) 0.2113(14) -0.0728(9) 0.023(6) Uiso 1 1 d . . . N16 N 0.2017(13) 0.1794(13) -0.1003(8) 0.031(5) Uiso 1 1 d . . . C17 C 0.1006(17) 0.3626(17) -0.0708(10) 0.034(7) Uiso 1 1 d . . . N17 N 0.0978(14) 0.4117(14) -0.0989(9) 0.038(6) Uiso 1 1 d . . . C18 C 0.2100(18) 0.3047(17) -0.0204(10) 0.036(7) Uiso 1 1 d . . . N18 N 0.2642(15) 0.3292(15) -0.0204(9) 0.042(6) Uiso 1 1 d . . . W2 W 0.22956(6) 0.46256(7) 0.57528(4) 0.0298(3) Uani 1 1 d . . . C21 C 0.2928(15) 0.4518(15) 0.6358(9) 0.025(6) Uiso 1 1 d . . . N21 N 0.3290(13) 0.4484(13) 0.6696(8) 0.034(6) Uiso 1 1 d . . . C22 C 0.2409(17) 0.5753(17) 0.5596(10) 0.035(7) Uiso 1 1 d . . . N22 N 0.2494(14) 0.6388(14) 0.5505(8) 0.037(6) Uiso 1 1 d . . . C23 C 0.2850(16) 0.3580(16) 0.5647(10) 0.031(6) Uiso 1 1 d . . . N23 N 0.3118(14) 0.3020(14) 0.5590(9) 0.037(6) Uiso 1 1 d . . . C24 C 0.1240(18) 0.5066(18) 0.5527(11) 0.042(8) Uiso 1 1 d . . . N24 N 0.0687(17) 0.5289(17) 0.5406(11) 0.057(8) Uiso 1 1 d . . . C25 C 0.1635(19) 0.5053(19) 0.6363(12) 0.046(8) Uiso 1 1 d . . . N25 N 0.135(2) 0.527(2) 0.6682(13) 0.078(10) Uiso 1 1 d . . . C26 C 0.3391(16) 0.4826(15) 0.5466(9) 0.027(6) Uiso 1 1 d . . . N26 N 0.3947(13) 0.4914(12) 0.5286(7) 0.026(5) Uiso 1 1 d . . . C27 C 0.2314(16) 0.4549(16) 0.4990(9) 0.029(6) Uiso 1 1 d . . . N27 N 0.2328(13) 0.4570(13) 0.4562(8) 0.030(5) Uiso 1 1 d . . . C28 C 0.158(2) 0.378(2) 0.6067(13) 0.054(9) Uiso 1 1 d . . . N28 N 0.126(2) 0.326(3) 0.6230(15) 0.100(13) Uiso 1 1 d . . . W3 W 0.27118(6) -0.10877(7) 0.00759(4) 0.0293(3) Uani 1 1 d . . . C31 C 0.366(2) -0.114(2) -0.0411(12) 0.048(9) Uiso 1 1 d . . . N31 N 0.419(2) -0.114(2) -0.0664(15) 0.098(13) Uiso 1 1 d . . . C32 C 0.2647(18) -0.0165(18) -0.0487(11) 0.040(8) Uiso 1 1 d . . . N32 N 0.2603(13) 0.0252(13) -0.0804(8) 0.032(6) Uiso 1 1 d . . . C33 C 0.2576(17) -0.0149(17) 0.0514(10) 0.035(7) Uiso 1 1 d . . . N33 N 0.2498(13) 0.0269(14) 0.0754(8) 0.033(6) Uiso 1 1 d . . . C34 C 0.1571(14) -0.0715(14) 0.0066(9) 0.023(6) Uiso 1 1 d . . . N34 N 0.0986(13) -0.0529(13) 0.0046(8) 0.029(5) Uiso 1 1 d . . . C35 C 0.3550(17) -0.1145(17) 0.0578(10) 0.036(7) Uiso 1 1 d . . . N35 N 0.3966(18) -0.1196(18) 0.0883(11) 0.063(9) Uiso 1 1 d . . . C36 C 0.2243(15) -0.1641(15) -0.0435(9) 0.024(6) Uiso 1 1 d . . . N36 N 0.1936(14) -0.1999(14) -0.0676(8) 0.036(6) Uiso 1 1 d . . . C37 C 0.2080(19) -0.1660(19) 0.0695(12) 0.046(8) Uiso 1 1 d . . . N37 N 0.1745(14) -0.1942(14) 0.0988(9) 0.038(6) Uiso 1 1 d . . . C38 C 0.312(2) -0.220(2) 0.0169(12) 0.049(9) Uiso 1 1 d . . . N38 N 0.330(2) -0.279(2) 0.0189(15) 0.095(13) Uiso 1 1 d . . . W4 W 0.59156(6) 0.30333(6) 0.63839(4) 0.0270(3) Uani 1 1 d . . . C41 C 0.5205(17) 0.3819(17) 0.6737(10) 0.038(7) Uiso 1 1 d . . . N41 N 0.4820(14) 0.4211(14) 0.6920(8) 0.034(6) Uiso 1 1 d . . . C42 C 0.5521(14) 0.3808(15) 0.5832(9) 0.023(6) Uiso 1 1 d . . . N42 N 0.5316(12) 0.4230(12) 0.5534(7) 0.022(5) Uiso 1 1 d . . . C43 C 0.4906(15) 0.2628(15) 0.6170(9) 0.026(6) Uiso 1 1 d . . . N43 N 0.4416(13) 0.2410(13) 0.6001(8) 0.030(5) Uiso 1 1 d . . . C44 C 0.5632(17) 0.2575(17) 0.7099(10) 0.038(7) Uiso 1 1 d . . . N44 N 0.5422(15) 0.2279(15) 0.7496(9) 0.045(7) Uiso 1 1 d . . . C45 C 0.6554(16) 0.3980(16) 0.6298(9) 0.029(6) Uiso 1 1 d . . . N45 N 0.6878(14) 0.4500(14) 0.6231(8) 0.034(6) Uiso 1 1 d . . . C46 C 0.6092(18) 0.1847(19) 0.6378(11) 0.042(8) Uiso 1 1 d . . . N46 N 0.6127(18) 0.1252(18) 0.6365(11) 0.061(8) Uiso 1 1 d . . . C47 C 0.6528(17) 0.2820(17) 0.5699(11) 0.039(7) Uiso 1 1 d . . . N47 N 0.6819(13) 0.2723(13) 0.5334(8) 0.033(6) Uiso 1 1 d . . . C48 C 0.6964(18) 0.2729(18) 0.6639(11) 0.040(8) Uiso 1 1 d . . . N48 N 0.7545(19) 0.2554(18) 0.6757(11) 0.064(9) Uiso 1 1 d . . . W5 W 0.02665(6) -0.00753(6) -0.19234(4) 0.0276(3) Uani 1 1 d . . . C51 C -0.0773(16) -0.0437(16) -0.1648(9) 0.030(6) Uiso 1 1 d . . . N51 N -0.1341(14) -0.0649(13) -0.1514(8) 0.034(6) Uiso 1 1 d . . . C52 C -0.0156(18) -0.0600(18) -0.2435(11) 0.040(8) Uiso 1 1 d . . . N52 N -0.0421(18) -0.0982(18) -0.2724(11) 0.065(9) Uiso 1 1 d . . . C53 C 0.0646(14) -0.1140(15) -0.1592(9) 0.023(6) Uiso 1 1 d . . . N53 N 0.0906(14) -0.1629(14) -0.1411(9) 0.039(6) Uiso 1 1 d . . . C54 C 0.1176(16) -0.0489(16) -0.2378(9) 0.029(6) Uiso 1 1 d . . . N54 N 0.1715(16) -0.0673(16) -0.2594(10) 0.052(7) Uiso 1 1 d . . . C55 C 0.1229(15) 0.0461(15) -0.1744(9) 0.027(6) Uiso 1 1 d . . . N55 N 0.1734(14) 0.0696(13) -0.1653(8) 0.033(6) Uiso 1 1 d . . . C56 C 0.0347(16) 0.0665(16) -0.2554(9) 0.029(6) Uiso 1 1 d . . . N56 N 0.0349(17) 0.1055(17) -0.2902(10) 0.055(8) Uiso 1 1 d . . . C57 C -0.0283(15) 0.0953(15) -0.1767(9) 0.026(6) Uiso 1 1 d . . . N57 N -0.0529(14) 0.1505(14) -0.1681(9) 0.039(6) Uiso 1 1 d . . . C58 C 0.0182(13) -0.0052(13) -0.1148(7) 0.013(5) Uiso 1 1 d . . . N58 N 0.0133(12) -0.0014(12) -0.0733(7) 0.022(5) Uiso 1 1 d . . . W6 W 0.51511(7) 0.70933(6) 0.61659(4) 0.0280(3) Uani 1 1 d . . . C61 C 0.4156(16) 0.7294(16) 0.5795(10) 0.032(7) Uiso 1 1 d . . . N61 N 0.3621(13) 0.7398(13) 0.5621(8) 0.030(5) Uiso 1 1 d . . . C62 C 0.5544(16) 0.7567(15) 0.5439(9) 0.029(6) Uiso 1 1 d . . . N62 N 0.5769(14) 0.7748(14) 0.5067(8) 0.036(6) Uiso 1 1 d . . . C63 C 0.5094(13) 0.6241(14) 0.5675(8) 0.018(5) Uiso 1 1 d . . . N63 N 0.5098(13) 0.5804(13) 0.5448(8) 0.028(5) Uiso 1 1 d . . . C64 C 0.6193(17) 0.6465(16) 0.6150(10) 0.034(7) Uiso 1 1 d . . . N64 N 0.6704(13) 0.6120(13) 0.6159(8) 0.034(6) Uiso 1 1 d . . . C65 C 0.5374(19) 0.6871(18) 0.6908(11) 0.044(8) Uiso 1 1 d . . . N65 N 0.5517(15) 0.6718(15) 0.7305(9) 0.043(7) Uiso 1 1 d . . . C66 C 0.5924(17) 0.7937(17) 0.6277(10) 0.036(7) Uiso 1 1 d . . . N66 N 0.6291(16) 0.8363(16) 0.6343(9) 0.046(7) Uiso 1 1 d . . . C67 C 0.4490(16) 0.6249(16) 0.6509(9) 0.029(6) Uiso 1 1 d . . . N67 N 0.4210(12) 0.5751(12) 0.6718(7) 0.023(5) Uiso 1 1 d . . . C68 C 0.4440(16) 0.7885(16) 0.6532(10) 0.031(6) Uiso 1 1 d . . . N68 N 0.4080(15) 0.8273(15) 0.6764(9) 0.042(6) Uiso 1 1 d . . . Ni7 Ni 0.0000 0.0000 0.0000 0.0227(11) Uani 1 2 d S . . Ni8 Ni 0.5000 0.5000 0.5000 0.0215(10) Uiso 1 2 d S . . Ni9 Ni 0.2334(2) 0.1069(2) 0.12327(13) 0.0326(9) Uani 1 1 d . . . O91 O 0.3333(13) 0.1462(13) 0.0927(8) 0.055(6) Uiso 1 1 d . . . N91 N 0.2866(15) 0.0500(16) 0.1796(9) 0.046(7) Uiso 1 1 d . . . N92 N 0.2322(17) 0.1810(17) 0.1736(10) 0.054(8) Uiso 1 1 d . . . C90 C 0.308(2) -0.018(2) 0.1803(15) 0.070(12) Uiso 1 1 d . . . H90 H 0.2997 -0.0438 0.1535 0.084 Uiso 1 1 calc R . . C91 C 0.343(3) -0.055(3) 0.2193(16) 0.080(13) Uiso 1 1 d . . . H91 H 0.3586 -0.1043 0.2198 0.096 Uiso 1 1 calc R . . C92 C 0.354(2) -0.013(2) 0.2575(15) 0.068(11) Uiso 1 1 d . . . H92 H 0.3817 -0.0334 0.2832 0.082 Uiso 1 1 calc R . . C93 C 0.326(2) 0.058(2) 0.2586(15) 0.069(12) Uiso 1 1 d . . . H93 H 0.3266 0.0842 0.2861 0.083 Uiso 1 1 calc R . . C94 C 0.297(2) 0.086(2) 0.2165(13) 0.054(9) Uiso 1 1 d . . . C95 C 0.261(2) 0.164(2) 0.2152(15) 0.066(11) Uiso 1 1 d . . . C96 C 0.261(2) 0.203(2) 0.2522(14) 0.060 Uiso 1 1 d . . . H96 H 0.2783 0.1832 0.2821 0.072 Uiso 1 1 calc R . . C97 C 0.231(3) 0.283(3) 0.2455(19) 0.093(15) Uiso 1 1 d . . . H97 H 0.2307 0.3157 0.2699 0.111 Uiso 1 1 calc R . . C98 C 0.205(3) 0.302(4) 0.200(2) 0.12(2) Uiso 1 1 d . . . H98 H 0.1879 0.3507 0.1916 0.140 Uiso 1 1 calc R . . C99 C 0.205(2) 0.252(2) 0.1660(15) 0.067(11) Uiso 1 1 d . . . H99 H 0.1845 0.2671 0.1361 0.081 Uiso 1 1 calc R . . Ni10 Ni 0.2656(2) 0.10544(19) -0.13871(12) 0.0284(8) Uani 1 1 d . . . O101 O 0.3556(11) 0.1446(11) -0.1087(6) 0.035(5) Uiso 1 1 d D . . C201 C 0.362(3) 0.140(3) -0.0586(8) 0.069(16) Uiso 0.70 1 d PD . . H20A H 0.4018 0.1025 -0.0559 0.082 Uiso 0.70 1 calc PR . . H20B H 0.3178 0.1143 -0.0468 0.082 Uiso 0.70 1 calc PR . . C202 C 0.373(6) 0.178(6) -0.014(3) 0.18(5) Uiso 0.70 1 d PD . . H20C H 0.3707 0.1425 0.0144 0.229 Uiso 0.70 1 calc PR . . H20D H 0.3340 0.2157 -0.0103 0.229 Uiso 0.70 1 calc PR . . H20E H 0.4200 0.2004 -0.0182 0.229 Uiso 0.70 1 calc PR . . N101 N 0.2853(13) 0.1752(13) -0.1994(8) 0.033(6) Uiso 1 1 d . . . N102 N 0.3361(14) 0.0431(14) -0.1813(9) 0.039(6) Uiso 1 1 d . . . C100 C 0.2517(15) 0.2422(15) -0.2113(9) 0.026(6) Uiso 1 1 d . . . H100 H 0.2138 0.2587 -0.1893 0.032 Uiso 1 1 calc R . . C101 C 0.2696(16) 0.2858(17) -0.2524(10) 0.034(7) Uiso 1 1 d . . . H101 H 0.2408 0.3284 -0.2608 0.041 Uiso 1 1 calc R . . C102 C 0.3296(17) 0.2678(17) -0.2818(11) 0.039(7) Uiso 1 1 d . . . H102 H 0.3460 0.3004 -0.3087 0.046 Uiso 1 1 calc R . . C103 C 0.3660(18) 0.2017(18) -0.2719(11) 0.042(8) Uiso 1 1 d . . . H103 H 0.4065 0.1876 -0.2928 0.050 Uiso 1 1 calc R . . C104 C 0.3435(17) 0.1563(17) -0.2318(10) 0.037(7) Uiso 1 1 d . . . C105 C 0.3746(18) 0.0805(17) -0.2185(11) 0.038(7) Uiso 1 1 d . . . C106 C 0.4284(17) 0.0499(17) -0.2481(11) 0.037(7) Uiso 1 1 d . . . H106 H 0.4506 0.0770 -0.2759 0.045 Uiso 1 1 calc R . . C107 C 0.450(2) -0.025(2) -0.2352(12) 0.050(9) Uiso 1 1 d . . . H107 H 0.4883 -0.0482 -0.2533 0.060 Uiso 1 1 calc R . . C108 C 0.413(2) -0.062(2) -0.1960(12) 0.051(9) Uiso 1 1 d . . . H108 H 0.4267 -0.1109 -0.1868 0.061 Uiso 1 1 calc R . . C109 C 0.3558(17) -0.0279(17) -0.1694(11) 0.039(7) Uiso 1 1 d . . . H109 H 0.3305 -0.0548 -0.1428 0.047 Uiso 1 1 calc R . . Ni11 Ni -0.0988(2) 0.2455(2) -0.14571(13) 0.0306(9) Uani 1 1 d . . . O111 O -0.1696(11) 0.2508(11) -0.2021(7) 0.037(5) Uiso 1 1 d D . . C211 C -0.2311(17) 0.209(2) -0.200(2) 0.09(2) Uiso 0.70 1 d PD . . H21A H -0.2223 0.1622 -0.1797 0.105 Uiso 0.70 1 calc PR . . H21B H -0.2401 0.1975 -0.2328 0.105 Uiso 0.70 1 calc PR . . C212 C -0.2965(15) 0.248(3) -0.1779(19) 0.062(15) Uiso 0.70 1 d PD . . H21C H -0.3389 0.2182 -0.1763 0.094 Uiso 0.70 1 calc PR . . H21D H -0.3058 0.2941 -0.1981 0.094 Uiso 0.70 1 calc PR . . H21E H -0.2877 0.2592 -0.1450 0.094 Uiso 0.70 1 calc PR . . N111 N -0.0305(14) 0.3105(14) -0.1912(8) 0.034(6) Uiso 1 1 d . . . N112 N -0.1357(14) 0.3466(14) -0.1286(9) 0.038(6) Uiso 1 1 d . . . C110 C 0.0238(16) 0.2894(17) -0.2222(10) 0.034(7) Uiso 1 1 d . . . H110 H 0.0280 0.2390 -0.2265 0.041 Uiso 1 1 calc R . . C111 C 0.0752(18) 0.3337(17) -0.2490(11) 0.039(7) Uiso 1 1 d . . . H111 H 0.1142 0.3148 -0.2693 0.047 Uiso 1 1 calc R . . C112 C 0.065(2) 0.408(2) -0.2437(12) 0.051(9) Uiso 1 1 d . . . H112 H 0.0949 0.4425 -0.2624 0.061 Uiso 1 1 calc R . . C113 C 0.011(2) 0.431(2) -0.2118(13) 0.058(10) Uiso 1 1 d . . . H113 H 0.0056 0.4814 -0.2069 0.069 Uiso 1 1 calc R . . C114 C -0.0372(19) 0.3820(19) -0.1859(11) 0.043(8) Uiso 1 1 d . . . C115 C -0.0997(16) 0.4057(16) -0.1517(9) 0.029(6) Uiso 1 1 d . . . C116 C -0.117(2) 0.475(2) -0.1420(13) 0.055(9) Uiso 1 1 d . . . H116 H -0.0893 0.5140 -0.1576 0.066 Uiso 1 1 calc R . . C117 C -0.175(2) 0.489(2) -0.1090(14) 0.064(11) Uiso 1 1 d . . . H117 H -0.1891 0.5375 -0.1023 0.076 Uiso 1 1 calc R . . C118 C -0.212(2) 0.433(2) -0.0869(12) 0.050(9) Uiso 1 1 d . . . H118 H -0.2507 0.4417 -0.0634 0.060 Uiso 1 1 calc R . . C119 C -0.1934(19) 0.3631(19) -0.0974(11) 0.044(8) Uiso 1 1 d . . . H119 H -0.2223 0.3249 -0.0822 0.053 Uiso 1 1 calc R . . Ni12 Ni 0.1321(2) -0.25810(19) -0.10802(12) 0.0311(9) Uani 1 1 d . . . O121 O 0.0716(11) -0.3162(11) -0.1490(7) 0.038(5) Uiso 1 1 d D . . C221 C 0.0053(14) -0.293(3) -0.1676(12) 0.068(14) Uiso 0.80 1 d PD . . H22A H -0.0155 -0.2502 -0.1512 0.082 Uiso 0.80 1 calc PR . . H22B H -0.0297 -0.3319 -0.1615 0.082 Uiso 0.80 1 calc PR . . C222 C 0.018(3) -0.272(3) -0.2212(11) 0.077(16) Uiso 0.80 1 d PD . . H22C H -0.0283 -0.2546 -0.2343 0.115 Uiso 0.80 1 calc PR . . H22D H 0.0375 -0.3140 -0.2373 0.115 Uiso 0.80 1 calc PR . . H22E H 0.0525 -0.2327 -0.2270 0.115 Uiso 0.80 1 calc PR . . N121 N 0.2218(14) -0.2630(14) -0.1570(8) 0.036(6) Uiso 1 1 d . . . N122 N 0.1814(13) -0.3567(13) -0.0825(8) 0.030(5) Uiso 1 1 d . . . C120 C 0.2396(18) -0.2145(19) -0.1929(11) 0.043(8) Uiso 1 1 d . . . H120 H 0.2059 -0.1751 -0.1997 0.052 Uiso 1 1 calc R . . C121 C 0.3050(18) -0.2165(19) -0.2219(11) 0.044(8) Uiso 1 1 d . . . H121 H 0.3174 -0.1788 -0.2466 0.053 Uiso 1 1 calc R . . C122 C 0.351(2) -0.2775(19) -0.2124(12) 0.050(9) Uiso 1 1 d . . . H122 H 0.3955 -0.2825 -0.2320 0.060 Uiso 1 1 calc R . . C123 C 0.3340(19) -0.3298(19) -0.1755(11) 0.044(8) Uiso 1 1 d . . . H123 H 0.3656 -0.3711 -0.1689 0.052 Uiso 1 1 calc R . . C124 C 0.2686(17) -0.3206(17) -0.1478(10) 0.037(7) Uiso 1 1 d . . . C125 C 0.2455(16) -0.3732(16) -0.1050(10) 0.032(7) Uiso 1 1 d . . . C126 C 0.2857(18) -0.4394(17) -0.0930(10) 0.038(7) Uiso 1 1 d . . . H126 H 0.3316 -0.4515 -0.1089 0.046 Uiso 1 1 calc R . . C127 C 0.2503(17) -0.4858(17) -0.0549(10) 0.037(7) Uiso 1 1 d . . . H127 H 0.2720 -0.5325 -0.0466 0.044 Uiso 1 1 calc R . . C128 C 0.1919(16) -0.4679(17) -0.0317(10) 0.035(7) Uiso 1 1 d . . . H128 H 0.1737 -0.4985 -0.0043 0.042 Uiso 1 1 calc R . . C129 C 0.1535(19) -0.4038(18) -0.0457(11) 0.044(8) Uiso 1 1 d . . . H129 H 0.1075 -0.3929 -0.0294 0.052 Uiso 1 1 calc R . . Ni13 Ni 0.3956(2) 0.4865(2) 0.71959(12) 0.0296(9) Uani 1 1 d . . . O131 O 0.4649(12) 0.5335(12) 0.7653(7) 0.044(5) Uiso 1 1 d . . . N131 N 0.3729(13) 0.4132(13) 0.7791(8) 0.034(6) Uiso 1 1 d . . . N132 N 0.3001(14) 0.5364(14) 0.7500(8) 0.036(6) Uiso 1 1 d . . . C130 C 0.4138(17) 0.3575(16) 0.7944(10) 0.034(7) Uiso 1 1 d . . . H130 H 0.4581 0.3474 0.7759 0.041 Uiso 1 1 calc R . . C131 C 0.3963(18) 0.3132(18) 0.8354(11) 0.042(8) Uiso 1 1 d . . . H131 H 0.4271 0.2725 0.8449 0.050 Uiso 1 1 calc R . . C132 C 0.3315(19) 0.329(2) 0.8635(12) 0.049(9) Uiso 1 1 d . . . H132 H 0.3160 0.2977 0.8913 0.059 Uiso 1 1 calc R . . C133 C 0.2922(19) 0.3897(18) 0.8499(11) 0.045(8) Uiso 1 1 d . . . H133 H 0.2497 0.4038 0.8690 0.054 Uiso 1 1 calc R . . C134 C 0.3147(17) 0.4309(17) 0.8077(10) 0.035(7) Uiso 1 1 d . . . C135 C 0.2698(19) 0.4970(19) 0.7877(12) 0.047(8) Uiso 1 1 d . . . C136 C 0.1954(17) 0.5143(18) 0.8063(11) 0.040(7) Uiso 1 1 d . . . H136 H 0.1722 0.4851 0.8327 0.048 Uiso 1 1 calc R . . C137 C 0.1599(19) 0.5746(18) 0.7842(11) 0.043(8) Uiso 1 1 d . . . H137 H 0.1112 0.5878 0.7947 0.051 Uiso 1 1 calc R . . C138 C 0.1980(18) 0.6156(18) 0.7458(11) 0.039(7) Uiso 1 1 d . . . H138 H 0.1761 0.6590 0.7311 0.047 Uiso 1 1 calc R . . C139 C 0.2662(18) 0.5934(18) 0.7295(11) 0.043(8) Uiso 1 1 d . . . H139 H 0.2899 0.6204 0.7023 0.051 Uiso 1 1 calc R . . Ni14 Ni 0.3659(2) 0.2029(2) 0.56068(12) 0.0301(8) Uani 1 1 d . . . O141 O 0.2869(13) 0.1607(13) 0.5218(8) 0.049(6) Uiso 1 1 d D . . C241 C 0.227(4) 0.202(5) 0.505(4) 0.04(3) Uiso 0.30 1 d PD . . H24A H 0.2119 0.2366 0.5300 0.052 Uiso 0.30 1 calc PR . . H24B H 0.1865 0.1689 0.5057 0.052 Uiso 0.30 1 calc PR . . C242 C 0.232(17) 0.246(15) 0.457(6) 0.22(14) Uiso 0.30 1 d PD . . H24C H 0.1875 0.2766 0.4532 0.325 Uiso 0.30 1 calc PR . . H24D H 0.2372 0.2127 0.4310 0.325 Uiso 0.30 1 calc PR . . H24E H 0.2741 0.2764 0.4541 0.325 Uiso 0.30 1 calc PR . . N141 N 0.4185(16) 0.0991(16) 0.5735(10) 0.048(7) Uiso 1 1 d . . . N142 N 0.3014(14) 0.1601(14) 0.6222(8) 0.037(6) Uiso 1 1 d . . . C140 C 0.4773(19) 0.0801(19) 0.5484(12) 0.046(8) Uiso 1 1 d . . . H140 H 0.4950 0.1106 0.5208 0.055 Uiso 1 1 calc R . . C141 C 0.516(2) 0.012(2) 0.5623(14) 0.061(10) Uiso 1 1 d . . . H141 H 0.5598 -0.0029 0.5449 0.074 Uiso 1 1 calc R . . C142 C 0.486(2) -0.029(2) 0.6020(13) 0.058(10) Uiso 1 1 d . . . H142 H 0.5101 -0.0738 0.6119 0.070 Uiso 1 1 calc R . . C143 C 0.4210(19) -0.007(2) 0.6294(12) 0.050(9) Uiso 1 1 d . . . H143 H 0.3979 -0.0359 0.6560 0.060 Uiso 1 1 calc R . . C144 C 0.3967(18) 0.0596(17) 0.6126(11) 0.038(7) Uiso 1 1 d . . . C145 C 0.3275(18) 0.0948(18) 0.6388(11) 0.039(7) Uiso 1 1 d . . . C146 C 0.2857(18) 0.0560(19) 0.6779(11) 0.043(8) Uiso 1 1 d . . . H146 H 0.2994 0.0074 0.6889 0.052 Uiso 1 1 calc R . . C147 C 0.227(2) 0.090(2) 0.6990(15) 0.067(11) Uiso 1 1 d . . . H147 H 0.2016 0.0650 0.7267 0.080 Uiso 1 1 calc R . . C148 C 0.200(2) 0.160(2) 0.6816(13) 0.058(10) Uiso 1 1 d . . . H148 H 0.1564 0.1829 0.6939 0.070 Uiso 1 1 calc R . . C149 C 0.2485(19) 0.1922(19) 0.6431(11) 0.045(8) Uiso 1 1 d . . . H149 H 0.2396 0.2420 0.6326 0.055 Uiso 1 1 calc R . . Ni15 Ni 0.2657(2) 0.7471(2) 0.53044(13) 0.0329(9) Uani 1 1 d . . . O151 O 0.2762(14) 0.8598(14) 0.5108(9) 0.063(7) Uiso 1 1 d D . . C251 C 0.303(2) 0.911(3) 0.538(2) 0.09(2) Uiso 0.70 1 d PD . . H25A H 0.3388 0.9407 0.5180 0.112 Uiso 0.70 1 calc PR . . H25B H 0.3268 0.8856 0.5662 0.112 Uiso 0.70 1 calc PR . . C252 C 0.240(3) 0.959(2) 0.5565(19) 0.069(16) Uiso 0.70 1 d PD . . H25C H 0.2587 0.9947 0.5758 0.103 Uiso 0.70 1 calc PR . . H25D H 0.2050 0.9293 0.5768 0.103 Uiso 0.70 1 calc PR . . H25E H 0.2171 0.9844 0.5288 0.103 Uiso 0.70 1 calc PR . . N151 N 0.1654(15) 0.7602(15) 0.5028(9) 0.044(7) Uiso 1 1 d . . . N152 N 0.2019(14) 0.7749(14) 0.5917(8) 0.037(6) Uiso 1 1 d . . . C150 C 0.152(3) 0.751(3) 0.4577(16) 0.078(13) Uiso 1 1 d . . . H150 H 0.1901 0.7370 0.4353 0.094 Uiso 1 1 calc R . . C151 C 0.083(3) 0.763(3) 0.443(2) 0.101(17) Uiso 1 1 d . . . H151 H 0.0760 0.7616 0.4095 0.122 Uiso 1 1 calc R . . C152 C 0.015(4) 0.778(4) 0.480(3) 0.14(2) Uiso 1 1 d . . . H152 H -0.0335 0.7830 0.4704 0.167 Uiso 1 1 calc R . . C153 C 0.030(3) 0.783(3) 0.525(2) 0.111(19) Uiso 1 1 d . . . H153 H -0.0074 0.7923 0.5496 0.133 Uiso 1 1 calc R . . C154 C 0.108(3) 0.774(3) 0.537(2) 0.101(17) Uiso 1 1 d . . . C155 C 0.137(2) 0.790(2) 0.5857(15) 0.069(11) Uiso 1 1 d . . . C156 C 0.085(3) 0.807(3) 0.6225(18) 0.093(15) Uiso 1 1 d . . . H156 H 0.0346 0.8132 0.6173 0.111 Uiso 1 1 calc R . . C157 C 0.110(3) 0.813(3) 0.6662(17) 0.080(13) Uiso 1 1 d . . . H157 H 0.0768 0.8233 0.6927 0.096 Uiso 1 1 calc R . . C158 C 0.180(3) 0.804(2) 0.6732(17) 0.077(13) Uiso 1 1 d . . . H158 H 0.1981 0.8127 0.7031 0.093 Uiso 1 1 calc R . . C159 C 0.228(2) 0.7813(19) 0.6332(12) 0.049(9) Uiso 1 1 d . . . H159 H 0.2778 0.7708 0.6372 0.058 Uiso 1 1 calc R . . Ni16 Ni 0.7554(2) 0.5382(2) 0.61792(13) 0.0331(9) Uani 1 1 d . . . O161 O 0.8298(14) 0.6229(14) 0.6142(8) 0.057(6) Uiso 1 1 d . . . N161 N 0.7478(15) 0.5236(15) 0.6915(9) 0.041(6) Uiso 1 1 d . . . N162 N 0.8434(15) 0.4661(15) 0.6290(9) 0.044(7) Uiso 1 1 d . . . C160 C 0.6998(18) 0.5518(18) 0.7233(11) 0.041(8) Uiso 1 1 d . . . H160 H 0.6745 0.5961 0.7137 0.049 Uiso 1 1 calc R . . C161 C 0.685(2) 0.518(2) 0.7713(13) 0.054(9) Uiso 1 1 d . . . H161 H 0.6468 0.5376 0.7922 0.065 Uiso 1 1 calc R . . C162 C 0.726(3) 0.456(3) 0.7877(17) 0.083(14) Uiso 1 1 d . . . H162 H 0.7174 0.4325 0.8195 0.099 Uiso 1 1 calc R . . C163 C 0.778(2) 0.433(2) 0.7570(14) 0.063(11) Uiso 1 1 d . . . H163 H 0.8076 0.3916 0.7666 0.075 Uiso 1 1 calc R . . C164 C 0.788(2) 0.468(2) 0.7101(14) 0.062(10) Uiso 1 1 d . . . C165 C 0.8491(17) 0.4403(17) 0.6738(10) 0.034(7) Uiso 1 1 d . . . C166 C 0.903(2) 0.395(2) 0.6887(16) 0.070(12) Uiso 1 1 d . . . H166 H 0.9065 0.3771 0.7219 0.084 Uiso 1 1 calc R . . C167 C 0.953(3) 0.374(3) 0.6507(16) 0.079(13) Uiso 1 1 d . . . H167 H 0.9903 0.3382 0.6578 0.095 Uiso 1 1 calc R . . C168 C 0.950(2) 0.403(2) 0.6065(14) 0.063(11) Uiso 1 1 d . . . H168 H 0.9878 0.3928 0.5826 0.076 Uiso 1 1 calc R . . C169 C 0.896(2) 0.446(2) 0.5942(14) 0.058(10) Uiso 1 1 d . . . H169 H 0.8919 0.4632 0.5611 0.069 Uiso 1 1 calc R . . O1W O 0.9734(12) 0.4502(12) 0.1164(7) 0.040(5) Uiso 1 1 d . . . O2W O 0.5048(14) 0.8535(14) 0.1556(8) 0.056(6) Uiso 1 1 d . . . O3W O 0.0657(17) 0.3841(17) 0.4644(10) 0.050(8) Uiso 0.75 1 d P . . O4W O 0.1056(17) 0.7781(17) 0.2879(11) 0.052(8) Uiso 0.75 1 d P . . O5W O 0.445(2) 0.049(2) 0.1069(14) 0.065(11) Uiso 0.65 1 d P . . O6W O 0.531(2) 0.477(2) 0.1396(14) 0.067(11) Uiso 0.65 1 d P . . O7W O 0.206(3) 0.238(3) 0.3682(17) 0.058(13) Uiso 0.50 1 d P . . O8W O 0.270(3) 0.939(3) 0.4255(17) 0.058(13) Uiso 0.50 1 d P . . O9W O 0.321(2) 0.075(2) 0.4504(15) 0.048(11) Uiso 0.50 1 d P . . O10W O 0.105(3) 0.147(3) 0.357(2) 0.065(16) Uiso 0.45 1 d P . . O11W O 0.937(3) 0.803(3) 0.3810(18) 0.062(14) Uiso 0.50 1 d P . . O13W O 0.317(4) 0.394(4) 0.067(3) 0.047(19) Uiso 0.30 1 d P . . O14W O 0.449(4) 0.238(4) 0.168(2) 0.046(16) Uiso 0.35 1 d P . . O15W O 0.450(5) 0.338(5) 0.166(3) 0.07(2) Uiso 0.30 1 d P . . O16W O 0.048(3) 0.407(3) 0.298(2) 0.049(14) Uiso 0.40 1 d P . . O17W O 0.069(5) 0.414(5) 0.254(3) 0.07(3) Uiso 0.30 1 d P . . O18W O 0.016(6) 0.377(6) 0.338(4) 0.07(3) Uiso 0.25 1 d P . . O19W O 0.405(5) 0.278(5) 0.147(3) 0.05(3) Uiso 0.25 1 d P . . O20W O 0.412(6) 0.582(6) 0.001(4) 0.06(3) Uiso 0.25 1 d P . . O21W O -0.026(4) 0.397(4) 0.276(3) 0.05(2) Uiso 0.30 1 d P . . O23W O 0.344(6) 0.430(6) 0.046(4) 0.06(3) Uiso 0.25 1 d P . . O24W O 0.985(4) 0.781(4) 0.354(3) 0.05(2) Uiso 0.30 1 d P . . O25W O 0.167(9) 0.947(9) 0.302(5) 0.05(4) Uiso 0.15 1 d P . . O26W O 0.153(10) 0.932(10) 0.345(6) 0.06(5) Uiso 0.15 1 d P . . O27W O 0.584(6) 0.432(6) 0.880(4) 0.05(3) Uiso 0.20 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0198(6) 0.0215(6) 0.0265(5) 0.0020(5) 0.0079(4) 0.0009(5) W2 0.0227(7) 0.0325(7) 0.0308(6) 0.0056(5) 0.0074(5) 0.0001(5) W3 0.0157(6) 0.0320(6) 0.0365(6) 0.0066(5) 0.0046(5) 0.0051(5) W4 0.0251(7) 0.0269(6) 0.0256(5) 0.0063(5) 0.0035(4) 0.0052(5) W5 0.0274(7) 0.0279(6) 0.0249(5) 0.0028(5) 0.0072(4) -0.0006(5) W6 0.0324(7) 0.0235(6) 0.0262(5) 0.0003(5) 0.0047(5) 0.0008(5) Ni7 0.021(3) 0.020(2) 0.024(2) 0.004(2) 0.0051(19) 0.004(2) Ni9 0.024(2) 0.039(2) 0.0334(18) 0.0045(17) 0.0014(15) -0.0062(18) Ni10 0.023(2) 0.0259(19) 0.0328(18) 0.0033(16) 0.0102(15) 0.0011(16) Ni11 0.025(2) 0.029(2) 0.0341(18) 0.0092(17) 0.0002(15) 0.0034(17) Ni12 0.030(2) 0.0254(19) 0.0336(18) -0.0004(16) 0.0158(16) 0.0017(17) Ni13 0.031(2) 0.0270(19) 0.0272(17) 0.0031(16) 0.0088(15) 0.0043(17) Ni14 0.030(2) 0.0268(19) 0.0309(18) 0.0045(16) 0.0057(15) -0.0042(17) Ni15 0.035(2) 0.030(2) 0.0310(18) -0.0004(17) 0.0034(16) 0.0118(18) Ni16 0.031(2) 0.033(2) 0.0333(18) 0.0002(17) -0.0008(16) 0.0006(18) _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 W1 C11 2.14(2) . ? W1 C18 2.16(3) . ? W1 C14 2.16(3) . ? W1 C12 2.17(3) . ? W1 C16 2.17(3) . ? W1 C15 2.17(2) . ? W1 C13 2.19(3) . ? W1 C17 2.19(3) . ? C11 N11 1.17(3) . ? N11 Ni11 2.07(2) . ? C12 N12 1.15(3) . ? N12 Ni7 2.01(2) . ? C13 N13 1.11(3) . ? N13 Ni12 2.05(2) 2 ? C14 N14 1.14(4) . ? C15 N15 1.15(3) . ? N15 Ni9 2.05(2) . ? C16 N16 1.12(3) . ? N16 Ni10 2.08(2) . ? C17 N17 1.14(4) . ? C18 N18 1.12(4) . ? W2 C22 2.11(3) . ? W2 C21 2.11(3) . ? W2 C27 2.13(3) . ? W2 C26 2.15(3) . ? W2 C28 2.16(4) . ? W2 C23 2.18(3) . ? W2 C24 2.19(3) . ? W2 C25 2.19(3) . ? C21 N21 1.19(3) . ? N21 Ni13 2.12(2) . ? C22 N22 1.19(4) . ? N22 Ni15 2.06(3) . ? C23 N23 1.15(4) . ? N23 Ni14 2.04(3) . ? C24 N24 1.15(4) . ? C25 N25 1.10(4) . ? C26 N26 1.11(3) . ? N26 Ni8 2.05(2) . ? C27 N27 1.18(3) . ? N27 Ni16 2.04(2) 2_666 ? C28 N28 1.18(5) . ? W3 C36 2.10(3) . ? W3 C31 2.13(4) . ? W3 C38 2.16(4) . ? W3 C35 2.16(3) . ? W3 C34 2.19(3) . ? W3 C32 2.20(3) . ? W3 C37 2.20(3) . ? W3 C33 2.21(3) . ? C31 N31 1.15(5) . ? C32 N32 1.12(4) . ? N32 Ni10 2.08(2) . ? C33 N33 1.07(3) . ? N33 Ni9 2.08(3) . ? C34 N34 1.12(3) . ? N34 Ni7 2.03(2) . ? C35 N35 1.18(4) . ? C36 N36 1.18(3) . ? N36 Ni12 2.07(3) . ? C37 N37 1.08(4) . ? N37 Ni11 2.03(3) 2 ? C38 N38 1.13(5) . ? W4 C44 2.11(3) . ? W4 C42 2.14(3) . ? W4 C45 2.14(3) . ? W4 C48 2.15(3) . ? W4 C41 2.16(3) . ? W4 C47 2.19(3) . ? W4 C43 2.19(3) . ? W4 C46 2.21(3) . ? C41 N41 1.12(4) . ? N41 Ni13 2.09(3) . ? C42 N42 1.15(3) . ? N42 Ni8 2.05(2) . ? C43 N43 1.16(3) . ? N43 Ni14 2.04(2) . ? C44 N44 1.22(4) . ? C45 N45 1.15(3) . ? N45 Ni16 2.09(3) . ? C46 N46 1.10(4) . ? C47 N47 1.13(4) . ? N47 Ni15 2.00(2) 2_666 ? C48 N48 1.17(4) . ? W5 C52 2.02(3) . ? W5 C56 2.11(3) . ? W5 C51 2.12(3) . ? W5 C58 2.15(2) . ? W5 C54 2.17(3) . ? W5 C57 2.18(3) . ? W5 C55 2.19(3) . ? W5 C53 2.20(3) . ? C51 N51 1.16(3) . ? N51 Ni9 2.09(3) 2 ? C52 N52 1.26(4) . ? C53 N53 1.10(3) . ? N53 Ni12 2.05(3) . ? C54 N54 1.17(4) . ? C55 N55 1.11(3) . ? N55 Ni10 2.07(3) . ? C56 N56 1.15(4) . ? C57 N57 1.14(3) . ? N57 Ni11 2.05(3) . ? C58 N58 1.16(3) . ? N58 Ni7 2.031(19) . ? W6 C67 2.13(3) . ? W6 C65 2.13(3) . ? W6 C61 2.18(3) . ? W6 C68 2.19(3) . ? W6 C62 2.20(3) . ? W6 C63 2.20(3) . ? W6 C64 2.20(3) . ? W6 C66 2.23(3) . ? C61 N61 1.14(3) . ? N61 Ni15 2.04(2) . ? C62 N62 1.11(3) . ? N62 Ni14 2.08(2) 2_666 ? C63 N63 1.07(3) . ? N63 Ni8 2.06(2) . ? C64 N64 1.11(4) . ? N64 Ni16 2.03(2) . ? C65 N65 1.16(4) . ? C66 N66 1.10(4) . ? C67 N67 1.16(3) . ? N67 Ni13 2.05(2) . ? C68 N68 1.16(4) . ? Ni7 N12 2.01(2) 2 ? Ni7 N58 2.031(19) 2 ? Ni7 N34 2.03(2) 2 ? Ni8 N26 2.05(2) 2_666 ? Ni8 N42 2.05(2) 2_666 ? Ni8 N63 2.06(2) 2_666 ? Ni9 N92 2.05(3) . ? Ni9 N91 2.08(3) . ? Ni9 N51 2.09(3) 2 ? Ni9 O91 2.10(3) . ? N91 C90 1.30(5) . ? N91 C94 1.30(4) . ? N92 C95 1.31(4) . ? N92 C99 1.39(5) . ? C90 C91 1.41(6) . ? C90 H90 0.9500 . ? C91 C92 1.41(6) . ? C91 H91 0.9500 . ? C92 C93 1.38(6) . ? C92 H92 0.9500 . ? C93 C94 1.36(5) . ? C93 H93 0.9500 . ? C94 C95 1.57(5) . ? C95 C96 1.31(5) . ? C96 C97 1.55(6) . ? C96 H96 0.9500 . ? C97 C98 1.40(7) . ? C97 H97 0.9500 . ? C98 C99 1.38(7) . ? C98 H98 0.9500 . ? C99 H99 0.9500 . ? Ni10 N101 2.04(2) . ? Ni10 N102 2.07(3) . ? Ni10 O101 2.11(2) . ? O101 C201 1.400(10) . ? C201 C202 1.499(10) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9800 . ? C202 H20D 0.9800 . ? C202 H20E 0.9800 . ? N101 C100 1.38(3) . ? N101 C104 1.40(4) . ? N102 C105 1.35(4) . ? N102 C109 1.36(4) . ? C100 C101 1.36(4) . ? C100 H100 0.9500 . ? C101 C102 1.37(4) . ? C101 H101 0.9500 . ? C102 C103 1.38(4) . ? C102 H102 0.9500 . ? C103 C104 1.37(4) . ? C103 H103 0.9500 . ? C104 C105 1.51(4) . ? C105 C106 1.37(4) . ? C106 C107 1.44(4) . ? C106 H106 0.9500 . ? C107 C108 1.37(5) . ? C107 H107 0.9500 . ? C108 C109 1.39(4) . ? C108 H108 0.9500 . ? C109 H109 0.9500 . ? Ni11 N37 2.03(3) 2 ? Ni11 N112 2.05(3) . ? Ni11 N111 2.05(3) . ? Ni11 O111 2.11(2) . ? O111 C211 1.403(10) . ? C211 C212 1.500(10) . ? C211 H21A 0.9900 . ? C211 H21B 0.9900 . ? C212 H21C 0.9800 . ? C212 H21D 0.9800 . ? C212 H21E 0.9800 . ? N111 C110 1.34(4) . ? N111 C114 1.34(4) . ? N112 C119 1.36(4) . ? N112 C115 1.38(4) . ? C110 C111 1.40(4) . ? C110 H110 0.9500 . ? C111 C112 1.41(5) . ? C111 H111 0.9500 . ? C112 C113 1.35(5) . ? C112 H112 0.9500 . ? C113 C114 1.41(5) . ? C113 H113 0.9500 . ? C114 C115 1.51(4) . ? C115 C116 1.36(4) . ? C116 C117 1.39(5) . ? C116 H116 0.9500 . ? C117 C118 1.33(5) . ? C117 H117 0.9500 . ? C118 C119 1.38(5) . ? C118 H118 0.9500 . ? C119 H119 0.9500 . ? Ni12 N13 2.05(2) 2 ? Ni12 N121 2.06(2) . ? Ni12 O121 2.07(2) . ? Ni12 N122 2.08(2) . ? O121 C221 1.403(10) . ? C221 C222 1.499(10) . ? C221 H22A 0.9900 . ? C221 H22B 0.9900 . ? C222 H22C 0.9800 . ? C222 H22D 0.9800 . ? C222 H22E 0.9800 . ? N121 C120 1.30(4) . ? N121 C124 1.36(4) . ? N122 C125 1.33(3) . ? N122 C129 1.36(4) . ? C120 C121 1.40(4) . ? C120 H120 0.9500 . ? C121 C122 1.40(5) . ? C121 H121 0.9500 . ? C122 C123 1.37(5) . ? C122 H122 0.9500 . ? C123 C124 1.39(4) . ? C123 H123 0.9500 . ? C124 C125 1.50(4) . ? C125 C126 1.43(4) . ? C126 C127 1.43(4) . ? C126 H126 0.9500 . ? C127 C128 1.26(4) . ? C127 H127 0.9500 . ? C128 C129 1.39(4) . ? C128 H128 0.9500 . ? C129 H129 0.9500 . ? Ni13 N131 2.06(2) . ? Ni13 N132 2.10(3) . ? Ni13 O131 2.15(2) . ? N131 C130 1.31(4) . ? N131 C134 1.33(4) . ? N132 C139 1.30(4) . ? N132 C135 1.32(4) . ? C130 C131 1.36(4) . ? C130 H130 0.9500 . ? C131 C132 1.41(4) . ? C131 H131 0.9500 . ? C132 C133 1.35(5) . ? C132 H132 0.9500 . ? C133 C134 1.38(4) . ? C133 H133 0.9500 . ? C134 C135 1.53(4) . ? C135 C136 1.46(4) . ? C136 C137 1.38(4) . ? C136 H136 0.9500 . ? C137 C138 1.40(4) . ? C137 H137 0.9500 . ? C138 C139 1.36(4) . ? C138 H138 0.9500 . ? C139 H139 0.9500 . ? Ni14 N62 2.08(2) 2_666 ? Ni14 N142 2.11(3) . ? Ni14 O141 2.11(2) . ? Ni14 N141 2.12(3) . ? O141 C241 1.400(10) . ? C241 C242 1.500(10) . ? C241 H24A 0.9900 . ? C241 H24B 0.9900 . ? C242 H24C 0.9800 . ? C242 H24D 0.9800 . ? C242 H24E 0.9800 . ? N141 C144 1.29(4) . ? N141 C140 1.29(4) . ? N142 C149 1.25(4) . ? N142 C145 1.33(4) . ? C140 C141 1.45(5) . ? C140 H140 0.9500 . ? C141 C142 1.36(5) . ? C141 H141 0.9500 . ? C142 C143 1.44(5) . ? C142 H142 0.9500 . ? C143 C144 1.34(4) . ? C143 H143 0.9500 . ? C144 C145 1.56(4) . ? C145 C146 1.43(4) . ? C146 C147 1.35(5) . ? C146 H146 0.9500 . ? C147 C148 1.42(5) . ? C147 H147 0.9500 . ? C148 C149 1.43(5) . ? C148 H148 0.9500 . ? C149 H149 0.9500 . ? Ni15 N47 2.00(2) 2_666 ? Ni15 N151 2.06(3) . ? Ni15 N152 2.08(2) . ? Ni15 O151 2.11(3) . ? O151 C251 1.404(10) . ? C251 C252 1.502(10) . ? C251 H25A 0.9900 . ? C251 H25B 0.9900 . ? C252 H25C 0.9800 . ? C252 H25D 0.9800 . ? C252 H25E 0.9800 . ? N151 C150 1.33(5) . ? N151 C154 1.39(6) . ? N152 C155 1.24(5) . ? N152 C159 1.30(4) . ? C150 C151 1.36(6) . ? C150 H150 0.9500 . ? C151 C152 1.60(8) . ? C151 H151 0.9500 . ? C152 C153 1.31(7) . ? C152 H152 0.9500 . ? C153 C154 1.50(7) . ? C153 H153 0.9500 . ? C154 C155 1.56(6) . ? C155 C156 1.38(6) . ? C156 C157 1.35(6) . ? C156 H156 0.9500 . ? C157 C158 1.32(6) . ? C157 H157 0.9500 . ? C158 C159 1.44(5) . ? C158 H158 0.9500 . ? C159 H159 0.9500 . ? Ni16 N161 2.02(2) . ? Ni16 N27 2.04(2) 2_666 ? Ni16 N162 2.08(3) . ? Ni16 O161 2.12(3) . ? N161 C160 1.32(4) . ? N161 C164 1.33(5) . ? N162 C165 1.30(4) . ? N162 C169 1.37(4) . ? C160 C161 1.42(4) . ? C160 H160 0.9500 . ? C161 C162 1.41(6) . ? C161 H161 0.9500 . ? C162 C163 1.31(6) . ? C162 H162 0.9500 . ? C163 C164 1.40(5) . ? C163 H163 0.9500 . ? C164 C165 1.55(5) . ? C165 C166 1.33(5) . ? C166 C167 1.42(6) . ? C166 H166 0.9500 . ? C167 C168 1.29(5) . ? C167 H167 0.9500 . ? C168 C169 1.29(5) . ? C168 H168 0.9500 . ? C169 H169 0.9500 . ? O11W O24W 1.21(8) . ? O13W O23W 0.97(11) . ? O14W O19W 1.20(10) . ? O15W O19W 1.57(13) . ? O16W O17W 1.24(10) . ? O16W O18W 1.30(11) . ? O16W O21W 1.56(10) . ? O25W O26W 1.2(2) . ? 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 C11 W1 C18 138.7(10) . . ? C11 W1 C14 121.0(10) . . ? C18 W1 C14 73.8(11) . . ? C11 W1 C12 71.9(10) . . ? C18 W1 C12 127.0(11) . . ? C14 W1 C12 135.8(10) . . ? C11 W1 C16 82.2(9) . . ? C18 W1 C16 71.9(11) . . ? C14 W1 C16 145.0(11) . . ? C12 W1 C16 73.5(10) . . ? C11 W1 C15 142.1(10) . . ? C18 W1 C15 73.2(10) . . ? C14 W1 C15 81.9(10) . . ? C12 W1 C15 71.1(10) . . ? C16 W1 C15 94.8(9) . . ? C11 W1 C13 76.6(9) . . ? C18 W1 C13 139.6(10) . . ? C14 W1 C13 69.0(11) . . ? C12 W1 C13 74.7(10) . . ? C16 W1 C13 145.9(10) . . ? C15 W1 C13 86.2(9) . . ? C11 W1 C17 71.5(10) . . ? C18 W1 C17 75.9(11) . . ? C14 W1 C17 77.1(11) . . ? C12 W1 C17 140.6(10) . . ? C16 W1 C17 87.8(10) . . ? C15 W1 C17 146.3(11) . . ? C13 W1 C17 109.8(10) . . ? N11 C11 W1 178(2) . . ? C11 N11 Ni11 173(2) . . ? N12 C12 W1 174(2) . . ? C12 N12 Ni7 175(2) . . ? N13 C13 W1 174(2) . . ? C13 N13 Ni12 176(2) . 2 ? N14 C14 W1 177(3) . . ? N15 C15 W1 176(2) . . ? C15 N15 Ni9 170(2) . . ? N16 C16 W1 175(3) . . ? C16 N16 Ni10 168(2) . . ? N17 C17 W1 177(3) . . ? N18 C18 W1 175(3) . . ? C22 W2 C21 95.6(11) . . ? C22 W2 C27 88.0(11) . . ? C21 W2 C27 144.7(11) . . ? C22 W2 C26 70.9(11) . . ? C21 W2 C26 74.1(10) . . ? C27 W2 C26 74.0(10) . . ? C22 W2 C28 145.6(13) . . ? C21 W2 C28 92.7(12) . . ? C27 W2 C28 103.9(12) . . ? C26 W2 C28 143.2(12) . . ? C22 W2 C23 142.3(11) . . ? C21 W2 C23 80.5(10) . . ? C27 W2 C23 75.6(10) . . ? C26 W2 C23 72.1(11) . . ? C28 W2 C23 71.9(13) . . ? C22 W2 C24 74.1(12) . . ? C21 W2 C24 141.3(11) . . ? C27 W2 C24 73.4(11) . . ? C26 W2 C24 132.3(11) . . ? C28 W2 C24 78.6(13) . . ? C23 W2 C24 130.0(12) . . ? C22 W2 C25 78.3(12) . . ? C21 W2 C25 72.3(11) . . ? C27 W2 C25 142.3(12) . . ? C26 W2 C25 131.1(12) . . ? C28 W2 C25 72.7(14) . . ? C23 W2 C25 133.6(11) . . ? C24 W2 C25 69.1(12) . . ? N21 C21 W2 178(2) . . ? C21 N21 Ni13 157(2) . . ? N22 C22 W2 178(3) . . ? C22 N22 Ni15 177(2) . . ? N23 C23 W2 178(3) . . ? C23 N23 Ni14 170(2) . . ? N24 C24 W2 179(3) . . ? N25 C25 W2 175(4) . . ? N26 C26 W2 175(2) . . ? C26 N26 Ni8 175(2) . . ? N27 C27 W2 174(3) . . ? C27 N27 Ni16 175(2) . 2_666 ? N28 C28 W2 173(4) . . ? C36 W3 C31 84.4(12) . . ? C36 W3 C38 73.3(12) . . ? C31 W3 C38 74.7(13) . . ? C36 W3 C35 144.7(11) . . ? C31 W3 C35 79.1(12) . . ? C38 W3 C35 72.3(13) . . ? C36 W3 C34 72.4(10) . . ? C31 W3 C34 139.2(11) . . ? C38 W3 C34 126.4(12) . . ? C35 W3 C34 137.2(10) . . ? C36 W3 C32 83.2(11) . . ? C31 W3 C32 71.9(12) . . ? C38 W3 C32 140.6(12) . . ? C35 W3 C32 119.9(12) . . ? C34 W3 C32 72.4(11) . . ? C36 W3 C37 93.1(11) . . ? C31 W3 C37 145.2(13) . . ? C38 W3 C37 71.3(13) . . ? C35 W3 C37 83.5(12) . . ? C34 W3 C37 70.9(11) . . ? C32 W3 C37 142.5(12) . . ? C36 W3 C33 144.6(11) . . ? C31 W3 C33 116.8(13) . . ? C38 W3 C33 137.2(12) . . ? C35 W3 C33 70.3(11) . . ? C34 W3 C33 73.5(10) . . ? C32 W3 C33 77.9(11) . . ? C37 W3 C33 84.4(12) . . ? N31 C31 W3 177(4) . . ? N32 C32 W3 173(3) . . ? C32 N32 Ni10 173(3) . . ? N33 C33 W3 175(3) . . ? C33 N33 Ni9 179(3) . . ? N34 C34 W3 178(2) . . ? C34 N34 Ni7 169(2) . . ? N35 C35 W3 174(3) . . ? N36 C36 W3 172(2) . . ? C36 N36 Ni12 175(2) . . ? N37 C37 W3 177(3) . . ? C37 N37 Ni11 170(3) . 2 ? N38 C38 W3 175(4) . . ? C44 W4 C42 141.1(11) . . ? C44 W4 C45 117.6(11) . . ? C42 W4 C45 69.6(10) . . ? C44 W4 C48 78.3(12) . . ? C42 W4 C48 135.1(11) . . ? C45 W4 C48 71.9(12) . . ? C44 W4 C41 72.7(12) . . ? C42 W4 C41 72.1(10) . . ? C45 W4 C41 77.6(11) . . ? C48 W4 C41 120.6(12) . . ? C44 W4 C47 143.3(12) . . ? C42 W4 C47 73.0(10) . . ? C45 W4 C47 82.2(11) . . ? C48 W4 C47 79.7(12) . . ? C41 W4 C47 144.0(11) . . ? C44 W4 C43 88.2(11) . . ? C42 W4 C43 72.7(10) . . ? C45 W4 C43 141.7(10) . . ? C48 W4 C43 145.0(11) . . ? C41 W4 C43 84.6(11) . . ? C47 W4 C43 93.4(11) . . ? C44 W4 C46 73.5(12) . . ? C42 W4 C46 128.9(11) . . ? C45 W4 C46 138.1(12) . . ? C48 W4 C46 71.5(12) . . ? C41 W4 C46 140.1(12) . . ? C47 W4 C46 71.8(12) . . ? C43 W4 C46 73.7(11) . . ? N41 C41 W4 178(3) . . ? C41 N41 Ni13 170(3) . . ? N42 C42 W4 179(2) . . ? C42 N42 Ni8 177(2) . . ? N43 C43 W4 172(2) . . ? C43 N43 Ni14 171(2) . . ? N44 C44 W4 174(3) . . ? N45 C45 W4 176(2) . . ? C45 N45 Ni16 172(2) . . ? N46 C46 W4 175(3) . . ? N47 C47 W4 177(3) . . ? C47 N47 Ni15 179(3) . 2_666 ? N48 C48 W4 177(3) . . ? C52 W5 C56 75.9(12) . . ? C52 W5 C51 71.2(12) . . ? C56 W5 C51 118.9(11) . . ? C52 W5 C58 139.4(11) . . ? C56 W5 C58 138.5(10) . . ? C51 W5 C58 71.8(9) . . ? C52 W5 C54 73.0(12) . . ? C56 W5 C54 74.6(10) . . ? C51 W5 C54 136.3(11) . . ? C58 W5 C54 127.7(9) . . ? C52 W5 C57 115.8(11) . . ? C56 W5 C57 70.7(10) . . ? C51 W5 C57 79.5(11) . . ? C58 W5 C57 72.8(9) . . ? C54 W5 C57 140.0(10) . . ? C52 W5 C55 144.4(11) . . ? C56 W5 C55 83.5(10) . . ? C51 W5 C55 144.2(10) . . ? C58 W5 C55 73.2(9) . . ? C54 W5 C55 73.7(10) . . ? C57 W5 C55 83.1(10) . . ? C52 W5 C53 88.0(11) . . ? C56 W5 C53 144.8(10) . . ? C51 W5 C53 83.6(10) . . ? C58 W5 C53 71.6(9) . . ? C54 W5 C53 70.7(10) . . ? C57 W5 C53 143.8(9) . . ? C55 W5 C53 92.8(10) . . ? N51 C51 W5 177(2) . . ? C51 N51 Ni9 176(2) . 2 ? N52 C52 W5 174(3) . . ? N53 C53 W5 171(3) . . ? C53 N53 Ni12 176(3) . . ? N54 C54 W5 173(3) . . ? N55 C55 W5 176(3) . . ? C55 N55 Ni10 172(2) . . ? N56 C56 W5 176(3) . . ? N57 C57 W5 176(3) . . ? C57 N57 Ni11 174(2) . . ? N58 C58 W5 178(2) . . ? C58 N58 Ni7 176(2) . . ? C67 W6 C65 70.0(12) . . ? C67 W6 C61 78.0(11) . . ? C65 W6 C61 133.9(12) . . ? C67 W6 C68 89.2(11) . . ? C65 W6 C68 76.7(11) . . ? C61 W6 C68 70.4(11) . . ? C67 W6 C62 140.7(10) . . ? C65 W6 C62 146.3(12) . . ? C61 W6 C62 77.0(11) . . ? C68 W6 C62 110.1(10) . . ? C67 W6 C63 70.0(9) . . ? C65 W6 C63 123.3(11) . . ? C61 W6 C63 72.0(10) . . ? C68 W6 C63 140.0(10) . . ? C62 W6 C63 73.6(10) . . ? C67 W6 C64 97.3(11) . . ? C65 W6 C64 75.0(12) . . ? C61 W6 C64 143.0(11) . . ? C68 W6 C64 146.6(11) . . ? C62 W6 C64 85.1(10) . . ? C63 W6 C64 72.0(10) . . ? C67 W6 C66 145.6(10) . . ? C65 W6 C66 76.0(12) . . ? C61 W6 C66 125.2(11) . . ? C68 W6 C66 78.0(11) . . ? C62 W6 C66 73.5(11) . . ? C63 W6 C66 137.0(10) . . ? C64 W6 C66 78.4(11) . . ? N61 C61 W6 177(2) . . ? C61 N61 Ni15 174(2) . . ? N62 C62 W6 174(3) . . ? C62 N62 Ni14 170(3) . 2_666 ? N63 C63 W6 176(2) . . ? C63 N63 Ni8 174(2) . . ? N64 C64 W6 176(3) . . ? C64 N64 Ni16 173(3) . . ? N65 C65 W6 176(3) . . ? N66 C66 W6 178(3) . . ? N67 C67 W6 171(2) . . ? C67 N67 Ni13 164(2) . . ? N68 C68 W6 174(2) . . ? N12 Ni7 N12 180.0(16) 2 . ? N12 Ni7 N58 90.5(8) 2 . ? N12 Ni7 N58 89.5(8) . . ? N12 Ni7 N58 89.5(8) 2 2 ? N12 Ni7 N58 90.5(8) . 2 ? N58 Ni7 N58 180.0(12) . 2 ? N12 Ni7 N34 89.8(9) 2 2 ? N12 Ni7 N34 90.2(9) . 2 ? N58 Ni7 N34 91.3(8) . 2 ? N58 Ni7 N34 88.7(8) 2 2 ? N12 Ni7 N34 90.2(9) 2 . ? N12 Ni7 N34 89.8(9) . . ? N58 Ni7 N34 88.7(8) . . ? N58 Ni7 N34 91.3(8) 2 . ? N34 Ni7 N34 180.0(18) 2 . ? N26 Ni8 N26 180.000(3) 2_666 . ? N26 Ni8 N42 90.8(8) 2_666 . ? N26 Ni8 N42 89.2(8) . . ? N26 Ni8 N42 89.2(8) 2_666 2_666 ? N26 Ni8 N42 90.8(8) . 2_666 ? N42 Ni8 N42 180.0(8) . 2_666 ? N26 Ni8 N63 92.2(9) 2_666 . ? N26 Ni8 N63 87.8(9) . . ? N42 Ni8 N63 90.2(8) . . ? N42 Ni8 N63 89.8(8) 2_666 . ? N26 Ni8 N63 87.8(9) 2_666 2_666 ? N26 Ni8 N63 92.2(9) . 2_666 ? N42 Ni8 N63 89.8(8) . 2_666 ? N42 Ni8 N63 90.2(8) 2_666 2_666 ? N63 Ni8 N63 180.0(8) . 2_666 ? N15 Ni9 N92 93.8(11) . . ? N15 Ni9 N33 93.0(9) . . ? N92 Ni9 N33 171.5(11) . . ? N15 Ni9 N91 170.6(11) . . ? N92 Ni9 N91 77.0(12) . . ? N33 Ni9 N91 96.2(10) . . ? N15 Ni9 N51 90.8(10) . 2 ? N92 Ni9 N51 93.7(11) . 2 ? N33 Ni9 N51 91.4(10) . 2 ? N91 Ni9 N51 91.2(10) . 2 ? N15 Ni9 O91 88.9(9) . . ? N92 Ni9 O91 88.7(11) . . ? N33 Ni9 O91 86.2(10) . . ? N91 Ni9 O91 89.5(10) . . ? N51 Ni9 O91 177.6(10) 2 . ? C90 N91 C94 119(3) . . ? C90 N91 Ni9 124(3) . . ? C94 N91 Ni9 117(2) . . ? C95 N92 C99 115(3) . . ? C95 N92 Ni9 121(3) . . ? C99 N92 Ni9 124(3) . . ? N91 C90 C91 122(4) . . ? N91 C90 H90 118.9 . . ? C91 C90 H90 118.9 . . ? C90 C91 C92 116(4) . . ? C90 C91 H91 122.1 . . ? C92 C91 H91 122.1 . . ? C93 C92 C91 122(4) . . ? C93 C92 H92 119.1 . . ? C91 C92 H92 119.1 . . ? C94 C93 C92 114(4) . . ? C94 C93 H93 123.1 . . ? C92 C93 H93 123.1 . . ? N91 C94 C93 127(4) . . ? N91 C94 C95 115(3) . . ? C93 C94 C95 117(3) . . ? C96 C95 N92 129(4) . . ? C96 C95 C94 122(4) . . ? N92 C95 C94 110(3) . . ? C95 C96 C97 118(4) . . ? C95 C96 H96 121.1 . . ? C97 C96 H96 121.1 . . ? C98 C97 C96 113(5) . . ? C98 C97 H97 123.5 . . ? C96 C97 H97 123.5 . . ? C99 C98 C97 121(6) . . ? C99 C98 H98 119.3 . . ? C97 C98 H98 119.3 . . ? C98 C99 N92 124(4) . . ? C98 C99 H99 118.2 . . ? N92 C99 H99 118.2 . . ? N101 Ni10 N102 78.3(10) . . ? N101 Ni10 N55 91.6(10) . . ? N102 Ni10 N55 93.6(10) . . ? N101 Ni10 N16 95.4(9) . . ? N102 Ni10 N16 172.7(10) . . ? N55 Ni10 N16 90.2(9) . . ? N101 Ni10 N32 171.0(10) . . ? N102 Ni10 N32 93.2(10) . . ? N55 Ni10 N32 91.8(9) . . ? N16 Ni10 N32 92.9(9) . . ? N101 Ni10 O101 89.5(9) . . ? N102 Ni10 O101 89.4(9) . . ? N55 Ni10 O101 176.9(9) . . ? N16 Ni10 O101 86.8(8) . . ? N32 Ni10 O101 87.4(9) . . ? C201 O101 Ni10 123(3) . . ? O101 C201 C202 149(7) . . ? O101 C201 H20A 99.4 . . ? C202 C201 H20A 99.4 . . ? O101 C201 H20B 99.4 . . ? C202 C201 H20B 99.4 . . ? H20A C201 H20B 104.0 . . ? C201 C202 H20C 109.5 . . ? C201 C202 H20D 109.5 . . ? H20C C202 H20D 109.5 . . ? C201 C202 H20E 109.5 . . ? H20C C202 H20E 109.5 . . ? H20D C202 H20E 109.5 . . ? C100 N101 C104 115(2) . . ? C100 N101 Ni10 128.2(19) . . ? C104 N101 Ni10 116.7(19) . . ? C105 N102 C109 118(3) . . ? C105 N102 Ni10 115(2) . . ? C109 N102 Ni10 125(2) . . ? C101 C100 N101 124(3) . . ? C101 C100 H100 118.0 . . ? N101 C100 H100 118.0 . . ? C100 C101 C102 119(3) . . ? C100 C101 H101 120.3 . . ? C102 C101 H101 120.3 . . ? C101 C102 C103 119(3) . . ? C101 C102 H102 120.4 . . ? C103 C102 H102 120.4 . . ? C104 C103 C102 120(3) . . ? C104 C103 H103 120.1 . . ? C102 C103 H103 120.1 . . ? C103 C104 N101 122(3) . . ? C103 C104 C105 126(3) . . ? N101 C104 C105 112(3) . . ? N102 C105 C106 124(3) . . ? N102 C105 C104 114(3) . . ? C106 C105 C104 121(3) . . ? C105 C106 C107 117(3) . . ? C105 C106 H106 121.5 . . ? C107 C106 H106 121.5 . . ? C108 C107 C106 118(3) . . ? C108 C107 H107 120.8 . . ? C106 C107 H107 120.8 . . ? C107 C108 C109 121(3) . . ? C107 C108 H108 119.4 . . ? C109 C108 H108 119.4 . . ? N102 C109 C108 121(3) . . ? N102 C109 H109 119.7 . . ? C108 C109 H109 119.7 . . ? N37 Ni11 N57 93.5(10) 2 . ? N37 Ni11 N112 93.2(10) 2 . ? N57 Ni11 N112 173.3(11) . . ? N37 Ni11 N111 171.9(10) 2 . ? N57 Ni11 N111 94.5(10) . . ? N112 Ni11 N111 78.8(10) . . ? N37 Ni11 N11 94.3(9) 2 . ? N57 Ni11 N11 91.8(9) . . ? N112 Ni11 N11 87.5(9) . . ? N111 Ni11 N11 86.8(9) . . ? N37 Ni11 O111 90.6(9) 2 . ? N57 Ni11 O111 89.5(9) . . ? N112 Ni11 O111 90.6(9) . . ? N111 Ni11 O111 88.1(9) . . ? N11 Ni11 O111 174.9(9) . . ? C211 O111 Ni11 123(3) . . ? O111 C211 C212 110.6(15) . . ? O111 C211 H21A 109.5 . . ? C212 C211 H21A 109.5 . . ? O111 C211 H21B 109.5 . . ? C212 C211 H21B 109.5 . . ? H21A C211 H21B 108.1 . . ? C211 C212 H21C 109.5 . . ? C211 C212 H21D 109.5 . . ? H21C C212 H21D 109.5 . . ? C211 C212 H21E 109.5 . . ? H21C C212 H21E 109.5 . . ? H21D C212 H21E 109.5 . . ? C110 N111 C114 116(3) . . ? C110 N111 Ni11 127(2) . . ? C114 N111 Ni11 116(2) . . ? C119 N112 C115 115(3) . . ? C119 N112 Ni11 127(2) . . ? C115 N112 Ni11 117.6(19) . . ? N111 C110 C111 127(3) . . ? N111 C110 H110 116.6 . . ? C111 C110 H110 116.6 . . ? C110 C111 C112 115(3) . . ? C110 C111 H111 122.6 . . ? C112 C111 H111 122.6 . . ? C113 C112 C111 120(4) . . ? C113 C112 H112 120.1 . . ? C111 C112 H112 120.1 . . ? C112 C113 C114 121(4) . . ? C112 C113 H113 119.5 . . ? C114 C113 H113 119.5 . . ? N111 C114 C113 121(3) . . ? N111 C114 C115 116(3) . . ? C113 C114 C115 123(3) . . ? C116 C115 N112 123(3) . . ? C116 C115 C114 126(3) . . ? N112 C115 C114 111(3) . . ? C115 C116 C117 120(4) . . ? C115 C116 H116 120.2 . . ? C117 C116 H116 120.2 . . ? C118 C117 C116 118(4) . . ? C118 C117 H117 120.8 . . ? C116 C117 H117 120.8 . . ? C117 C118 C119 121(4) . . ? C117 C118 H118 119.4 . . ? C119 C118 H118 119.4 . . ? N112 C119 C118 122(3) . . ? N112 C119 H119 118.8 . . ? C118 C119 H119 118.8 . . ? N53 Ni12 N13 91.7(10) . 2 ? N53 Ni12 N121 94.2(10) . . ? N13 Ni12 N121 174.0(9) 2 . ? N53 Ni12 O121 90.0(9) . . ? N13 Ni12 O121 88.7(9) 2 . ? N121 Ni12 O121 92.2(9) . . ? N53 Ni12 N36 90.0(10) . . ? N13 Ni12 N36 92.0(9) 2 . ? N121 Ni12 N36 87.1(10) . . ? O121 Ni12 N36 179.3(9) . . ? N53 Ni12 N122 172.9(9) . . ? N13 Ni12 N122 94.9(9) 2 . ? N121 Ni12 N122 79.2(9) . . ? O121 Ni12 N122 87.7(9) . . ? N36 Ni12 N122 92.2(9) . . ? C221 O121 Ni12 126(3) . . ? O121 C221 C222 109.1(15) . . ? O121 C221 H22A 109.9 . . ? C222 C221 H22A 109.9 . . ? O121 C221 H22B 109.9 . . ? C222 C221 H22B 109.9 . . ? H22A C221 H22B 108.3 . . ? C221 C222 H22C 109.5 . . ? C221 C222 H22D 109.5 . . ? H22C C222 H22D 109.5 . . ? C221 C222 H22E 109.5 . . ? H22C C222 H22E 109.5 . . ? H22D C222 H22E 109.5 . . ? C120 N121 C124 118(3) . . ? C120 N121 Ni12 127(2) . . ? C124 N121 Ni12 115(2) . . ? C125 N122 C129 119(3) . . ? C125 N122 Ni12 115.5(19) . . ? C129 N122 Ni12 126(2) . . ? N121 C120 C121 124(3) . . ? N121 C120 H120 117.8 . . ? C121 C120 H120 117.8 . . ? C120 C121 C122 116(3) . . ? C120 C121 H121 122.0 . . ? C122 C121 H121 122.0 . . ? C123 C122 C121 121(3) . . ? C123 C122 H122 119.3 . . ? C121 C122 H122 119.3 . . ? C122 C123 C124 118(3) . . ? C122 C123 H123 121.2 . . ? C124 C123 H123 121.2 . . ? N121 C124 C123 122(3) . . ? N121 C124 C125 115(3) . . ? C123 C124 C125 122(3) . . ? N122 C125 C126 123(3) . . ? N122 C125 C124 115(3) . . ? C126 C125 C124 122(3) . . ? C125 C126 C127 114(3) . . ? C125 C126 H126 123.2 . . ? C127 C126 H126 123.2 . . ? C128 C127 C126 123(3) . . ? C128 C127 H127 118.4 . . ? C126 C127 H127 118.4 . . ? C127 C128 C129 121(3) . . ? C127 C128 H128 119.6 . . ? C129 C128 H128 119.6 . . ? N122 C129 C128 120(3) . . ? N122 C129 H129 119.9 . . ? C128 C129 H129 119.9 . . ? N67 Ni13 N131 167.1(9) . . ? N67 Ni13 N41 93.9(9) . . ? N131 Ni13 N41 93.0(9) . . ? N67 Ni13 N132 94.0(9) . . ? N131 Ni13 N132 80.1(10) . . ? N41 Ni13 N132 170.8(10) . . ? N67 Ni13 N21 90.9(9) . . ? N131 Ni13 N21 100.2(10) . . ? N41 Ni13 N21 88.9(9) . . ? N132 Ni13 N21 86.4(9) . . ? N67 Ni13 O131 83.8(8) . . ? N131 Ni13 O131 85.1(9) . . ? N41 Ni13 O131 91.5(9) . . ? N132 Ni13 O131 93.9(9) . . ? N21 Ni13 O131 174.7(9) . . ? C130 N131 C134 118(3) . . ? C130 N131 Ni13 127(2) . . ? C134 N131 Ni13 115.0(19) . . ? C139 N132 C135 121(3) . . ? C139 N132 Ni13 125(2) . . ? C135 N132 Ni13 113(2) . . ? N131 C130 C131 123(3) . . ? N131 C130 H130 118.3 . . ? C131 C130 H130 118.3 . . ? C130 C131 C132 118(3) . . ? C130 C131 H131 120.8 . . ? C132 C131 H131 120.8 . . ? C133 C132 C131 118(3) . . ? C133 C132 H132 120.9 . . ? C131 C132 H132 120.9 . . ? C132 C133 C134 119(3) . . ? C132 C133 H133 120.7 . . ? C134 C133 H133 120.7 . . ? N131 C134 C133 123(3) . . ? N131 C134 C135 115(3) . . ? C133 C134 C135 122(3) . . ? N132 C135 C136 120(3) . . ? N132 C135 C134 116(3) . . ? C136 C135 C134 123(3) . . ? C137 C136 C135 118(3) . . ? C137 C136 H136 121.2 . . ? C135 C136 H136 121.2 . . ? C136 C137 C138 118(3) . . ? C136 C137 H137 121.0 . . ? C138 C137 H137 121.0 . . ? C139 C138 C137 120(3) . . ? C139 C138 H138 119.9 . . ? C137 C138 H138 119.9 . . ? N132 C139 C138 122(3) . . ? N132 C139 H139 118.8 . . ? C138 C139 H139 118.8 . . ? N43 Ni14 N23 89.5(10) . . ? N43 Ni14 N62 95.7(10) . 2_666 ? N23 Ni14 N62 94.5(10) . 2_666 ? N43 Ni14 N142 94.5(9) . . ? N23 Ni14 N142 93.1(10) . . ? N62 Ni14 N142 167.4(10) 2_666 . ? N43 Ni14 O141 178.1(9) . . ? N23 Ni14 O141 91.5(10) . . ? N62 Ni14 O141 85.9(9) 2_666 . ? N142 Ni14 O141 83.9(9) . . ? N43 Ni14 N141 86.8(10) . . ? N23 Ni14 N141 171.7(10) . . ? N62 Ni14 N141 93.3(10) 2_666 . ? N142 Ni14 N141 79.8(10) . . ? O141 Ni14 N141 92.0(10) . . ? C241 O141 Ni14 123(5) . . ? O141 C241 C242 121(10) . . ? O141 C241 H24A 107.2 . . ? C242 C241 H24A 107.2 . . ? O141 C241 H24B 107.2 . . ? C242 C241 H24B 107.2 . . ? H24A C241 H24B 106.8 . . ? C241 C242 H24C 109.5 . . ? C241 C242 H24D 109.5 . . ? H24C C242 H24D 109.5 . . ? C241 C242 H24E 109.5 . . ? H24C C242 H24E 109.5 . . ? H24D C242 H24E 109.5 . . ? C144 N141 C140 120(3) . . ? C144 N141 Ni14 117(2) . . ? C140 N141 Ni14 122(2) . . ? C149 N142 C145 123(3) . . ? C149 N142 Ni14 126(2) . . ? C145 N142 Ni14 111(2) . . ? N141 C140 C141 120(3) . . ? N141 C140 H140 119.9 . . ? C141 C140 H140 119.9 . . ? C142 C141 C140 116(4) . . ? C142 C141 H141 122.0 . . ? C140 C141 H141 122.0 . . ? C141 C142 C143 123(4) . . ? C141 C142 H142 118.4 . . ? C143 C142 H142 118.4 . . ? C144 C143 C142 111(3) . . ? C144 C143 H143 124.4 . . ? C142 C143 H143 124.4 . . ? N141 C144 C143 129(3) . . ? N141 C144 C145 111(3) . . ? C143 C144 C145 119(3) . . ? N142 C145 C146 117(3) . . ? N142 C145 C144 120(3) . . ? C146 C145 C144 122(3) . . ? C147 C146 C145 119(3) . . ? C147 C146 H146 120.5 . . ? C145 C146 H146 120.5 . . ? C146 C147 C148 123(4) . . ? C146 C147 H147 118.5 . . ? C148 C147 H147 118.5 . . ? C147 C148 C149 111(4) . . ? C147 C148 H148 124.4 . . ? C149 C148 H148 124.4 . . ? N142 C149 C148 125(3) . . ? N142 C149 H149 117.3 . . ? C148 C149 H149 117.3 . . ? N47 Ni15 N61 90.3(9) 2_666 . ? N47 Ni15 N22 93.0(10) 2_666 . ? N61 Ni15 N22 91.0(10) . . ? N47 Ni15 N151 94.0(10) 2_666 . ? N61 Ni15 N151 175.2(10) . . ? N22 Ni15 N151 91.0(11) . . ? N47 Ni15 N152 172.8(10) 2_666 . ? N61 Ni15 N152 95.9(9) . . ? N22 Ni15 N152 90.5(10) . . ? N151 Ni15 N152 79.7(10) . . ? N47 Ni15 O151 89.0(10) 2_666 . ? N61 Ni15 O151 91.5(10) . . ? N22 Ni15 O151 176.8(10) . . ? N151 Ni15 O151 86.4(11) . . ? N152 Ni15 O151 87.2(10) . . ? C251 O151 Ni15 128(3) . . ? O151 C251 C252 109.3(15) . . ? O151 C251 H25A 109.8 . . ? C252 C251 H25A 109.8 . . ? O151 C251 H25B 109.8 . . ? C252 C251 H25B 109.8 . . ? H25A C251 H25B 108.3 . . ? C251 C252 H25C 109.5 . . ? C251 C252 H25D 109.5 . . ? H25C C252 H25D 109.5 . . ? C251 C252 H25E 109.5 . . ? H25C C252 H25E 109.5 . . ? H25D C252 H25E 109.5 . . ? C150 N151 C154 119(4) . . ? C150 N151 Ni15 126(3) . . ? C154 N151 Ni15 115(3) . . ? C155 N152 C159 120(3) . . ? C155 N152 Ni15 116(3) . . ? C159 N152 Ni15 124(2) . . ? N151 C150 C151 121(5) . . ? N151 C150 H150 119.5 . . ? C151 C150 H150 119.5 . . ? C150 C151 C152 122(5) . . ? C150 C151 H151 119.0 . . ? C152 C151 H151 119.0 . . ? C153 C152 C151 115(6) . . ? C153 C152 H152 122.4 . . ? C151 C152 H152 122.4 . . ? C152 C153 C154 118(6) . . ? C152 C153 H153 120.9 . . ? C154 C153 H153 120.9 . . ? N151 C154 C153 124(5) . . ? N151 C154 C155 111(4) . . ? C153 C154 C155 125(5) . . ? N152 C155 C156 125(4) . . ? N152 C155 C154 117(4) . . ? C156 C155 C154 117(4) . . ? C157 C156 C155 116(5) . . ? C157 C156 H156 122.1 . . ? C155 C156 H156 122.1 . . ? C158 C157 C156 122(5) . . ? C158 C157 H157 119.0 . . ? C156 C157 H157 119.0 . . ? C157 C158 C159 117(4) . . ? C157 C158 H158 121.6 . . ? C159 C158 H158 121.6 . . ? N152 C159 C158 120(4) . . ? N152 C159 H159 120.1 . . ? C158 C159 H159 120.1 . . ? N161 Ni16 N64 93.3(10) . . ? N161 Ni16 N27 174.5(10) . 2_666 ? N64 Ni16 N27 91.5(9) . 2_666 ? N161 Ni16 N162 79.9(10) . . ? N64 Ni16 N162 172.6(10) . . ? N27 Ni16 N162 95.4(10) 2_666 . ? N161 Ni16 N45 84.8(10) . . ? N64 Ni16 N45 93.0(10) . . ? N27 Ni16 N45 92.4(9) 2_666 . ? N162 Ni16 N45 89.2(10) . . ? N161 Ni16 O161 94.0(10) . . ? N64 Ni16 O161 90.8(10) . . ? N27 Ni16 O161 88.5(9) 2_666 . ? N162 Ni16 O161 87.0(10) . . ? N45 Ni16 O161 176.1(10) . . ? C160 N161 C164 114(3) . . ? C160 N161 Ni16 130(2) . . ? C164 N161 Ni16 115(2) . . ? C165 N162 C169 119(3) . . ? C165 N162 Ni16 115(2) . . ? C169 N162 Ni16 126(2) . . ? N161 C160 C161 123(3) . . ? N161 C160 H160 118.7 . . ? C161 C160 H160 118.7 . . ? C162 C161 C160 120(4) . . ? C162 C161 H161 120.2 . . ? C160 C161 H161 120.2 . . ? C163 C162 C161 117(4) . . ? C163 C162 H162 121.6 . . ? C161 C162 H162 121.6 . . ? C162 C163 C164 120(4) . . ? C162 C163 H163 119.8 . . ? C164 C163 H163 119.8 . . ? N161 C164 C163 126(4) . . ? N161 C164 C165 114(3) . . ? C163 C164 C165 120(3) . . ? N162 C165 C166 124(3) . . ? N162 C165 C164 114(3) . . ? C166 C165 C164 121(3) . . ? C165 C166 C167 114(4) . . ? C165 C166 H166 123.0 . . ? C167 C166 H166 123.0 . . ? C168 C167 C166 121(5) . . ? C168 C167 H167 119.3 . . ? C166 C167 H167 119.3 . . ? C169 C168 C167 121(4) . . ? C169 C168 H168 119.4 . . ? C167 C168 H168 119.4 . . ? C168 C169 N162 120(4) . . ? C168 C169 H169 119.9 . . ? N162 C169 H169 119.9 . . ? O17W O16W O18W 157(9) . . ? O17W O16W O21W 81(6) . . ? O18W O16W O21W 84(7) . . ? O14W O19W O15W 82(7) . . ? _diffrn_measured_fraction_theta_max 0.656 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.656 _refine_diff_density_max 7.337 _refine_diff_density_min -3.005 _refine_diff_density_rms 0.356 #===END data_2a _database_code_depnum_ccdc_archive 'CCDC 876829' #TrackingRef '- clusters1-4_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; {Ni[Ni(4,4'dmbpy)(H2O)]8[W(CN)8]6}*18H2O ; _chemical_name_common (Ni(Ni(4,4'dmbpy)(H2O))8(W(CN)8)6)*18H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C152 H116 N64 Ni9 O12 W6' _chemical_formula_weight 4662.35 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' W W -0.8490 6.8722 '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 19.195(5) _cell_length_b 19.843(5) _cell_length_c 20.321(5) _cell_angle_alpha 93.918(5) _cell_angle_beta 111.191(5) _cell_angle_gamma 115.588(5) _cell_volume 6273(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2268 _exptl_absorpt_coefficient_mu 3.447 _exptl_absorpt_correction_T_min 0.3394 _exptl_absorpt_correction_T_max 0.7244 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details '(DENZO-SMN; Otwinowski & Minor, 1997)' _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 KappaCCD _diffrn_measurement_method '\f and \o scans to fill Ewald sphere' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 47802 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.50 _reflns_number_total 28489 _reflns_number_gt 20399 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (ALTOMARE et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.6387P] 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 28489 _refine_ls_number_parameters 1096 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.356587(12) 0.535274(11) 0.671554(10) 0.03275(5) Uani 1 1 d . . . W2 W 0.486449(13) 0.733343(12) 0.390718(11) 0.03622(6) Uani 1 1 d . . . W3 W 0.193102(12) 0.297440(12) 0.287873(10) 0.03818(6) Uani 1 1 d . . . Ni1 Ni 0.5000 0.5000 0.5000 0.02766(16) Uani 1 2 d S . . Ni2 Ni 0.59245(4) 0.81420(4) 0.68086(4) 0.04327(15) Uani 1 1 d . . . Ni3 Ni 0.36842(4) 0.49258(4) 0.16744(3) 0.04214(15) Uani 1 1 d . . . Ni4 Ni 0.20214(4) 0.23495(4) 0.53953(4) 0.04041(15) Uani 1 1 d . . . Ni5 Ni 0.18986(4) 0.54861(4) 0.40148(4) 0.04214(15) Uani 1 1 d . . . C11 C 0.4099(3) 0.5161(3) 0.5997(2) 0.0339(10) Uani 1 1 d . . . N11 N 0.4384(3) 0.5073(2) 0.5619(2) 0.0357(9) Uani 1 1 d . . . C12 C 0.4552(3) 0.6467(3) 0.6760(3) 0.0421(11) Uani 1 1 d . . . N12 N 0.5049(3) 0.7055(3) 0.6773(3) 0.0477(11) Uani 1 1 d . . . C13 C 0.4707(3) 0.5313(3) 0.7419(3) 0.0405(11) Uani 1 1 d . . . N13 N 0.5278(3) 0.5243(3) 0.7750(2) 0.0497(11) Uani 1 1 d . . . C14 C 0.2910(3) 0.4126(3) 0.6212(3) 0.0413(11) Uani 1 1 d . . . N14 N 0.2547(3) 0.3477(3) 0.5943(3) 0.0467(10) Uani 1 1 d . . . C15 C 0.2914(3) 0.5534(3) 0.5681(3) 0.0389(11) Uani 1 1 d . . . N15 N 0.2571(3) 0.5576(3) 0.5114(3) 0.0459(10) Uani 1 1 d . . . C16 C 0.2244(4) 0.4966(4) 0.6517(3) 0.0493(13) Uani 1 1 d . . . N16 N 0.1537(3) 0.4732(4) 0.6399(3) 0.0692(16) Uani 1 1 d . . . C17 C 0.3347(4) 0.4847(4) 0.7592(3) 0.0536(14) Uani 1 1 d . . . N17 N 0.3243(4) 0.4575(4) 0.8044(3) 0.0737(17) Uani 1 1 d . . . C18 C 0.3661(4) 0.6272(4) 0.7436(4) 0.0602(16) Uani 1 1 d . . . N18 N 0.3705(5) 0.6756(4) 0.7817(4) 0.087(2) Uani 1 1 d . . . C21 C 0.4894(3) 0.6380(3) 0.4356(2) 0.0341(10) Uani 1 1 d . . . N21 N 0.4897(3) 0.5881(2) 0.4584(2) 0.0365(9) Uani 1 1 d . . . C22 C 0.5218(3) 0.7696(3) 0.5068(3) 0.0429(11) Uani 1 1 d . . . N22 N 0.5428(3) 0.7864(3) 0.5682(3) 0.0528(12) Uani 1 1 d . . . C23 C 0.4330(3) 0.6368(3) 0.2975(3) 0.0408(11) Uani 1 1 d . . . N23 N 0.4115(3) 0.5877(3) 0.2499(2) 0.0516(11) Uani 1 1 d . . . C24 C 0.6120(3) 0.7453(3) 0.4198(3) 0.0437(12) Uani 1 1 d . . . N24 N 0.6780(3) 0.7519(3) 0.4353(3) 0.0512(11) Uani 1 1 d . . . C25 C 0.3637(3) 0.6620(3) 0.3931(3) 0.0418(11) Uani 1 1 d . . . N25 N 0.3006(3) 0.6247(3) 0.3947(3) 0.0537(12) Uani 1 1 d . . . C26 C 0.4035(6) 0.7782(5) 0.3414(6) 0.086(3) Uani 1 1 d . . . N26 N 0.3578(6) 0.8017(6) 0.3134(7) 0.138(4) Uani 1 1 d . . . C27 C 0.5201(5) 0.7776(4) 0.3059(4) 0.0603(16) Uani 1 1 d . . . N27 N 0.5384(5) 0.7989(4) 0.2609(4) 0.092(2) Uani 1 1 d . . . C28 C 0.5729(5) 0.8579(4) 0.4330(4) 0.071(2) Uani 1 1 d . . . N28 N 0.6210(6) 0.9222(4) 0.4539(5) 0.111(3) Uani 1 1 d . . . C31 C 0.3195(3) 0.3773(3) 0.3715(3) 0.0348(10) Uani 1 1 d . . . N31 N 0.3857(3) 0.4203(2) 0.4162(2) 0.0363(9) Uani 1 1 d . . . C32 C 0.2734(4) 0.2446(3) 0.3022(3) 0.0492(13) Uani 1 1 d . . . N32 N 0.3186(3) 0.2200(3) 0.3095(3) 0.0609(13) Uani 1 1 d . . . C33 C 0.2582(3) 0.3788(3) 0.2371(3) 0.0448(12) Uani 1 1 d . . . N33 N 0.2956(3) 0.4207(3) 0.2122(2) 0.0507(11) Uani 1 1 d . . . C34 C 0.1915(3) 0.2773(3) 0.3888(3) 0.0440(12) Uani 1 1 d . . . N34 N 0.1940(3) 0.2656(3) 0.4451(3) 0.0522(12) Uani 1 1 d . . . C35 C 0.1937(3) 0.3977(3) 0.3367(3) 0.0430(12) Uani 1 1 d . . . N35 N 0.1971(3) 0.4525(3) 0.3649(3) 0.0531(12) Uani 1 1 d . . . C36 C 0.0784(5) 0.2961(5) 0.2202(5) 0.089(3) Uani 1 1 d . . . N36 N 0.0162(6) 0.2957(7) 0.1795(6) 0.160(5) Uani 1 1 d . . . C37 C 0.1538(5) 0.2341(4) 0.1763(3) 0.071(2) Uani 1 1 d . . . N37 N 0.1345(5) 0.2006(5) 0.1204(3) 0.108(3) Uani 1 1 d . . . C38 C 0.0999(5) 0.1782(4) 0.2698(4) 0.074(2) Uani 1 1 d . . . N38 N 0.0530(6) 0.1159(5) 0.2612(5) 0.127(4) Uani 1 1 d . . . N201 N 0.5200(3) 0.8665(3) 0.6828(3) 0.0539(12) Uani 1 1 d . . . C202 C 0.5621(5) 0.9448(4) 0.6938(4) 0.0634(16) Uani 1 1 d . . . C203 C 0.5233(5) 0.9891(4) 0.7000(5) 0.076(2) Uani 1 1 d . . . H203 H 0.5519 1.0422 0.7057 0.091 Uiso 1 1 calc R . . C204 C 0.4429(5) 0.9540(5) 0.6979(5) 0.079(2) Uani 1 1 d . . . C205 C 0.4028(5) 0.8749(5) 0.6872(5) 0.086(2) Uani 1 1 d . . . H205 H 0.3481 0.8494 0.6851 0.104 Uiso 1 1 calc R . . C206 C 0.4422(5) 0.8328(4) 0.6796(5) 0.075(2) Uani 1 1 d . . . H206 H 0.4131 0.7793 0.6719 0.090 Uiso 1 1 calc R . . C207 C 0.4031(6) 1.0013(6) 0.7097(7) 0.111(3) Uani 1 1 d . . . H20A H 0.4408 1.0549 0.7159 0.166 Uiso 1 1 calc R . . H20B H 0.3937 0.9956 0.7527 0.166 Uiso 1 1 calc R . . H20C H 0.3493 0.9839 0.6680 0.166 Uiso 1 1 calc R . . N208 N 0.6770(3) 0.9287(3) 0.6938(3) 0.0571(13) Uani 1 1 d . . . C209 C 0.6489(5) 0.9779(4) 0.6981(4) 0.0645(17) Uani 1 1 d . . . C210 C 0.7019(6) 1.0585(5) 0.7121(6) 0.101(3) Uani 1 1 d . . . H210 H 0.6808 1.0924 0.7149 0.121 Uiso 1 1 calc R . . C211 C 0.7852(6) 1.0864(5) 0.7215(7) 0.107(3) Uani 1 1 d . . . C212 C 0.8155(6) 1.0355(6) 0.7181(6) 0.100(3) Uani 1 1 d . . . H212 H 0.8723 1.0536 0.7266 0.120 Uiso 1 1 calc R . . C213 C 0.7588(5) 0.9550(5) 0.7014(5) 0.083(2) Uani 1 1 d . . . H213 H 0.7774 0.9199 0.6957 0.099 Uiso 1 1 calc R . . C214 C 0.8455(9) 1.1737(6) 0.7383(11) 0.197(8) Uani 1 1 d . . . H21A H 0.9010 1.1825 0.7445 0.296 Uiso 1 1 calc R . . H21B H 0.8506 1.2004 0.7825 0.296 Uiso 1 1 calc R . . H21C H 0.8226 1.1929 0.6985 0.296 Uiso 1 1 calc R . . O215 O 0.6423(4) 0.8455(3) 0.7980(3) 0.0815(15) Uani 1 1 d . . . N301 N 0.3236(3) 0.4039(3) 0.0770(2) 0.0570(13) Uani 1 1 d . . . C302 C 0.3423(4) 0.4294(4) 0.0220(3) 0.0596(16) Uani 1 1 d . . . C303 C 0.3067(6) 0.3763(5) -0.0457(4) 0.097(3) Uani 1 1 d . . . H303 H 0.3220 0.3928 -0.0825 0.116 Uiso 1 1 calc R . . C304 C 0.2500(8) 0.3012(6) -0.0571(5) 0.126(4) Uani 1 1 d . . . C305 C 0.2356(7) 0.2762(6) 0.0008(5) 0.120(4) Uani 1 1 d . . . H305 H 0.2026 0.2238 -0.0038 0.145 Uiso 1 1 calc R . . C306 C 0.2715(5) 0.3307(4) 0.0651(4) 0.076(2) Uani 1 1 d . . . H306 H 0.2578 0.3145 0.1028 0.091 Uiso 1 1 calc R . . C307 C 0.2088(13) 0.2439(8) -0.1319(6) 0.247(12) Uani 1 1 d . . . H30A H 0.1697 0.1935 -0.1313 0.371 Uiso 1 1 calc R . . H30B H 0.2527 0.2410 -0.1421 0.371 Uiso 1 1 calc R . . H30C H 0.1783 0.2611 -0.1691 0.371 Uiso 1 1 calc R . . N308 N 0.4244(3) 0.5543(3) 0.1055(2) 0.0498(11) Uani 1 1 d . . . C309 C 0.4023(4) 0.5120(4) 0.0393(3) 0.0539(14) Uani 1 1 d . . . C310 C 0.4337(5) 0.5450(5) -0.0089(4) 0.078(2) Uani 1 1 d . . . H310 H 0.4193 0.5139 -0.0531 0.093 Uiso 1 1 calc R . . C311 C 0.4859(5) 0.6239(5) 0.0088(4) 0.074(2) Uani 1 1 d . . . C312 C 0.5054(5) 0.6676(5) 0.0760(4) 0.083(2) Uani 1 1 d . . . H312 H 0.5395 0.7212 0.0893 0.099 Uiso 1 1 calc R . . C313 C 0.4743(4) 0.6317(4) 0.1233(4) 0.0684(19) Uani 1 1 d . . . H313 H 0.4883 0.6616 0.1681 0.082 Uiso 1 1 calc R . . C314 C 0.5157(7) 0.6638(7) -0.0447(5) 0.118(4) Uani 1 1 d . . . H31A H 0.4963 0.6255 -0.0881 0.176 Uiso 1 1 calc R . . H31B H 0.5772 0.6934 -0.0224 0.176 Uiso 1 1 calc R . . H31C H 0.4923 0.6978 -0.0574 0.176 Uiso 1 1 calc R . . O315 O 0.2606(3) 0.5067(3) 0.1072(3) 0.0717(13) Uani 1 1 d . . . N401 N 0.1384(3) 0.1199(3) 0.4813(3) 0.0469(11) Uani 1 1 d . . . C402 C 0.0528(3) 0.0845(3) 0.4537(3) 0.0485(13) Uani 1 1 d . . . C403 C 0.0013(4) 0.0097(4) 0.4075(4) 0.0599(16) Uani 1 1 d . . . H403 H -0.0581 -0.0134 0.3881 0.072 Uiso 1 1 calc R . . C404 C 0.0397(5) -0.0299(4) 0.3906(4) 0.0663(18) Uani 1 1 d . . . C405 C 0.1291(5) 0.0077(4) 0.4223(4) 0.074(2) Uani 1 1 d . . . H405 H 0.1573 -0.0174 0.4136 0.089 Uiso 1 1 calc R . . C406 C 0.1744(4) 0.0809(4) 0.4657(4) 0.0638(17) Uani 1 1 d . . . H406 H 0.2339 0.1054 0.4856 0.077 Uiso 1 1 calc R . . C407 C -0.0133(6) -0.1103(5) 0.3399(5) 0.098(3) Uani 1 1 d . . . H40A H 0.0240 -0.1285 0.3348 0.147 Uiso 1 1 calc R . . H40B H -0.0487 -0.1094 0.2928 0.147 Uiso 1 1 calc R . . H40C H -0.0488 -0.1444 0.3597 0.147 Uiso 1 1 calc R . . N408 N 0.0757(3) 0.2061(3) 0.5132(3) 0.0472(11) Uani 1 1 d . . . C409 C 0.0170(4) 0.1314(3) 0.4742(3) 0.0507(13) Uani 1 1 d . . . C410 C -0.0687(4) 0.1026(4) 0.4581(4) 0.0646(17) Uani 1 1 d . . . H410 H -0.1081 0.0509 0.4327 0.078 Uiso 1 1 calc R . . C411 C -0.0957(4) 0.1507(5) 0.4798(5) 0.076(2) Uani 1 1 d . . . C412 C -0.0359(5) 0.2264(5) 0.5177(5) 0.081(2) Uani 1 1 d . . . H412 H -0.0524 0.2600 0.5329 0.097 Uiso 1 1 calc R . . C413 C 0.0482(4) 0.2524(4) 0.5328(4) 0.0654(17) Uani 1 1 d . . . H413 H 0.0880 0.3041 0.5576 0.079 Uiso 1 1 calc R . . C414 C -0.1904(5) 0.1194(6) 0.4612(7) 0.124(4) Uani 1 1 d . . . H41A H -0.2223 0.0656 0.4349 0.186 Uiso 1 1 calc R . . H41B H -0.2117 0.1479 0.4315 0.186 Uiso 1 1 calc R . . H41C H -0.1970 0.1249 0.5056 0.186 Uiso 1 1 calc R . . O415 O 0.2050(3) 0.1957(3) 0.6340(2) 0.0600(11) Uani 1 1 d . . . C416 C 0.2337(6) 0.2439(6) 0.7024(4) 0.090(3) Uani 1 1 d . . . H41D H 0.2102 0.2122 0.7314 0.108 Uiso 1 1 calc R . . H41E H 0.2116 0.2798 0.6954 0.108 Uiso 1 1 calc R . . C417 C 0.3283(6) 0.2888(7) 0.7443(6) 0.113(3) Uani 1 1 d . . . H41F H 0.3432 0.3204 0.7903 0.169 Uiso 1 1 calc R . . H41G H 0.3523 0.3213 0.7167 0.169 Uiso 1 1 calc R . . H41H H 0.3508 0.2537 0.7529 0.169 Uiso 1 1 calc R . . N501 N 0.0711(3) 0.4750(3) 0.3963(2) 0.0463(10) Uani 1 1 d . . . C502 C 0.0058(4) 0.4483(4) 0.3307(3) 0.0529(14) Uani 1 1 d . . . C503 C -0.0792(4) 0.3987(4) 0.3186(4) 0.0660(17) Uani 1 1 d . . . H503 H -0.1238 0.3789 0.2717 0.079 Uiso 1 1 calc R . . C504 C -0.0950(4) 0.3799(4) 0.3787(5) 0.074(2) Uani 1 1 d . . . C505 C -0.0265(4) 0.4072(4) 0.4454(4) 0.0646(17) Uani 1 1 d . . . H505 H -0.0350 0.3932 0.4858 0.078 Uiso 1 1 calc R . . C506 C 0.0543(4) 0.4550(4) 0.4535(4) 0.0572(15) Uani 1 1 d . . . H506 H 0.0996 0.4746 0.5000 0.069 Uiso 1 1 calc R . . C507 C -0.1851(5) 0.3274(6) 0.3701(6) 0.103(3) Uani 1 1 d . . . H50A H -0.2254 0.3137 0.3200 0.154 Uiso 1 1 calc R . . H50B H -0.1984 0.3541 0.4009 0.154 Uiso 1 1 calc R . . H50C H -0.1885 0.2812 0.3841 0.154 Uiso 1 1 calc R . . N508 N 0.1092(3) 0.5293(4) 0.2925(3) 0.0595(13) Uani 1 1 d . . . C509 C 0.0282(4) 0.4741(4) 0.2715(3) 0.0584(15) Uani 1 1 d . . . C510 C -0.0283(5) 0.4442(6) 0.1972(4) 0.084(2) Uani 1 1 d . . . H510 H -0.0844 0.4052 0.1828 0.101 Uiso 1 1 calc R . . C511 C -0.0028(6) 0.4714(7) 0.1447(5) 0.107(4) Uani 1 1 d . . . C512 C 0.0795(6) 0.5306(8) 0.1696(5) 0.120(4) Uani 1 1 d . . . H512 H 0.0991 0.5522 0.1363 0.144 Uiso 1 1 calc R . . C513 C 0.1333(5) 0.5584(6) 0.2426(4) 0.094(3) Uani 1 1 d . . . H513 H 0.1888 0.5991 0.2580 0.113 Uiso 1 1 calc R . . C514 C -0.0647(8) 0.4394(10) 0.0622(5) 0.166(7) Uani 1 1 d . . . H51A H -0.0352 0.4659 0.0347 0.248 Uiso 1 1 calc R . . H51B H -0.1127 0.4476 0.0535 0.248 Uiso 1 1 calc R . . H51C H -0.0847 0.3849 0.0471 0.248 Uiso 1 1 calc R . . O515 O 0.1711(3) 0.6410(3) 0.4331(3) 0.0608(11) Uani 1 1 d . . . O1 O 0.2509(5) 0.0833(4) 0.6500(5) 0.124(2) Uani 1 1 d . . . O2 O 0.0069(3) 0.6184(3) 0.3595(3) 0.0752(14) Uani 1 1 d . . . C3 C -0.0159(8) 0.6341(9) 0.2866(10) 0.159(6) Uani 1 1 d . . . H3A H 0.0371 0.6677 0.2840 0.190 Uiso 1 1 calc R . . H3B H -0.0437 0.5854 0.2500 0.190 Uiso 1 1 calc R . . C4 C -0.0672(10) 0.6669(10) 0.2669(9) 0.167(6) Uani 1 1 d . . . H4A H -0.0770 0.6732 0.2185 0.250 Uiso 1 1 calc R . . H4B H -0.0398 0.7166 0.3009 0.250 Uiso 1 1 calc R . . H4C H -0.1211 0.6339 0.2675 0.250 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 W1 0.03637(10) 0.03405(11) 0.03218(9) 0.00882(7) 0.02026(8) 0.01652(8) W2 0.04332(11) 0.03096(11) 0.04194(10) 0.01557(8) 0.02338(9) 0.01963(8) W3 0.03261(10) 0.03696(11) 0.03475(10) 0.00572(8) 0.01303(8) 0.01057(8) Ni1 0.0298(4) 0.0262(4) 0.0292(4) 0.0086(3) 0.0154(3) 0.0133(3) Ni2 0.0491(4) 0.0306(3) 0.0486(4) 0.0048(3) 0.0254(3) 0.0157(3) Ni3 0.0466(3) 0.0478(4) 0.0304(3) 0.0129(3) 0.0169(3) 0.0214(3) Ni4 0.0382(3) 0.0333(3) 0.0444(3) 0.0089(3) 0.0233(3) 0.0092(3) Ni5 0.0383(3) 0.0510(4) 0.0453(3) 0.0186(3) 0.0205(3) 0.0259(3) C11 0.036(2) 0.028(2) 0.035(2) 0.0063(18) 0.0161(19) 0.0126(19) N11 0.040(2) 0.036(2) 0.040(2) 0.0151(17) 0.0258(18) 0.0191(18) C12 0.045(3) 0.037(3) 0.046(3) 0.006(2) 0.023(2) 0.019(2) N12 0.058(3) 0.032(2) 0.053(3) 0.006(2) 0.029(2) 0.019(2) C13 0.047(3) 0.044(3) 0.035(2) 0.010(2) 0.024(2) 0.021(2) N13 0.048(3) 0.063(3) 0.041(2) 0.021(2) 0.018(2) 0.030(2) C14 0.047(3) 0.038(3) 0.046(3) 0.014(2) 0.029(2) 0.019(2) N14 0.046(2) 0.039(3) 0.052(3) 0.012(2) 0.023(2) 0.017(2) C15 0.035(2) 0.043(3) 0.042(3) 0.010(2) 0.020(2) 0.020(2) N15 0.040(2) 0.054(3) 0.050(3) 0.016(2) 0.022(2) 0.027(2) C16 0.053(3) 0.056(4) 0.052(3) 0.017(3) 0.033(3) 0.029(3) N16 0.047(3) 0.099(5) 0.077(4) 0.035(3) 0.040(3) 0.035(3) C17 0.062(3) 0.065(4) 0.038(3) 0.017(3) 0.028(3) 0.029(3) N17 0.101(4) 0.080(4) 0.057(3) 0.033(3) 0.056(3) 0.039(4) C18 0.076(4) 0.050(4) 0.067(4) 0.007(3) 0.045(3) 0.031(3) N18 0.121(6) 0.077(5) 0.086(4) 0.009(4) 0.066(4) 0.053(4) C21 0.034(2) 0.038(3) 0.033(2) 0.010(2) 0.0174(19) 0.017(2) N21 0.043(2) 0.035(2) 0.042(2) 0.0125(18) 0.0262(18) 0.0208(18) C22 0.049(3) 0.030(3) 0.053(3) 0.013(2) 0.027(2) 0.019(2) N22 0.064(3) 0.039(3) 0.052(3) 0.002(2) 0.029(2) 0.021(2) C23 0.048(3) 0.039(3) 0.041(3) 0.018(2) 0.022(2) 0.022(2) N23 0.060(3) 0.052(3) 0.041(2) 0.013(2) 0.023(2) 0.026(2) C24 0.045(3) 0.032(3) 0.053(3) 0.017(2) 0.027(2) 0.013(2) N24 0.044(3) 0.050(3) 0.056(3) 0.015(2) 0.028(2) 0.014(2) C25 0.040(3) 0.048(3) 0.045(3) 0.018(2) 0.019(2) 0.027(2) N25 0.043(2) 0.064(3) 0.064(3) 0.027(3) 0.025(2) 0.031(2) C26 0.090(5) 0.086(6) 0.138(7) 0.073(6) 0.071(6) 0.066(5) N26 0.117(7) 0.161(9) 0.208(11) 0.120(9) 0.085(7) 0.104(7) C27 0.087(5) 0.048(4) 0.070(4) 0.032(3) 0.049(4) 0.039(3) N27 0.140(6) 0.077(5) 0.096(5) 0.049(4) 0.085(5) 0.052(4) C28 0.095(5) 0.036(4) 0.069(4) 0.015(3) 0.043(4) 0.016(3) N28 0.122(6) 0.052(4) 0.119(6) 0.021(4) 0.052(5) 0.011(4) C31 0.033(2) 0.031(3) 0.041(2) 0.013(2) 0.017(2) 0.015(2) N31 0.037(2) 0.033(2) 0.037(2) 0.0087(17) 0.0166(18) 0.0148(18) C32 0.048(3) 0.039(3) 0.047(3) 0.000(2) 0.019(2) 0.013(2) N32 0.056(3) 0.047(3) 0.075(3) 0.003(3) 0.028(3) 0.024(3) C33 0.041(3) 0.052(3) 0.036(2) 0.012(2) 0.019(2) 0.016(2) N33 0.054(3) 0.057(3) 0.036(2) 0.013(2) 0.020(2) 0.023(2) C34 0.039(3) 0.030(3) 0.048(3) 0.004(2) 0.017(2) 0.007(2) N34 0.053(3) 0.050(3) 0.046(2) 0.011(2) 0.025(2) 0.017(2) C35 0.033(2) 0.053(3) 0.041(3) 0.008(2) 0.014(2) 0.022(2) N35 0.052(3) 0.064(3) 0.052(3) 0.016(2) 0.023(2) 0.035(3) C36 0.056(4) 0.068(5) 0.092(6) -0.011(4) -0.004(4) 0.024(4) N36 0.096(6) 0.157(10) 0.141(8) -0.017(7) -0.044(6) 0.078(6) C37 0.070(4) 0.065(4) 0.045(3) 0.004(3) 0.024(3) 0.008(3) N37 0.106(5) 0.098(6) 0.048(3) -0.017(3) 0.024(4) 0.003(4) C38 0.068(4) 0.055(4) 0.058(4) 0.009(3) 0.025(3) 0.000(3) N38 0.129(7) 0.062(5) 0.095(5) 0.003(4) 0.036(5) -0.017(5) N201 0.064(3) 0.040(3) 0.065(3) 0.015(2) 0.032(3) 0.028(2) C202 0.077(4) 0.042(4) 0.079(4) 0.020(3) 0.040(4) 0.030(3) C203 0.089(5) 0.047(4) 0.099(6) 0.018(4) 0.039(4) 0.041(4) C204 0.075(5) 0.061(5) 0.104(6) 0.020(4) 0.031(4) 0.043(4) C205 0.077(5) 0.067(5) 0.130(7) 0.025(5) 0.052(5) 0.041(4) C206 0.074(5) 0.050(4) 0.108(6) 0.024(4) 0.049(4) 0.029(4) C207 0.097(6) 0.080(6) 0.163(10) 0.019(6) 0.046(7) 0.060(6) N208 0.067(3) 0.035(3) 0.065(3) 0.005(2) 0.038(3) 0.015(2) C209 0.072(4) 0.034(3) 0.083(5) 0.013(3) 0.037(4) 0.020(3) C210 0.103(7) 0.051(5) 0.157(9) 0.028(5) 0.078(7) 0.026(4) C211 0.096(6) 0.049(5) 0.165(10) 0.027(6) 0.067(7) 0.017(5) C212 0.089(6) 0.074(6) 0.135(8) 0.024(6) 0.073(6) 0.019(5) C213 0.070(5) 0.057(4) 0.115(6) 0.012(4) 0.058(5) 0.014(4) C214 0.149(11) 0.053(6) 0.38(3) 0.058(11) 0.149(15) 0.014(7) O215 0.093(4) 0.074(4) 0.061(3) -0.001(2) 0.024(3) 0.037(3) N301 0.072(3) 0.058(3) 0.035(2) 0.009(2) 0.027(2) 0.024(3) C302 0.074(4) 0.064(4) 0.041(3) 0.010(3) 0.029(3) 0.031(3) C303 0.138(8) 0.075(6) 0.053(4) 0.000(4) 0.056(5) 0.023(5) C304 0.182(11) 0.067(6) 0.077(6) -0.015(5) 0.067(7) 0.016(6) C305 0.159(9) 0.074(6) 0.083(6) -0.004(5) 0.077(6) 0.004(6) C306 0.108(6) 0.056(4) 0.058(4) 0.013(3) 0.054(4) 0.019(4) C307 0.39(3) 0.102(10) 0.093(8) -0.041(7) 0.137(13) -0.022(12) N308 0.048(2) 0.055(3) 0.040(2) 0.020(2) 0.019(2) 0.019(2) C309 0.058(3) 0.061(4) 0.039(3) 0.012(3) 0.023(3) 0.025(3) C310 0.091(5) 0.099(6) 0.056(4) 0.033(4) 0.047(4) 0.043(5) C311 0.070(4) 0.082(5) 0.063(4) 0.035(4) 0.031(4) 0.026(4) C312 0.078(5) 0.073(5) 0.067(4) 0.027(4) 0.031(4) 0.011(4) C313 0.068(4) 0.070(5) 0.056(3) 0.025(3) 0.028(3) 0.021(4) C314 0.113(7) 0.135(9) 0.096(6) 0.062(6) 0.066(6) 0.032(7) O315 0.065(3) 0.083(4) 0.065(3) 0.028(3) 0.019(2) 0.041(3) N401 0.042(2) 0.032(2) 0.059(3) 0.008(2) 0.025(2) 0.0103(19) C402 0.044(3) 0.038(3) 0.050(3) 0.005(2) 0.025(2) 0.006(2) C403 0.050(3) 0.044(3) 0.064(4) 0.004(3) 0.031(3) 0.002(3) C404 0.075(4) 0.044(4) 0.074(4) 0.008(3) 0.047(4) 0.014(3) C405 0.070(4) 0.051(4) 0.103(6) 0.001(4) 0.051(4) 0.022(3) C406 0.057(4) 0.051(4) 0.084(5) 0.007(3) 0.041(3) 0.021(3) C407 0.091(6) 0.060(5) 0.117(7) -0.012(5) 0.059(5) 0.010(4) N408 0.044(2) 0.038(3) 0.055(3) 0.011(2) 0.026(2) 0.014(2) C409 0.047(3) 0.039(3) 0.052(3) 0.011(2) 0.020(3) 0.012(2) C410 0.040(3) 0.051(4) 0.083(4) 0.004(3) 0.020(3) 0.013(3) C411 0.046(3) 0.079(5) 0.100(6) 0.022(4) 0.033(4) 0.027(4) C412 0.070(4) 0.063(5) 0.124(7) 0.025(5) 0.048(5) 0.040(4) C413 0.068(4) 0.047(4) 0.090(5) 0.019(3) 0.044(4) 0.026(3) C414 0.050(4) 0.105(8) 0.189(11) -0.003(7) 0.046(6) 0.027(5) O415 0.066(3) 0.059(3) 0.049(2) 0.021(2) 0.031(2) 0.021(2) C416 0.089(6) 0.096(7) 0.064(4) 0.016(4) 0.035(4) 0.027(5) C417 0.097(7) 0.122(9) 0.091(6) 0.019(6) 0.022(5) 0.047(6) N501 0.043(2) 0.050(3) 0.048(2) 0.013(2) 0.020(2) 0.024(2) C502 0.045(3) 0.059(4) 0.058(3) 0.020(3) 0.016(3) 0.032(3) C503 0.052(3) 0.073(5) 0.072(4) 0.021(4) 0.024(3) 0.032(3) C504 0.052(4) 0.061(4) 0.113(6) 0.036(4) 0.040(4) 0.025(3) C505 0.059(4) 0.064(4) 0.079(4) 0.031(4) 0.039(4) 0.028(3) C506 0.057(3) 0.069(4) 0.061(3) 0.023(3) 0.034(3) 0.035(3) C507 0.056(4) 0.099(7) 0.131(8) 0.034(6) 0.045(5) 0.015(4) N508 0.049(3) 0.080(4) 0.051(3) 0.023(3) 0.017(2) 0.036(3) C509 0.054(3) 0.070(4) 0.051(3) 0.020(3) 0.015(3) 0.035(3) C510 0.064(4) 0.110(7) 0.063(4) 0.026(4) 0.018(4) 0.039(5) C511 0.077(5) 0.168(11) 0.064(5) 0.028(6) 0.023(4) 0.056(6) C512 0.087(6) 0.192(12) 0.069(5) 0.061(7) 0.041(5) 0.049(7) C513 0.067(5) 0.142(9) 0.068(5) 0.052(5) 0.029(4) 0.044(5) C514 0.109(8) 0.274(19) 0.054(5) 0.028(8) 0.008(5) 0.070(10) O515 0.059(2) 0.056(3) 0.076(3) 0.014(2) 0.029(2) 0.036(2) O1 0.118(5) 0.083(5) 0.171(7) 0.045(5) 0.055(5) 0.054(4) O2 0.061(3) 0.084(4) 0.101(4) 0.042(3) 0.043(3) 0.044(3) C3 0.112(9) 0.155(13) 0.258(19) 0.092(13) 0.100(11) 0.085(9) C4 0.175(13) 0.187(15) 0.209(15) 0.113(13) 0.091(12) 0.133(13) _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 W1 C14 2.154(6) . ? W1 C18 2.158(6) . ? W1 C11 2.160(5) . ? W1 C15 2.169(5) . ? W1 C12 2.171(6) . ? W1 C16 2.175(6) . ? W1 C13 2.178(6) . ? W1 C17 2.186(5) . ? W2 C26 2.128(8) . ? W2 C24 2.162(6) . ? W2 C27 2.164(6) . ? W2 C21 2.168(5) . ? W2 C23 2.170(6) . ? W2 C22 2.175(6) . ? W2 C28 2.176(7) . ? W2 C25 2.184(5) . ? W3 C36 2.119(8) . ? W3 C34 2.124(5) . ? W3 C31 2.149(5) . ? W3 C35 2.154(6) . ? W3 C33 2.156(5) . ? W3 C32 2.160(7) . ? W3 C38 2.164(7) . ? W3 C37 2.201(7) . ? Ni1 N31 2.037(4) . ? Ni1 N31 2.037(4) 2_666 ? Ni1 N21 2.046(4) . ? Ni1 N21 2.046(4) 2_666 ? Ni1 N11 2.048(4) 2_666 ? Ni1 N11 2.048(4) . ? Ni2 N32 2.049(6) 2_666 ? Ni2 N12 2.060(5) . ? Ni2 N22 2.061(5) . ? Ni2 N208 2.071(5) . ? Ni2 N201 2.072(5) . ? Ni2 O215 2.145(5) . ? Ni3 N33 2.047(5) . ? Ni3 N23 2.067(5) . ? Ni3 N308 2.071(4) . ? Ni3 N301 2.080(5) . ? Ni3 N13 2.097(5) 2_666 ? Ni3 O315 2.140(5) . ? Ni4 N34 2.026(5) . ? Ni4 N14 2.040(5) . ? Ni4 N24 2.059(5) 2_666 ? Ni4 N401 2.069(5) . ? Ni4 N408 2.079(5) . ? Ni4 O415 2.112(4) . ? Ni5 N501 2.066(5) . ? Ni5 N25 2.069(5) . ? Ni5 N35 2.078(5) . ? Ni5 N508 2.083(5) . ? Ni5 N15 2.086(5) . ? Ni5 O515 2.117(4) . ? C11 N11 1.136(6) . ? C12 N12 1.135(7) . ? C13 N13 1.134(7) . ? N13 Ni3 2.097(5) 2_666 ? C14 N14 1.138(7) . ? C15 N15 1.131(6) . ? C16 N16 1.147(7) . ? C17 N17 1.131(7) . ? C18 N18 1.145(8) . ? C21 N21 1.124(6) . ? C22 N22 1.139(7) . ? C23 N23 1.136(7) . ? C24 N24 1.131(7) . ? N24 Ni4 2.059(5) 2_666 ? C25 N25 1.129(7) . ? C26 N26 1.157(10) . ? C27 N27 1.137(8) . ? C28 N28 1.134(9) . ? C31 N31 1.135(6) . ? C32 N32 1.138(8) . ? N32 Ni2 2.049(6) 2_666 ? C33 N33 1.126(7) . ? C34 N34 1.171(7) . ? C35 N35 1.160(7) . ? C36 N36 1.179(10) . ? C37 N37 1.117(9) . ? C38 N38 1.124(9) . ? N201 C206 1.321(9) . ? N201 C202 1.361(8) . ? C202 C203 1.402(10) . ? C202 C209 1.469(10) . ? C203 C204 1.373(11) . ? C203 H203 0.9300 . ? C204 C205 1.375(11) . ? C204 C207 1.498(11) . ? C205 C206 1.381(10) . ? C205 H205 0.9300 . ? C206 H206 0.9300 . ? C207 H20A 0.9600 . ? C207 H20B 0.9600 . ? C207 H20C 0.9600 . ? N208 C209 1.315(9) . ? N208 C213 1.364(9) . ? C209 C210 1.414(10) . ? C210 C211 1.377(13) . ? C210 H210 0.9300 . ? C211 C212 1.375(14) . ? C211 C214 1.536(12) . ? C212 C213 1.417(11) . ? C212 H212 0.9300 . ? C213 H213 0.9300 . ? C214 H21A 0.9600 . ? C214 H21B 0.9600 . ? C214 H21C 0.9600 . ? N301 C306 1.300(8) . ? N301 C302 1.357(7) . ? C302 C303 1.402(9) . ? C302 C309 1.461(9) . ? C303 C304 1.352(12) . ? C303 H303 0.9300 . ? C304 C305 1.380(13) . ? C304 C307 1.531(12) . ? C305 C306 1.366(10) . ? C305 H305 0.9300 . ? C306 H306 0.9300 . ? C307 H30A 0.9600 . ? C307 H30B 0.9600 . ? C307 H30C 0.9600 . ? N308 C313 1.345(9) . ? N308 C309 1.349(7) . ? C309 C310 1.387(8) . ? C310 C311 1.375(11) . ? C310 H310 0.9300 . ? C311 C312 1.395(11) . ? C311 C314 1.520(10) . ? C312 C313 1.388(9) . ? C312 H312 0.9300 . ? C313 H313 0.9300 . ? C314 H31A 0.9600 . ? C314 H31B 0.9600 . ? C314 H31C 0.9600 . ? N401 C406 1.327(8) . ? N401 C402 1.338(7) . ? C402 C403 1.390(8) . ? C402 C409 1.491(9) . ? C403 C404 1.387(10) . ? C403 H403 0.9300 . ? C404 C405 1.395(10) . ? C404 C407 1.503(10) . ? C405 C406 1.350(9) . ? C405 H405 0.9300 . ? C406 H406 0.9300 . ? C407 H40A 0.9600 . ? C407 H40B 0.9600 . ? C407 H40C 0.9600 . ? N408 C413 1.341(8) . ? N408 C409 1.359(7) . ? C409 C410 1.383(8) . ? C410 C411 1.382(10) . ? C410 H410 0.9300 . ? C411 C412 1.372(11) . ? C411 C414 1.527(10) . ? C412 C413 1.367(10) . ? C412 H412 0.9300 . ? C413 H413 0.9300 . ? C414 H41A 0.9600 . ? C414 H41B 0.9600 . ? C414 H41C 0.9600 . ? O415 C416 1.399(9) . ? C416 C417 1.482(12) . ? C416 H41D 0.9700 . ? C416 H41E 0.9700 . ? C417 H41F 0.9600 . ? C417 H41G 0.9600 . ? C417 H41H 0.9600 . ? N501 C502 1.323(7) . ? N501 C506 1.356(7) . ? C502 C503 1.407(9) . ? C502 C509 1.471(9) . ? C503 C504 1.398(10) . ? C503 H503 0.9300 . ? C504 C505 1.362(10) . ? C504 C507 1.520(9) . ? C505 C506 1.363(9) . ? C505 H505 0.9300 . ? C506 H506 0.9300 . ? C507 H50A 0.9600 . ? C507 H50B 0.9600 . ? C507 H50C 0.9600 . ? N508 C513 1.329(9) . ? N508 C509 1.336(8) . ? C509 C510 1.395(9) . ? C510 C511 1.378(12) . ? C510 H510 0.9300 . ? C511 C512 1.368(13) . ? C511 C514 1.546(12) . ? C512 C513 1.364(11) . ? C512 H512 0.9300 . ? C513 H513 0.9300 . ? C514 H51A 0.9600 . ? C514 H51B 0.9600 . ? C514 H51C 0.9600 . ? O2 C3 1.481(16) . ? C3 C4 1.363(16) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 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 C14 W1 C18 146.6(2) . . ? C14 W1 C11 71.88(17) . . ? C18 W1 C11 141.5(2) . . ? C14 W1 C15 90.2(2) . . ? C18 W1 C15 98.2(2) . . ? C11 W1 C15 72.76(18) . . ? C14 W1 C12 143.41(18) . . ? C18 W1 C12 70.0(2) . . ? C11 W1 C12 71.54(18) . . ? C15 W1 C12 78.6(2) . . ? C14 W1 C16 75.9(2) . . ? C18 W1 C16 76.4(2) . . ? C11 W1 C16 130.85(19) . . ? C15 W1 C16 71.28(19) . . ? C12 W1 C16 130.4(2) . . ? C14 W1 C13 90.9(2) . . ? C18 W1 C13 99.7(2) . . ? C11 W1 C13 74.79(18) . . ? C15 W1 C13 145.42(17) . . ? C12 W1 C13 80.1(2) . . ? C16 W1 C13 142.0(2) . . ? C14 W1 C17 77.2(2) . . ? C18 W1 C17 76.6(3) . . ? C11 W1 C17 132.8(2) . . ? C15 W1 C17 142.5(2) . . ? C12 W1 C17 130.8(2) . . ? C16 W1 C17 71.4(2) . . ? C13 W1 C17 71.0(2) . . ? C26 W2 C24 145.5(3) . . ? C26 W2 C27 74.3(3) . . ? C24 W2 C27 76.1(2) . . ? C26 W2 C21 142.3(2) . . ? C24 W2 C21 72.07(18) . . ? C27 W2 C21 132.1(2) . . ? C26 W2 C23 97.2(3) . . ? C24 W2 C23 89.7(2) . . ? C27 W2 C23 70.9(2) . . ? C21 W2 C23 73.97(18) . . ? C26 W2 C22 103.2(3) . . ? C24 W2 C22 88.6(2) . . ? C27 W2 C22 140.7(2) . . ? C21 W2 C22 73.32(19) . . ? C23 W2 C22 146.11(19) . . ? C26 W2 C28 77.9(4) . . ? C24 W2 C28 76.1(3) . . ? C27 W2 C28 71.3(3) . . ? C21 W2 C28 131.2(2) . . ? C23 W2 C28 141.8(2) . . ? C22 W2 C28 69.9(2) . . ? C26 W2 C25 71.8(3) . . ? C24 W2 C25 142.65(19) . . ? C27 W2 C25 132.8(2) . . ? C21 W2 C25 70.61(18) . . ? C23 W2 C25 81.6(2) . . ? C22 W2 C25 79.46(19) . . ? C28 W2 C25 130.1(3) . . ? C36 W3 C34 110.0(3) . . ? C36 W3 C31 139.7(3) . . ? C34 W3 C31 73.94(18) . . ? C36 W3 C35 71.7(3) . . ? C34 W3 C35 77.2(2) . . ? C31 W3 C35 70.32(18) . . ? C36 W3 C33 88.5(3) . . ? C34 W3 C33 145.06(19) . . ? C31 W3 C33 73.04(18) . . ? C35 W3 C33 81.2(2) . . ? C36 W3 C32 147.0(3) . . ? C34 W3 C32 87.0(2) . . ? C31 W3 C32 71.10(19) . . ? C35 W3 C32 140.99(19) . . ? C33 W3 C32 92.9(2) . . ? C36 W3 C38 79.5(3) . . ? C34 W3 C38 70.3(2) . . ? C31 W3 C38 134.8(2) . . ? C35 W3 C38 125.2(3) . . ? C33 W3 C38 144.1(2) . . ? C32 W3 C38 80.2(3) . . ? C36 W3 C37 73.7(3) . . ? C34 W3 C37 140.8(2) . . ? C31 W3 C37 129.3(2) . . ? C35 W3 C37 136.3(3) . . ? C33 W3 C37 71.9(2) . . ? C32 W3 C37 75.5(3) . . ? C38 W3 C37 72.3(3) . . ? N31 Ni1 N31 180.000(1) . 2_666 ? N31 Ni1 N21 90.68(17) . . ? N31 Ni1 N21 89.32(17) 2_666 . ? N31 Ni1 N21 89.32(17) . 2_666 ? N31 Ni1 N21 90.68(17) 2_666 2_666 ? N21 Ni1 N21 180.0(2) . 2_666 ? N31 Ni1 N11 89.68(16) . 2_666 ? N31 Ni1 N11 90.32(16) 2_666 2_666 ? N21 Ni1 N11 88.85(16) . 2_666 ? N21 Ni1 N11 91.15(15) 2_666 2_666 ? N31 Ni1 N11 90.32(16) . . ? N31 Ni1 N11 89.68(16) 2_666 . ? N21 Ni1 N11 91.15(15) . . ? N21 Ni1 N11 88.85(16) 2_666 . ? N11 Ni1 N11 180.000(1) 2_666 . ? N32 Ni2 N12 91.8(2) 2_666 . ? N32 Ni2 N22 92.6(2) 2_666 . ? N12 Ni2 N22 91.16(19) . . ? N32 Ni2 N208 92.9(2) 2_666 . ? N12 Ni2 N208 173.04(19) . . ? N22 Ni2 N208 93.8(2) . . ? N32 Ni2 N201 170.3(2) 2_666 . ? N12 Ni2 N201 96.0(2) . . ? N22 Ni2 N201 92.9(2) . . ? N208 Ni2 N201 78.8(2) . . ? N32 Ni2 O215 89.1(2) 2_666 . ? N12 Ni2 O215 89.4(2) . . ? N22 Ni2 O215 178.2(2) . . ? N208 Ni2 O215 85.5(2) . . ? N201 Ni2 O215 85.3(2) . . ? N33 Ni3 N23 90.73(19) . . ? N33 Ni3 N308 170.38(18) . . ? N23 Ni3 N308 96.4(2) . . ? N33 Ni3 N301 93.6(2) . . ? N23 Ni3 N301 174.1(2) . . ? N308 Ni3 N301 78.9(2) . . ? N33 Ni3 N13 91.98(19) . 2_666 ? N23 Ni3 N13 92.6(2) . 2_666 ? N308 Ni3 N13 94.16(19) . 2_666 ? N301 Ni3 N13 91.3(2) . 2_666 ? N33 Ni3 O315 87.4(2) . . ? N23 Ni3 O315 88.7(2) . . ? N308 Ni3 O315 86.33(19) . . ? N301 Ni3 O315 87.4(2) . . ? N13 Ni3 O315 178.5(2) 2_666 . ? N34 Ni4 N14 90.5(2) . . ? N34 Ni4 N24 91.83(19) . 2_666 ? N14 Ni4 N24 91.04(19) . 2_666 ? N34 Ni4 N401 89.0(2) . . ? N14 Ni4 N401 174.97(19) . . ? N24 Ni4 N401 93.98(19) 2_666 . ? N34 Ni4 N408 91.51(19) . . ? N14 Ni4 N408 95.84(19) . . ? N24 Ni4 N408 172.3(2) 2_666 . ? N401 Ni4 N408 79.16(18) . . ? N34 Ni4 O415 176.40(19) . . ? N14 Ni4 O415 92.89(18) . . ? N24 Ni4 O415 89.24(18) 2_666 . ? N401 Ni4 O415 87.50(18) . . ? N408 Ni4 O415 87.03(18) . . ? N501 Ni5 N25 172.83(19) . . ? N501 Ni5 N35 89.2(2) . . ? N25 Ni5 N35 92.5(2) . . ? N501 Ni5 N508 78.44(19) . . ? N25 Ni5 N508 94.7(2) . . ? N35 Ni5 N508 86.1(2) . . ? N501 Ni5 N15 94.47(17) . . ? N25 Ni5 N15 92.39(18) . . ? N35 Ni5 N15 93.07(19) . . ? N508 Ni5 N15 172.87(19) . . ? N501 Ni5 O515 86.76(18) . . ? N25 Ni5 O515 91.2(2) . . ? N35 Ni5 O515 175.14(18) . . ? N508 Ni5 O515 90.5(2) . . ? N15 Ni5 O515 89.93(18) . . ? N11 C11 W1 178.8(4) . . ? C11 N11 Ni1 174.9(4) . . ? N12 C12 W1 177.9(5) . . ? C12 N12 Ni2 177.7(5) . . ? N13 C13 W1 175.0(5) . . ? C13 N13 Ni3 177.6(5) . 2_666 ? N14 C14 W1 178.4(5) . . ? C14 N14 Ni4 171.4(4) . . ? N15 C15 W1 174.4(5) . . ? C15 N15 Ni5 171.5(5) . . ? N16 C16 W1 177.1(6) . . ? N17 C17 W1 178.3(6) . . ? N18 C18 W1 179.4(7) . . ? N21 C21 W2 179.1(4) . . ? C21 N21 Ni1 175.2(4) . . ? N22 C22 W2 176.2(5) . . ? C22 N22 Ni2 173.3(5) . . ? N23 C23 W2 174.5(5) . . ? C23 N23 Ni3 175.6(5) . . ? N24 C24 W2 179.6(6) . . ? C24 N24 Ni4 178.2(5) . 2_666 ? N25 C25 W2 179.4(5) . . ? C25 N25 Ni5 173.8(5) . . ? N26 C26 W2 178.7(11) . . ? N27 C27 W2 177.6(6) . . ? N28 C28 W2 176.2(8) . . ? N31 C31 W3 178.6(5) . . ? C31 N31 Ni1 175.8(4) . . ? N32 C32 W3 176.6(5) . . ? C32 N32 Ni2 173.8(5) . 2_666 ? N33 C33 W3 176.6(5) . . ? C33 N33 Ni3 175.7(5) . . ? N34 C34 W3 176.8(5) . . ? C34 N34 Ni4 172.6(5) . . ? N35 C35 W3 177.4(5) . . ? C35 N35 Ni5 171.9(5) . . ? N36 C36 W3 176.3(10) . . ? N37 C37 W3 178.2(9) . . ? N38 C38 W3 178.4(9) . . ? C206 N201 C202 118.9(6) . . ? C206 N201 Ni2 126.9(5) . . ? C202 N201 Ni2 114.0(4) . . ? N201 C202 C203 120.9(6) . . ? N201 C202 C209 115.5(6) . . ? C203 C202 C209 123.6(6) . . ? C204 C203 C202 120.0(7) . . ? C204 C203 H203 120.0 . . ? C202 C203 H203 120.0 . . ? C203 C204 C205 117.2(7) . . ? C203 C204 C207 120.6(8) . . ? C205 C204 C207 122.1(8) . . ? C204 C205 C206 121.2(8) . . ? C204 C205 H205 119.4 . . ? C206 C205 H205 119.4 . . ? N201 C206 C205 121.7(7) . . ? N201 C206 H206 119.2 . . ? C205 C206 H206 119.2 . . ? C204 C207 H20A 109.5 . . ? C204 C207 H20B 109.5 . . ? H20A C207 H20B 109.5 . . ? C204 C207 H20C 109.5 . . ? H20A C207 H20C 109.5 . . ? H20B C207 H20C 109.5 . . ? C209 N208 C213 119.9(6) . . ? C209 N208 Ni2 115.6(4) . . ? C213 N208 Ni2 124.4(5) . . ? N208 C209 C210 121.7(7) . . ? N208 C209 C202 115.9(6) . . ? C210 C209 C202 122.1(7) . . ? C211 C210 C209 119.2(9) . . ? C211 C210 H210 120.4 . . ? C209 C210 H210 120.4 . . ? C212 C211 C210 119.4(8) . . ? C212 C211 C214 119.5(10) . . ? C210 C211 C214 121.0(10) . . ? C211 C212 C213 118.9(8) . . ? C211 C212 H212 120.5 . . ? C213 C212 H212 120.5 . . ? N208 C213 C212 120.6(8) . . ? N208 C213 H213 119.7 . . ? C212 C213 H213 119.7 . . ? C211 C214 H21A 109.5 . . ? C211 C214 H21B 109.5 . . ? H21A C214 H21B 109.5 . . ? C211 C214 H21C 109.5 . . ? H21A C214 H21C 109.5 . . ? H21B C214 H21C 109.5 . . ? C306 N301 C302 119.0(5) . . ? C306 N301 Ni3 126.4(4) . . ? C302 N301 Ni3 113.7(4) . . ? N301 C302 C303 119.6(6) . . ? N301 C302 C309 116.2(5) . . ? C303 C302 C309 124.2(6) . . ? C304 C303 C302 119.9(7) . . ? C304 C303 H303 120.1 . . ? C302 C303 H303 120.1 . . ? C303 C304 C305 119.0(8) . . ? C303 C304 C307 119.8(9) . . ? C305 C304 C307 120.9(9) . . ? C306 C305 C304 118.0(8) . . ? C306 C305 H305 121.0 . . ? C304 C305 H305 121.0 . . ? N301 C306 C305 124.0(6) . . ? N301 C306 H306 118.0 . . ? C305 C306 H306 118.0 . . ? C304 C307 H30A 109.5 . . ? C304 C307 H30B 109.5 . . ? H30A C307 H30B 109.5 . . ? C304 C307 H30C 109.5 . . ? H30A C307 H30C 109.5 . . ? H30B C307 H30C 109.5 . . ? C313 N308 C309 118.7(5) . . ? C313 N308 Ni3 125.9(4) . . ? C309 N308 Ni3 115.3(4) . . ? N308 C309 C310 122.1(6) . . ? N308 C309 C302 115.1(5) . . ? C310 C309 C302 122.7(6) . . ? C311 C310 C309 120.0(7) . . ? C311 C310 H310 120.0 . . ? C309 C310 H310 120.0 . . ? C310 C311 C312 117.4(6) . . ? C310 C311 C314 122.0(8) . . ? C312 C311 C314 120.3(8) . . ? C313 C312 C311 120.5(7) . . ? C313 C312 H312 119.7 . . ? C311 C312 H312 119.7 . . ? N308 C313 C312 121.1(7) . . ? N308 C313 H313 119.4 . . ? C312 C313 H313 119.4 . . ? C311 C314 H31A 109.5 . . ? C311 C314 H31B 109.5 . . ? H31A C314 H31B 109.5 . . ? C311 C314 H31C 109.5 . . ? H31A C314 H31C 109.5 . . ? H31B C314 H31C 109.5 . . ? C406 N401 C402 118.4(5) . . ? C406 N401 Ni4 125.9(4) . . ? C402 N401 Ni4 115.5(4) . . ? N401 C402 C403 121.8(6) . . ? N401 C402 C409 115.5(5) . . ? C403 C402 C409 122.6(5) . . ? C404 C403 C402 119.1(6) . . ? C404 C403 H403 120.4 . . ? C402 C403 H403 120.4 . . ? C403 C404 C405 117.5(6) . . ? C403 C404 C407 121.1(7) . . ? C405 C404 C407 121.3(7) . . ? C406 C405 C404 119.6(7) . . ? C406 C405 H405 120.2 . . ? C404 C405 H405 120.2 . . ? N401 C406 C405 123.4(6) . . ? N401 C406 H406 118.3 . . ? C405 C406 H406 118.3 . . ? C404 C407 H40A 109.5 . . ? C404 C407 H40B 109.5 . . ? H40A C407 H40B 109.5 . . ? C404 C407 H40C 109.5 . . ? H40A C407 H40C 109.5 . . ? H40B C407 H40C 109.5 . . ? C413 N408 C409 118.5(5) . . ? C413 N408 Ni4 126.8(4) . . ? C409 N408 Ni4 114.7(4) . . ? N408 C409 C410 120.8(6) . . ? N408 C409 C402 115.0(5) . . ? C410 C409 C402 124.2(5) . . ? C411 C410 C409 119.9(6) . . ? C411 C410 H410 120.1 . . ? C409 C410 H410 120.1 . . ? C412 C411 C410 118.6(6) . . ? C412 C411 C414 121.4(8) . . ? C410 C411 C414 120.0(7) . . ? C413 C412 C411 119.6(7) . . ? C413 C412 H412 120.2 . . ? C411 C412 H412 120.2 . . ? N408 C413 C412 122.6(7) . . ? N408 C413 H413 118.7 . . ? C412 C413 H413 118.7 . . ? C411 C414 H41A 109.5 . . ? C411 C414 H41B 109.5 . . ? H41A C414 H41B 109.5 . . ? C411 C414 H41C 109.5 . . ? H41A C414 H41C 109.5 . . ? H41B C414 H41C 109.5 . . ? C416 O415 Ni4 124.1(5) . . ? O415 C416 C417 114.2(8) . . ? O415 C416 H41D 108.7 . . ? C417 C416 H41D 108.7 . . ? O415 C416 H41E 108.7 . . ? C417 C416 H41E 108.7 . . ? H41D C416 H41E 107.6 . . ? C416 C417 H41F 109.5 . . ? C416 C417 H41G 109.5 . . ? H41F C417 H41G 109.5 . . ? C416 C417 H41H 109.5 . . ? H41F C417 H41H 109.5 . . ? H41G C417 H41H 109.5 . . ? C502 N501 C506 118.1(5) . . ? C502 N501 Ni5 115.5(4) . . ? C506 N501 Ni5 126.3(4) . . ? N501 C502 C503 122.2(6) . . ? N501 C502 C509 115.3(5) . . ? C503 C502 C509 122.4(6) . . ? C504 C503 C502 118.5(6) . . ? C504 C503 H503 120.7 . . ? C502 C503 H503 120.7 . . ? C505 C504 C503 118.1(6) . . ? C505 C504 C507 120.3(8) . . ? C503 C504 C507 121.6(8) . . ? C504 C505 C506 120.5(7) . . ? C504 C505 H505 119.8 . . ? C506 C505 H505 119.8 . . ? N501 C506 C505 122.5(6) . . ? N501 C506 H506 118.7 . . ? C505 C506 H506 118.7 . . ? C504 C507 H50A 109.5 . . ? C504 C507 H50B 109.5 . . ? H50A C507 H50B 109.5 . . ? C504 C507 H50C 109.5 . . ? H50A C507 H50C 109.5 . . ? H50B C507 H50C 109.5 . . ? C513 N508 C509 119.3(6) . . ? C513 N508 Ni5 126.2(5) . . ? C509 N508 Ni5 113.8(4) . . ? N508 C509 C510 119.7(6) . . ? N508 C509 C502 115.7(5) . . ? C510 C509 C502 124.5(6) . . ? C511 C510 C509 121.3(8) . . ? C511 C510 H510 119.3 . . ? C509 C510 H510 119.3 . . ? C512 C511 C510 116.4(8) . . ? C512 C511 C514 121.5(10) . . ? C510 C511 C514 122.1(9) . . ? C513 C512 C511 120.8(8) . . ? C513 C512 H512 119.6 . . ? C511 C512 H512 119.6 . . ? N508 C513 C512 122.2(8) . . ? N508 C513 H513 118.9 . . ? C512 C513 H513 118.9 . . ? C511 C514 H51A 109.5 . . ? C511 C514 H51B 109.5 . . ? H51A C514 H51B 109.5 . . ? C511 C514 H51C 109.5 . . ? H51A C514 H51C 109.5 . . ? H51B C514 H51C 109.5 . . ? C4 C3 O2 118.6(13) . . ? C4 C3 H3A 107.7 . . ? O2 C3 H3A 107.7 . . ? C4 C3 H3B 107.7 . . ? O2 C3 H3B 107.7 . . ? H3A C3 H3B 107.1 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.334 _refine_diff_density_min -1.369 _refine_diff_density_rms 0.121 #===END data_2b _database_code_depnum_ccdc_archive 'CCDC 876830' #TrackingRef '- clusters1-4_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; {Ni[Ni(4,4'dmbpy)(H2O)]8[W(CN)8]6}*18H2O ; _chemical_name_common (Ni(Ni(4,4'dmbpy)(H2O))8(W(CN)8)6)*18H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C160 H140 N66 Ni9 O24 W6' _chemical_formula_weight 5002.64 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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 18.9503(2) _cell_length_b 19.5178(2) _cell_length_c 20.1197(2) _cell_angle_alpha 93.1280(10) _cell_angle_beta 112.1450(10) _cell_angle_gamma 115.2360(10) _cell_volume 6025.51(14) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2450 _exptl_absorpt_coefficient_mu 3.597 _exptl_absorpt_correction_T_min 0.4117 _exptl_absorpt_correction_T_max 0.6721 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details '(DENZO-SMN; Otwinowski & Minor, 1997)' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\f and \o scans to fill Ewald sphere' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 44302 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.11 _reflns_number_total 26189 _reflns_number_gt 21458 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (ALTOMARE et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+42.4471P] 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 26189 _refine_ls_number_parameters 1231 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1594 _refine_ls_wR_factor_gt 0.1443 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 W1 W 0.642642(16) 0.464013(15) 0.327478(13) 0.02320(7) Uani 1 1 d . . . W2 W 0.483720(17) 0.736970(15) 0.387571(14) 0.02554(7) Uani 1 1 d . . . W3 W 0.812895(16) 0.700522(16) 0.715122(14) 0.02725(8) Uani 1 1 d . . . Ni1 Ni 0.5000 0.5000 0.5000 0.0188(2) Uani 1 2 d S . . Ni2 Ni 0.80012(5) 0.76763(5) 0.45977(5) 0.02905(19) Uani 1 1 d . . . Ni3 Ni 0.81485(5) 0.44636(5) 0.60013(5) 0.02802(18) Uani 1 1 d . . . Ni4 Ni 0.59706(6) 0.81702(5) 0.68241(5) 0.02998(19) Uani 1 1 d . . . Ni5 Ni 0.36389(6) 0.49563(5) 0.16205(4) 0.02812(18) Uani 1 1 d . . . C11 C 0.5919(4) 0.4859(4) 0.4013(3) 0.0222(12) Uani 1 1 d . . . N11 N 0.5627(3) 0.4941(3) 0.4392(3) 0.0239(11) Uani 1 1 d . . . C12 C 0.7105(4) 0.5876(4) 0.3775(4) 0.0287(14) Uani 1 1 d . . . N12 N 0.7473(4) 0.6547(4) 0.4036(3) 0.0339(13) Uani 1 1 d . . . C13 C 0.7101(4) 0.4439(4) 0.4319(4) 0.0248(13) Uani 1 1 d . . . N13 N 0.7468(4) 0.4398(4) 0.4901(3) 0.0307(12) Uani 1 1 d . . . C14 C 0.5431(4) 0.3527(4) 0.3250(4) 0.0266(13) Uani 1 1 d . . . N14 N 0.4925(4) 0.2938(4) 0.3247(3) 0.0315(13) Uani 1 1 d . . . C15 C 0.5259(5) 0.4688(4) 0.2567(4) 0.0299(14) Uani 1 1 d . . . N15 N 0.4678(4) 0.4770(4) 0.2219(3) 0.0328(13) Uani 1 1 d . . . C16 C 0.7759(5) 0.5012(5) 0.3471(4) 0.0354(16) Uani 1 1 d . . . N16 N 0.8472(5) 0.5244(5) 0.3586(4) 0.0475(17) Uani 1 1 d . . . C17 C 0.6293(6) 0.3702(5) 0.2540(4) 0.0393(17) Uani 1 1 d . . . N17 N 0.6222(6) 0.3195(4) 0.2147(4) 0.0530(19) Uani 1 1 d . . . C18 C 0.6635(5) 0.5157(5) 0.2391(4) 0.0325(15) Uani 1 1 d . . . N18 N 0.6746(5) 0.5457(4) 0.1940(4) 0.0432(16) Uani 1 1 d . . . C21 C 0.4876(4) 0.6403(4) 0.4334(3) 0.0221(12) Uani 1 1 d . . . N21 N 0.4888(3) 0.5896(3) 0.4570(3) 0.0242(11) Uani 1 1 d . . . C22 C 0.6114(4) 0.7498(4) 0.4179(4) 0.0314(15) Uani 1 1 d . . . N22 N 0.6784(4) 0.7555(4) 0.4331(4) 0.0386(15) Uani 1 1 d . . . C23 C 0.3617(5) 0.6678(4) 0.3920(4) 0.0309(14) Uani 1 1 d . . . N23 N 0.2976(4) 0.6295(4) 0.3945(3) 0.0353(13) Uani 1 1 d . . . C24 C 0.5242(5) 0.7742(4) 0.5048(4) 0.0305(14) Uani 1 1 d . . . N24 N 0.5490(4) 0.7935(4) 0.5683(4) 0.0369(14) Uani 1 1 d . . . C25 C 0.4306(5) 0.6407(4) 0.2942(4) 0.0299(14) Uani 1 1 d . . . N25 N 0.4080(4) 0.5902(4) 0.2452(3) 0.0328(13) Uani 1 1 d . . . C26 C 0.3933(8) 0.7733(8) 0.3262(8) 0.080(4) Uani 1 1 d . . . N26 N 0.3409(9) 0.7889(10) 0.2910(9) 0.127(6) Uani 1 1 d . . . C27 C 0.5683(8) 0.8628(6) 0.4266(6) 0.060(3) Uani 1 1 d . . . N27 N 0.6149(8) 0.9277(6) 0.4469(6) 0.087(4) Uani 1 1 d . . . C28 C 0.5207(8) 0.7822(6) 0.3022(6) 0.058(2) Uani 1 1 d . . . N28 N 0.5399(8) 0.8046(6) 0.2564(6) 0.081(3) Uani 1 1 d . . . C31 C 0.6834(4) 0.6219(4) 0.6310(3) 0.0232(12) Uani 1 1 d . . . N31 N 0.6151(3) 0.5786(3) 0.5855(3) 0.0252(11) Uani 1 1 d . . . C32 C 0.8115(4) 0.7210(4) 0.6115(4) 0.0302(14) Uani 1 1 d . . . N32 N 0.8077(4) 0.7335(4) 0.5553(3) 0.0333(13) Uani 1 1 d . . . C33 C 0.8118(4) 0.5989(5) 0.6651(4) 0.0306(15) Uani 1 1 d . . . N33 N 0.8070(4) 0.5426(4) 0.6365(3) 0.0322(13) Uani 1 1 d . . . C34 C 0.7344(5) 0.7564(4) 0.7004(4) 0.0337(16) Uani 1 1 d . . . N34 N 0.6883(4) 0.7828(4) 0.6935(4) 0.0394(15) Uani 1 1 d . . . C35 C 0.7481(4) 0.6180(4) 0.7668(3) 0.0291(14) Uani 1 1 d . . . N35 N 0.7103(4) 0.5765(4) 0.7933(3) 0.0329(13) Uani 1 1 d . . . C36 C 0.8529(6) 0.7653(5) 0.8256(5) 0.047(2) Uani 1 1 d . . . N36 N 0.8734(6) 0.8000(5) 0.8841(4) 0.062(2) Uani 1 1 d . . . C37 C 0.9093(5) 0.8195(5) 0.7330(5) 0.0414(18) Uani 1 1 d . . . N37 N 0.9593(6) 0.8822(5) 0.7429(5) 0.067(2) Uani 1 1 d . . . C38 C 0.9288(5) 0.6984(5) 0.7856(5) 0.0454(19) Uani 1 1 d . . . N38 N 0.9912(5) 0.6981(5) 0.8278(5) 0.066(2) Uani 1 1 d . . . N201 N 0.8635(4) 0.8826(4) 0.5199(4) 0.0359(14) Uani 1 1 d . . . C202 C 0.8262(6) 0.9205(5) 0.5389(6) 0.051(2) Uani 1 1 d . . . H202 H 0.7646 0.8953 0.5186 0.062 Uiso 1 1 calc R . . C203 C 0.8735(7) 0.9938(5) 0.5861(7) 0.063(3) Uani 1 1 d . . . H203 H 0.8443 1.0183 0.5979 0.075 Uiso 1 1 calc R . . C204 C 0.9627(7) 1.0323(5) 0.6165(7) 0.063(3) Uani 1 1 d . . . C205 C 1.0014(6) 0.9925(5) 0.5960(5) 0.048(2) Uani 1 1 d . . . H205 H 1.0629 1.0167 0.6152 0.057 Uiso 1 1 calc R . . C206 C 0.9503(5) 0.9188(4) 0.5483(4) 0.0369(17) Uani 1 1 d . . . C207 C 0.9864(5) 0.8715(4) 0.5257(4) 0.0358(16) Uani 1 1 d . . . C208 C 1.0741(5) 0.9024(5) 0.5420(5) 0.0440(19) Uani 1 1 d . . . H208 H 1.1144 0.9554 0.5690 0.053 Uiso 1 1 calc R . . C209 C 1.1016(6) 0.8545(6) 0.5182(6) 0.053(2) Uani 1 1 d . . . C210 C 1.0427(6) 0.7798(5) 0.4799(6) 0.050(2) Uani 1 1 d . . . H210 H 1.0603 0.7462 0.4632 0.060 Uiso 1 1 calc R . . C211 C 0.9551(5) 0.7515(5) 0.4647(5) 0.0399(17) Uani 1 1 d . . . H211 H 0.9141 0.6985 0.4378 0.048 Uiso 1 1 calc R . . N212 N 0.9278(4) 0.7970(4) 0.4870(3) 0.0327(13) Uani 1 1 d . . . C213 C 1.0185(9) 1.1120(6) 0.6705(9) 0.100(6) Uani 1 1 d . . . H21A H 1.0800 1.1282 0.6853 0.150 Uiso 1 1 calc R . . H21B H 1.0077 1.1098 0.7145 0.150 Uiso 1 1 calc R . . H21C H 1.0042 1.1500 0.6469 0.150 Uiso 1 1 calc R . . C214 C 1.1966(7) 0.8890(7) 0.5350(9) 0.083(4) Uani 1 1 d . . . H21D H 1.2282 0.9440 0.5632 0.124 Uiso 1 1 calc R . . H21E H 1.2017 0.8859 0.4884 0.124 Uiso 1 1 calc R . . H21F H 1.2215 0.8596 0.5644 0.124 Uiso 1 1 calc R . . O215 O 0.7968(4) 0.8077(4) 0.3651(3) 0.0464(14) Uani 1 1 d . . . C216 C 0.7685(10) 0.7631(9) 0.2988(8) 0.087(4) Uani 1 1 d . . . H21G H 0.7946 0.7280 0.3054 0.105 Uiso 1 1 calc R . . H21H H 0.7899 0.7973 0.2686 0.105 Uiso 1 1 calc R . . C217 C 0.6676(11) 0.7117(14) 0.2546(8) 0.126(8) Uani 1 1 d . . . H21I H 0.6531 0.6809 0.2067 0.188 Uiso 1 1 calc R . . H21J H 0.6408 0.7456 0.2461 0.188 Uiso 1 1 calc R . . H21K H 0.6456 0.6762 0.2831 0.188 Uiso 1 1 calc R . . N301 N 0.9357(4) 0.5215(4) 0.6069(3) 0.0315(12) Uani 1 1 d . . . C302 C 0.9512(5) 0.5443(5) 0.5493(4) 0.0342(15) Uani 1 1 d . . . H302 H 0.9041 0.5244 0.5009 0.041 Uiso 1 1 calc R . . C303 C 1.0332(5) 0.5955(5) 0.5591(5) 0.0400(18) Uani 1 1 d . . . H303 H 1.0419 0.6102 0.5174 0.048 Uiso 1 1 calc R . . C304 C 1.1035(5) 0.6261(5) 0.6283(5) 0.0409(18) Uani 1 1 d . . . C305 C 1.0861(5) 0.6015(5) 0.6872(5) 0.0398(17) Uani 1 1 d . . . H305 H 1.1324 0.6200 0.7358 0.048 Uiso 1 1 calc R . . C306 C 1.0023(5) 0.5507(5) 0.6752(4) 0.0351(16) Uani 1 1 d . . . C307 C 0.9792(5) 0.5204(5) 0.7346(4) 0.0378(17) Uani 1 1 d . . . C308 C 1.0373(6) 0.5475(6) 0.8099(5) 0.054(2) Uani 1 1 d . . . H308 H 1.0955 0.5875 0.8259 0.064 Uiso 1 1 calc R . . C309 C 1.0102(6) 0.5159(7) 0.8618(5) 0.064(3) Uani 1 1 d . . . C310 C 0.9262(6) 0.4566(7) 0.8358(5) 0.067(3) Uani 1 1 d . . . H310 H 0.9062 0.4324 0.8695 0.080 Uiso 1 1 calc R . . C311 C 0.8705(6) 0.4317(6) 0.7605(5) 0.055(2) Uani 1 1 d . . . H311 H 0.8124 0.3910 0.7438 0.066 Uiso 1 1 calc R . . N312 N 0.8956(4) 0.4631(4) 0.7107(4) 0.0375(14) Uani 1 1 d . . . C313 C 1.1935(6) 0.6817(6) 0.6401(7) 0.058(2) Uani 1 1 d . . . H31A H 1.2338 0.6964 0.6928 0.087 Uiso 1 1 calc R . . H31B H 1.1947 0.7287 0.6245 0.087 Uiso 1 1 calc R . . H31C H 1.2110 0.6564 0.6107 0.087 Uiso 1 1 calc R . . C314 C 1.0722(8) 0.5477(10) 0.9443(6) 0.092(5) Uani 1 1 d . . . H31D H 1.1285 0.5898 0.9513 0.137 Uiso 1 1 calc R . . H31E H 1.0801 0.5055 0.9643 0.137 Uiso 1 1 calc R . . H31F H 1.0479 0.5682 0.9702 0.137 Uiso 1 1 calc R . . O315 O 0.8322(3) 0.3532(3) 0.5666(3) 0.0411(12) Uani 1 1 d D . . H315 H 0.8835 0.3601 0.5909 0.05(3) Uiso 1 1 d R A . C316 C 0.781(2) 0.2758(14) 0.5762(19) 0.050(11) Uiso 0.23(2) 1 d PD A 3 H31G H 0.7648 0.2821 0.6166 0.061 Uiso 0.23(2) 1 calc PR A 3 H31H H 0.8152 0.2477 0.5888 0.061 Uiso 0.23(2) 1 calc PR A 3 C317 C 0.697(2) 0.229(2) 0.5004(17) 0.041(10) Uiso 0.23(2) 1 d PD A 3 H31I H 0.6612 0.1769 0.5044 0.061 Uiso 0.23(2) 1 calc PR A 3 H31J H 0.7141 0.2233 0.4609 0.061 Uiso 0.23(2) 1 calc PR A 3 H31K H 0.6639 0.2573 0.4888 0.061 Uiso 0.23(2) 1 calc PR A 3 C318 C 0.7482(14) 0.2168(12) 0.5873(11) 0.096(7) Uiso 0.77(2) 1 d PD A 4 H31L H 0.7013 0.1636 0.5588 0.145 Uiso 0.77(2) 1 calc PR A 4 H31M H 0.7319 0.2390 0.6203 0.145 Uiso 0.77(2) 1 calc PR A 4 H31N H 0.8016 0.2150 0.6170 0.145 Uiso 0.77(2) 1 calc PR A 4 C319 C 0.7641(18) 0.2702(11) 0.5316(14) 0.148(11) Uiso 0.77(2) 1 d PD A 4 H31O H 0.7800 0.2466 0.4985 0.177 Uiso 0.77(2) 1 calc PR A 4 H31P H 0.7086 0.2688 0.5001 0.177 Uiso 0.77(2) 1 calc PR A 4 N401 N 0.5202(5) 0.8656(4) 0.6844(4) 0.0382(14) Uani 1 1 d . . . C404 C 0.4392(9) 0.9498(7) 0.7051(7) 0.072(3) Uani 1 1 d . . . N412 N 0.6881(5) 0.9329(4) 0.6989(4) 0.0451(17) Uani 1 1 d . . . C413 C 0.3963(11) 0.9948(10) 0.7183(9) 0.100(5) Uani 1 1 d . B . H41A H 0.3411 0.9587 0.7182 0.150 Uiso 1 1 calc R . . H41B H 0.3851 1.0216 0.6789 0.150 Uiso 1 1 calc R . . H41C H 0.4346 1.0336 0.7665 0.150 Uiso 1 1 calc R . . N427 N 0.6412(5) 0.8433(5) 0.7982(4) 0.0505(19) Uani 1 1 d . . . C402 C 0.4438(12) 0.8338(8) 0.6824(10) 0.046(4) Uani 0.520(8) 1 d P B 1 H402 H 0.4133 0.7782 0.6719 0.055 Uiso 0.520(8) 1 calc PR B 1 C403 C 0.4032(10) 0.8735(10) 0.6939(9) 0.045(4) Uani 0.520(8) 1 d P B 1 H403 H 0.3480 0.8453 0.6939 0.054 Uiso 0.520(8) 1 calc PR B 1 C405 C 0.5309(13) 0.9926(10) 0.7112(11) 0.056(5) Uani 0.520(8) 1 d P B 1 H405 H 0.5618 1.0481 0.7219 0.067 Uiso 0.520(8) 1 calc PR B 1 C406 C 0.5669(12) 0.9479(9) 0.7007(10) 0.047(4) Uani 0.520(8) 1 d P B 1 C407 C 0.6600(12) 0.9821(9) 0.7110(10) 0.048(4) Uani 0.520(8) 1 d P B 1 C408 C 0.7090(16) 1.0608(12) 0.7266(17) 0.088(8) Uani 0.520(8) 1 d P B 1 H408 H 0.6861 1.0942 0.7327 0.106 Uiso 0.520(8) 1 calc PR B 1 C409 C 0.7978(15) 1.0939(11) 0.7340(16) 0.081(8) Uani 0.520(8) 1 d P B 1 C410 C 0.8262(15) 1.0364(12) 0.7277(15) 0.077(7) Uani 0.520(8) 1 d P B 1 H410 H 0.8846 1.0525 0.7368 0.092 Uiso 0.520(8) 1 calc PR B 1 C411 C 0.7653(12) 0.9568(10) 0.7080(11) 0.055(5) Uani 0.520(8) 1 d P B 1 H411 H 0.7828 0.9191 0.7012 0.066 Uiso 0.520(8) 1 calc PR B 1 C414 C 0.8657(18) 1.1738(16) 0.748(2) 0.16(2) Uani 0.520(8) 1 d P B 1 H41D H 0.9175 1.1728 0.7497 0.241 Uiso 0.520(8) 1 calc PR B 1 H41E H 0.8806 1.2049 0.7962 0.241 Uiso 0.520(8) 1 calc PR B 1 H41F H 0.8447 1.1973 0.7088 0.241 Uiso 0.520(8) 1 calc PR B 1 C417 C 0.4677(14) 0.8796(13) 0.6277(12) 0.056(5) Uani 0.480(8) 1 d P B 2 H417 H 0.4628 0.8644 0.5799 0.067 Uiso 0.480(8) 1 calc PR B 2 C418 C 0.4196(19) 0.9149(17) 0.6338(15) 0.079(7) Uani 0.480(8) 1 d P B 2 H418 H 0.3753 0.9152 0.5911 0.094 Uiso 0.480(8) 1 calc PR B 2 C420 C 0.4801(14) 0.9203(14) 0.7646(14) 0.061(6) Uani 0.480(8) 1 d P B 2 H420 H 0.4775 0.9270 0.8106 0.073 Uiso 0.480(8) 1 calc PR B 2 C421 C 0.5228(12) 0.8820(10) 0.7522(10) 0.042(4) Uani 0.480(8) 1 d P B 2 C422 C 0.5832(13) 0.8668(11) 0.8128(11) 0.047(4) Uani 0.480(8) 1 d P B 2 C423 C 0.5959(11) 0.8803(10) 0.8852(9) 0.038(4) Uani 0.480(8) 1 d P B 2 H423 H 0.5629 0.8998 0.8975 0.045 Uiso 0.480(8) 1 calc PR B 2 C424 C 0.651(2) 0.8677(16) 0.9368(18) 0.085(9) Uani 0.480(8) 1 d P B 2 C425 C 0.6950(17) 0.8423(17) 0.9203(12) 0.076(7) Uani 0.480(8) 1 d P B 2 H425 H 0.7348 0.8320 0.9581 0.091 Uiso 0.480(8) 1 calc PR B 2 C426 C 0.6869(16) 0.8290(14) 0.8478(10) 0.063(6) Uani 0.480(8) 1 d P B 2 H426 H 0.7196 0.8074 0.8380 0.075 Uiso 0.480(8) 1 calc PR B 2 C429 C 0.670(3) 0.884(3) 1.0207(14) 0.134(17) Uani 0.480(8) 1 d P B 2 H42A H 0.6327 0.9046 1.0269 0.201 Uiso 0.480(8) 1 calc PR B 2 H42B H 0.7311 0.9234 1.0508 0.201 Uiso 0.480(8) 1 calc PR B 2 H42C H 0.6576 0.8358 1.0367 0.201 Uiso 0.480(8) 1 calc PR B 2 N501 N 0.4241(4) 0.5577(4) 0.1016(3) 0.0324(13) Uani 1 1 d . . . C502 C 0.4746(6) 0.6346(5) 0.1178(5) 0.0447(19) Uani 1 1 d . . . H502 H 0.4884 0.6656 0.1635 0.054 Uiso 1 1 calc R . . C503 C 0.5083(6) 0.6719(5) 0.0721(5) 0.049(2) Uani 1 1 d . . . H503 H 0.5442 0.7272 0.0866 0.059 Uiso 1 1 calc R . . C504 C 0.4897(6) 0.6289(6) 0.0057(5) 0.049(2) Uani 1 1 d . . . C505 C 0.4366(6) 0.5495(5) -0.0120(4) 0.0434(19) Uani 1 1 d . . . H505 H 0.4221 0.5177 -0.0576 0.052 Uiso 1 1 calc R . . C506 C 0.4036(5) 0.5146(5) 0.0358(4) 0.0380(17) Uani 1 1 d . . . C507 C 0.3442(6) 0.4298(5) 0.0182(4) 0.0430(19) Uani 1 1 d . . . C508 C 0.3129(7) 0.3779(6) -0.0480(5) 0.058(3) Uani 1 1 d . . . H508 H 0.3301 0.3958 -0.0852 0.070 Uiso 1 1 calc R . . C509 C 0.2563(9) 0.2996(7) -0.0601(6) 0.078(4) Uani 1 1 d . . . C510 C 0.2318(9) 0.2772(7) -0.0046(7) 0.077(4) Uani 1 1 d . . . H510 H 0.1916 0.2242 -0.0115 0.093 Uiso 1 1 calc R . . C511 C 0.2652(7) 0.3311(6) 0.0595(5) 0.059(3) Uani 1 1 d . . . H511 H 0.2490 0.3140 0.0973 0.070 Uiso 1 1 calc R . . N512 N 0.3191(4) 0.4060(4) 0.0720(3) 0.0391(15) Uani 1 1 d . . . C513 C 0.5232(7) 0.6674(7) -0.0477(6) 0.065(3) Uani 1 1 d . . . H51A H 0.5028 0.6271 -0.0917 0.097 Uiso 1 1 calc R . . H51B H 0.5870 0.6957 -0.0231 0.097 Uiso 1 1 calc R . . H51C H 0.5014 0.7043 -0.0626 0.097 Uiso 1 1 calc R . . C514 C 0.2212(13) 0.2421(8) -0.1318(8) 0.120(7) Uani 1 1 d . . . H51D H 0.1830 0.1896 -0.1305 0.179 Uiso 1 1 calc R . . H51E H 0.2696 0.2420 -0.1389 0.179 Uiso 1 1 calc R . . H51F H 0.1881 0.2573 -0.1730 0.179 Uiso 1 1 calc R . . O515 O 0.2565(4) 0.5127(4) 0.0974(3) 0.0453(14) Uani 1 1 d . . . O61E O 0.9946(4) 0.3747(3) 0.6437(3) 0.0424(13) Uiso 1 1 d . . . H61E H 1.0422 0.4051 0.6429 0.08(4) Uiso 1 1 d R . . C62E C 1.0207(10) 0.3651(9) 0.7179(8) 0.087(4) Uiso 1 1 d . . . H62A H 1.0516 0.4176 0.7526 0.105 Uiso 1 1 calc R . . H62B H 0.9672 0.3337 0.7237 0.105 Uiso 1 1 calc R . . C63E C 1.0749(11) 0.3292(10) 0.7415(9) 0.098(4) Uiso 1 1 d . . . H63A H 1.0872 0.3260 0.7928 0.148 Uiso 1 1 calc R . . H63B H 1.1297 0.3607 0.7388 0.148 Uiso 1 1 calc R . . H63C H 1.0450 0.2763 0.7091 0.148 Uiso 1 1 calc R . . O71E O 1.0561(12) 0.7811(11) 0.6753(11) 0.174(6) Uiso 1 1 d . . . C73E C 1.2046(11) 0.8701(10) 0.7438(9) 0.100(5) Uiso 1 1 d . . . H73A H 1.2577 0.8886 0.7902 0.150 Uiso 1 1 calc R . . H73B H 1.1908 0.9129 0.7354 0.150 Uiso 1 1 calc R . . H73C H 1.2136 0.8529 0.7024 0.150 Uiso 1 1 calc R . . C72E C 1.1388(14) 0.8102(13) 0.7482(13) 0.138(7) Uiso 1 1 d . . . H72A H 1.1295 0.8273 0.7899 0.165 Uiso 1 1 calc R . . H72B H 1.1528 0.7672 0.7575 0.165 Uiso 1 1 calc R . . O1H O 0.7483(6) 0.9180(5) 0.3448(5) 0.075(2) Uiso 1 1 d . . . O2H O 0.9082(7) 0.6001(6) 0.9313(6) 0.098(3) Uiso 1 1 d . . . O3H O 0.7637(10) 0.9774(9) 0.2329(8) 0.143(5) Uiso 1 1 d . . . O4H O 1.1609(12) 0.7565(11) 0.9320(11) 0.181(7) Uiso 1 1 d . . . O5H O 1.2674(16) 0.6705(14) 0.9192(14) 0.234(10) Uiso 1 1 d . . . O6H O 0.5920(11) 0.8682(10) 0.1464(10) 0.076(4) Uiso 0.50 1 d P . . O7H O 1.3840(9) 0.7809(8) 0.8935(8) 0.057(3) Uiso 0.50 1 d P . . O8H O 1.1019(13) 1.0342(12) 0.7933(12) 0.095(6) Uiso 0.50 1 d P . . O9H O 0.2985(15) 0.6656(14) 0.0800(13) 0.107(7) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02602(13) 0.03114(14) 0.01907(12) 0.00776(10) 0.01505(10) 0.01480(11) W2 0.02990(14) 0.02690(14) 0.02406(13) 0.01058(10) 0.01560(11) 0.01364(11) W3 0.02079(13) 0.03293(15) 0.01993(13) 0.00301(10) 0.00780(10) 0.00772(11) Ni1 0.0188(5) 0.0244(5) 0.0148(5) 0.0050(4) 0.0097(4) 0.0099(4) Ni2 0.0251(4) 0.0290(4) 0.0305(4) 0.0076(4) 0.0172(4) 0.0069(3) Ni3 0.0241(4) 0.0385(5) 0.0264(4) 0.0125(4) 0.0125(3) 0.0175(4) Ni4 0.0327(4) 0.0278(4) 0.0277(4) 0.0009(3) 0.0166(4) 0.0111(4) Ni5 0.0297(4) 0.0379(5) 0.0167(4) 0.0085(3) 0.0106(3) 0.0160(4) C11 0.023(3) 0.025(3) 0.021(3) 0.007(2) 0.013(2) 0.011(2) N11 0.024(3) 0.025(3) 0.021(3) 0.007(2) 0.010(2) 0.011(2) C12 0.026(3) 0.040(4) 0.021(3) 0.011(3) 0.016(3) 0.011(3) N12 0.031(3) 0.038(3) 0.032(3) 0.012(3) 0.020(3) 0.009(3) C13 0.026(3) 0.035(3) 0.026(3) 0.012(3) 0.017(3) 0.019(3) N13 0.027(3) 0.039(3) 0.032(3) 0.010(3) 0.017(3) 0.019(3) C14 0.027(3) 0.034(4) 0.022(3) 0.004(3) 0.014(3) 0.016(3) N14 0.035(3) 0.036(3) 0.029(3) 0.008(2) 0.016(3) 0.020(3) C15 0.040(4) 0.038(4) 0.023(3) 0.013(3) 0.022(3) 0.021(3) N15 0.036(3) 0.042(3) 0.023(3) 0.010(2) 0.014(3) 0.020(3) C16 0.036(4) 0.046(4) 0.036(4) 0.017(3) 0.025(3) 0.021(3) N16 0.044(4) 0.070(5) 0.050(4) 0.029(4) 0.033(3) 0.033(4) C17 0.053(5) 0.045(4) 0.038(4) 0.017(3) 0.031(4) 0.028(4) N17 0.076(5) 0.046(4) 0.054(4) 0.006(3) 0.044(4) 0.030(4) C18 0.033(3) 0.044(4) 0.023(3) 0.008(3) 0.018(3) 0.016(3) N18 0.047(4) 0.056(4) 0.028(3) 0.015(3) 0.025(3) 0.019(3) C21 0.023(3) 0.025(3) 0.019(3) 0.008(2) 0.011(2) 0.011(2) N21 0.023(3) 0.029(3) 0.021(2) 0.004(2) 0.013(2) 0.011(2) C22 0.027(3) 0.033(4) 0.037(4) 0.012(3) 0.021(3) 0.010(3) N22 0.035(3) 0.043(4) 0.035(3) 0.012(3) 0.023(3) 0.008(3) C23 0.029(3) 0.035(4) 0.032(3) 0.014(3) 0.013(3) 0.018(3) N23 0.030(3) 0.045(4) 0.034(3) 0.015(3) 0.016(3) 0.019(3) C24 0.036(4) 0.028(3) 0.033(4) 0.010(3) 0.020(3) 0.016(3) N24 0.046(4) 0.033(3) 0.033(3) 0.004(3) 0.023(3) 0.016(3) C25 0.035(3) 0.041(4) 0.023(3) 0.015(3) 0.016(3) 0.022(3) N25 0.035(3) 0.045(4) 0.022(3) 0.013(3) 0.015(2) 0.020(3) C26 0.073(7) 0.097(9) 0.125(11) 0.081(9) 0.067(8) 0.060(7) N26 0.101(9) 0.188(15) 0.182(15) 0.141(13) 0.088(10) 0.113(11) C27 0.078(7) 0.042(5) 0.056(6) 0.016(4) 0.033(5) 0.022(5) N27 0.103(8) 0.048(5) 0.067(6) 0.017(5) 0.031(6) 0.006(5) C28 0.081(7) 0.066(6) 0.048(5) 0.031(5) 0.040(5) 0.040(6) N28 0.125(9) 0.079(7) 0.084(7) 0.050(6) 0.081(7) 0.054(7) C31 0.027(3) 0.023(3) 0.024(3) 0.005(2) 0.016(3) 0.012(3) N31 0.023(3) 0.031(3) 0.021(3) 0.008(2) 0.012(2) 0.011(2) C32 0.025(3) 0.031(3) 0.026(3) 0.004(3) 0.012(3) 0.007(3) N32 0.029(3) 0.033(3) 0.029(3) 0.006(2) 0.014(2) 0.007(3) C33 0.021(3) 0.044(4) 0.022(3) 0.008(3) 0.008(3) 0.014(3) N33 0.027(3) 0.043(4) 0.029(3) 0.011(3) 0.014(2) 0.017(3) C34 0.027(3) 0.036(4) 0.025(3) -0.005(3) 0.011(3) 0.007(3) N34 0.036(3) 0.041(4) 0.036(3) -0.004(3) 0.016(3) 0.015(3) C35 0.026(3) 0.038(4) 0.016(3) 0.006(3) 0.006(3) 0.013(3) N35 0.033(3) 0.045(3) 0.018(3) 0.006(2) 0.011(2) 0.017(3) C36 0.039(4) 0.050(5) 0.033(4) 0.004(4) 0.016(3) 0.006(4) N36 0.063(5) 0.056(5) 0.032(4) -0.007(3) 0.018(4) 0.005(4) C37 0.040(4) 0.038(4) 0.037(4) 0.002(3) 0.017(3) 0.011(4) N37 0.069(6) 0.048(5) 0.055(5) 0.004(4) 0.029(4) 0.006(4) C38 0.035(4) 0.042(4) 0.042(4) 0.007(4) 0.008(4) 0.012(4) N38 0.035(4) 0.067(5) 0.060(5) 0.004(4) -0.008(4) 0.021(4) N201 0.035(3) 0.032(3) 0.045(4) 0.011(3) 0.027(3) 0.012(3) C202 0.048(5) 0.040(4) 0.079(7) 0.014(4) 0.043(5) 0.019(4) C203 0.068(6) 0.035(4) 0.100(8) 0.011(5) 0.065(6) 0.014(4) C204 0.075(7) 0.036(5) 0.083(7) 0.004(5) 0.062(6) 0.009(5) C205 0.046(5) 0.032(4) 0.063(5) 0.004(4) 0.042(4) 0.002(3) C206 0.040(4) 0.031(4) 0.043(4) 0.012(3) 0.031(4) 0.009(3) C207 0.032(4) 0.034(4) 0.034(4) 0.007(3) 0.018(3) 0.008(3) C208 0.027(4) 0.036(4) 0.055(5) 0.000(4) 0.021(4) 0.003(3) C209 0.033(4) 0.052(5) 0.067(6) 0.011(5) 0.025(4) 0.013(4) C210 0.039(4) 0.050(5) 0.071(6) 0.016(4) 0.031(4) 0.025(4) C211 0.035(4) 0.041(4) 0.043(4) 0.009(3) 0.020(3) 0.016(3) N212 0.028(3) 0.034(3) 0.034(3) 0.009(3) 0.017(3) 0.010(3) C213 0.104(10) 0.031(5) 0.159(14) -0.018(6) 0.108(11) -0.011(6) C214 0.041(5) 0.073(8) 0.126(11) 0.001(7) 0.043(7) 0.019(5) O215 0.046(3) 0.062(4) 0.046(3) 0.031(3) 0.034(3) 0.025(3) C216 0.098(10) 0.106(11) 0.081(9) 0.033(8) 0.051(8) 0.058(9) C217 0.119(13) 0.26(2) 0.064(8) 0.065(12) 0.052(9) 0.134(16) N301 0.032(3) 0.037(3) 0.036(3) 0.015(3) 0.018(3) 0.022(3) C302 0.033(4) 0.042(4) 0.037(4) 0.014(3) 0.018(3) 0.023(3) C303 0.038(4) 0.042(4) 0.057(5) 0.022(4) 0.033(4) 0.022(4) C304 0.039(4) 0.038(4) 0.061(5) 0.023(4) 0.028(4) 0.025(4) C305 0.028(4) 0.038(4) 0.053(5) 0.015(4) 0.017(3) 0.016(3) C306 0.026(3) 0.043(4) 0.041(4) 0.016(3) 0.016(3) 0.020(3) C307 0.031(4) 0.049(4) 0.035(4) 0.019(3) 0.012(3) 0.022(3) C308 0.036(4) 0.071(6) 0.046(5) 0.022(5) 0.014(4) 0.022(4) C309 0.045(5) 0.092(8) 0.041(5) 0.030(5) 0.011(4) 0.028(5) C310 0.047(5) 0.108(9) 0.036(5) 0.040(5) 0.016(4) 0.029(6) C311 0.046(5) 0.072(6) 0.036(4) 0.028(4) 0.018(4) 0.019(5) N312 0.032(3) 0.055(4) 0.033(3) 0.024(3) 0.017(3) 0.024(3) C313 0.041(5) 0.050(5) 0.084(7) 0.024(5) 0.034(5) 0.017(4) C314 0.055(6) 0.136(13) 0.041(6) 0.028(7) 0.005(5) 0.025(7) O315 0.031(3) 0.045(3) 0.052(3) 0.010(3) 0.017(2) 0.024(2) N401 0.052(4) 0.031(3) 0.041(4) 0.010(3) 0.026(3) 0.023(3) C404 0.092(8) 0.077(8) 0.063(7) 0.011(6) 0.029(6) 0.060(7) N412 0.051(4) 0.030(3) 0.045(4) -0.004(3) 0.030(3) 0.007(3) C413 0.130(13) 0.112(11) 0.104(11) 0.023(9) 0.050(10) 0.099(11) N427 0.054(4) 0.055(4) 0.030(3) -0.009(3) 0.017(3) 0.019(4) C402 0.063(10) 0.021(7) 0.059(10) 0.010(7) 0.035(9) 0.018(7) C403 0.034(8) 0.040(8) 0.047(9) 0.002(7) 0.011(7) 0.013(7) C405 0.071(12) 0.031(8) 0.055(10) 0.002(7) 0.012(9) 0.030(8) C406 0.054(10) 0.031(8) 0.056(10) 0.018(7) 0.029(8) 0.017(7) C407 0.059(10) 0.025(7) 0.051(10) 0.008(7) 0.026(8) 0.011(7) C408 0.075(15) 0.036(10) 0.14(2) 0.032(13) 0.036(16) 0.021(10) C409 0.060(13) 0.031(9) 0.12(2) -0.002(11) 0.045(14) -0.007(9) C410 0.067(13) 0.050(11) 0.098(17) 0.005(11) 0.058(13) -0.001(10) C411 0.059(11) 0.031(8) 0.062(11) -0.010(7) 0.037(9) 0.004(8) C414 0.063(16) 0.067(17) 0.24(4) 0.10(2) 0.01(2) -0.020(13) C417 0.058(12) 0.063(12) 0.053(11) 0.022(10) 0.021(10) 0.037(10) C418 0.092(19) 0.095(19) 0.072(16) 0.030(14) 0.037(15) 0.062(17) C420 0.054(11) 0.073(14) 0.078(15) 0.016(12) 0.036(11) 0.045(11) C421 0.046(9) 0.037(9) 0.051(10) 0.008(7) 0.028(8) 0.020(8) C422 0.057(11) 0.043(9) 0.054(11) 0.009(8) 0.035(9) 0.026(9) C423 0.043(9) 0.053(10) 0.025(7) 0.004(7) 0.024(7) 0.023(8) C424 0.10(2) 0.066(15) 0.09(2) -0.002(14) 0.067(19) 0.025(15) C425 0.078(16) 0.100(19) 0.042(11) 0.036(12) 0.023(11) 0.038(15) C426 0.084(15) 0.083(15) 0.028(9) 0.008(9) 0.013(10) 0.057(14) C429 0.22(4) 0.19(4) 0.035(13) 0.014(18) 0.030(19) 0.15(4) N501 0.034(3) 0.040(3) 0.020(3) 0.008(2) 0.011(2) 0.017(3) C502 0.050(5) 0.044(5) 0.038(4) 0.013(4) 0.025(4) 0.017(4) C503 0.057(5) 0.042(5) 0.042(5) 0.018(4) 0.027(4) 0.014(4) C504 0.041(4) 0.066(6) 0.032(4) 0.022(4) 0.016(4) 0.018(4) C505 0.049(5) 0.059(5) 0.023(3) 0.014(3) 0.019(3) 0.023(4) C506 0.044(4) 0.048(4) 0.019(3) 0.012(3) 0.015(3) 0.018(4) C507 0.047(4) 0.053(5) 0.020(3) 0.011(3) 0.014(3) 0.017(4) C508 0.078(7) 0.052(5) 0.034(4) 0.005(4) 0.032(5) 0.017(5) C509 0.100(9) 0.061(7) 0.045(6) -0.007(5) 0.039(6) 0.010(6) C510 0.093(8) 0.052(6) 0.066(7) 0.001(5) 0.055(7) 0.002(6) C511 0.073(6) 0.051(5) 0.042(5) 0.006(4) 0.040(5) 0.012(5) N512 0.047(4) 0.042(4) 0.022(3) 0.005(3) 0.021(3) 0.012(3) C513 0.059(6) 0.066(6) 0.045(5) 0.025(5) 0.026(5) 0.006(5) C514 0.169(16) 0.069(8) 0.064(8) -0.015(7) 0.067(10) 0.000(9) O515 0.041(3) 0.070(4) 0.029(3) 0.020(3) 0.013(2) 0.031(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C12 2.145(7) . ? W1 C17 2.152(8) . ? W1 C11 2.161(6) . ? W1 C13 2.167(6) . ? W1 C14 2.169(7) . ? W1 C16 2.171(7) . ? W1 C18 2.173(7) . ? W1 C15 2.178(7) . ? W2 C26 2.121(11) . ? W2 C22 2.155(7) . ? W2 C25 2.156(7) . ? W2 C24 2.158(7) . ? W2 C21 2.162(6) . ? W2 C23 2.163(7) . ? W2 C27 2.169(10) . ? W2 C28 2.183(9) . ? W3 C32 2.138(7) . ? W3 C38 2.139(9) . ? W3 C34 2.139(8) . ? W3 C31 2.149(7) . ? W3 C35 2.155(7) . ? W3 C37 2.157(8) . ? W3 C33 2.161(8) . ? W3 C36 2.172(8) . ? Ni1 N31 2.025(5) 2_666 ? Ni1 N31 2.025(5) . ? Ni1 N11 2.030(5) . ? Ni1 N11 2.030(5) 2_666 ? Ni1 N21 2.049(6) 2_666 ? Ni1 N21 2.049(6) . ? Ni2 N12 2.032(7) . ? Ni2 N32 2.043(6) . ? Ni2 N22 2.061(7) . ? Ni2 N201 2.062(6) . ? Ni2 N212 2.066(6) . ? Ni2 O215 2.087(5) . ? Ni3 N23 2.061(6) 2_666 ? Ni3 N33 2.063(7) . ? Ni3 N13 2.064(6) . ? Ni3 N301 2.073(6) . ? Ni3 N312 2.079(6) . ? Ni3 O315 2.101(6) . ? Ni4 N34 2.048(7) . ? Ni4 N14 2.058(6) 2_666 ? Ni4 N401 2.060(7) . ? Ni4 N24 2.064(6) . ? Ni4 N412 2.088(7) . ? Ni4 N427 2.103(7) . ? Ni5 N35 2.042(6) 2_666 ? Ni5 N25 2.048(6) . ? Ni5 N501 2.068(6) . ? Ni5 N512 2.071(6) . ? Ni5 N15 2.080(6) . ? Ni5 O515 2.140(6) . ? C11 N11 1.137(8) . ? C12 N12 1.161(10) . ? C13 N13 1.141(9) . ? C14 N14 1.138(9) . ? N14 Ni4 2.058(6) 2_666 ? C15 N15 1.146(10) . ? C16 N16 1.147(10) . ? C17 N17 1.158(11) . ? C18 N18 1.143(10) . ? C21 N21 1.125(8) . ? C22 N22 1.141(10) . ? C23 N23 1.146(9) . ? N23 Ni3 2.061(6) 2_666 ? C24 N24 1.157(10) . ? C25 N25 1.159(10) . ? C26 N26 1.154(15) . ? C27 N27 1.126(13) . ? C28 N28 1.155(12) . ? C31 N31 1.147(8) . ? C32 N32 1.151(9) . ? C33 N33 1.165(10) . ? C34 N34 1.162(10) . ? C35 N35 1.137(9) . ? N35 Ni5 2.042(6) 2_666 ? C36 N36 1.158(11) . ? C37 N37 1.130(12) . ? C38 N38 1.170(11) . ? N201 C206 1.338(10) . ? N201 C202 1.345(11) . ? C202 C203 1.367(13) . ? C202 H202 0.9500 . ? C203 C204 1.373(15) . ? C203 H203 0.9500 . ? C204 C205 1.410(13) . ? C204 C213 1.505(14) . ? C205 C206 1.375(11) . ? C205 H205 0.9500 . ? C206 C207 1.500(11) . ? C207 N212 1.343(10) . ? C207 C208 1.394(10) . ? C208 C209 1.391(13) . ? C208 H208 0.9500 . ? C209 C210 1.344(13) . ? C209 C214 1.514(12) . ? C210 C211 1.404(11) . ? C210 H210 0.9500 . ? C211 N212 1.335(10) . ? C211 H211 0.9500 . ? C213 H21A 0.9800 . ? C213 H21B 0.9800 . ? C213 H21C 0.9800 . ? C214 H21D 0.9800 . ? C214 H21E 0.9800 . ? C214 H21F 0.9800 . ? O215 C216 1.327(15) . ? C216 C217 1.56(2) . ? C216 H21G 0.9900 . ? C216 H21H 0.9900 . ? C217 H21I 0.9800 . ? C217 H21J 0.9800 . ? C217 H21K 0.9800 . ? N301 C306 1.341(10) . ? N301 C302 1.352(9) . ? C302 C303 1.370(10) . ? C302 H302 0.9500 . ? C303 C304 1.378(12) . ? C303 H303 0.9500 . ? C304 C305 1.402(12) . ? C304 C313 1.493(11) . ? C305 C306 1.380(10) . ? C305 H305 0.9500 . ? C306 C307 1.490(11) . ? C307 N312 1.360(10) . ? C307 C308 1.395(12) . ? C308 C309 1.393(13) . ? C308 H308 0.9500 . ? C309 C310 1.371(14) . ? C309 C314 1.521(14) . ? C310 C311 1.386(13) . ? C310 H310 0.9500 . ? C311 N312 1.336(10) . ? C311 H311 0.9500 . ? C313 H31A 0.9800 . ? C313 H31B 0.9800 . ? C313 H31C 0.9800 . ? C314 H31D 0.9800 . ? C314 H31E 0.9800 . ? C314 H31F 0.9800 . ? O315 C316 1.478(19) . ? O315 C319 1.480(17) . ? O315 H315 0.8525 . ? C316 C317 1.570(19) . ? C316 H31G 0.9900 . ? C316 H31H 0.9900 . ? C317 H31I 0.9800 . ? C317 H31J 0.9800 . ? C317 H31K 0.9800 . ? C318 C319 1.596(18) . ? C318 H31L 0.9800 . ? C318 H31M 0.9800 . ? C318 H31N 0.9800 . ? C319 H31O 0.9900 . ? C319 H31P 0.9900 . ? N401 C402 1.291(19) . ? N401 C417 1.33(2) . ? N401 C421 1.360(19) . ? N401 C406 1.408(17) . ? C404 C403 1.31(2) . ? C404 C418 1.39(3) . ? C404 C420 1.46(3) . ? C404 C413 1.501(15) . ? C404 C405 1.52(3) . ? N412 C411 1.26(2) . ? N412 C407 1.333(19) . ? C413 H41A 0.9800 . ? C413 H41B 0.9800 . ? C413 H41C 0.9800 . ? N427 C426 1.19(2) . ? N427 C422 1.470(19) . ? C402 C403 1.37(2) . ? C402 H402 0.9500 . ? C403 H403 0.9500 . ? C405 C406 1.37(3) . ? C405 H405 0.9500 . ? C406 C407 1.52(3) . ? C407 C408 1.35(2) . ? C408 C409 1.46(3) . ? C408 H408 0.9500 . ? C409 C410 1.45(4) . ? C409 C414 1.46(3) . ? C410 C411 1.40(2) . ? C410 H410 0.9500 . ? C411 H411 0.9500 . ? C414 H41D 0.9800 . ? C414 H41E 0.9800 . ? C414 H41F 0.9800 . ? C417 C418 1.39(3) . ? C417 H417 0.9500 . ? C418 H418 0.9500 . ? C420 C421 1.39(3) . ? C420 H420 0.9500 . ? C421 C422 1.47(3) . ? C422 C423 1.37(2) . ? C423 C424 1.29(4) . ? C423 H423 0.9500 . ? C424 C425 1.27(4) . ? C424 C429 1.57(4) . ? C425 C426 1.41(3) . ? C425 H425 0.9500 . ? C426 H426 0.9500 . ? C429 H42A 0.9800 . ? C429 H42B 0.9800 . ? C429 H42C 0.9800 . ? N501 C502 1.327(11) . ? N501 C506 1.350(9) . ? C502 C503 1.379(11) . ? C502 H502 0.9500 . ? C503 C504 1.374(13) . ? C503 H503 0.9500 . ? C504 C505 1.372(13) . ? C504 C513 1.522(11) . ? C505 C506 1.393(10) . ? C505 H505 0.9500 . ? C506 C507 1.476(12) . ? C507 N512 1.367(9) . ? C507 C508 1.378(12) . ? C508 C509 1.383(15) . ? C508 H508 0.9500 . ? C509 C510 1.386(15) . ? C509 C514 1.499(15) . ? C510 C511 1.356(14) . ? C510 H510 0.9500 . ? C511 N512 1.317(11) . ? C511 H511 0.9500 . ? C513 H51A 0.9800 . ? C513 H51B 0.9800 . ? C513 H51C 0.9800 . ? C514 H51D 0.9800 . ? C514 H51E 0.9800 . ? C514 H51F 0.9800 . ? O61E C62E 1.435(15) . ? O61E H61E 0.8484 . ? C62E C63E 1.44(2) . ? C62E H62A 0.9900 . ? C62E H62B 0.9900 . ? C63E H63A 0.9800 . ? C63E H63B 0.9800 . ? C63E H63C 0.9800 . ? O71E C72E 1.53(3) . ? C73E C72E 1.33(2) . ? C73E H73A 0.9800 . ? C73E H73B 0.9800 . ? C73E H73C 0.9800 . ? C72E H72A 0.9900 . ? C72E H72B 0.9900 . ? 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 C12 W1 C17 146.7(3) . . ? C12 W1 C11 71.5(2) . . ? C17 W1 C11 141.7(3) . . ? C12 W1 C13 90.6(3) . . ? C17 W1 C13 98.1(3) . . ? C11 W1 C13 73.2(2) . . ? C12 W1 C14 143.1(2) . . ? C17 W1 C14 70.2(3) . . ? C11 W1 C14 71.6(2) . . ? C13 W1 C14 78.1(2) . . ? C12 W1 C16 75.6(3) . . ? C17 W1 C16 77.1(3) . . ? C11 W1 C16 130.3(3) . . ? C13 W1 C16 70.9(3) . . ? C14 W1 C16 130.5(3) . . ? C12 W1 C18 76.5(3) . . ? C17 W1 C18 77.0(3) . . ? C11 W1 C18 132.2(3) . . ? C13 W1 C18 142.2(3) . . ? C14 W1 C18 131.7(3) . . ? C16 W1 C18 71.4(3) . . ? C12 W1 C15 91.4(3) . . ? C17 W1 C15 98.9(3) . . ? C11 W1 C15 74.7(2) . . ? C13 W1 C15 145.3(2) . . ? C14 W1 C15 79.7(3) . . ? C16 W1 C15 142.6(3) . . ? C18 W1 C15 71.4(3) . . ? C26 W2 C22 145.3(3) . . ? C26 W2 C25 91.1(5) . . ? C22 W2 C25 89.7(3) . . ? C26 W2 C24 110.1(5) . . ? C22 W2 C24 86.8(3) . . ? C25 W2 C24 146.7(3) . . ? C26 W2 C21 140.4(4) . . ? C22 W2 C21 72.5(2) . . ? C25 W2 C21 73.9(2) . . ? C24 W2 C21 73.4(2) . . ? C26 W2 C23 71.0(3) . . ? C22 W2 C23 143.4(3) . . ? C25 W2 C23 83.4(3) . . ? C24 W2 C23 80.0(3) . . ? C21 W2 C23 71.0(2) . . ? C26 W2 C27 80.9(5) . . ? C22 W2 C27 76.5(4) . . ? C25 W2 C27 140.3(3) . . ? C24 W2 C27 70.4(3) . . ? C21 W2 C27 133.1(3) . . ? C23 W2 C27 128.7(4) . . ? C26 W2 C28 73.4(4) . . ? C22 W2 C28 74.2(4) . . ? C25 W2 C28 70.6(3) . . ? C24 W2 C28 138.9(4) . . ? C21 W2 C28 130.7(3) . . ? C23 W2 C28 135.0(4) . . ? C27 W2 C28 69.9(4) . . ? C32 W3 C38 111.8(3) . . ? C32 W3 C34 86.0(3) . . ? C38 W3 C34 146.7(3) . . ? C32 W3 C31 73.6(2) . . ? C38 W3 C31 139.7(3) . . ? C34 W3 C31 71.0(2) . . ? C32 W3 C35 144.6(3) . . ? C38 W3 C35 86.9(3) . . ? C34 W3 C35 94.1(3) . . ? C31 W3 C35 73.0(2) . . ? C32 W3 C37 70.5(3) . . ? C38 W3 C37 79.6(3) . . ? C34 W3 C37 80.6(3) . . ? C31 W3 C37 135.2(3) . . ? C35 W3 C37 144.6(3) . . ? C32 W3 C33 76.8(3) . . ? C38 W3 C33 71.6(3) . . ? C34 W3 C33 141.5(3) . . ? C31 W3 C33 71.2(2) . . ? C35 W3 C33 81.5(3) . . ? C37 W3 C33 123.5(3) . . ? C32 W3 C36 139.9(3) . . ? C38 W3 C36 74.3(4) . . ? C34 W3 C36 74.2(3) . . ? C31 W3 C36 128.4(3) . . ? C35 W3 C36 72.8(3) . . ? C37 W3 C36 72.0(3) . . ? C33 W3 C36 138.0(3) . . ? N31 Ni1 N31 180.000(1) 2_666 . ? N31 Ni1 N11 89.9(2) 2_666 . ? N31 Ni1 N11 90.1(2) . . ? N31 Ni1 N11 90.1(2) 2_666 2_666 ? N31 Ni1 N11 89.9(2) . 2_666 ? N11 Ni1 N11 180.000(1) . 2_666 ? N31 Ni1 N21 90.0(2) 2_666 2_666 ? N31 Ni1 N21 90.0(2) . 2_666 ? N11 Ni1 N21 91.5(2) . 2_666 ? N11 Ni1 N21 88.5(2) 2_666 2_666 ? N31 Ni1 N21 90.0(2) 2_666 . ? N31 Ni1 N21 90.0(2) . . ? N11 Ni1 N21 88.5(2) . . ? N11 Ni1 N21 91.5(2) 2_666 . ? N21 Ni1 N21 180.0(3) 2_666 . ? N12 Ni2 N32 90.3(2) . . ? N12 Ni2 N22 91.3(3) . . ? N32 Ni2 N22 91.9(2) . . ? N12 Ni2 N201 175.3(3) . . ? N32 Ni2 N201 88.9(3) . . ? N22 Ni2 N201 93.3(3) . . ? N12 Ni2 N212 96.1(3) . . ? N32 Ni2 N212 92.1(2) . . ? N22 Ni2 N212 171.5(3) . . ? N201 Ni2 N212 79.3(3) . . ? N12 Ni2 O215 92.2(3) . . ? N32 Ni2 O215 177.4(3) . . ? N22 Ni2 O215 89.0(2) . . ? N201 Ni2 O215 88.6(3) . . ? N212 Ni2 O215 86.7(2) . . ? N23 Ni3 N33 91.8(3) 2_666 . ? N23 Ni3 N13 91.9(2) 2_666 . ? N33 Ni3 N13 92.4(2) . . ? N23 Ni3 N301 173.3(2) 2_666 . ? N33 Ni3 N301 89.0(2) . . ? N13 Ni3 N301 94.8(2) . . ? N23 Ni3 N312 94.5(2) 2_666 . ? N33 Ni3 N312 86.4(3) . . ? N13 Ni3 N312 173.5(2) . . ? N301 Ni3 N312 78.9(2) . . ? N23 Ni3 O315 91.6(2) 2_666 . ? N33 Ni3 O315 176.0(2) . . ? N13 Ni3 O315 89.4(2) . . ? N301 Ni3 O315 87.4(2) . . ? N312 Ni3 O315 91.3(3) . . ? N34 Ni4 N14 92.1(3) . 2_666 ? N34 Ni4 N401 171.4(3) . . ? N14 Ni4 N401 93.8(3) 2_666 . ? N34 Ni4 N24 92.8(3) . . ? N14 Ni4 N24 91.3(2) 2_666 . ? N401 Ni4 N24 93.3(3) . . ? N34 Ni4 N412 90.1(3) . . ? N14 Ni4 N412 174.7(2) 2_666 . ? N401 Ni4 N412 83.5(3) . . ? N24 Ni4 N412 93.4(3) . . ? N34 Ni4 N427 90.4(3) . . ? N14 Ni4 N427 88.7(3) 2_666 . ? N401 Ni4 N427 83.5(3) . . ? N24 Ni4 N427 176.8(3) . . ? N412 Ni4 N427 86.4(3) . . ? N35 Ni5 N25 90.3(2) 2_666 . ? N35 Ni5 N501 171.4(2) 2_666 . ? N25 Ni5 N501 96.7(2) . . ? N35 Ni5 N512 93.5(2) 2_666 . ? N25 Ni5 N512 175.2(3) . . ? N501 Ni5 N512 79.2(2) . . ? N35 Ni5 N15 91.7(2) 2_666 . ? N25 Ni5 N15 91.9(2) . . ? N501 Ni5 N15 92.9(2) . . ? N512 Ni5 N15 91.0(3) . . ? N35 Ni5 O515 88.9(2) 2_666 . ? N25 Ni5 O515 89.8(2) . . ? N501 Ni5 O515 86.3(2) . . ? N512 Ni5 O515 87.3(3) . . ? N15 Ni5 O515 178.2(2) . . ? N11 C11 W1 177.1(6) . . ? C11 N11 Ni1 174.6(5) . . ? N12 C12 W1 179.0(6) . . ? C12 N12 Ni2 170.2(5) . . ? N13 C13 W1 173.5(6) . . ? C13 N13 Ni3 172.5(6) . . ? N14 C14 W1 178.2(6) . . ? C14 N14 Ni4 175.2(6) . 2_666 ? N15 C15 W1 175.0(6) . . ? C15 N15 Ni5 177.8(6) . . ? N16 C16 W1 176.7(8) . . ? N17 C17 W1 179.7(8) . . ? N18 C18 W1 177.1(7) . . ? N21 C21 W2 179.4(5) . . ? C21 N21 Ni1 175.7(5) . . ? N22 C22 W2 178.9(7) . . ? C22 N22 Ni2 178.9(7) . . ? N23 C23 W2 178.2(6) . . ? C23 N23 Ni3 175.3(6) . 2_666 ? N24 C24 W2 176.9(7) . . ? C24 N24 Ni4 173.0(6) . . ? N25 C25 W2 175.1(6) . . ? C25 N25 Ni5 176.0(6) . . ? N26 C26 W2 176.4(16) . . ? N27 C27 W2 177.1(12) . . ? N28 C28 W2 178.6(10) . . ? N31 C31 W3 178.1(6) . . ? C31 N31 Ni1 174.7(5) . . ? N32 C32 W3 176.4(7) . . ? C32 N32 Ni2 172.9(6) . . ? N33 C33 W3 176.9(6) . . ? C33 N33 Ni3 171.4(6) . . ? N34 C34 W3 175.7(7) . . ? C34 N34 Ni4 173.2(7) . . ? N35 C35 W3 175.4(6) . . ? C35 N35 Ni5 176.1(6) . 2_666 ? N36 C36 W3 179.3(10) . . ? N37 C37 W3 179.0(9) . . ? N38 C38 W3 175.8(9) . . ? C206 N201 C202 118.2(7) . . ? C206 N201 Ni2 115.6(5) . . ? C202 N201 Ni2 125.8(6) . . ? N201 C202 C203 122.7(9) . . ? N201 C202 H202 118.7 . . ? C203 C202 H202 118.7 . . ? C202 C203 C204 120.5(9) . . ? C202 C203 H203 119.7 . . ? C204 C203 H203 119.7 . . ? C203 C204 C205 116.5(9) . . ? C203 C204 C213 123.1(10) . . ? C205 C204 C213 120.3(10) . . ? C206 C205 C204 120.2(8) . . ? C206 C205 H205 119.9 . . ? C204 C205 H205 119.9 . . ? N201 C206 C205 121.8(8) . . ? N201 C206 C207 114.6(7) . . ? C205 C206 C207 123.5(7) . . ? N212 C207 C208 121.7(7) . . ? N212 C207 C206 115.2(6) . . ? C208 C207 C206 123.1(7) . . ? C209 C208 C207 119.1(8) . . ? C209 C208 H208 120.4 . . ? C207 C208 H208 120.4 . . ? C210 C209 C208 118.8(8) . . ? C210 C209 C214 122.5(9) . . ? C208 C209 C214 118.6(9) . . ? C209 C210 C211 120.0(8) . . ? C209 C210 H210 120.0 . . ? C211 C210 H210 120.0 . . ? N212 C211 C210 121.7(8) . . ? N212 C211 H211 119.1 . . ? C210 C211 H211 119.1 . . ? C211 N212 C207 118.6(7) . . ? C211 N212 Ni2 126.2(5) . . ? C207 N212 Ni2 114.9(5) . . ? C204 C213 H21A 109.5 . . ? C204 C213 H21B 109.5 . . ? H21A C213 H21B 109.5 . . ? C204 C213 H21C 109.5 . . ? H21A C213 H21C 109.5 . . ? H21B C213 H21C 109.5 . . ? C209 C214 H21D 109.5 . . ? C209 C214 H21E 109.5 . . ? H21D C214 H21E 109.5 . . ? C209 C214 H21F 109.5 . . ? H21D C214 H21F 109.5 . . ? H21E C214 H21F 109.5 . . ? C216 O215 Ni2 125.2(8) . . ? O215 C216 C217 115.5(11) . . ? O215 C216 H21G 108.4 . . ? C217 C216 H21G 108.4 . . ? O215 C216 H21H 108.4 . . ? C217 C216 H21H 108.4 . . ? H21G C216 H21H 107.5 . . ? C216 C217 H21I 109.5 . . ? C216 C217 H21J 109.5 . . ? H21I C217 H21J 109.5 . . ? C216 C217 H21K 109.5 . . ? H21I C217 H21K 109.5 . . ? H21J C217 H21K 109.5 . . ? C306 N301 C302 119.0(6) . . ? C306 N301 Ni3 115.6(5) . . ? C302 N301 Ni3 125.4(5) . . ? N301 C302 C303 121.4(7) . . ? N301 C302 H302 119.3 . . ? C303 C302 H302 119.3 . . ? C302 C303 C304 121.4(8) . . ? C302 C303 H303 119.3 . . ? C304 C303 H303 119.3 . . ? C303 C304 C305 116.2(7) . . ? C303 C304 C313 122.2(8) . . ? C305 C304 C313 121.6(8) . . ? C306 C305 C304 120.7(8) . . ? C306 C305 H305 119.7 . . ? C304 C305 H305 119.7 . . ? N301 C306 C305 121.3(7) . . ? N301 C306 C307 115.0(6) . . ? C305 C306 C307 123.6(7) . . ? N312 C307 C308 120.8(7) . . ? N312 C307 C306 115.2(7) . . ? C308 C307 C306 124.0(7) . . ? C309 C308 C307 120.2(9) . . ? C309 C308 H308 119.9 . . ? C307 C308 H308 119.9 . . ? C310 C309 C308 117.6(9) . . ? C310 C309 C314 122.1(10) . . ? C308 C309 C314 120.3(10) . . ? C309 C310 C311 120.3(9) . . ? C309 C310 H310 119.9 . . ? C311 C310 H310 119.9 . . ? N312 C311 C310 122.3(9) . . ? N312 C311 H311 118.8 . . ? C310 C311 H311 118.8 . . ? C311 N312 C307 118.7(7) . . ? C311 N312 Ni3 126.3(6) . . ? C307 N312 Ni3 114.2(5) . . ? C304 C313 H31A 109.5 . . ? C304 C313 H31B 109.5 . . ? H31A C313 H31B 109.5 . . ? C304 C313 H31C 109.5 . . ? H31A C313 H31C 109.5 . . ? H31B C313 H31C 109.5 . . ? C309 C314 H31D 109.5 . . ? C309 C314 H31E 109.5 . . ? H31D C314 H31E 109.5 . . ? C309 C314 H31F 109.5 . . ? H31D C314 H31F 109.5 . . ? H31E C314 H31F 109.5 . . ? C316 O315 C319 31.9(15) . . ? C316 O315 Ni3 117.8(18) . . ? C319 O315 Ni3 126.6(14) . . ? C316 O315 H315 100.3 . . ? C319 O315 H315 114.7 . . ? Ni3 O315 H315 113.8 . . ? O315 C316 C317 107(2) . . ? O315 C316 H31G 110.4 . . ? C317 C316 H31G 110.4 . . ? O315 C316 H31H 110.4 . . ? C317 C316 H31H 110.4 . . ? H31G C316 H31H 108.6 . . ? C316 C317 H31I 109.5 . . ? C316 C317 H31J 109.5 . . ? H31I C317 H31J 109.5 . . ? C316 C317 H31K 109.5 . . ? H31I C317 H31K 109.5 . . ? H31J C317 H31K 109.5 . . ? C319 C318 H31L 109.5 . . ? C319 C318 H31M 109.5 . . ? H31L C318 H31M 109.5 . . ? C319 C318 H31N 109.5 . . ? H31L C318 H31N 109.5 . . ? H31M C318 H31N 109.5 . . ? O315 C319 C318 115.9(18) . . ? O315 C319 H31O 108.3 . . ? C318 C319 H31O 108.3 . . ? O315 C319 H31P 108.3 . . ? C318 C319 H31P 108.3 . . ? H31O C319 H31P 107.4 . . ? C402 N401 C417 71.5(13) . . ? C402 N401 C421 67.4(11) . . ? C417 N401 C421 118.1(13) . . ? C402 N401 C406 118.3(11) . . ? C417 N401 C406 78.9(13) . . ? C421 N401 C406 82.1(11) . . ? C402 N401 Ni4 130.3(8) . . ? C417 N401 Ni4 127.8(11) . . ? C421 N401 Ni4 114.1(9) . . ? C406 N401 Ni4 110.9(9) . . ? C403 C404 C418 69.8(15) . . ? C403 C404 C420 63.6(13) . . ? C418 C404 C420 116.1(16) . . ? C403 C404 C413 122.0(15) . . ? C418 C404 C413 121.8(15) . . ? C420 C404 C413 119.3(13) . . ? C403 C404 C405 117.2(12) . . ? C418 C404 C405 82.6(16) . . ? C420 C404 C405 82.4(13) . . ? C413 C404 C405 120.5(13) . . ? C411 N412 C407 122.0(12) . . ? C411 N412 Ni4 126.0(10) . . ? C407 N412 Ni4 111.1(8) . . ? C404 C413 H41A 109.5 . . ? C404 C413 H41B 109.5 . . ? H41A C413 H41B 109.5 . . ? C404 C413 H41C 109.5 . . ? H41A C413 H41C 109.5 . . ? H41B C413 H41C 109.5 . . ? C426 N427 C422 116.9(14) . . ? C426 N427 Ni4 134.4(11) . . ? C422 N427 Ni4 106.6(9) . . ? N401 C402 C403 125.3(14) . . ? N401 C402 H402 117.3 . . ? C403 C402 H402 117.3 . . ? C404 C403 C402 120.9(15) . . ? C404 C403 H403 119.5 . . ? C402 C403 H403 119.5 . . ? C406 C405 C404 117.4(14) . . ? C406 C405 H405 121.3 . . ? C404 C405 H405 121.3 . . ? C405 C406 N401 120.7(16) . . ? C405 C406 C407 123.5(15) . . ? N401 C406 C407 115.7(14) . . ? N412 C407 C408 122.4(19) . . ? N412 C407 C406 118.3(13) . . ? C408 C407 C406 119.1(19) . . ? C407 C408 C409 119(2) . . ? C407 C408 H408 120.4 . . ? C409 C408 H408 120.4 . . ? C410 C409 C414 112(2) . . ? C410 C409 C408 114.5(17) . . ? C414 C409 C408 133(3) . . ? C411 C410 C409 118(2) . . ? C411 C410 H410 120.8 . . ? C409 C410 H410 120.8 . . ? N412 C411 C410 122.9(18) . . ? N412 C411 H411 118.5 . . ? C410 C411 H411 118.5 . . ? C409 C414 H41D 109.5 . . ? C409 C414 H41E 109.5 . . ? H41D C414 H41E 109.5 . . ? C409 C414 H41F 109.5 . . ? H41D C414 H41F 109.5 . . ? H41E C414 H41F 109.5 . . ? N401 C417 C418 125(2) . . ? N401 C417 H417 117.7 . . ? C418 C417 H417 117.7 . . ? C417 C418 C404 117(2) . . ? C417 C418 H418 121.5 . . ? C404 C418 H418 121.5 . . ? C421 C420 C404 118.2(19) . . ? C421 C420 H420 120.9 . . ? C404 C420 H420 120.9 . . ? N401 C421 C420 121.5(18) . . ? N401 C421 C422 115.6(14) . . ? C420 C421 C422 122.4(18) . . ? C423 C422 N427 116.4(17) . . ? C423 C422 C421 124.4(16) . . ? N427 C422 C421 118.9(14) . . ? C424 C423 C422 122.4(18) . . ? C424 C423 H423 118.8 . . ? C422 C423 H423 118.8 . . ? C425 C424 C423 119(3) . . ? C425 C424 C429 117(3) . . ? C423 C424 C429 125(2) . . ? C424 C425 C426 122(3) . . ? C424 C425 H425 119.0 . . ? C426 C425 H425 119.0 . . ? N427 C426 C425 123(2) . . ? N427 C426 H426 118.5 . . ? C425 C426 H426 118.5 . . ? C424 C429 H42A 109.5 . . ? C424 C429 H42B 109.5 . . ? H42A C429 H42B 109.5 . . ? C424 C429 H42C 109.5 . . ? H42A C429 H42C 109.5 . . ? H42B C429 H42C 109.5 . . ? C502 N501 C506 117.5(7) . . ? C502 N501 Ni5 127.3(5) . . ? C506 N501 Ni5 115.0(5) . . ? N501 C502 C503 123.7(8) . . ? N501 C502 H502 118.2 . . ? C503 C502 H502 118.2 . . ? C504 C503 C502 119.8(8) . . ? C504 C503 H503 120.1 . . ? C502 C503 H503 120.1 . . ? C505 C504 C503 117.0(7) . . ? C505 C504 C513 121.1(8) . . ? C503 C504 C513 121.9(9) . . ? C504 C505 C506 121.0(8) . . ? C504 C505 H505 119.5 . . ? C506 C505 H505 119.5 . . ? N501 C506 C505 121.1(8) . . ? N501 C506 C507 115.9(6) . . ? C505 C506 C507 123.0(7) . . ? N512 C507 C508 121.5(8) . . ? N512 C507 C506 114.9(7) . . ? C508 C507 C506 123.6(7) . . ? C507 C508 C509 119.6(8) . . ? C507 C508 H508 120.2 . . ? C509 C508 H508 120.2 . . ? C508 C509 C510 117.6(9) . . ? C508 C509 C514 120.5(10) . . ? C510 C509 C514 121.9(11) . . ? C511 C510 C509 119.9(10) . . ? C511 C510 H510 120.0 . . ? C509 C510 H510 120.0 . . ? N512 C511 C510 123.4(8) . . ? N512 C511 H511 118.3 . . ? C510 C511 H511 118.3 . . ? C511 N512 C507 118.0(7) . . ? C511 N512 Ni5 127.0(5) . . ? C507 N512 Ni5 114.8(5) . . ? C504 C513 H51A 109.5 . . ? C504 C513 H51B 109.5 . . ? H51A C513 H51B 109.5 . . ? C504 C513 H51C 109.5 . . ? H51A C513 H51C 109.5 . . ? H51B C513 H51C 109.5 . . ? C509 C514 H51D 109.5 . . ? C509 C514 H51E 109.5 . . ? H51D C514 H51E 109.5 . . ? C509 C514 H51F 109.5 . . ? H51D C514 H51F 109.5 . . ? H51E C514 H51F 109.5 . . ? C62E O61E H61E 104.0 . . ? C63E C62E O61E 118.1(13) . . ? C63E C62E H62A 107.8 . . ? O61E C62E H62A 107.8 . . ? C63E C62E H62B 107.8 . . ? O61E C62E H62B 107.8 . . ? H62A C62E H62B 107.1 . . ? C62E C63E H63A 109.5 . . ? C62E C63E H63B 109.5 . . ? H63A C63E H63B 109.5 . . ? C62E C63E H63C 109.5 . . ? H63A C63E H63C 109.5 . . ? H63B C63E H63C 109.5 . . ? C72E C73E H73A 109.5 . . ? C72E C73E H73B 109.5 . . ? H73A C73E H73B 109.5 . . ? C72E C73E H73C 109.5 . . ? H73A C73E H73C 109.5 . . ? H73B C73E H73C 109.5 . . ? C73E C72E O71E 109.4(19) . . ? C73E C72E H72A 109.8 . . ? O71E C72E H72A 109.8 . . ? C73E C72E H72B 109.8 . . ? O71E C72E H72B 109.8 . . ? H72A C72E H72B 108.3 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O315 H315 O61E 0.85 1.85 2.699(8) 179.7 . O61E H61E N16 0.85 1.97 2.820(9) 179.8 2_766 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.657 _refine_diff_density_min -1.468 _refine_diff_density_rms 0.200 #===END data_3a _database_code_depnum_ccdc_archive 'CCDC 876831' #TrackingRef '- clusters1-4_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; {Ni[Ni(5,5'dmbpy)(H2O)]8[W(CN)8]6}*8H2O ; _chemical_name_common (Ni(Ni(5,5'dmbpy)(H2O))8(W(CN)8)6)*8H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C148 H96 N64 Ni9 O18 W6' _chemical_formula_weight 4690.15 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' _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 19.120(5) _cell_length_b 19.474(5) _cell_length_c 19.769(5) _cell_angle_alpha 100.320(5) _cell_angle_beta 105.230(5) _cell_angle_gamma 118.465(5) _cell_volume 5828(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 3.712 _exptl_absorpt_correction_T_min 0.3566 _exptl_absorpt_correction_T_max 0.6059 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details '(DENZO-SMN; Otwinowski & Minor, 1997)' _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 KappaCCD _diffrn_measurement_method '\f and \o scans to fill Ewald sphere' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 43198 _diffrn_reflns_av_R_equivalents 0.0855 _diffrn_reflns_av_sigmaI/netI 0.1154 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.55 _reflns_number_total 26210 _reflns_number_gt 16093 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (ALTOMARE et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+45.1327P] 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 SHELXL _refine_ls_extinction_coef 0.00039(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 26210 _refine_ls_number_parameters 1081 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1326 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1770 _refine_ls_wR_factor_gt 0.1445 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.34946(2) 0.19692(2) 0.51818(2) 0.02814(11) Uani 1 1 d . . . W2 W 0.48353(3) 0.36982(3) 0.23064(2) 0.03453(12) Uani 1 1 d . . . W3 W 0.81172(2) 0.55382(3) 0.63247(2) 0.03038(11) Uani 1 1 d . . . Ni1 Ni 0.5000 0.5000 0.5000 0.0222(3) Uani 1 2 d S . . Ni2 Ni 0.18091(9) 0.17423(8) 0.24426(8) 0.0371(3) Uani 1 1 d . . . Ni3 Ni 0.79847(9) 0.64839(9) 0.39597(9) 0.0368(3) Uani 1 1 d . . . Ni4 Ni 0.61399(9) 0.41522(9) 0.77895(8) 0.0382(3) Uani 1 1 d . . . Ni5 Ni 0.59957(9) 0.24631(8) 0.42091(8) 0.0351(3) Uani 1 1 d . . . C11 C 0.4183(6) 0.3222(6) 0.5173(6) 0.029(2) Uani 1 1 d . . . N11 N 0.4530(5) 0.3880(5) 0.5158(5) 0.035(2) Uani 1 1 d . . . C12 C 0.2874(7) 0.1967(6) 0.4104(7) 0.035(2) Uani 1 1 d . . . N12 N 0.2525(6) 0.1959(6) 0.3520(5) 0.042(2) Uani 1 1 d . . . C13 C 0.2800(6) 0.2501(6) 0.5439(6) 0.034(2) Uani 1 1 d . . . N13 N 0.2467(6) 0.2834(6) 0.5620(6) 0.044(2) Uani 1 1 d . . . C14 C 0.4524(7) 0.2798(7) 0.6274(6) 0.036(2) Uani 1 1 d . . . N14 N 0.5092(7) 0.3259(6) 0.6844(6) 0.046(2) Uani 1 1 d . . . C15 C 0.4409(7) 0.2046(6) 0.4699(6) 0.033(2) Uani 1 1 d . . . N15 N 0.4938(6) 0.2123(6) 0.4484(5) 0.037(2) Uani 1 1 d . . . C16 C 0.2861(8) 0.1393(7) 0.5875(8) 0.048(3) Uani 1 1 d . . . N16 N 0.2537(9) 0.1106(8) 0.6244(9) 0.080(4) Uani 1 1 d . . . C17 C 0.3974(8) 0.1222(7) 0.5536(8) 0.045(3) Uani 1 1 d . . . N17 N 0.4232(9) 0.0832(8) 0.5707(8) 0.071(4) Uani 1 1 d . . . C18 C 0.2530(8) 0.0709(7) 0.4428(7) 0.049(3) Uani 1 1 d . . . N18 N 0.2001(9) 0.0040(7) 0.3986(7) 0.077(4) Uani 1 1 d . . . C21 C 0.4812(6) 0.4166(6) 0.3354(6) 0.031(2) Uani 1 1 d . . . N21 N 0.4847(5) 0.4447(5) 0.3949(5) 0.0322(18) Uani 1 1 d . . . C22 C 0.3578(7) 0.2857(8) 0.2271(7) 0.043(3) Uani 1 1 d . . . N22 N 0.2905(6) 0.2418(6) 0.2259(6) 0.047(2) Uani 1 1 d . . . C23 C 0.6084(8) 0.4828(8) 0.3008(7) 0.043(3) Uani 1 1 d . . . N23 N 0.6763(7) 0.5437(7) 0.3376(6) 0.048(2) Uani 1 1 d . . . C24 C 0.4509(8) 0.4602(8) 0.2228(7) 0.044(3) Uani 1 1 d . . . N24 N 0.4311(7) 0.5074(7) 0.2210(6) 0.051(2) Uani 1 1 d . . . C25 C 0.5332(8) 0.3205(7) 0.3048(7) 0.043(3) Uani 1 1 d . . . N25 N 0.5578(7) 0.2936(6) 0.3464(6) 0.044(2) Uani 1 1 d . . . C26 C 0.451(2) 0.2477(16) 0.1694(11) 0.121(9) Uani 1 1 d . . . N26 N 0.431(2) 0.1799(18) 0.1315(14) 0.190(13) Uani 1 1 d . . . C27 C 0.3989(11) 0.3284(11) 0.1166(9) 0.073(4) Uani 1 1 d . . . N27 N 0.3531(14) 0.3059(15) 0.0546(10) 0.134(8) Uani 1 1 d . . . C28 C 0.5664(16) 0.395(3) 0.1760(14) 0.27(3) Uani 1 1 d . . . N28 N 0.6169(16) 0.414(3) 0.1484(15) 0.39(4) Uani 1 1 d . . . C31 C 0.6902(6) 0.5378(6) 0.5753(6) 0.033(2) Uani 1 1 d . . . N31 N 0.6235(5) 0.5271(5) 0.5462(5) 0.0348(19) Uani 1 1 d . . . C32 C 0.8191(7) 0.6622(7) 0.6943(6) 0.037(2) Uani 1 1 d . . . N32 N 0.8218(6) 0.7206(6) 0.7219(6) 0.046(2) Uani 1 1 d . . . C33 C 0.8134(6) 0.5900(6) 0.5356(7) 0.035(2) Uani 1 1 d . . . N33 N 0.8134(6) 0.6117(6) 0.4856(5) 0.040(2) Uani 1 1 d . . . C34 C 0.7296(7) 0.4976(7) 0.6877(6) 0.040(2) Uani 1 1 d . . . N34 N 0.6851(6) 0.4681(6) 0.7196(5) 0.044(2) Uani 1 1 d . . . C35 C 0.7238(7) 0.4265(8) 0.5557(7) 0.039(2) Uani 1 1 d . . . N35 N 0.6757(6) 0.3609(6) 0.5096(6) 0.045(2) Uani 1 1 d . . . C36 C 0.8865(8) 0.5101(8) 0.5968(8) 0.051(3) Uani 1 1 d . . . N36 N 0.9276(8) 0.4898(8) 0.5783(8) 0.072(4) Uani 1 1 d . . . C37 C 0.8882(9) 0.5556(11) 0.7355(9) 0.064(4) Uani 1 1 d . . . N37 N 0.9288(10) 0.5552(12) 0.7891(8) 0.097(5) Uani 1 1 d . . . C38 C 0.9411(8) 0.6629(8) 0.6683(8) 0.050(3) Uani 1 1 d . . . N38 N 1.0087(8) 0.7201(8) 0.6850(9) 0.079(4) Uani 1 1 d . . . N201 N 0.0947(6) 0.1372(6) 0.1357(6) 0.045(2) Uani 1 1 d . . . C202 C 0.0119(8) 0.0841(8) 0.1220(8) 0.056(3) Uani 1 1 d . . . C203 C -0.0536(10) 0.0529(11) 0.0506(10) 0.074(4) Uani 1 1 d . . . H203 H -0.1120 0.0180 0.0413 0.089 Uiso 1 1 calc R . . C204 C -0.0295(13) 0.0750(13) -0.0028(10) 0.091(6) Uani 1 1 d . . . H204 H -0.0723 0.0520 -0.0510 0.110 Uiso 1 1 calc R . . C205 C 0.0555(12) 0.1300(11) 0.0085(8) 0.076(5) Uani 1 1 d . . . C206 C 0.1163(10) 0.1601(9) 0.0829(8) 0.063(4) Uani 1 1 d . . . H206 H 0.1747 0.1981 0.0945 0.075 Uiso 1 1 calc R . . C207 C 0.0887(14) 0.1603(15) -0.0484(10) 0.101(7) Uani 1 1 d . . . H20A H 0.0408 0.1352 -0.0960 0.152 Uiso 1 1 calc R . . H20B H 0.1284 0.1448 -0.0533 0.152 Uiso 1 1 calc R . . H20C H 0.1181 0.2200 -0.0320 0.152 Uiso 1 1 calc R . . N208 N 0.0647(6) 0.0963(6) 0.2487(6) 0.046(2) Uani 1 1 d . . . C209 C -0.0054(8) 0.0606(8) 0.1862(9) 0.062(4) Uani 1 1 d . . . C210 C -0.0882(9) 0.0027(10) 0.1832(12) 0.083(6) Uani 1 1 d . . . H210 H -0.1375 -0.0221 0.1391 0.100 Uiso 1 1 calc R . . C211 C -0.0956(10) -0.0166(10) 0.2452(13) 0.083(6) Uani 1 1 d . . . H211 H -0.1500 -0.0560 0.2421 0.100 Uiso 1 1 calc R . . C212 C -0.0274(10) 0.0195(9) 0.3091(11) 0.067(4) Uani 1 1 d . . . C213 C 0.0533(9) 0.0775(8) 0.3087(10) 0.064(4) Uani 1 1 d . . . H213 H 0.1023 0.1047 0.3535 0.076 Uiso 1 1 calc R . . C214 C -0.0301(13) 0.0031(13) 0.3810(12) 0.091(6) Uani 1 1 d . . . H21A H 0.0278 0.0358 0.4196 0.137 Uiso 1 1 calc R . . H21B H -0.0539 -0.0552 0.3722 0.137 Uiso 1 1 calc R . . H21C H -0.0658 0.0184 0.3967 0.137 Uiso 1 1 calc R . . O215 O 0.1796(6) 0.0639(5) 0.2051(5) 0.057(2) Uani 1 1 d . . . N301 N 0.9250(6) 0.7531(6) 0.4425(7) 0.048(3) Uani 1 1 d . . . C302 C 0.9481(9) 0.7880(8) 0.3921(10) 0.056(4) Uani 1 1 d . . . C303 C 1.0323(11) 0.8560(10) 0.4136(12) 0.077(5) Uani 1 1 d . . . H303 H 1.0488 0.8799 0.3791 0.092 Uiso 1 1 calc R . . C304 C 1.0904(12) 0.8872(11) 0.4860(14) 0.085(6) Uani 1 1 d . . . H304 H 1.1463 0.9338 0.5012 0.102 Uiso 1 1 calc R . . C305 C 1.0668(8) 0.8496(8) 0.5389(11) 0.071(5) Uani 1 1 d . . . C306 C 0.9819(8) 0.7819(8) 0.5099(9) 0.056(3) Uani 1 1 d . . . H306 H 0.9641 0.7545 0.5419 0.067 Uiso 1 1 calc R . . C307 C 1.1323(11) 0.8856(12) 0.6180(13) 0.105(7) Uani 1 1 d . . . H30A H 1.1863 0.9324 0.6234 0.157 Uiso 1 1 calc R . . H30B H 1.1409 0.8436 0.6295 0.157 Uiso 1 1 calc R . . H30C H 1.1115 0.9038 0.6519 0.157 Uiso 1 1 calc R . . N308 N 0.7992(7) 0.6882(7) 0.3056(7) 0.053(3) Uani 1 1 d . . . C309 C 0.8803(11) 0.7529(9) 0.3177(10) 0.065(4) Uani 1 1 d . . . C310 C 0.8924(15) 0.7791(14) 0.2564(14) 0.102(7) Uani 1 1 d . . . H310 H 0.9460 0.8235 0.2626 0.122 Uiso 1 1 calc R . . C311 C 0.820(2) 0.7350(18) 0.1853(16) 0.120(9) Uani 1 1 d . . . H311 H 0.8286 0.7487 0.1442 0.144 Uiso 1 1 calc R . . C312 C 0.7410(16) 0.6752(14) 0.1758(11) 0.090(6) Uani 1 1 d . . . C313 C 0.7343(12) 0.6510(11) 0.2381(9) 0.071(4) Uani 1 1 d . . . H313 H 0.6808 0.6060 0.2316 0.085 Uiso 1 1 calc R . . C314 C 0.6663(17) 0.6239(18) 0.0976(12) 0.133(10) Uani 1 1 d . . . H31A H 0.6153 0.5822 0.1015 0.200 Uiso 1 1 calc R . . H31B H 0.6824 0.5971 0.0650 0.200 Uiso 1 1 calc R . . H31C H 0.6543 0.6603 0.0775 0.200 Uiso 1 1 calc R . . O315 O 0.8449(7) 0.5797(7) 0.3509(6) 0.069(3) Uani 1 1 d . . . N401 N 0.5578(7) 0.3659(7) 0.8482(6) 0.051(3) Uani 1 1 d . . . C402 C 0.6116(12) 0.4091(11) 0.9237(10) 0.072(4) Uani 1 1 d . . . C403 C 0.5792(17) 0.3811(15) 0.9752(11) 0.103(7) Uani 1 1 d . . . H403 H 0.6138 0.4094 1.0264 0.123 Uiso 1 1 calc R . . C404 C 0.4940(17) 0.3099(16) 0.9506(14) 0.110(8) Uani 1 1 d . . . H404 H 0.4733 0.2919 0.9858 0.131 Uiso 1 1 calc R . . C405 C 0.4425(14) 0.2678(13) 0.8772(13) 0.088(6) Uani 1 1 d . . . C406 C 0.4774(10) 0.2994(10) 0.8269(10) 0.073(5) Uani 1 1 d . . . H406 H 0.4424 0.2722 0.7757 0.087 Uiso 1 1 calc R . . C407 C 0.3497(15) 0.1895(14) 0.8475(14) 0.127(9) Uani 1 1 d . . . H40A H 0.3253 0.1684 0.7935 0.190 Uiso 1 1 calc R . . H40B H 0.3145 0.2038 0.8651 0.190 Uiso 1 1 calc R . . H40C H 0.3516 0.1474 0.8652 0.190 Uiso 1 1 calc R . . N408 N 0.7160(7) 0.4956(7) 0.8822(6) 0.052(3) Uani 1 1 d . . . C409 C 0.6956(11) 0.4781(12) 0.9403(8) 0.073(5) Uani 1 1 d . . . C410 C 0.7597(14) 0.5289(14) 1.0130(9) 0.099(7) Uani 1 1 d . . . H410 H 0.7458 0.5196 1.0536 0.119 Uiso 1 1 calc R . . C411 C 0.835(2) 0.5862(17) 1.0253(13) 0.130(10) Uani 1 1 d . . . H411 H 0.8754 0.6154 1.0748 0.155 Uiso 1 1 calc R . . C412 C 0.8621(11) 0.6101(12) 0.9651(11) 0.089(6) Uani 1 1 d . . . C413 C 0.7962(10) 0.5597(10) 0.8946(8) 0.069(4) Uani 1 1 d . . . H413 H 0.8074 0.5703 0.8533 0.083 Uiso 1 1 calc R . . C414 C 0.9509(13) 0.6779(13) 0.9723(15) 0.126(9) Uani 1 1 d . . . H41A H 0.9899 0.7069 1.0244 0.189 Uiso 1 1 calc R . . H41B H 0.9455 0.7168 0.9513 0.189 Uiso 1 1 calc R . . H41C H 0.9732 0.6528 0.9458 0.189 Uiso 1 1 calc R . . O415 O 0.6597(7) 0.3348(7) 0.7796(7) 0.073(3) Uani 1 1 d D . . C416 C 0.663(2) 0.292(2) 0.7140(17) 0.22(2) Uani 1 1 d D . . C417 C 0.744(2) 0.312(2) 0.710(3) 0.205(18) Uani 1 1 d . . . N501 N 0.6509(6) 0.1962(5) 0.4878(6) 0.039(2) Uani 1 1 d . . . C502 C 0.7275(8) 0.2124(8) 0.4888(8) 0.050(3) Uani 1 1 d . . . C503 C 0.7691(10) 0.1823(11) 0.5290(9) 0.069(4) Uani 1 1 d . . . H503 H 0.8238 0.1961 0.5317 0.082 Uiso 1 1 calc R . . C504 C 0.7293(12) 0.1319(12) 0.5651(12) 0.091(6) Uani 1 1 d . . . H504 H 0.7564 0.1096 0.5907 0.109 Uiso 1 1 calc R . . C505 C 0.6500(9) 0.1136(8) 0.5639(8) 0.054(3) Uani 1 1 d . . . C506 C 0.6152(9) 0.1488(7) 0.5244(7) 0.048(3) Uani 1 1 d . . . H506 H 0.5621 0.1385 0.5232 0.057 Uiso 1 1 calc R . . C507 C 0.6056(11) 0.0576(10) 0.6022(10) 0.072(4) Uani 1 1 d . . . H50A H 0.6416 0.0403 0.6265 0.109 Uiso 1 1 calc R . . H50B H 0.5509 0.0092 0.5658 0.109 Uiso 1 1 calc R . . H50C H 0.5958 0.0873 0.6390 0.109 Uiso 1 1 calc R . . N508 N 0.7087(6) 0.2764(6) 0.3978(6) 0.048(2) Uani 1 1 d . . . C509 C 0.7600(8) 0.2587(9) 0.4412(9) 0.059(4) Uani 1 1 d . . . C510 C 0.8415(9) 0.2854(9) 0.4383(11) 0.071(5) Uani 1 1 d . . . H510 H 0.8804 0.2779 0.4704 0.085 Uiso 1 1 calc R . . C511 C 0.8636(11) 0.3234(11) 0.3865(12) 0.087(6) Uani 1 1 d . . . H511 H 0.9162 0.3391 0.3828 0.104 Uiso 1 1 calc R . . C512 C 0.8104(10) 0.3366(10) 0.3438(10) 0.067(4) Uani 1 1 d . . . C513 C 0.7329(10) 0.3136(10) 0.3502(9) 0.064(4) Uani 1 1 d . . . H513 H 0.6960 0.3245 0.3200 0.076 Uiso 1 1 calc R . . C514 C 0.8309(13) 0.3749(13) 0.2866(13) 0.100(7) Uani 1 1 d . . . H51A H 0.7843 0.3796 0.2604 0.150 Uiso 1 1 calc R . . H51B H 0.8377 0.3402 0.2514 0.150 Uiso 1 1 calc R . . H51C H 0.8838 0.4295 0.3113 0.150 Uiso 1 1 calc R . . O515 O 0.5244(6) 0.1269(5) 0.3321(5) 0.056(2) Uani 1 1 d . . . O1 O 0.0918(9) -0.0761(9) 0.2423(8) 0.104(4) Uiso 1 1 d . . . O2 O 0.7992(15) 0.5189(15) 0.2007(13) 0.177(8) Uiso 1 1 d . . . O3 O 0.9504(8) 0.5517(8) 0.4451(7) 0.091(4) Uiso 1 1 d . . . O4 O 0.530(3) 0.119(3) 0.188(2) 0.313(18) Uiso 1 1 d . . . O5 O 0.5786(11) 0.0207(10) 0.3440(9) 0.122(5) 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 W1 0.0273(2) 0.02393(19) 0.0384(2) 0.01679(17) 0.01738(17) 0.01377(16) W2 0.0379(2) 0.0416(2) 0.0289(2) 0.01219(18) 0.01658(18) 0.0238(2) W3 0.02287(19) 0.0339(2) 0.0377(2) 0.01556(18) 0.01239(17) 0.01691(17) Ni1 0.0211(7) 0.0217(7) 0.0273(9) 0.0116(7) 0.0122(7) 0.0121(6) Ni2 0.0321(7) 0.0307(7) 0.0357(8) 0.0086(6) 0.0080(6) 0.0124(6) Ni3 0.0358(7) 0.0403(7) 0.0510(9) 0.0264(7) 0.0287(7) 0.0236(6) Ni4 0.0416(8) 0.0450(8) 0.0343(8) 0.0215(6) 0.0162(6) 0.0254(7) Ni5 0.0353(7) 0.0339(7) 0.0485(8) 0.0180(6) 0.0231(6) 0.0236(6) C11 0.032(5) 0.032(5) 0.032(5) 0.020(4) 0.018(4) 0.019(4) N11 0.027(4) 0.036(5) 0.049(6) 0.027(4) 0.022(4) 0.015(4) C12 0.031(5) 0.024(5) 0.048(7) 0.012(5) 0.015(5) 0.014(4) N12 0.041(5) 0.042(5) 0.035(5) 0.009(4) 0.012(4) 0.021(4) C13 0.024(5) 0.033(5) 0.045(6) 0.017(5) 0.019(5) 0.011(4) N13 0.038(5) 0.052(6) 0.058(6) 0.028(5) 0.028(5) 0.029(5) C14 0.037(6) 0.042(6) 0.035(6) 0.024(5) 0.017(5) 0.022(5) N14 0.049(6) 0.045(5) 0.039(6) 0.022(5) 0.020(5) 0.020(5) C15 0.036(5) 0.031(5) 0.036(6) 0.015(4) 0.015(5) 0.020(4) N15 0.041(5) 0.039(5) 0.042(5) 0.017(4) 0.022(4) 0.026(4) C16 0.061(8) 0.032(6) 0.063(8) 0.021(6) 0.034(7) 0.028(6) N16 0.099(10) 0.072(8) 0.118(12) 0.068(9) 0.085(10) 0.048(8) C17 0.044(6) 0.042(6) 0.064(8) 0.034(6) 0.033(6) 0.024(5) N17 0.084(9) 0.071(8) 0.105(11) 0.058(8) 0.046(8) 0.061(7) C18 0.059(8) 0.036(6) 0.048(7) 0.025(6) 0.015(6) 0.023(6) N18 0.078(9) 0.032(6) 0.055(8) 0.007(5) 0.006(7) -0.003(6) C21 0.032(5) 0.040(5) 0.031(5) 0.014(4) 0.016(4) 0.025(5) N21 0.028(4) 0.031(4) 0.036(5) 0.012(4) 0.012(4) 0.016(4) C22 0.038(6) 0.051(7) 0.041(7) 0.023(5) 0.015(5) 0.022(5) N22 0.044(6) 0.047(6) 0.048(6) 0.020(5) 0.020(5) 0.022(5) C23 0.058(8) 0.056(7) 0.038(6) 0.026(6) 0.033(6) 0.037(7) N23 0.048(6) 0.045(6) 0.063(7) 0.030(5) 0.029(5) 0.026(5) C24 0.057(7) 0.054(7) 0.034(6) 0.025(5) 0.022(6) 0.035(6) N24 0.064(7) 0.051(6) 0.047(6) 0.023(5) 0.024(5) 0.037(6) C25 0.052(7) 0.041(6) 0.047(7) 0.018(5) 0.032(6) 0.027(6) N25 0.061(6) 0.048(6) 0.053(6) 0.026(5) 0.034(5) 0.043(5) C26 0.23(3) 0.128(19) 0.054(11) 0.043(12) 0.068(15) 0.13(2) N26 0.33(4) 0.17(2) 0.113(18) 0.027(17) 0.07(2) 0.18(3) C27 0.081(11) 0.086(11) 0.045(9) 0.022(8) 0.026(8) 0.042(9) N27 0.135(17) 0.163(19) 0.051(10) 0.021(11) 0.006(10) 0.068(15) C28 0.096(17) 0.33(5) 0.093(18) -0.10(2) 0.074(15) -0.03(2) N28 0.122(19) 0.43(5) 0.13(2) -0.15(3) 0.098(17) -0.12(3) C31 0.032(5) 0.040(6) 0.038(6) 0.023(5) 0.020(5) 0.022(5) N31 0.027(4) 0.036(5) 0.041(5) 0.017(4) 0.013(4) 0.016(4) C32 0.031(5) 0.043(6) 0.041(6) 0.018(5) 0.015(5) 0.021(5) N32 0.045(6) 0.032(5) 0.052(6) 0.015(4) 0.015(5) 0.019(4) C33 0.025(5) 0.035(5) 0.051(7) 0.020(5) 0.020(5) 0.017(4) N33 0.033(5) 0.044(5) 0.040(5) 0.019(4) 0.011(4) 0.018(4) C34 0.041(6) 0.050(6) 0.038(6) 0.022(5) 0.016(5) 0.030(5) N34 0.042(5) 0.051(6) 0.032(5) 0.019(4) 0.011(4) 0.022(5) C35 0.037(6) 0.049(7) 0.051(7) 0.025(6) 0.028(5) 0.030(6) N35 0.048(6) 0.035(5) 0.062(7) 0.020(5) 0.032(5) 0.023(5) C36 0.040(6) 0.064(8) 0.069(9) 0.028(7) 0.032(6) 0.037(6) N36 0.062(7) 0.073(8) 0.100(11) 0.027(7) 0.040(7) 0.048(7) C37 0.049(8) 0.100(12) 0.064(9) 0.046(9) 0.027(7) 0.049(8) N37 0.078(9) 0.167(16) 0.066(9) 0.066(10) 0.020(8) 0.078(11) C38 0.035(6) 0.055(7) 0.055(8) 0.015(6) 0.019(6) 0.022(6) N38 0.046(7) 0.059(7) 0.108(11) 0.023(8) 0.034(7) 0.013(6) N201 0.044(5) 0.034(5) 0.041(6) 0.009(4) 0.009(5) 0.016(4) C202 0.046(7) 0.043(7) 0.048(8) -0.005(6) 0.001(6) 0.019(6) C203 0.045(8) 0.082(11) 0.061(10) 0.013(9) 0.002(7) 0.025(8) C204 0.091(14) 0.093(13) 0.050(10) -0.005(9) -0.017(9) 0.056(12) C205 0.091(13) 0.072(10) 0.039(8) 0.012(7) 0.000(8) 0.044(10) C206 0.071(9) 0.056(8) 0.054(9) 0.015(7) 0.014(7) 0.037(7) C207 0.119(16) 0.136(18) 0.053(11) 0.029(11) 0.025(11) 0.079(15) N208 0.039(5) 0.041(5) 0.056(7) 0.018(5) 0.018(5) 0.020(5) C209 0.040(7) 0.046(7) 0.085(11) 0.006(7) 0.021(7) 0.021(6) C210 0.033(7) 0.054(9) 0.112(15) -0.002(9) 0.023(8) 0.003(7) C211 0.047(9) 0.053(9) 0.127(17) 0.025(10) 0.045(11) 0.009(7) C212 0.059(9) 0.044(7) 0.113(14) 0.028(8) 0.049(10) 0.031(7) C213 0.053(8) 0.050(7) 0.107(13) 0.047(8) 0.043(8) 0.031(7) C214 0.124(15) 0.116(15) 0.132(17) 0.090(14) 0.099(14) 0.095(13) O215 0.065(6) 0.044(5) 0.064(6) 0.013(4) 0.028(5) 0.032(5) N301 0.036(5) 0.038(5) 0.082(8) 0.031(5) 0.031(6) 0.022(4) C302 0.051(7) 0.051(7) 0.103(12) 0.047(8) 0.057(8) 0.034(6) C303 0.071(10) 0.060(9) 0.130(16) 0.063(11) 0.069(12) 0.034(8) C304 0.070(11) 0.075(11) 0.15(2) 0.056(13) 0.073(13) 0.052(10) C305 0.035(7) 0.037(7) 0.140(16) 0.035(8) 0.038(9) 0.017(6) C306 0.047(7) 0.050(7) 0.091(11) 0.038(8) 0.041(8) 0.030(6) C307 0.053(10) 0.069(11) 0.141(19) 0.018(12) 0.012(11) 0.019(9) N308 0.058(7) 0.068(7) 0.064(7) 0.041(6) 0.041(6) 0.043(6) C309 0.089(11) 0.063(9) 0.087(12) 0.047(8) 0.064(10) 0.053(9) C310 0.112(16) 0.128(17) 0.14(2) 0.102(17) 0.103(17) 0.074(15) C311 0.19(3) 0.17(2) 0.14(2) 0.13(2) 0.13(2) 0.14(2) C312 0.135(18) 0.109(15) 0.082(13) 0.058(12) 0.064(13) 0.087(15) C313 0.090(12) 0.092(12) 0.073(11) 0.055(10) 0.046(10) 0.065(10) C314 0.16(2) 0.20(3) 0.072(14) 0.057(16) 0.026(15) 0.12(2) O315 0.095(8) 0.084(7) 0.074(7) 0.033(6) 0.050(6) 0.072(7) N401 0.068(7) 0.066(7) 0.036(6) 0.026(5) 0.023(5) 0.046(6) C402 0.097(13) 0.071(10) 0.068(11) 0.035(9) 0.044(10) 0.051(10) C403 0.16(2) 0.129(18) 0.057(11) 0.053(12) 0.070(13) 0.089(17) C404 0.14(2) 0.136(19) 0.108(18) 0.086(16) 0.093(17) 0.078(17) C405 0.127(16) 0.098(13) 0.099(15) 0.066(12) 0.083(14) 0.073(13) C406 0.063(9) 0.069(9) 0.091(12) 0.058(9) 0.037(9) 0.028(8) C407 0.132(19) 0.113(17) 0.14(2) 0.077(16) 0.102(18) 0.039(15) N408 0.051(6) 0.058(6) 0.044(6) 0.019(5) 0.016(5) 0.030(5) C409 0.081(11) 0.109(14) 0.035(8) 0.018(8) 0.014(7) 0.065(11) C410 0.092(14) 0.102(15) 0.037(9) -0.016(9) 0.001(9) 0.035(12) C411 0.14(2) 0.113(19) 0.061(14) -0.011(13) -0.016(14) 0.063(18) C412 0.062(10) 0.085(12) 0.070(12) -0.013(10) -0.004(9) 0.034(10) C413 0.062(9) 0.080(11) 0.045(8) 0.010(7) 0.013(7) 0.035(8) C414 0.080(14) 0.084(14) 0.16(2) -0.015(14) 0.035(14) 0.033(12) O415 0.092(8) 0.087(8) 0.091(8) 0.046(7) 0.056(7) 0.071(7) C416 0.20(3) 0.15(3) 0.43(6) 0.13(3) 0.19(4) 0.15(3) C417 0.18(3) 0.12(2) 0.36(6) 0.07(3) 0.14(4) 0.10(2) N501 0.041(5) 0.031(4) 0.051(6) 0.013(4) 0.018(4) 0.025(4) C502 0.045(7) 0.044(7) 0.059(8) 0.015(6) 0.017(6) 0.028(6) C503 0.057(8) 0.091(11) 0.088(12) 0.040(9) 0.029(8) 0.059(9) C504 0.102(13) 0.097(13) 0.144(18) 0.078(13) 0.069(13) 0.083(12) C505 0.061(8) 0.056(8) 0.057(8) 0.025(7) 0.024(7) 0.038(7) C506 0.059(7) 0.037(6) 0.054(8) 0.016(6) 0.020(6) 0.032(6) C507 0.094(12) 0.066(9) 0.081(11) 0.052(9) 0.041(10) 0.049(9) N508 0.041(5) 0.048(6) 0.065(7) 0.022(5) 0.033(5) 0.026(5) C509 0.040(7) 0.058(8) 0.084(10) 0.019(7) 0.023(7) 0.034(6) C510 0.043(7) 0.060(8) 0.134(15) 0.038(9) 0.050(9) 0.038(7) C511 0.068(10) 0.083(11) 0.147(18) 0.057(12) 0.076(12) 0.047(9) C512 0.070(9) 0.084(11) 0.083(11) 0.038(9) 0.056(9) 0.051(9) C513 0.067(9) 0.087(10) 0.068(10) 0.036(8) 0.047(8) 0.051(8) C514 0.097(14) 0.094(13) 0.138(19) 0.055(13) 0.087(14) 0.047(11) O515 0.056(5) 0.044(5) 0.071(6) 0.019(4) 0.026(5) 0.031(4) _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 W1 C18 2.139(12) . ? W1 C13 2.140(10) . ? W1 C12 2.147(12) . ? W1 C14 2.152(12) . ? W1 C11 2.156(9) . ? W1 C15 2.160(10) . ? W1 C16 2.175(12) . ? W1 C17 2.179(12) . ? W2 C28 2.065(19) . ? W2 C21 2.129(10) . ? W2 C27 2.131(16) . ? W2 C22 2.141(11) . ? W2 C24 2.145(12) . ? W2 C25 2.148(13) . ? W2 C23 2.151(14) . ? W2 C26 2.16(2) . ? W3 C34 2.132(12) . ? W3 C31 2.139(10) . ? W3 C35 2.148(13) . ? W3 C37 2.156(14) . ? W3 C33 2.158(11) . ? W3 C38 2.160(12) . ? W3 C32 2.161(12) . ? W3 C36 2.178(11) . ? Ni1 N21 2.034(9) . ? Ni1 N21 2.034(9) 2_666 ? Ni1 N11 2.047(8) 2_666 ? Ni1 N11 2.047(8) . ? Ni1 N31 2.048(8) 2_666 ? Ni1 N31 2.048(8) . ? Ni2 N12 2.045(10) . ? Ni2 N208 2.046(10) . ? Ni2 N22 2.048(10) . ? Ni2 N32 2.067(10) 2_666 ? Ni2 N201 2.074(10) . ? Ni2 O215 2.134(8) . ? Ni3 N33 2.029(10) . ? Ni3 N23 2.036(11) . ? Ni3 N13 2.068(10) 2_666 ? Ni3 N308 2.072(11) . ? Ni3 N301 2.077(10) . ? Ni3 O315 2.119(8) . ? Ni4 N14 2.020(11) . ? Ni4 N401 2.052(11) . ? Ni4 N34 2.054(10) . ? Ni4 N24 2.063(11) 2_666 ? Ni4 N408 2.067(11) . ? Ni4 O415 2.126(10) . ? Ni5 N25 2.055(10) . ? Ni5 N15 2.063(9) . ? Ni5 N35 2.082(11) . ? Ni5 N508 2.082(9) . ? Ni5 N501 2.088(9) . ? Ni5 O515 2.140(9) . ? C11 N11 1.138(12) . ? C12 N12 1.165(14) . ? C13 N13 1.175(13) . ? N13 Ni3 2.068(10) 2_666 ? C14 N14 1.149(14) . ? C15 N15 1.154(13) . ? C16 N16 1.133(16) . ? C17 N17 1.137(15) . ? C18 N18 1.164(16) . ? C21 N21 1.176(13) . ? C22 N22 1.147(14) . ? C23 N23 1.160(16) . ? C24 N24 1.152(15) . ? N24 Ni4 2.063(11) 2_666 ? C25 N25 1.167(15) . ? C26 N26 1.21(3) . ? C27 N27 1.16(2) . ? C28 N28 1.17(3) . ? C31 N31 1.149(12) . ? C32 N32 1.140(14) . ? N32 Ni2 2.067(10) 2_666 ? C33 N33 1.142(14) . ? C34 N34 1.182(14) . ? C35 N35 1.154(15) . ? C36 N36 1.141(15) . ? C37 N37 1.141(17) . ? C38 N38 1.136(16) . ? N201 C206 1.293(18) . ? N201 C202 1.328(16) . ? C202 C203 1.404(19) . ? C202 C209 1.49(2) . ? C203 C204 1.32(3) . ? C204 C205 1.38(3) . ? C205 C206 1.42(2) . ? C205 C207 1.51(3) . ? N208 C209 1.319(17) . ? N208 C213 1.343(18) . ? C209 C210 1.416(19) . ? C210 C211 1.37(3) . ? C211 C212 1.32(2) . ? C212 C213 1.416(18) . ? C212 C214 1.52(2) . ? N301 C306 1.290(18) . ? N301 C302 1.354(16) . ? C302 C303 1.391(19) . ? C302 C309 1.45(2) . ? C303 C304 1.37(3) . ? C304 C305 1.43(3) . ? C305 C306 1.378(18) . ? C305 C307 1.50(3) . ? N308 C313 1.332(19) . ? N308 C309 1.373(18) . ? C309 C310 1.43(2) . ? C310 C311 1.43(3) . ? C311 C312 1.33(3) . ? C312 C313 1.41(2) . ? C312 C314 1.53(3) . ? N401 C406 1.336(18) . ? N401 C402 1.38(2) . ? C402 C403 1.39(2) . ? C402 C409 1.41(2) . ? C403 C404 1.42(3) . ? C404 C405 1.34(3) . ? C405 C406 1.41(2) . ? C405 C407 1.54(3) . ? N408 C413 1.355(19) . ? N408 C409 1.356(19) . ? C409 C410 1.40(2) . ? C410 C411 1.25(3) . ? C411 C412 1.48(3) . ? C412 C413 1.38(2) . ? C412 C414 1.52(3) . ? O415 C416 1.444(18) . ? C416 C417 1.44(4) . ? N501 C506 1.318(15) . ? N501 C502 1.337(15) . ? C502 C503 1.373(18) . ? C502 C509 1.47(2) . ? C503 C504 1.37(2) . ? C504 C505 1.38(2) . ? C505 C506 1.370(17) . ? C505 C507 1.494(19) . ? N508 C513 1.334(17) . ? N508 C509 1.343(17) . ? C509 C510 1.410(17) . ? C510 C511 1.41(2) . ? C511 C512 1.30(2) . ? C512 C513 1.377(18) . ? C512 C514 1.50(2) . ? 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 C18 W1 C13 106.1(5) . . ? C18 W1 C12 70.3(4) . . ? C13 W1 C12 78.9(4) . . ? C18 W1 C14 147.7(4) . . ? C13 W1 C14 88.1(4) . . ? C12 W1 C14 141.8(4) . . ? C18 W1 C11 140.4(4) . . ? C13 W1 C11 74.1(4) . . ? C12 W1 C11 70.9(4) . . ? C14 W1 C11 71.0(4) . . ? C18 W1 C15 91.9(5) . . ? C13 W1 C15 145.9(4) . . ? C12 W1 C15 80.2(4) . . ? C14 W1 C15 91.8(4) . . ? C11 W1 C15 73.7(4) . . ? C18 W1 C16 77.2(5) . . ? C13 W1 C16 70.9(4) . . ? C12 W1 C16 126.7(5) . . ? C14 W1 C16 80.6(4) . . ? C11 W1 C16 135.2(4) . . ? C15 W1 C16 142.6(4) . . ? C18 W1 C17 74.5(5) . . ? C13 W1 C17 140.9(4) . . ? C12 W1 C17 133.5(4) . . ? C14 W1 C17 76.4(4) . . ? C11 W1 C17 130.6(4) . . ? C15 W1 C17 71.4(4) . . ? C16 W1 C17 71.3(4) . . ? C28 W2 C21 141.1(7) . . ? C28 W2 C27 77.1(10) . . ? C21 W2 C27 133.5(5) . . ? C28 W2 C22 146.8(7) . . ? C21 W2 C22 72.0(4) . . ? C27 W2 C22 76.6(6) . . ? C28 W2 C24 101.9(16) . . ? C21 W2 C24 73.1(4) . . ? C27 W2 C24 73.3(6) . . ? C22 W2 C24 89.7(5) . . ? C28 W2 C25 98.9(15) . . ? C21 W2 C25 73.5(4) . . ? C27 W2 C25 138.6(6) . . ? C22 W2 C25 87.7(4) . . ? C24 W2 C25 145.6(4) . . ? C28 W2 C23 69.7(7) . . ? C21 W2 C23 71.5(4) . . ? C27 W2 C23 131.9(6) . . ? C22 W2 C23 143.5(4) . . ? C24 W2 C23 80.4(5) . . ? C25 W2 C23 81.5(4) . . ? C28 W2 C26 75.9(14) . . ? C21 W2 C26 131.1(6) . . ? C27 W2 C26 70.2(8) . . ? C22 W2 C26 76.3(9) . . ? C24 W2 C26 143.0(7) . . ? C25 W2 C26 68.9(6) . . ? C23 W2 C26 129.8(8) . . ? C34 W3 C31 72.8(4) . . ? C34 W3 C35 77.3(4) . . ? C31 W3 C35 72.4(4) . . ? C34 W3 C37 71.1(5) . . ? C31 W3 C37 142.4(4) . . ? C35 W3 C37 108.7(6) . . ? C34 W3 C33 143.1(4) . . ? C31 W3 C33 70.6(4) . . ? C35 W3 C33 87.4(4) . . ? C37 W3 C33 145.7(4) . . ? C34 W3 C38 134.9(5) . . ? C31 W3 C38 128.1(5) . . ? C35 W3 C38 142.6(4) . . ? C37 W3 C38 74.6(6) . . ? C33 W3 C38 74.6(5) . . ? C34 W3 C32 80.7(4) . . ? C31 W3 C32 74.0(4) . . ? C35 W3 C32 144.0(4) . . ? C37 W3 C32 90.3(5) . . ? C33 W3 C32 93.6(4) . . ? C38 W3 C32 71.1(4) . . ? C34 W3 C36 124.8(5) . . ? C31 W3 C36 133.5(5) . . ? C35 W3 C36 71.3(4) . . ? C37 W3 C36 77.5(5) . . ? C33 W3 C36 79.6(4) . . ? C38 W3 C36 73.3(5) . . ? C32 W3 C36 144.2(5) . . ? N21 Ni1 N21 180.000(2) . 2_666 ? N21 Ni1 N11 89.7(4) . 2_666 ? N21 Ni1 N11 90.3(4) 2_666 2_666 ? N21 Ni1 N11 90.3(4) . . ? N21 Ni1 N11 89.7(4) 2_666 . ? N11 Ni1 N11 180.000(1) 2_666 . ? N21 Ni1 N31 88.0(3) . 2_666 ? N21 Ni1 N31 92.0(3) 2_666 2_666 ? N11 Ni1 N31 89.4(3) 2_666 2_666 ? N11 Ni1 N31 90.6(3) . 2_666 ? N21 Ni1 N31 92.0(3) . . ? N21 Ni1 N31 88.0(3) 2_666 . ? N11 Ni1 N31 90.6(3) 2_666 . ? N11 Ni1 N31 89.4(3) . . ? N31 Ni1 N31 180.000(2) 2_666 . ? N12 Ni2 N208 93.8(4) . . ? N12 Ni2 N22 92.0(4) . . ? N208 Ni2 N22 172.6(4) . . ? N12 Ni2 N32 92.0(4) . 2_666 ? N208 Ni2 N32 93.5(4) . 2_666 ? N22 Ni2 N32 90.9(4) . 2_666 ? N12 Ni2 N201 172.0(4) . . ? N208 Ni2 N201 78.8(4) . . ? N22 Ni2 N201 95.2(4) . . ? N32 Ni2 N201 91.3(4) 2_666 . ? N12 Ni2 O215 90.2(4) . . ? N208 Ni2 O215 85.7(4) . . ? N22 Ni2 O215 89.7(4) . . ? N32 Ni2 O215 177.7(4) 2_666 . ? N201 Ni2 O215 86.4(4) . . ? N33 Ni3 N23 91.4(4) . . ? N33 Ni3 N13 92.4(4) . 2_666 ? N23 Ni3 N13 92.5(4) . 2_666 ? N33 Ni3 N308 172.2(4) . . ? N23 Ni3 N308 93.5(4) . . ? N13 Ni3 N308 93.5(4) 2_666 . ? N33 Ni3 N301 94.3(4) . . ? N23 Ni3 N301 172.6(4) . . ? N13 Ni3 N301 92.0(4) 2_666 . ? N308 Ni3 N301 80.3(5) . . ? N33 Ni3 O315 88.9(4) . . ? N23 Ni3 O315 87.7(4) . . ? N13 Ni3 O315 178.7(4) 2_666 . ? N308 Ni3 O315 85.2(4) . . ? N301 Ni3 O315 87.7(4) . . ? N14 Ni4 N401 93.4(4) . . ? N14 Ni4 N34 92.5(4) . . ? N401 Ni4 N34 172.5(4) . . ? N14 Ni4 N24 91.2(4) . 2_666 ? N401 Ni4 N24 92.7(4) . 2_666 ? N34 Ni4 N24 91.7(4) . 2_666 ? N14 Ni4 N408 172.8(4) . . ? N401 Ni4 N408 80.1(4) . . ? N34 Ni4 N408 93.7(4) . . ? N24 Ni4 N408 92.3(4) 2_666 . ? N14 Ni4 O415 88.8(5) . . ? N401 Ni4 O415 86.6(4) . . ? N34 Ni4 O415 89.0(4) . . ? N24 Ni4 O415 179.4(4) 2_666 . ? N408 Ni4 O415 87.7(5) . . ? N25 Ni5 N15 91.2(4) . . ? N25 Ni5 N35 93.3(4) . . ? N15 Ni5 N35 91.9(4) . . ? N25 Ni5 N508 92.8(4) . . ? N15 Ni5 N508 176.0(4) . . ? N35 Ni5 N508 88.3(4) . . ? N25 Ni5 N501 172.2(4) . . ? N15 Ni5 N501 95.9(4) . . ? N35 Ni5 N501 89.7(4) . . ? N508 Ni5 N501 80.2(4) . . ? N25 Ni5 O515 88.8(4) . . ? N15 Ni5 O515 88.9(4) . . ? N35 Ni5 O515 177.7(4) . . ? N508 Ni5 O515 90.8(4) . . ? N501 Ni5 O515 88.0(4) . . ? N11 C11 W1 178.6(9) . . ? C11 N11 Ni1 171.9(9) . . ? N12 C12 W1 178.9(10) . . ? C12 N12 Ni2 170.9(9) . . ? N13 C13 W1 175.6(10) . . ? C13 N13 Ni3 173.5(10) . 2_666 ? N14 C14 W1 177.2(9) . . ? C14 N14 Ni4 174.1(9) . . ? N15 C15 W1 175.7(10) . . ? C15 N15 Ni5 170.7(9) . . ? N16 C16 W1 178.8(12) . . ? N17 C17 W1 178.3(12) . . ? N18 C18 W1 176.3(11) . . ? N21 C21 W2 176.4(8) . . ? C21 N21 Ni1 175.8(8) . . ? N22 C22 W2 178.8(12) . . ? C22 N22 Ni2 169.7(10) . . ? N23 C23 W2 178.8(10) . . ? C23 N23 Ni3 175.6(10) . . ? N24 C24 W2 176.3(11) . . ? C24 N24 Ni4 174.3(11) . 2_666 ? N25 C25 W2 177.1(9) . . ? C25 N25 Ni5 178.9(9) . . ? N26 C26 W2 176(2) . . ? N27 C27 W2 180(2) . . ? N28 C28 W2 176(3) . . ? N31 C31 W3 177.1(9) . . ? C31 N31 Ni1 174.3(8) . . ? N32 C32 W3 174.8(10) . . ? C32 N32 Ni2 171.4(10) . 2_666 ? N33 C33 W3 176.9(9) . . ? C33 N33 Ni3 172.5(9) . . ? N34 C34 W3 178.6(11) . . ? C34 N34 Ni4 176.0(9) . . ? N35 C35 W3 174.0(10) . . ? C35 N35 Ni5 173.4(9) . . ? N36 C36 W3 177.8(12) . . ? N37 C37 W3 178.5(16) . . ? N38 C38 W3 178.0(13) . . ? C206 N201 C202 120.4(12) . . ? C206 N201 Ni2 125.2(9) . . ? C202 N201 Ni2 114.3(9) . . ? N201 C202 C203 120.6(15) . . ? N201 C202 C209 115.9(11) . . ? C203 C202 C209 123.4(14) . . ? C204 C203 C202 117.6(15) . . ? C203 C204 C205 123.9(15) . . ? C204 C205 C206 114.1(17) . . ? C204 C205 C207 127.6(16) . . ? C206 C205 C207 118.4(17) . . ? N201 C206 C205 123.3(16) . . ? C209 N208 C213 117.3(12) . . ? C209 N208 Ni2 116.5(10) . . ? C213 N208 Ni2 126.2(9) . . ? N208 C209 C210 120.3(16) . . ? N208 C209 C202 114.5(11) . . ? C210 C209 C202 125.2(15) . . ? C211 C210 C209 120.0(17) . . ? C212 C211 C210 121.4(14) . . ? C211 C212 C213 115.9(17) . . ? C211 C212 C214 124.9(15) . . ? C213 C212 C214 119.2(17) . . ? N208 C213 C212 125.1(16) . . ? C306 N301 C302 119.8(11) . . ? C306 N301 Ni3 126.9(9) . . ? C302 N301 Ni3 113.1(10) . . ? N301 C302 C303 120.1(16) . . ? N301 C302 C309 116.6(11) . . ? C303 C302 C309 123.2(14) . . ? C304 C303 C302 118.9(16) . . ? C303 C304 C305 121.1(16) . . ? C306 C305 C304 114.0(17) . . ? C306 C305 C307 126.4(16) . . ? C304 C305 C307 119.7(15) . . ? N301 C306 C305 126.1(14) . . ? C313 N308 C309 120.3(13) . . ? C313 N308 Ni3 126.6(10) . . ? C309 N308 Ni3 112.5(10) . . ? N308 C309 C310 118.2(17) . . ? N308 C309 C302 116.7(12) . . ? C310 C309 C302 125.0(16) . . ? C309 C310 C311 118.2(17) . . ? C312 C311 C310 122.4(18) . . ? C311 C312 C313 116(2) . . ? C311 C312 C314 121(2) . . ? C313 C312 C314 122(2) . . ? N308 C313 C312 124.4(18) . . ? C406 N401 C402 120.0(13) . . ? C406 N401 Ni4 126.5(10) . . ? C402 N401 Ni4 113.5(10) . . ? N401 C402 C403 117.9(18) . . ? N401 C402 C409 115.6(14) . . ? C403 C402 C409 126.5(18) . . ? C402 C403 C404 120.5(19) . . ? C405 C404 C403 121.1(17) . . ? C404 C405 C406 116.4(19) . . ? C404 C405 C407 123.2(17) . . ? C406 C405 C407 120.4(19) . . ? N401 C406 C405 124.0(18) . . ? C413 N408 C409 120.8(13) . . ? C413 N408 Ni4 126.5(10) . . ? C409 N408 Ni4 112.7(10) . . ? N408 C409 C410 117.7(18) . . ? N408 C409 C402 118.1(13) . . ? C410 C409 C402 124.2(18) . . ? C411 C410 C409 122(2) . . ? C410 C411 C412 123(2) . . ? C413 C412 C411 112.2(18) . . ? C413 C412 C414 119(2) . . ? C411 C412 C414 129(2) . . ? N408 C413 C412 123.6(17) . . ? C416 O415 Ni4 123.0(13) . . ? C417 C416 O415 121(3) . . ? C506 N501 C502 118.6(10) . . ? C506 N501 Ni5 128.0(8) . . ? C502 N501 Ni5 113.2(8) . . ? N501 C502 C503 120.4(13) . . ? N501 C502 C509 116.1(11) . . ? C503 C502 C509 123.4(12) . . ? C504 C503 C502 119.4(14) . . ? C503 C504 C505 120.9(14) . . ? C506 C505 C504 115.2(14) . . ? C506 C505 C507 123.6(13) . . ? C504 C505 C507 121.2(13) . . ? N501 C506 C505 125.4(12) . . ? C513 N508 C509 120.1(11) . . ? C513 N508 Ni5 127.7(9) . . ? C509 N508 Ni5 112.1(9) . . ? N508 C509 C510 118.1(14) . . ? N508 C509 C502 117.9(11) . . ? C510 C509 C502 124.0(13) . . ? C511 C510 C509 119.5(15) . . ? C512 C511 C510 119.9(14) . . ? C511 C512 C513 119.5(15) . . ? C511 C512 C514 121.2(15) . . ? C513 C512 C514 119.2(16) . . ? N508 C513 C512 122.7(15) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 2.316 _refine_diff_density_min -0.976 _refine_diff_density_rms 0.200 #===END data_3b _database_code_depnum_ccdc_archive 'CCDC 876832' #TrackingRef '- clusters1-4_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; {Ni[Ni(5,5'dmbpy)(H2O)]8[W(CN)8]6}*8H2O ; _chemical_name_common (Ni(Ni(5,5'dmbpy)(H2O))8(W(CN)8)6)*8H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C148 H89 N65 Ni9 O12 W6' _chemical_formula_weight 4601.10 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' W W -0.8490 6.8722 '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 19.899(5) _cell_length_b 20.113(5) _cell_length_c 31.475(5) _cell_angle_alpha 89.305(5) _cell_angle_beta 90.024(5) _cell_angle_gamma 73.132(5) _cell_volume 12054(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4448.0 _exptl_absorpt_coefficient_mu 3.586 _exptl_absorpt_correction_T_min 0.6730 _exptl_absorpt_correction_T_max 0.8412 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details '(DENZO-SMN; Otwinowski & Minor, 1997)' _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 KappaCCD _diffrn_measurement_method '\f and \o scans to fill Ewald sphere' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 79308 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.1322 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 27.47 _reflns_number_total 54307 _reflns_number_gt 27806 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (ALTOMARE et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+119.9078P] 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 54307 _refine_ls_number_parameters 1100 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.1964 _refine_ls_R_factor_gt 0.0955 _refine_ls_wR_factor_ref 0.2551 _refine_ls_wR_factor_gt 0.2047 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.004 _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 W1 W 0.38790(3) -0.11933(3) 0.622425(17) 0.05049(15) Uani 1 1 d . . . W2 W 0.59370(3) 0.14497(3) 0.614613(16) 0.04930(15) Uani 1 1 d . . . W3 W 0.25919(3) 0.20034(3) 0.487975(17) 0.04971(15) Uani 1 1 d . . . Ni1 Ni 0.5000 0.0000 0.5000 0.0369(5) Uani 1 2 d S . . Ni2 Ni 0.20332(9) -0.04321(10) 0.49624(6) 0.0576(5) Uani 1 1 d . . . Ni3 Ni 0.64649(10) -0.11879(10) 0.66754(5) 0.0555(4) Uani 1 1 d . . . Ni4 Ni 0.46788(10) 0.31301(9) 0.48602(6) 0.0564(4) Uani 1 1 d . . . Ni5 Ni 0.32978(10) 0.15250(10) 0.65129(5) 0.0576(5) Uani 1 1 d . . . C11 C 0.4498(5) -0.0382(5) 0.5466(3) 0.028(2) Uiso 1 1 d . . . N11 N 0.4270(7) -0.0647(7) 0.5726(4) 0.068(3) Uiso 1 1 d . . . C12 C 0.3126(8) -0.0964(8) 0.5730(5) 0.061(4) Uiso 1 1 d . . . N12 N 0.2714(7) -0.0806(7) 0.5455(4) 0.068(3) Uiso 1 1 d . . . C13 C 0.4896(7) -0.1151(7) 0.6405(4) 0.055(3) Uiso 1 1 d . . . N13 N 0.5450(7) -0.1104(6) 0.6495(4) 0.065(3) Uiso 1 1 d . . . C14 C 0.4506(7) -0.1972(7) 0.5813(4) 0.055(3) Uiso 1 1 d . . . N14 N 0.4808(6) -0.2390(6) 0.5576(4) 0.064(3) Uiso 1 1 d . . . C15 C 0.3595(7) -0.0124(7) 0.6410(4) 0.054(3) Uiso 1 1 d . . . N15 N 0.3459(6) 0.0450(7) 0.6479(4) 0.065(3) Uiso 1 1 d . . . C16 C 0.3541(11) -0.2096(12) 0.6246(7) 0.103(6) Uiso 1 1 d . . . N16 N 0.3321(12) -0.2599(13) 0.6250(7) 0.151(8) Uiso 1 1 d . . . C17 C 0.2862(11) -0.0952(10) 0.6518(6) 0.094(6) Uiso 1 1 d . . . N17 N 0.2295(11) -0.0831(10) 0.6668(6) 0.122(6) Uiso 1 1 d . . . C18 C 0.4072(11) -0.1503(11) 0.6860(7) 0.099(6) Uiso 1 1 d . . . N18 N 0.4203(14) -0.1702(14) 0.7225(9) 0.174(9) Uiso 1 1 d . . . C21 C 0.5462(5) 0.0449(5) 0.5449(3) 0.028(2) Uiso 1 1 d . . . N21 N 0.5654(6) 0.0781(7) 0.5688(4) 0.067(3) Uiso 1 1 d . . . C22 C 0.6761(7) 0.1173(7) 0.5689(4) 0.053(3) Uiso 1 1 d . . . N22 N 0.7222(6) 0.0972(6) 0.5461(4) 0.064(3) Uiso 1 1 d . . . C23 C 0.6184(7) 0.0438(7) 0.6435(4) 0.052(3) Uiso 1 1 d . . . N23 N 0.6323(6) -0.0133(6) 0.6564(4) 0.062(3) Uiso 1 1 d . . . C24 C 0.5343(7) 0.2106(7) 0.5652(4) 0.053(3) Uiso 1 1 d . . . N24 N 0.5033(6) 0.2452(6) 0.5371(4) 0.062(3) Uiso 1 1 d . . . C25 C 0.4883(7) 0.1441(7) 0.6285(4) 0.053(3) Uiso 1 1 d . . . N25 N 0.4322(6) 0.1421(6) 0.6360(4) 0.060(3) Uiso 1 1 d . . . C26 C 0.6159(10) 0.2411(11) 0.6128(6) 0.094(6) Uiso 1 1 d . . . N26 N 0.6307(12) 0.2932(12) 0.6109(7) 0.144(7) Uiso 1 1 d . . . C27 C 0.6900(10) 0.1304(9) 0.6479(6) 0.081(5) Uiso 1 1 d . . . N27 N 0.7447(10) 0.1217(10) 0.6659(6) 0.121(6) Uiso 1 1 d . . . C28 C 0.5663(9) 0.1840(9) 0.6762(6) 0.077(5) Uiso 1 1 d . . . N28 N 0.5490(9) 0.2053(9) 0.7105(6) 0.111(5) Uiso 1 1 d . . . C31 C 0.4168(5) 0.0868(5) 0.4967(3) 0.029(2) Uiso 1 1 d . . . N31 N 0.3646(7) 0.1252(7) 0.4944(4) 0.067(3) Uiso 1 1 d . . . C32 C 0.2440(7) 0.0997(8) 0.4879(4) 0.056(3) Uiso 1 1 d . . . N32 N 0.2363(6) 0.0442(7) 0.4892(4) 0.064(3) Uiso 1 1 d . . . C33 C 0.2953(8) 0.1640(8) 0.4258(5) 0.060(4) Uiso 1 1 d . . . N33 N 0.3162(6) 0.1443(6) 0.3929(4) 0.060(3) Uiso 1 1 d . . . C34 C 0.3344(7) 0.2581(7) 0.4801(4) 0.055(3) Uiso 1 1 d . . . N34 N 0.3773(6) 0.2849(6) 0.4791(4) 0.063(3) Uiso 1 1 d . . . C35 C 0.2828(7) 0.1794(7) 0.5538(4) 0.056(3) Uiso 1 1 d . . . N35 N 0.2985(6) 0.1673(6) 0.5890(4) 0.061(3) Uiso 1 1 d . . . C36 C 0.1572(11) 0.2072(11) 0.5102(7) 0.097(6) Uiso 1 1 d . . . N36 N 0.1036(12) 0.2097(12) 0.5264(7) 0.142(7) Uiso 1 1 d . . . C37 C 0.1928(11) 0.2664(11) 0.4432(7) 0.102(6) Uiso 1 1 d . . . N37 N 0.1568(14) 0.3001(14) 0.4155(8) 0.170(9) Uiso 1 1 d . . . C38 C 0.2189(10) 0.2954(11) 0.5170(6) 0.094(6) Uiso 1 1 d . . . N38 N 0.1988(11) 0.3496(11) 0.5341(7) 0.130(7) Uiso 1 1 d . . . N201 N 0.1221(6) 0.0124(6) 0.5345(4) 0.066(3) Uiso 1 1 d . . . C202 C 0.1234(9) 0.0160(9) 0.5772(5) 0.076(5) Uiso 1 1 d . . . H202 H 0.1646 -0.0078 0.5913 0.092 Uiso 1 1 calc R . . C203 C 0.0672(9) 0.0530(9) 0.6012(5) 0.078(5) Uiso 1 1 d . . . C204 C 0.0105(10) 0.0903(10) 0.5784(6) 0.086(5) Uiso 1 1 d . . . H204 H -0.0278 0.1186 0.5928 0.103 Uiso 1 1 calc R . . C205 C 0.0078(9) 0.0879(9) 0.5376(5) 0.077(5) Uiso 1 1 d . . . H205 H -0.0331 0.1127 0.5235 0.093 Uiso 1 1 calc R . . C206 C 0.0630(8) 0.0502(8) 0.5145(5) 0.068(4) Uiso 1 1 d . . . C207 C 0.0678(9) 0.0412(9) 0.4683(5) 0.072(4) Uiso 1 1 d . . . C208 C 0.0126(10) 0.0771(9) 0.4404(6) 0.083(5) Uiso 1 1 d . . . H208 H -0.0279 0.1078 0.4513 0.099 Uiso 1 1 calc R . . C209 C 0.0189(11) 0.0666(10) 0.3980(6) 0.095(6) Uiso 1 1 d . . . H209 H -0.0182 0.0884 0.3800 0.114 Uiso 1 1 calc R . . C210 C 0.0794(10) 0.0244(10) 0.3814(6) 0.084(5) Uiso 1 1 d . . . C211 C 0.1335(9) -0.0097(9) 0.4100(5) 0.075(4) Uiso 1 1 d . . . H211 H 0.1751 -0.0385 0.3993 0.090 Uiso 1 1 calc R . . N212 N 0.1268(6) -0.0020(6) 0.4513(4) 0.066(3) Uiso 1 1 d . . . C213 C 0.0739(12) 0.0523(12) 0.6487(7) 0.119(7) Uiso 1 1 d . . . H21A H 0.0306 0.0799 0.6608 0.179 Uiso 1 1 calc R . . H21B H 0.1112 0.0711 0.6566 0.179 Uiso 1 1 calc R . . H21C H 0.0841 0.0054 0.6592 0.179 Uiso 1 1 calc R . . C214 C 0.0912(12) 0.0095(12) 0.3344(7) 0.119(7) Uiso 1 1 d . . . H21D H 0.1368 -0.0226 0.3303 0.179 Uiso 1 1 calc R . . H21E H 0.0882 0.0520 0.3193 0.179 Uiso 1 1 calc R . . H21F H 0.0560 -0.0101 0.3239 0.179 Uiso 1 1 calc R . . O215 O 0.1626(6) -0.1293(6) 0.5033(3) 0.078(3) Uiso 1 1 d . . . N301 N 0.7450(6) -0.1375(6) 0.6938(4) 0.064(3) Uiso 1 1 d . . . C302 C 0.8058(9) -0.1593(9) 0.6729(6) 0.078(5) Uiso 1 1 d . . . H302 H 0.8042 -0.1621 0.6434 0.094 Uiso 1 1 calc R . . C303 C 0.8714(11) -0.1782(11) 0.6925(6) 0.094(6) Uiso 1 1 d . . . C304 C 0.8704(12) -0.1755(11) 0.7358(7) 0.105(6) Uiso 1 1 d . . . H304 H 0.9132 -0.1891 0.7501 0.126 Uiso 1 1 calc R . . C305 C 0.8126(10) -0.1548(10) 0.7587(7) 0.096(6) Uiso 1 1 d . . . H305 H 0.8144 -0.1529 0.7882 0.115 Uiso 1 1 calc R . . C306 C 0.7467(8) -0.1354(8) 0.7363(5) 0.070(4) Uiso 1 1 d . . . C307 C 0.6776(8) -0.1155(8) 0.7572(5) 0.066(4) Uiso 1 1 d . . . C308 C 0.6720(11) -0.1117(10) 0.8015(6) 0.096(6) Uiso 1 1 d . . . H308 H 0.7106 -0.1191 0.8195 0.116 Uiso 1 1 calc R . . C309 C 0.6057(12) -0.0962(11) 0.8155(7) 0.112(7) Uiso 1 1 d . . . H309 H 0.5999 -0.0932 0.8448 0.134 Uiso 1 1 calc R . . C310 C 0.5461(11) -0.0844(11) 0.7920(7) 0.099(6) Uiso 1 1 d . . . C311 C 0.5592(10) -0.0872(9) 0.7471(6) 0.084(5) Uiso 1 1 d . . . H311 H 0.5213 -0.0772 0.7284 0.100 Uiso 1 1 calc R . . N312 N 0.6228(7) -0.1033(6) 0.7316(4) 0.066(3) Uiso 1 1 d . . . C313 C 0.9350(12) -0.2039(13) 0.6650(8) 0.129(8) Uiso 1 1 d . . . H31A H 0.9209 -0.2001 0.6357 0.194 Uiso 1 1 calc R . . H31B H 0.9584 -0.2516 0.6720 0.194 Uiso 1 1 calc R . . H31C H 0.9665 -0.1764 0.6697 0.194 Uiso 1 1 calc R . . C314 C 0.4705(14) -0.0725(15) 0.8064(9) 0.159(10) Uiso 1 1 d . . . H31D H 0.4404 -0.0668 0.7820 0.238 Uiso 1 1 calc R . . H31E H 0.4564 -0.0314 0.8233 0.238 Uiso 1 1 calc R . . H31F H 0.4671 -0.1117 0.8230 0.238 Uiso 1 1 calc R . . O315 O 0.6579(5) -0.2256(5) 0.6790(3) 0.071(3) Uiso 1 1 d . . . C316 C 0.6339(14) -0.2674(15) 0.6490(9) 0.136(9) Uiso 1 1 d . . . C317 C 0.660(3) -0.342(3) 0.6570(16) 0.27(2) Uiso 1 1 d . . . N401 N 0.5521(7) 0.3504(7) 0.4968(4) 0.069(3) Uiso 1 1 d . . . C402 C 0.6143(9) 0.3253(9) 0.4805(5) 0.079(5) Uiso 1 1 d . . . H402 H 0.6211 0.2885 0.4618 0.094 Uiso 1 1 calc R . . C403 C 0.6726(10) 0.3503(10) 0.4894(6) 0.086(5) Uiso 1 1 d . . . C404 C 0.6595(11) 0.4049(10) 0.5175(6) 0.096(6) Uiso 1 1 d . . . H404 H 0.6954 0.4231 0.5257 0.115 Uiso 1 1 calc R . . C405 C 0.5926(10) 0.4322(10) 0.5331(6) 0.087(5) Uiso 1 1 d . . . H405 H 0.5836 0.4702 0.5511 0.105 Uiso 1 1 calc R . . C406 C 0.5389(9) 0.4053(9) 0.5231(5) 0.073(4) Uiso 1 1 d . . . C407 C 0.4706(9) 0.4282(9) 0.5399(5) 0.074(4) Uiso 1 1 d . . . C408 C 0.4479(10) 0.4867(9) 0.5680(5) 0.084(5) Uiso 1 1 d . . . H408 H 0.4783 0.5114 0.5767 0.101 Uiso 1 1 calc R . . C409 C 0.3793(11) 0.5041(11) 0.5812(7) 0.101(6) Uiso 1 1 d . . . H409 H 0.3646 0.5392 0.6011 0.121 Uiso 1 1 calc R . . C410 C 0.3303(10) 0.4719(10) 0.5665(6) 0.090(5) Uiso 1 1 d . . . C411 C 0.3588(9) 0.4157(9) 0.5389(5) 0.077(5) Uiso 1 1 d . . . H411 H 0.3287 0.3916 0.5288 0.092 Uiso 1 1 calc R . . N412 N 0.4246(6) 0.3949(6) 0.5264(4) 0.064(3) Uiso 1 1 d . . . C413 C 0.7447(13) 0.3181(13) 0.4690(8) 0.135(9) Uiso 1 1 d . . . H41A H 0.7425 0.2806 0.4510 0.202 Uiso 1 1 calc R . . H41B H 0.7793 0.3009 0.4908 0.202 Uiso 1 1 calc R . . H41C H 0.7574 0.3529 0.4523 0.202 Uiso 1 1 calc R . . C414 C 0.2559(12) 0.4943(12) 0.5798(7) 0.120(7) Uiso 1 1 d . . . H41D H 0.2311 0.4656 0.5666 0.180 Uiso 1 1 calc R . . H41E H 0.2350 0.5419 0.5714 0.180 Uiso 1 1 calc R . . H41F H 0.2534 0.4899 0.6101 0.180 Uiso 1 1 calc R . . O415 O 0.4378(6) 0.3870(6) 0.4357(3) 0.075(3) Uiso 1 1 d . . . N501 N 0.3480(7) 0.1450(7) 0.7164(4) 0.068(3) Uiso 1 1 d . . . C502 C 0.4103(10) 0.1315(9) 0.7346(6) 0.084(5) Uiso 1 1 d . . . H502 H 0.4497 0.1211 0.7173 0.101 Uiso 1 1 calc R . . C503 C 0.4201(12) 0.1319(11) 0.7801(7) 0.106(6) Uiso 1 1 d . . . C504 C 0.3563(12) 0.1435(12) 0.8021(8) 0.116(7) Uiso 1 1 d . . . H504 H 0.3584 0.1398 0.8316 0.140 Uiso 1 1 calc R . . C505 C 0.2946(12) 0.1589(11) 0.7842(7) 0.103(6) Uiso 1 1 d . . . H505 H 0.2543 0.1694 0.8008 0.123 Uiso 1 1 calc R . . C506 C 0.2890(9) 0.1595(9) 0.7398(5) 0.076(4) Uiso 1 1 d . . . C507 C 0.2221(8) 0.1765(8) 0.7163(5) 0.069(4) Uiso 1 1 d . . . C508 C 0.1566(10) 0.1936(10) 0.7355(6) 0.094(6) Uiso 1 1 d . . . H508 H 0.1526 0.1904 0.7648 0.112 Uiso 1 1 calc R . . C509 C 0.0995(12) 0.2148(11) 0.7111(7) 0.107(6) Uiso 1 1 d . . . H509 H 0.0557 0.2280 0.7241 0.128 Uiso 1 1 calc R . . C510 C 0.1026(11) 0.2180(10) 0.6676(6) 0.094(6) Uiso 1 1 d . . . C511 C 0.1710(9) 0.1948(9) 0.6500(6) 0.081(5) Uiso 1 1 d . . . H511 H 0.1758 0.1938 0.6206 0.097 Uiso 1 1 calc R . . N512 N 0.2276(7) 0.1749(7) 0.6736(4) 0.067(3) Uiso 1 1 d . . . C513 C 0.4906(12) 0.1194(13) 0.7984(8) 0.131(8) Uiso 1 1 d . . . H51A H 0.4874 0.1211 0.8288 0.196 Uiso 1 1 calc R . . H51B H 0.5110 0.1544 0.7883 0.196 Uiso 1 1 calc R . . H51C H 0.5196 0.0745 0.7900 0.196 Uiso 1 1 calc R . . C514 C 0.0389(12) 0.2404(12) 0.6377(7) 0.125(8) Uiso 1 1 d . . . H51D H 0.0546 0.2371 0.6088 0.187 Uiso 1 1 calc R . . H51E H 0.0127 0.2876 0.6435 0.187 Uiso 1 1 calc R . . H51F H 0.0095 0.2106 0.6421 0.187 Uiso 1 1 calc R . . O515 O 0.3176(5) 0.2601(6) 0.6563(3) 0.073(3) Uiso 1 1 d . . . C516 C 0.3446(9) 0.3019(9) 0.6258(5) 0.081(5) Uiso 1 1 d . . . H51G H 0.3700 0.2724 0.6034 0.097 Uiso 1 1 calc R . . H51H H 0.3056 0.3371 0.6129 0.097 Uiso 1 1 calc R . . C517 C 0.3907(11) 0.3349(12) 0.6470(7) 0.113(7) Uiso 1 1 d . . . H51I H 0.4082 0.3618 0.6267 0.170 Uiso 1 1 calc R . . H51J H 0.4294 0.3000 0.6596 0.170 Uiso 1 1 calc R . . H51K H 0.3652 0.3649 0.6688 0.170 Uiso 1 1 calc R . . W1' W 0.17577(3) 0.29825(3) 0.090362(17) 0.05922(17) Uani 1 1 d . . . W2' W 0.05656(3) 0.34919(3) -0.139608(16) 0.05277(15) Uani 1 1 d . . . W3' W 0.21105(3) 0.60176(4) -0.04124(2) 0.06529(18) Uani 1 1 d D . . Ni1' Ni 0.0000 0.5000 0.0000 0.0390(5) Uani 1 2 d S . . Ni2' Ni 0.22241(10) 0.54108(12) 0.12449(6) 0.0683(5) Uani 1 1 d . . . Ni3' Ni 0.01175(13) 0.19489(10) -0.00950(6) 0.0718(6) Uani 1 1 d . . . Ni4' Ni 0.05728(11) 0.60813(11) -0.18161(6) 0.0665(5) Uani 1 1 d . . . Ni5' Ni 0.29682(10) 0.32570(12) -0.05788(6) 0.0712(6) Uani 1 1 d . . . C11' C 0.1041(7) 0.3827(7) 0.0577(4) 0.052(3) Uiso 1 1 d . . . N11' N 0.0651(6) 0.4264(6) 0.0387(3) 0.052(3) Uiso 1 1 d . . . C12' C 0.2067(8) 0.3893(8) 0.1047(5) 0.063(4) Uiso 1 1 d . . . N12' N 0.2180(7) 0.4407(7) 0.1124(4) 0.070(3) Uiso 1 1 d . . . C13' C 0.1159(8) 0.2536(8) 0.0476(5) 0.061(4) Uiso 1 1 d . . . N13' N 0.0802(7) 0.2326(7) 0.0261(4) 0.075(4) Uiso 1 1 d . . . C14' C 0.0837(8) 0.3266(8) 0.1275(4) 0.059(4) Uiso 1 1 d . . . N14' N 0.0335(7) 0.3452(7) 0.1476(4) 0.070(3) Uiso 1 1 d . . . C15' C 0.2213(8) 0.3104(8) 0.0297(5) 0.070(4) Uiso 1 1 d . . . N15' N 0.2451(7) 0.3173(7) -0.0028(4) 0.077(4) Uiso 1 1 d . . . C16' C 0.2085(9) 0.2913(9) 0.1552(5) 0.075(4) Uiso 1 1 d . . . N16' N 0.2275(9) 0.2890(9) 0.1905(6) 0.105(5) Uiso 1 1 d . . . C17' C 0.1760(11) 0.1994(12) 0.1130(7) 0.100(6) Uiso 1 1 d . . . N17' N 0.1742(12) 0.1441(13) 0.1254(7) 0.150(8) Uiso 1 1 d . . . C18' C 0.2843(12) 0.2406(11) 0.0905(7) 0.102(6) Uiso 1 1 d . . . N18' N 0.3450(12) 0.2101(12) 0.0899(7) 0.142(7) Uiso 1 1 d . . . C21' C 0.0388(7) 0.4080(7) -0.0820(4) 0.051(3) Uiso 1 1 d . . . N21' N 0.0275(5) 0.4370(6) -0.0507(3) 0.051(3) Uiso 1 1 d . . . C22' C -0.0538(8) 0.3951(7) -0.1326(4) 0.057(3) Uiso 1 1 d . . . N22' N -0.1134(7) 0.4207(7) -0.1291(4) 0.070(3) Uiso 1 1 d . . . C23' C 0.0345(8) 0.2840(8) -0.0909(5) 0.066(4) Uiso 1 1 d . . . N23' N 0.0245(7) 0.2489(7) -0.0629(4) 0.077(4) Uiso 1 1 d . . . C24' C 0.0493(7) 0.4540(8) -0.1592(4) 0.058(3) Uiso 1 1 d . . . N24' N 0.0495(7) 0.5085(7) -0.1677(4) 0.072(3) Uiso 1 1 d . . . C25' C 0.1566(8) 0.3349(8) -0.1101(4) 0.060(4) Uiso 1 1 d . . . N25' N 0.2090(7) 0.3306(7) -0.0929(4) 0.073(4) Uiso 1 1 d . . . C26' C 0.1278(9) 0.3433(9) -0.1898(6) 0.080(5) Uiso 1 1 d . . . N26' N 0.1678(10) 0.3438(10) -0.2183(6) 0.118(6) Uiso 1 1 d . . . C27' C 0.1068(11) 0.2451(11) -0.1525(6) 0.096(6) Uiso 1 1 d . . . N27' N 0.1392(11) 0.1843(11) -0.1565(6) 0.126(6) Uiso 1 1 d . . . C28' C 0.0029(12) 0.3293(12) -0.1929(7) 0.106(6) Uiso 1 1 d . . . N28' N -0.0271(13) 0.3158(12) -0.2224(8) 0.155(8) Uiso 1 1 d . . . C31' C 0.1264(7) 0.5601(7) -0.0252(4) 0.052(3) Uiso 1 1 d . . . N31' N 0.0817(6) 0.5390(6) -0.0153(4) 0.059(3) Uiso 1 1 d . . . C32' C 0.2169(8) 0.5790(8) 0.0254(5) 0.066(4) Uiso 1 1 d . . . N32' N 0.2200(7) 0.5645(7) 0.0603(4) 0.079(4) Uiso 1 1 d . . . C33' C 0.1228(8) 0.6848(8) -0.0184(5) 0.067(4) Uiso 1 1 d . . . N33' N 0.0752(8) 0.7269(8) -0.0080(4) 0.082(4) Uiso 1 1 d . . . C34' C 0.1491(8) 0.6072(8) -0.0977(5) 0.065(4) Uiso 1 1 d . . . N34' N 0.1168(7) 0.6071(7) -0.1275(4) 0.077(4) Uiso 1 1 d . . . C35' C 0.2523(8) 0.4915(9) -0.0490(5) 0.070(4) Uiso 1 1 d . . . N35' N 0.2691(7) 0.4334(7) -0.0538(4) 0.076(4) Uiso 1 1 d . . . C36' C 0.308(2) 0.602(2) -0.0154(12) 0.189(14) Uiso 1 1 d . . . N36' N 0.356(2) 0.616(2) 0.0004(13) 0.261(17) Uiso 1 1 d . . . C37' C 0.2829(13) 0.5903(13) -0.0909(8) 0.123(8) Uiso 1 1 d . . . N37' N 0.3241(14) 0.5771(14) -0.1191(9) 0.174(9) Uiso 1 1 d . . . C38' C 0.220(3) 0.7003(15) -0.0645(16) 0.27(2) Uiso 1 1 d D . . N38' N 0.216(3) 0.7542(15) -0.0788(17) 0.36(3) Uiso 1 1 d D . . N601 N 0.3315(8) 0.5117(8) 0.1303(5) 0.084(4) Uiso 1 1 d . . . C602 C 0.3755(11) 0.5101(11) 0.0990(7) 0.104(6) Uiso 1 1 d . . . H602 H 0.3580 0.5171 0.0714 0.124 Uiso 1 1 calc R . . C603 C 0.4496(13) 0.4981(12) 0.1055(8) 0.116(7) Uiso 1 1 d . . . C604 C 0.4702(15) 0.4853(14) 0.1455(9) 0.137(9) Uiso 1 1 d . . . H604 H 0.5180 0.4744 0.1513 0.165 Uiso 1 1 calc R . . C605 C 0.4283(14) 0.4869(13) 0.1771(9) 0.136(9) Uiso 1 1 d . . . H605 H 0.4470 0.4772 0.2043 0.163 Uiso 1 1 calc R . . C606 C 0.3533(11) 0.5032(11) 0.1713(7) 0.100(6) Uiso 1 1 d . . . C607 C 0.3008(10) 0.5071(10) 0.2035(6) 0.091(5) Uiso 1 1 d . . . C608 C 0.3147(14) 0.4968(13) 0.2466(8) 0.128(8) Uiso 1 1 d . . . H608 H 0.3608 0.4828 0.2564 0.154 Uiso 1 1 calc R . . C609 C 0.2639(14) 0.5065(13) 0.2730(9) 0.130(8) Uiso 1 1 d . . . H609 H 0.2747 0.5011 0.3018 0.156 Uiso 1 1 calc R . . C610 C 0.1952(13) 0.5242(12) 0.2615(7) 0.110(7) Uiso 1 1 d . . . C611 C 0.1844(11) 0.5308(10) 0.2169(6) 0.094(6) Uiso 1 1 d . . . H611 H 0.1387 0.5413 0.2067 0.113 Uiso 1 1 calc R . . N612 N 0.2355(7) 0.5228(7) 0.1893(4) 0.077(4) Uiso 1 1 d . . . C613 C 0.4955(16) 0.4965(16) 0.0639(9) 0.170(12) Uiso 1 1 d . . . H61A H 0.4652 0.5077 0.0395 0.256 Uiso 1 1 calc R . . H61B H 0.5278 0.4510 0.0608 0.256 Uiso 1 1 calc R . . H61C H 0.5213 0.5300 0.0664 0.256 Uiso 1 1 calc R . . C614 C 0.1295(16) 0.5378(16) 0.2899(10) 0.172(12) Uiso 1 1 d . . . H61D H 0.0881 0.5502 0.2723 0.259 Uiso 1 1 calc R . . H61E H 0.1283 0.5751 0.3089 0.259 Uiso 1 1 calc R . . H61F H 0.1312 0.4966 0.3060 0.259 Uiso 1 1 calc R . . O615 O 0.2270(7) 0.6441(7) 0.1372(4) 0.101(4) Uiso 1 1 d . . . N801 N 0.0074(7) 0.6105(7) -0.2403(4) 0.067(3) Uiso 1 1 d . . . C802 C -0.0607(9) 0.6299(9) -0.2470(6) 0.081(5) Uiso 1 1 d . . . H802 H -0.0898 0.6437 -0.2237 0.097 Uiso 1 1 calc R . . C803 C -0.0928(10) 0.6313(10) -0.2871(6) 0.089(5) Uiso 1 1 d . . . C804 C -0.0456(12) 0.6100(12) -0.3192(8) 0.117(7) Uiso 1 1 d . . . H804 H -0.0629 0.6105 -0.3467 0.140 Uiso 1 1 calc R . . C805 C 0.0268(12) 0.5875(11) -0.3133(7) 0.110(7) Uiso 1 1 d . . . H805 H 0.0567 0.5731 -0.3362 0.132 Uiso 1 1 calc R . . C806 C 0.0537(9) 0.5869(9) -0.2719(5) 0.078(5) Uiso 1 1 d . . . C807 C 0.1245(10) 0.5659(9) -0.2613(6) 0.081(5) Uiso 1 1 d . . . C808 C 0.1804(14) 0.5398(14) -0.2898(9) 0.138(9) Uiso 1 1 d . . . H808 H 0.1697 0.5314 -0.3176 0.166 Uiso 1 1 calc R . . C809 C 0.2479(15) 0.5264(14) -0.2789(9) 0.141(9) Uiso 1 1 d . . . H809 H 0.2819 0.5162 -0.3000 0.169 Uiso 1 1 calc R . . C810 C 0.2690(12) 0.5275(12) -0.2361(7) 0.110(7) Uiso 1 1 d . . . C811 C 0.2094(10) 0.5505(10) -0.2082(6) 0.092(5) Uiso 1 1 d . . . H811 H 0.2184 0.5525 -0.1793 0.110 Uiso 1 1 calc R . . N812 N 0.1414(7) 0.5694(7) -0.2210(4) 0.076(4) Uiso 1 1 d . . . C813 C -0.1684(11) 0.6575(11) -0.2945(7) 0.111(7) Uiso 1 1 d . . . H81A H -0.1920 0.6706 -0.2680 0.167 Uiso 1 1 calc R . . H81B H -0.1847 0.6218 -0.3072 0.167 Uiso 1 1 calc R . . H81C H -0.1782 0.6972 -0.3133 0.167 Uiso 1 1 calc R . . C814 C 0.3443(12) 0.5096(13) -0.2205(8) 0.132(8) Uiso 1 1 d . . . H81D H 0.3447 0.5149 -0.1902 0.197 Uiso 1 1 calc R . . H81E H 0.3674 0.5401 -0.2338 0.197 Uiso 1 1 calc R . . H81F H 0.3684 0.4623 -0.2275 0.197 Uiso 1 1 calc R . . O815 O 0.0669(7) 0.7086(7) -0.1970(4) 0.108(4) Uiso 1 1 d . . . N901 N 0.3600(7) 0.3263(7) -0.1106(4) 0.079(4) Uiso 1 1 d . . . C902 C 0.3415(10) 0.3252(9) -0.1503(5) 0.081(5) Uiso 1 1 d . . . H902 H 0.2953 0.3269 -0.1562 0.097 Uiso 1 1 calc R . . C903 C 0.3878(12) 0.3215(11) -0.1847(7) 0.102(6) Uiso 1 1 d . . . C904 C 0.4519(13) 0.3204(12) -0.1724(8) 0.126(8) Uiso 1 1 d . . . H904 H 0.4845 0.3173 -0.1940 0.151 Uiso 1 1 calc R . . C905 C 0.4756(13) 0.3230(12) -0.1330(8) 0.123(8) Uiso 1 1 d . . . H905 H 0.5211 0.3243 -0.1274 0.148 Uiso 1 1 calc R . . C906 C 0.4253(11) 0.3238(11) -0.0997(6) 0.096(6) Uiso 1 1 d . . . C907 C 0.4429(11) 0.3211(11) -0.0549(7) 0.099(6) Uiso 1 1 d . . . C908 C 0.5100(14) 0.3199(13) -0.0380(9) 0.137(9) Uiso 1 1 d . . . H908 H 0.5473 0.3199 -0.0559 0.164 Uiso 1 1 calc R . . C909 C 0.5177(15) 0.3189(13) 0.0052(9) 0.137(9) Uiso 1 1 d . . . H909 H 0.5600 0.3220 0.0164 0.164 Uiso 1 1 calc R . . C910 C 0.4686(13) 0.3138(13) 0.0317(8) 0.118(7) Uiso 1 1 d . . . C911 C 0.3993(12) 0.3169(11) 0.0126(7) 0.107(6) Uiso 1 1 d . . . H911 H 0.3619 0.3166 0.0303 0.128 Uiso 1 1 calc R . . N912 N 0.3901(8) 0.3200(8) -0.0284(5) 0.085(4) Uiso 1 1 d . . . C913 C 0.3596(13) 0.3184(13) -0.2296(7) 0.128(8) Uiso 1 1 d . . . H91A H 0.3106 0.3214 -0.2283 0.192 Uiso 1 1 calc R . . H91B H 0.3848 0.2753 -0.2424 0.192 Uiso 1 1 calc R . . H91C H 0.3657 0.3564 -0.2464 0.192 Uiso 1 1 calc R . . C914 C 0.4752(16) 0.3100(16) 0.0781(9) 0.171(12) Uiso 1 1 d . . . H91D H 0.4322 0.3062 0.0902 0.257 Uiso 1 1 calc R . . H91E H 0.4846 0.3512 0.0882 0.257 Uiso 1 1 calc R . . H91F H 0.5131 0.2700 0.0861 0.257 Uiso 1 1 calc R . . O915 O 0.3289(7) 0.2145(7) -0.0615(4) 0.108(4) Uiso 1 1 d . . . N701 N -0.0035(6) 0.1325(7) 0.0402(4) 0.083(4) Uiso 1 1 d D . . N712 N -0.0515(8) 0.1479(9) -0.0425(6) 0.118(6) Uiso 1 1 d D . . N724 N 0.0927(8) 0.1070(8) -0.0270(5) 0.103(5) Uiso 1 1 d D . . C704 C -0.0267(11) 0.0387(12) 0.0983(7) 0.171(12) Uiso 1 1 d D . . C702 C 0.0242(12) 0.1311(13) 0.0802(7) 0.122(15) Uiso 0.517(12) 1 d PD A 1 C703 C 0.0127(13) 0.0836(14) 0.1113(9) 0.20(3) Uiso 0.517(12) 1 d PD A 1 C705 C -0.0537(13) 0.0421(13) 0.0582(8) 0.140(18) Uiso 0.517(12) 1 d PD A 1 C706 C -0.0400(10) 0.0901(11) 0.0302(7) 0.116(14) Uiso 0.517(12) 1 d PD A 1 C707 C -0.0631(11) 0.1005(12) -0.0142(7) 0.105(13) Uiso 0.517(12) 1 d PD A 1 C708 C -0.1029(14) 0.0555(13) -0.0249(11) 0.107(13) Uiso 0.517(12) 1 d PD A 1 C709 C -0.1268(16) 0.0623(19) -0.0668(13) 0.19(3) Uiso 0.517(12) 1 d PD A 1 C710 C -0.1136(16) 0.111(2) -0.0951(11) 0.21(3) Uiso 0.517(12) 1 d PD A 1 C711 C -0.068(3) 0.150(2) -0.0826(9) 0.149(19) Uiso 0.517(12) 1 d PD A 1 C713 C 0.036(4) 0.104(4) 0.1546(16) 0.24(4) Uiso 0.517(12) 1 d PD A 1 C714 C -0.111(5) 0.122(5) -0.1423(13) 0.26(4) Uiso 0.517(12) 1 d PD A 1 C715 C -0.0524(11) 0.1532(14) 0.0700(7) 0.112(15) Uiso 0.483(12) 1 d PD A 2 C716 C -0.0652(13) 0.1071(14) 0.1006(8) 0.124(16) Uiso 0.483(12) 1 d PD A 2 C717 C 0.0246(13) 0.0162(13) 0.0664(8) 0.112(15) Uiso 0.483(12) 1 d PD A 2 C718 C 0.0346(10) 0.0648(11) 0.0365(6) 0.089(11) Uiso 0.483(12) 1 d PD A 2 C719 C 0.0845(12) 0.0556(14) 0.0001(6) 0.095(12) Uiso 0.483(12) 1 d PD A 2 C720 C 0.1288(17) -0.0123(14) -0.0063(10) 0.126(17) Uiso 0.483(12) 1 d PD A 2 C721 C 0.1757(17) -0.0222(18) -0.0401(11) 0.18(3) Uiso 0.483(12) 1 d PD A 2 C722 C 0.1803(15) 0.032(2) -0.0674(10) 0.26(4) Uiso 0.483(12) 1 d PD A 2 C723 C 0.123(2) 0.0926(18) -0.0647(9) 0.125(17) Uiso 0.483(12) 1 d PD A 2 C726 C 0.210(3) 0.014(3) -0.1112(14) 0.20(3) Uiso 0.483(12) 1 d PD A 2 C725 C -0.123(4) 0.113(5) 0.132(2) 0.24(4) Uiso 0.483(12) 1 d PD A 2 O1W O 0.2069(8) 0.3504(8) 0.6949(5) 0.126(5) Uiso 1 1 d . B 2 O2W O 0.6544(8) -0.2754(8) 0.7587(5) 0.128(5) Uiso 1 1 d . . 2 O3W O 0.8401(10) 0.1713(11) 0.4091(6) 0.118(6) Uiso 0.75 1 d P C 2 O4W O 0.3045(14) 0.4696(14) 0.4172(8) 0.104(8) Uiso 0.50 1 d P D 2 O5W O 0.4721(14) 0.6164(14) 0.6308(8) 0.104(8) Uiso 0.50 1 d P E 2 O6W O 0.806(2) 0.220(2) 0.5629(13) 0.177(15) Uiso 0.50 1 d P F 2 O7W O 0.706(3) 0.397(3) 0.6258(16) 0.091(14) Uiso 0.25 1 d P . 2 O8W O 0.346(3) 0.578(3) 0.3598(16) 0.093(14) Uiso 0.25 1 d P . 2 O9W O 0.408(3) 0.289(3) 0.213(2) 0.123(19) Uiso 0.25 1 d P . 2 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 W1 0.0519(3) 0.0548(3) 0.0460(3) 0.0068(2) 0.0038(2) -0.0176(3) W2 0.0549(3) 0.0504(3) 0.0444(3) -0.0061(2) -0.0068(2) -0.0180(3) W3 0.0425(3) 0.0502(3) 0.0515(3) 0.0003(2) -0.0012(2) -0.0058(2) Ni1 0.0365(11) 0.0412(12) 0.0332(10) 0.0002(9) -0.0010(9) -0.0116(9) Ni2 0.0406(9) 0.0683(12) 0.0680(11) 0.0006(9) -0.0023(8) -0.0225(9) Ni3 0.0605(11) 0.0612(11) 0.0416(9) 0.0071(8) -0.0122(8) -0.0129(9) Ni4 0.0670(12) 0.0398(9) 0.0629(11) 0.0009(8) -0.0054(9) -0.0165(9) Ni5 0.0623(11) 0.0626(11) 0.0445(9) -0.0093(8) 0.0141(8) -0.0123(9) W1' 0.0656(4) 0.0588(4) 0.0438(3) 0.0045(3) -0.0031(3) -0.0033(3) W2' 0.0598(3) 0.0606(4) 0.0392(3) -0.0102(2) 0.0109(2) -0.0192(3) W3' 0.0612(4) 0.0865(5) 0.0609(4) -0.0028(3) 0.0137(3) -0.0414(4) Ni1' 0.0401(12) 0.0454(12) 0.0318(10) -0.0024(9) 0.0050(9) -0.0130(10) Ni2' 0.0580(11) 0.0896(15) 0.0595(11) -0.0051(10) -0.0065(9) -0.0245(11) Ni3' 0.1073(17) 0.0537(11) 0.0615(11) -0.0047(9) 0.0133(11) -0.0343(12) Ni4' 0.0775(13) 0.0755(13) 0.0476(10) 0.0081(9) 0.0110(9) -0.0241(11) Ni5' 0.0516(11) 0.0920(15) 0.0629(12) -0.0087(11) 0.0107(9) -0.0096(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C18 2.09(2) . ? W1 C16 2.11(2) . ? W1 C12 2.112(15) . ? W1 C13 2.127(14) . ? W1 C17 2.15(2) . ? W1 C15 2.147(14) . ? W1 C14 2.144(14) . ? W1 N11 2.175(13) . ? W2 C26 2.11(2) . ? W2 C28 2.112(18) . ? W2 C27 2.126(19) . ? W2 C22 2.136(14) . ? W2 C23 2.142(14) . ? W2 C24 2.145(14) . ? W2 C25 2.148(14) . ? W2 N21 2.164(13) . ? W3 C38 2.07(2) . ? W3 C37 2.10(2) . ? W3 C36 2.11(2) . ? W3 C32 2.131(15) . ? W3 C35 2.133(14) . ? W3 C33 2.147(14) . ? W3 C34 2.156(14) . ? W3 N31 2.208(13) . ? Ni1 C31 2.029(10) . ? Ni1 C31 2.029(10) 2_656 ? Ni1 C11 2.039(10) . ? Ni1 C11 2.039(10) 2_656 ? Ni1 C21 2.042(10) . ? Ni1 C21 2.042(10) 2_656 ? Ni2 N12 2.045(13) . ? Ni2 N32 2.056(13) . ? Ni2 N22 2.061(12) 2_656 ? Ni2 N212 2.060(12) . ? Ni2 N201 2.074(12) . ? Ni2 O215 2.122(11) . ? Ni3 N13 2.057(13) . ? Ni3 N33 2.058(12) 2_656 ? Ni3 N301 2.058(12) . ? Ni3 N312 2.078(12) . ? Ni3 N23 2.083(13) . ? Ni3 O315 2.121(11) . ? Ni4 N34 2.052(13) . ? Ni4 N401 2.056(13) . ? Ni4 N412 2.074(12) . ? Ni4 N14 2.077(12) 2_656 ? Ni4 N24 2.082(12) . ? Ni4 O415 2.124(11) . ? Ni5 N25 2.045(12) . ? Ni5 N35 2.048(12) . ? Ni5 N512 2.077(13) . ? Ni5 N501 2.077(12) . ? Ni5 N15 2.095(13) . ? Ni5 O515 2.114(11) . ? C11 N11 1.136(15) . ? C12 N12 1.167(17) . ? C13 N13 1.168(16) . ? C14 N14 1.161(16) . ? N14 Ni4 2.077(12) 2_656 ? C15 N15 1.132(16) . ? C16 N16 1.21(3) . ? C17 N17 1.18(2) . ? C18 N18 1.21(3) . ? C21 N21 1.150(14) . ? C22 N22 1.147(16) . ? N22 Ni2 2.061(12) 2_656 ? C23 N23 1.168(16) . ? C24 N24 1.175(16) . ? C25 N25 1.153(16) . ? C26 N26 1.17(3) . ? C27 N27 1.19(2) . ? C28 N28 1.18(2) . ? C31 N31 1.101(14) . ? C32 N32 1.172(17) . ? C33 N33 1.149(16) . ? N33 Ni3 2.058(12) 2_656 ? C34 N34 1.135(16) . ? C35 N35 1.156(16) . ? C36 N36 1.17(3) . ? C37 N37 1.20(3) . ? C38 N38 1.18(2) . ? N201 C202 1.345(19) . ? N201 C206 1.353(18) . ? C202 C203 1.38(2) . ? C202 H202 0.9300 . ? C203 C204 1.36(2) . ? C203 C213 1.50(3) . ? C204 C205 1.29(2) . ? C204 H204 0.9300 . ? C205 C206 1.36(2) . ? C205 H205 0.9300 . ? C206 C207 1.46(2) . ? C207 N212 1.357(19) . ? C207 C208 1.42(2) . ? C208 C209 1.36(2) . ? C208 H208 0.9300 . ? C209 C210 1.36(2) . ? C209 H209 0.9300 . ? C210 C211 1.41(2) . ? C210 C214 1.52(3) . ? C211 N212 1.313(18) . ? C211 H211 0.9300 . ? C213 H21A 0.9600 . ? C213 H21B 0.9600 . ? C213 H21C 0.9600 . ? C214 H21D 0.9600 . ? C214 H21E 0.9600 . ? C214 H21F 0.9600 . ? N301 C302 1.338(19) . ? N301 C306 1.340(18) . ? C302 C303 1.39(2) . ? C302 H302 0.9300 . ? C303 C304 1.36(3) . ? C303 C313 1.50(3) . ? C304 C305 1.32(3) . ? C304 H304 0.9300 . ? C305 C306 1.43(2) . ? C305 H305 0.9300 . ? C306 C307 1.47(2) . ? C307 N312 1.318(18) . ? C307 C308 1.40(2) . ? C308 C309 1.34(3) . ? C308 H308 0.9300 . ? C309 C310 1.36(3) . ? C309 H309 0.9300 . ? C310 C311 1.44(2) . ? C310 C314 1.52(3) . ? C311 N312 1.31(2) . ? C311 H311 0.9300 . ? C313 H31A 0.9600 . ? C313 H31B 0.9600 . ? C313 H31C 0.9600 . ? C314 H31D 0.9600 . ? C314 H31E 0.9600 . ? C314 H31F 0.9600 . ? O315 C316 1.44(3) . ? C316 C317 1.45(5) . ? N401 C402 1.301(19) . ? N401 C406 1.352(19) . ? C402 C403 1.42(2) . ? C402 H402 0.9300 . ? C403 C404 1.38(2) . ? C403 C413 1.54(3) . ? C404 C405 1.38(2) . ? C404 H404 0.9300 . ? C405 C406 1.37(2) . ? C405 H405 0.9300 . ? C406 C407 1.41(2) . ? C407 N412 1.351(19) . ? C407 C408 1.44(2) . ? C408 C409 1.37(2) . ? C408 H408 0.9300 . ? C409 C410 1.40(3) . ? C409 H409 0.9300 . ? C410 C411 1.42(2) . ? C410 C414 1.48(3) . ? C411 N412 1.315(19) . ? C411 H411 0.9300 . ? C413 H41A 0.9600 . ? C413 H41B 0.9600 . ? C413 H41C 0.9600 . ? C414 H41D 0.9600 . ? C414 H41E 0.9600 . ? C414 H41F 0.9600 . ? N501 C502 1.32(2) . ? N501 C506 1.346(19) . ? C502 C503 1.45(3) . ? C502 H502 0.9300 . ? C503 C504 1.41(3) . ? C503 C513 1.47(3) . ? C504 C505 1.30(3) . ? C504 H504 0.9300 . ? C505 C506 1.40(2) . ? C505 H505 0.9300 . ? C506 C507 1.47(2) . ? C507 N512 1.347(19) . ? C507 C508 1.39(2) . ? C508 C509 1.33(3) . ? C508 H508 0.9300 . ? C509 C510 1.37(3) . ? C509 H509 0.9300 . ? C510 C511 1.42(2) . ? C510 C514 1.53(3) . ? C511 N512 1.308(19) . ? C511 H511 0.9300 . ? C513 H51A 0.9600 . ? C513 H51B 0.9600 . ? C513 H51C 0.9600 . ? C514 H51D 0.9600 . ? C514 H51E 0.9600 . ? C514 H51F 0.9600 . ? O515 C516 1.470(19) . ? C516 C517 1.45(2) . ? C516 H51G 0.9700 . ? C516 H51H 0.9700 . ? C517 H51I 0.9600 . ? C517 H51J 0.9600 . ? C517 H51K 0.9600 . ? W1' C17' 2.10(2) . ? W1' C14' 2.112(15) . ? W1' C11' 2.128(14) . ? W1' C18' 2.13(2) . ? W1' C16' 2.131(17) . ? W1' C12' 2.148(16) . ? W1' C15' 2.156(16) . ? W1' C13' 2.164(15) . ? W2' C27' 2.09(2) . ? W2' C28' 2.09(2) . ? W2' C26' 2.103(18) . ? W2' C22' 2.134(14) . ? W2' C23' 2.133(16) . ? W2' C25' 2.137(15) . ? W2' C21' 2.149(13) . ? W2' C24' 2.154(15) . ? W3' C37' 2.09(3) . ? W3' C36' 2.10(4) . ? W3' C32' 2.137(16) . ? W3' C31' 2.146(14) . ? W3' C35' 2.147(17) . ? W3' C34' 2.147(16) . ? W3' C38' 2.163(16) . ? W3' C33' 2.173(16) . ? Ni1' N21' 2.025(11) 2_565 ? Ni1' N21' 2.025(11) . ? Ni1' N11' 2.048(11) 2_565 ? Ni1' N11' 2.048(11) . ? Ni1' N31' 2.054(12) 2_565 ? Ni1' N31' 2.054(12) . ? Ni2' N32' 2.067(14) . ? Ni2' N612 2.072(14) . ? Ni2' N12' 2.085(14) . ? Ni2' N601 2.086(15) . ? Ni2' N22' 2.085(13) 2_565 ? Ni2' O615 2.142(13) . ? Ni3' N23' 2.047(14) . ? Ni3' N33' 2.053(15) 2_565 ? Ni3' N712 2.066(18) . ? Ni3' N701 2.071(13) . ? Ni3' N13' 2.075(14) . ? Ni3' N724 2.096(16) . ? Ni4' N812 2.053(14) . ? Ni4' N34' 2.071(14) . ? Ni4' N14' 2.082(13) 2_565 ? Ni4' N801 2.090(12) . ? Ni4' N24' 2.096(14) . ? Ni4' O815 2.135(14) . ? Ni5' N15' 2.047(14) . ? Ni5' N25' 2.042(14) . ? Ni5' N912 2.048(15) . ? Ni5' N35' 2.079(14) . ? Ni5' N901 2.083(14) . ? Ni5' O915 2.145(14) . ? C11' N11' 1.150(15) . ? C12' N12' 1.149(17) . ? C13' N13' 1.149(17) . ? C14' N14' 1.152(17) . ? N14' Ni4' 2.082(13) 2_565 ? C15' N15' 1.150(18) . ? C16' N16' 1.17(2) . ? C17' N17' 1.19(3) . ? C18' N18' 1.19(3) . ? C21' N21' 1.140(15) . ? C22' N22' 1.154(17) . ? N22' Ni2' 2.085(13) 2_565 ? C23' N23' 1.174(18) . ? C24' N24' 1.125(17) . ? C25' N25' 1.156(17) . ? C26' N26' 1.20(2) . ? C27' N27' 1.21(2) . ? C28' N28' 1.18(3) . ? C31' N31' 1.133(16) . ? C32' N32' 1.130(18) . ? C33' N33' 1.123(18) . ? N33' Ni3' 2.053(15) 2_565 ? C34' N34' 1.136(18) . ? C35' N35' 1.131(18) . ? C36' N36' 1.18(5) . ? C37' N37' 1.19(3) . ? C38' N38' 1.148(17) . ? N601 C602 1.31(2) . ? N601 C606 1.35(2) . ? C602 C603 1.44(3) . ? C602 H602 0.9300 . ? C603 C604 1.32(3) . ? C603 C613 1.59(3) . ? C604 C605 1.29(3) . ? C604 H604 0.9300 . ? C605 C606 1.44(3) . ? C605 H605 0.9300 . ? C606 C607 1.44(3) . ? C607 N612 1.32(2) . ? C607 C608 1.39(3) . ? C608 C609 1.28(3) . ? C608 H608 0.9300 . ? C609 C610 1.36(3) . ? C609 H609 0.9300 . ? C610 C611 1.42(3) . ? C610 C614 1.54(3) . ? C611 N612 1.31(2) . ? C611 H611 0.9300 . ? C613 H61A 0.9600 . ? C613 H61B 0.9600 . ? C613 H61C 0.9600 . ? C614 H61D 0.9600 . ? C614 H61E 0.9600 . ? C614 H61F 0.9600 . ? N801 C802 1.312(19) . ? N801 C806 1.35(2) . ? C802 C803 1.41(2) . ? C802 H802 0.9300 . ? C803 C804 1.37(3) . ? C803 C813 1.46(3) . ? C804 C805 1.39(3) . ? C804 H804 0.9300 . ? C805 C806 1.41(3) . ? C805 H805 0.9300 . ? C806 C807 1.39(2) . ? C807 N812 1.32(2) . ? C807 C808 1.41(3) . ? C808 C809 1.33(3) . ? C808 H808 0.9300 . ? C809 C810 1.41(3) . ? C809 H809 0.9300 . ? C810 C811 1.44(3) . ? C810 C814 1.52(3) . ? C811 N812 1.36(2) . ? C811 H811 0.9300 . ? C813 H81A 0.9600 . ? C813 H81B 0.9600 . ? C813 H81C 0.9600 . ? C814 H81D 0.9600 . ? C814 H81E 0.9600 . ? C814 H81F 0.9600 . ? N901 C902 1.30(2) . ? N901 C906 1.33(2) . ? C902 C903 1.41(3) . ? C902 H902 0.9300 . ? C903 C904 1.33(3) . ? C903 C913 1.53(3) . ? C904 C905 1.33(3) . ? C904 H904 0.9300 . ? C905 C906 1.45(3) . ? C905 H905 0.9300 . ? C906 C907 1.45(3) . ? C907 N912 1.35(2) . ? C907 C908 1.43(3) . ? C908 C909 1.37(3) . ? C908 H908 0.9300 . ? C909 C910 1.31(3) . ? C909 H909 0.9300 . ? C910 C914 1.47(3) . ? C910 C911 1.49(3) . ? C911 N912 1.30(2) . ? C911 H911 0.9300 . ? C913 H91A 0.9600 . ? C913 H91B 0.9600 . ? C913 H91C 0.9600 . ? C914 H91D 0.9600 . ? C914 H91E 0.9600 . ? C914 H91F 0.9600 . ? N701 C706 1.311(17) . ? N701 C715 1.331(17) . ? N701 C718 1.360(17) . ? N701 C702 1.370(17) . ? N712 C711 1.304(18) . ? N712 C707 1.364(17) . ? N724 C723 1.329(17) . ? N724 C719 1.377(17) . ? C704 C705 1.366(18) . ? C704 C716 1.370(18) . ? C704 C717 1.415(17) . ? C704 C703 1.419(18) . ? C702 C703 1.422(18) . ? C703 C713 1.54(2) . ? C705 C706 1.385(18) . ? C706 C707 1.465(18) . ? C707 C708 1.409(18) . ? C708 C709 1.393(18) . ? C709 C710 1.394(18) . ? C710 C711 1.414(18) . ? C710 C714 1.50(2) . ? C715 C716 1.403(18) . ? C716 C725 1.50(2) . ? C717 C718 1.403(18) . ? C718 C719 1.496(18) . ? C719 C720 1.409(18) . ? C720 C721 1.393(18) . ? C721 C722 1.399(18) . ? C722 C723 1.414(18) . ? C722 C726 1.503(18) . ? O2W O9W 1.60(6) 2_656 ? O7W O8W 1.11(6) 2_666 ? O8W O7W 1.11(6) 2_666 ? O9W O2W 1.60(6) 2_656 ? 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 C18 W1 C16 78.5(8) . . ? C18 W1 C12 145.3(7) . . ? C16 W1 C12 79.7(7) . . ? C18 W1 C13 70.2(7) . . ? C16 W1 C13 124.9(7) . . ? C12 W1 C13 144.2(5) . . ? C18 W1 C17 74.6(8) . . ? C16 W1 C17 70.8(8) . . ? C12 W1 C17 73.0(6) . . ? C13 W1 C17 135.9(6) . . ? C18 W1 C15 89.9(7) . . ? C16 W1 C15 143.0(7) . . ? C12 W1 C15 91.5(5) . . ? C13 W1 C15 82.0(5) . . ? C17 W1 C15 72.2(6) . . ? C18 W1 C14 110.4(7) . . ? C16 W1 C14 69.4(7) . . ? C12 W1 C14 86.3(5) . . ? C13 W1 C14 80.5(5) . . ? C17 W1 C14 137.7(6) . . ? C15 W1 C14 146.5(5) . . ? C18 W1 N11 140.4(7) . . ? C16 W1 N11 134.4(7) . . ? C12 W1 N11 72.6(5) . . ? C13 W1 N11 71.7(5) . . ? C17 W1 N11 130.3(6) . . ? C15 W1 N11 74.1(5) . . ? C14 W1 N11 73.3(5) . . ? C26 W2 C28 76.9(7) . . ? C26 W2 C27 73.4(7) . . ? C28 W2 C27 74.0(7) . . ? C26 W2 C22 83.0(6) . . ? C28 W2 C22 144.8(6) . . ? C27 W2 C22 72.7(6) . . ? C26 W2 C23 145.9(6) . . ? C28 W2 C23 86.3(6) . . ? C27 W2 C23 73.6(6) . . ? C22 W2 C23 94.9(5) . . ? C26 W2 C24 69.4(6) . . ? C28 W2 C24 113.3(6) . . ? C27 W2 C24 138.7(6) . . ? C22 W2 C24 85.4(5) . . ? C23 W2 C24 144.6(5) . . ? C26 W2 C25 118.5(7) . . ? C28 W2 C25 70.6(6) . . ? C27 W2 C25 137.9(6) . . ? C22 W2 C25 144.5(5) . . ? C23 W2 C25 82.1(5) . . ? C24 W2 C25 77.6(5) . . ? C26 W2 N21 136.2(6) . . ? C28 W2 N21 140.0(6) . . ? C27 W2 N21 129.1(6) . . ? C22 W2 N21 72.6(5) . . ? C23 W2 N21 73.6(5) . . ? C24 W2 N21 72.7(5) . . ? C25 W2 N21 72.6(5) . . ? C38 W3 C37 73.3(8) . . ? C38 W3 C36 71.4(8) . . ? C37 W3 C36 76.3(8) . . ? C38 W3 C32 139.3(7) . . ? C37 W3 C32 110.8(7) . . ? C36 W3 C32 70.6(7) . . ? C38 W3 C35 75.4(7) . . ? C37 W3 C35 145.8(7) . . ? C36 W3 C35 81.0(7) . . ? C32 W3 C35 84.7(5) . . ? C38 W3 C33 136.9(7) . . ? C37 W3 C33 72.3(7) . . ? C36 W3 C33 123.1(7) . . ? C32 W3 C33 78.0(5) . . ? C35 W3 C33 141.9(5) . . ? C38 W3 C34 72.3(7) . . ? C37 W3 C34 89.7(7) . . ? C36 W3 C34 143.5(7) . . ? C32 W3 C34 145.3(5) . . ? C35 W3 C34 93.7(5) . . ? C33 W3 C34 82.4(5) . . ? C38 W3 N31 129.1(6) . . ? C37 W3 N31 141.7(7) . . ? C36 W3 N31 136.1(7) . . ? C32 W3 N31 73.7(5) . . ? C35 W3 N31 70.9(5) . . ? C33 W3 N31 71.7(5) . . ? C34 W3 N31 73.0(5) . . ? C31 Ni1 C31 180.000(2) . 2_656 ? C31 Ni1 C11 89.2(4) . . ? C31 Ni1 C11 90.8(4) 2_656 . ? C31 Ni1 C11 90.8(4) . 2_656 ? C31 Ni1 C11 89.2(4) 2_656 2_656 ? C11 Ni1 C11 180.0(4) . 2_656 ? C31 Ni1 C21 90.4(4) . . ? C31 Ni1 C21 89.6(4) 2_656 . ? C11 Ni1 C21 90.0(4) . . ? C11 Ni1 C21 90.0(4) 2_656 . ? C31 Ni1 C21 89.6(4) . 2_656 ? C31 Ni1 C21 90.4(4) 2_656 2_656 ? C11 Ni1 C21 90.0(4) . 2_656 ? C11 Ni1 C21 90.0(4) 2_656 2_656 ? C21 Ni1 C21 180.000(2) . 2_656 ? N12 Ni2 N32 92.7(5) . . ? N12 Ni2 N22 90.0(5) . 2_656 ? N32 Ni2 N22 91.6(5) . 2_656 ? N12 Ni2 N212 174.1(5) . . ? N32 Ni2 N212 88.4(5) . . ? N22 Ni2 N212 95.8(5) 2_656 . ? N12 Ni2 N201 94.8(5) . . ? N32 Ni2 N201 89.4(5) . . ? N22 Ni2 N201 175.0(5) 2_656 . ? N212 Ni2 N201 79.3(5) . . ? N12 Ni2 O215 89.8(5) . . ? N32 Ni2 O215 176.4(5) . . ? N22 Ni2 O215 91.1(5) 2_656 . ? N212 Ni2 O215 88.9(5) . . ? N201 Ni2 O215 87.8(5) . . ? N13 Ni3 N33 92.3(5) . 2_656 ? N13 Ni3 N301 170.3(5) . . ? N33 Ni3 N301 94.0(5) 2_656 . ? N13 Ni3 N312 94.6(5) . . ? N33 Ni3 N312 171.5(5) 2_656 . ? N301 Ni3 N312 78.6(5) . . ? N13 Ni3 N23 92.0(5) . . ? N33 Ni3 N23 92.4(5) 2_656 . ? N301 Ni3 N23 95.1(5) . . ? N312 Ni3 N23 92.4(5) . . ? N13 Ni3 O315 86.5(5) . . ? N33 Ni3 O315 88.2(4) 2_656 . ? N301 Ni3 O315 86.3(4) . . ? N312 Ni3 O315 87.2(4) . . ? N23 Ni3 O315 178.4(4) . . ? N34 Ni4 N401 173.6(5) . . ? N34 Ni4 N412 95.2(5) . . ? N401 Ni4 N412 78.4(5) . . ? N34 Ni4 N14 91.0(5) . 2_656 ? N401 Ni4 N14 95.2(5) . 2_656 ? N412 Ni4 N14 172.4(5) . 2_656 ? N34 Ni4 N24 93.5(5) . . ? N401 Ni4 N24 87.3(5) . . ? N412 Ni4 N24 91.6(5) . . ? N14 Ni4 N24 92.3(5) 2_656 . ? N34 Ni4 O415 91.2(4) . . ? N401 Ni4 O415 87.8(5) . . ? N412 Ni4 O415 86.3(4) . . ? N14 Ni4 O415 89.3(4) 2_656 . ? N24 Ni4 O415 175.0(4) . . ? N25 Ni5 N35 92.4(5) . . ? N25 Ni5 N512 170.8(5) . . ? N35 Ni5 N512 93.3(5) . . ? N25 Ni5 N501 94.5(5) . . ? N35 Ni5 N501 172.4(5) . . ? N512 Ni5 N501 79.5(5) . . ? N25 Ni5 N15 91.7(5) . . ? N35 Ni5 N15 92.2(5) . . ? N512 Ni5 N15 95.3(5) . . ? N501 Ni5 N15 91.0(5) . . ? N25 Ni5 O515 86.6(4) . . ? N35 Ni5 O515 89.7(4) . . ? N512 Ni5 O515 86.2(5) . . ? N501 Ni5 O515 87.4(5) . . ? N15 Ni5 O515 177.5(5) . . ? N11 C11 Ni1 173.7(10) . . ? C11 N11 W1 177.4(11) . . ? N12 C12 W1 176.7(13) . . ? C12 N12 Ni2 173.4(13) . . ? N13 C13 W1 177.4(13) . . ? C13 N13 Ni3 170.9(12) . . ? N14 C14 W1 175.8(12) . . ? C14 N14 Ni4 178.2(12) . 2_656 ? N15 C15 W1 175.0(13) . . ? C15 N15 Ni5 170.4(12) . . ? N16 C16 W1 177(2) . . ? N17 C17 W1 177.7(19) . . ? N18 C18 W1 178(2) . . ? N21 C21 Ni1 171.0(10) . . ? C21 N21 W2 175.8(11) . . ? N22 C22 W2 174.3(13) . . ? C22 N22 Ni2 167.7(12) . 2_656 ? N23 C23 W2 175.1(12) . . ? C23 N23 Ni3 167.7(11) . . ? N24 C24 W2 177.6(12) . . ? C24 N24 Ni4 167.7(11) . . ? N25 C25 W2 178.5(13) . . ? C25 N25 Ni5 172.2(12) . . ? N26 C26 W2 177(2) . . ? N27 C27 W2 178.8(18) . . ? N28 C28 W2 177.9(16) . . ? N31 C31 Ni1 166.7(11) . . ? C31 N31 W3 178.2(12) . . ? N32 C32 W3 177.9(12) . . ? C32 N32 Ni2 168.5(12) . . ? N33 C33 W3 178.3(13) . . ? C33 N33 Ni3 174.5(12) . 2_656 ? N34 C34 W3 173.6(13) . . ? C34 N34 Ni4 166.1(12) . . ? N35 C35 W3 177.2(12) . . ? C35 N35 Ni5 175.4(12) . . ? N36 C36 W3 173(2) . . ? N37 C37 W3 175(2) . . ? N38 C38 W3 177(2) . . ? C202 N201 C206 117.1(14) . . ? C202 N201 Ni2 126.3(11) . . ? C206 N201 Ni2 116.5(10) . . ? N201 C202 C203 123.8(16) . . ? N201 C202 H202 118.1 . . ? C203 C202 H202 118.1 . . ? C204 C203 C202 115.0(17) . . ? C204 C203 C213 125.5(17) . . ? C202 C203 C213 119.4(17) . . ? C205 C204 C203 122.4(19) . . ? C205 C204 H204 118.8 . . ? C203 C204 H204 118.8 . . ? C204 C205 C206 121.8(18) . . ? C204 C205 H205 119.1 . . ? C206 C205 H205 119.1 . . ? N201 C206 C205 119.7(15) . . ? N201 C206 C207 111.9(14) . . ? C205 C206 C207 128.4(16) . . ? N212 C207 C208 118.4(15) . . ? N212 C207 C206 119.5(14) . . ? C208 C207 C206 122.1(15) . . ? C209 C208 C207 120.1(18) . . ? C209 C208 H208 120.0 . . ? C207 C208 H208 120.0 . . ? C208 C209 C210 120.5(19) . . ? C208 C209 H209 119.8 . . ? C210 C209 H209 119.8 . . ? C209 C210 C211 117.9(18) . . ? C209 C210 C214 124.1(18) . . ? C211 C210 C214 118.0(17) . . ? N212 C211 C210 122.2(16) . . ? N212 C211 H211 118.9 . . ? C210 C211 H211 118.9 . . ? C211 N212 C207 120.9(14) . . ? C211 N212 Ni2 126.2(11) . . ? C207 N212 Ni2 112.6(10) . . ? C203 C213 H21A 109.5 . . ? C203 C213 H21B 109.5 . . ? H21A C213 H21B 109.5 . . ? C203 C213 H21C 109.5 . . ? H21A C213 H21C 109.5 . . ? H21B C213 H21C 109.5 . . ? C210 C214 H21D 109.5 . . ? C210 C214 H21E 109.5 . . ? H21D C214 H21E 109.5 . . ? C210 C214 H21F 109.5 . . ? H21D C214 H21F 109.5 . . ? H21E C214 H21F 109.5 . . ? C302 N301 C306 118.5(14) . . ? C302 N301 Ni3 125.8(11) . . ? C306 N301 Ni3 115.1(10) . . ? N301 C302 C303 123.9(17) . . ? N301 C302 H302 118.0 . . ? C303 C302 H302 118.0 . . ? C304 C303 C302 115.3(19) . . ? C304 C303 C313 127(2) . . ? C302 C303 C313 117.9(18) . . ? C305 C304 C303 124(2) . . ? C305 C304 H304 117.9 . . ? C303 C304 H304 117.9 . . ? C304 C305 C306 117.4(19) . . ? C304 C305 H305 121.3 . . ? C306 C305 H305 121.3 . . ? N301 C306 C305 120.5(15) . . ? N301 C306 C307 115.3(14) . . ? C305 C306 C307 124.2(15) . . ? N312 C307 C308 123.2(16) . . ? N312 C307 C306 115.7(14) . . ? C308 C307 C306 121.1(15) . . ? C309 C308 C307 113.7(19) . . ? C309 C308 H308 123.2 . . ? C307 C308 H308 123.2 . . ? C308 C309 C310 128(2) . . ? C308 C309 H309 116.1 . . ? C310 C309 H309 116.1 . . ? C309 C310 C311 113(2) . . ? C309 C310 C314 130(2) . . ? C311 C310 C314 117(2) . . ? N312 C311 C310 122.1(17) . . ? N312 C311 H311 118.9 . . ? C310 C311 H311 118.9 . . ? C311 N312 C307 120.4(14) . . ? C311 N312 Ni3 124.3(11) . . ? C307 N312 Ni3 115.1(10) . . ? C303 C313 H31A 109.5 . . ? C303 C313 H31B 109.5 . . ? H31A C313 H31B 109.5 . . ? C303 C313 H31C 109.5 . . ? H31A C313 H31C 109.5 . . ? H31B C313 H31C 109.5 . . ? C310 C314 H31D 109.5 . . ? C310 C314 H31E 109.5 . . ? H31D C314 H31E 109.5 . . ? C310 C314 H31F 109.5 . . ? H31D C314 H31F 109.5 . . ? H31E C314 H31F 109.5 . . ? C316 O315 Ni3 122.1(13) . . ? O315 C316 C317 114(3) . . ? C402 N401 C406 120.1(15) . . ? C402 N401 Ni4 125.2(11) . . ? C406 N401 Ni4 114.7(11) . . ? N401 C402 C403 124.4(17) . . ? N401 C402 H402 117.8 . . ? C403 C402 H402 117.8 . . ? C404 C403 C402 115.2(18) . . ? C404 C403 C413 123.1(19) . . ? C402 C403 C413 121.6(18) . . ? C405 C404 C403 119.3(19) . . ? C405 C404 H404 120.4 . . ? C403 C404 H404 120.4 . . ? C404 C405 C406 122.1(18) . . ? C404 C405 H405 118.9 . . ? C406 C405 H405 118.9 . . ? N401 C406 C405 118.7(16) . . ? N401 C406 C407 116.3(15) . . ? C405 C406 C407 124.8(16) . . ? N412 C407 C406 116.4(15) . . ? N412 C407 C408 120.4(15) . . ? C406 C407 C408 123.1(16) . . ? C409 C408 C407 116.8(18) . . ? C409 C408 H408 121.6 . . ? C407 C408 H408 121.6 . . ? C408 C409 C410 124(2) . . ? C408 C409 H409 118.2 . . ? C410 C409 H409 118.2 . . ? C409 C410 C411 114.2(18) . . ? C409 C410 C414 122.1(19) . . ? C411 C410 C414 123.7(18) . . ? N412 C411 C410 124.9(17) . . ? N412 C411 H411 117.6 . . ? C410 C411 H411 117.6 . . ? C411 N412 C407 120.1(14) . . ? C411 N412 Ni4 125.9(11) . . ? C407 N412 Ni4 114.0(10) . . ? C403 C413 H41A 109.5 . . ? C403 C413 H41B 109.5 . . ? H41A C413 H41B 109.5 . . ? C403 C413 H41C 109.5 . . ? H41A C413 H41C 109.5 . . ? H41B C413 H41C 109.5 . . ? C410 C414 H41D 109.5 . . ? C410 C414 H41E 109.5 . . ? H41D C414 H41E 109.5 . . ? C410 C414 H41F 109.5 . . ? H41D C414 H41F 109.5 . . ? H41E C414 H41F 109.5 . . ? C502 N501 C506 121.1(15) . . ? C502 N501 Ni5 125.0(12) . . ? C506 N501 Ni5 113.8(11) . . ? N501 C502 C503 123.1(18) . . ? N501 C502 H502 118.4 . . ? C503 C502 H502 118.4 . . ? C504 C503 C502 112(2) . . ? C504 C503 C513 127(2) . . ? C502 C503 C513 121(2) . . ? C505 C504 C503 125(2) . . ? C505 C504 H504 117.6 . . ? C503 C504 H504 117.6 . . ? C504 C505 C506 120(2) . . ? C504 C505 H505 120.1 . . ? C506 C505 H505 120.1 . . ? N501 C506 C505 119.0(17) . . ? N501 C506 C507 116.7(15) . . ? C505 C506 C507 124.3(17) . . ? N512 C507 C508 120.4(15) . . ? N512 C507 C506 115.5(14) . . ? C508 C507 C506 124.1(16) . . ? C509 C508 C507 119(2) . . ? C509 C508 H508 120.6 . . ? C507 C508 H508 120.6 . . ? C508 C509 C510 123(2) . . ? C508 C509 H509 118.7 . . ? C510 C509 H509 118.7 . . ? C509 C510 C511 115.5(19) . . ? C509 C510 C514 125(2) . . ? C511 C510 C514 119.2(18) . . ? N512 C511 C510 122.4(17) . . ? N512 C511 H511 118.8 . . ? C510 C511 H511 118.8 . . ? C511 N512 C507 120.0(14) . . ? C511 N512 Ni5 125.1(11) . . ? C507 N512 Ni5 114.4(10) . . ? C503 C513 H51A 109.5 . . ? C503 C513 H51B 109.5 . . ? H51A C513 H51B 109.5 . . ? C503 C513 H51C 109.5 . . ? H51A C513 H51C 109.5 . . ? H51B C513 H51C 109.5 . . ? C510 C514 H51D 109.5 . . ? C510 C514 H51E 109.5 . . ? H51D C514 H51E 109.5 . . ? C510 C514 H51F 109.5 . . ? H51D C514 H51F 109.5 . . ? H51E C514 H51F 109.5 . . ? C516 O515 Ni5 125.3(9) . . ? C517 C516 O515 110.3(15) . . ? C517 C516 H51G 109.6 . . ? O515 C516 H51G 109.6 . . ? C517 C516 H51H 109.6 . . ? O515 C516 H51H 109.6 . . ? H51G C516 H51H 108.1 . . ? C516 C517 H51I 109.5 . . ? C516 C517 H51J 109.5 . . ? H51I C517 H51J 109.5 . . ? C516 C517 H51K 109.5 . . ? H51I C517 H51K 109.5 . . ? H51J C517 H51K 109.5 . . ? C17' W1' C14' 80.6(7) . . ? C17' W1' C11' 136.6(7) . . ? C14' W1' C11' 73.7(5) . . ? C17' W1' C18' 76.3(8) . . ? C14' W1' C18' 144.2(7) . . ? C11' W1' C18' 140.3(7) . . ? C17' W1' C16' 73.0(7) . . ? C14' W1' C16' 73.1(6) . . ? C11' W1' C16' 128.8(6) . . ? C18' W1' C16' 74.1(7) . . ? C17' W1' C12' 144.3(7) . . ? C14' W1' C12' 95.0(6) . . ? C11' W1' C12' 73.4(5) . . ? C18' W1' C12' 88.2(7) . . ? C16' W1' C12' 71.8(6) . . ? C17' W1' C15' 120.7(7) . . ? C14' W1' C15' 145.3(6) . . ? C11' W1' C15' 72.4(5) . . ? C18' W1' C15' 70.4(7) . . ? C16' W1' C15' 136.3(6) . . ? C12' W1' C15' 82.2(6) . . ? C17' W1' C13' 70.3(7) . . ? C14' W1' C13' 85.5(5) . . ? C11' W1' C13' 73.3(5) . . ? C18' W1' C13' 111.4(7) . . ? C16' W1' C13' 140.0(6) . . ? C12' W1' C13' 145.1(6) . . ? C15' W1' C13' 78.0(6) . . ? C27' W2' C28' 76.4(8) . . ? C27' W2' C26' 70.7(7) . . ? C28' W2' C26' 76.0(8) . . ? C27' W2' C22' 126.1(7) . . ? C28' W2' C22' 69.6(7) . . ? C26' W2' C22' 134.3(6) . . ? C27' W2' C23' 69.8(7) . . ? C28' W2' C23' 104.3(7) . . ? C26' W2' C23' 139.1(6) . . ? C22' W2' C23' 79.6(6) . . ? C27' W2' C25' 78.4(7) . . ? C28' W2' C25' 146.0(7) . . ? C26' W2' C25' 74.4(6) . . ? C22' W2' C25' 144.4(5) . . ? C23' W2' C25' 87.7(6) . . ? C27' W2' C21' 133.0(7) . . ? C28' W2' C21' 141.0(7) . . ? C26' W2' C21' 132.1(6) . . ? C22' W2' C21' 71.6(5) . . ? C23' W2' C21' 72.7(5) . . ? C25' W2' C21' 72.8(5) . . ? C27' W2' C24' 143.3(7) . . ? C28' W2' C24' 94.2(7) . . ? C26' W2' C24' 72.6(6) . . ? C22' W2' C24' 80.7(5) . . ? C23' W2' C24' 146.1(6) . . ? C25' W2' C24' 92.6(5) . . ? C21' W2' C24' 75.0(5) . . ? C37' W3' C36' 71.8(12) . . ? C37' W3' C32' 135.8(8) . . ? C36' W3' C32' 68.2(11) . . ? C37' W3' C31' 136.1(8) . . ? C36' W3' C31' 137.6(11) . . ? C32' W3' C31' 71.9(5) . . ? C37' W3' C35' 75.3(8) . . ? C36' W3' C35' 88.4(11) . . ? C32' W3' C35' 85.5(6) . . ? C31' W3' C35' 74.6(6) . . ? C37' W3' C34' 75.5(8) . . ? C36' W3' C34' 146.7(11) . . ? C32' W3' C34' 144.7(6) . . ? C31' W3' C34' 73.0(5) . . ? C35' W3' C34' 89.4(6) . . ? C37' W3' C38' 67.5(16) . . ? C36' W3' C38' 78.6(17) . . ? C32' W3' C38' 120.2(15) . . ? C31' W3' C38' 136.0(14) . . ? C35' W3' C38' 142.8(15) . . ? C34' W3' C38' 83.3(14) . . ? C37' W3' C33' 135.7(8) . . ? C36' W3' C33' 114.1(11) . . ? C32' W3' C33' 79.2(6) . . ? C31' W3' C33' 70.7(5) . . ? C35' W3' C33' 144.9(6) . . ? C34' W3' C33' 85.4(6) . . ? C38' W3' C33' 70.9(15) . . ? N21' Ni1' N21' 180.0(6) 2_565 . ? N21' Ni1' N11' 90.9(4) 2_565 2_565 ? N21' Ni1' N11' 89.1(4) . 2_565 ? N21' Ni1' N11' 89.1(4) 2_565 . ? N21' Ni1' N11' 90.9(4) . . ? N11' Ni1' N11' 180.0(7) 2_565 . ? N21' Ni1' N31' 87.5(4) 2_565 2_565 ? N21' Ni1' N31' 92.5(4) . 2_565 ? N11' Ni1' N31' 90.3(4) 2_565 2_565 ? N11' Ni1' N31' 89.7(4) . 2_565 ? N21' Ni1' N31' 92.5(4) 2_565 . ? N21' Ni1' N31' 87.5(4) . . ? N11' Ni1' N31' 89.7(4) 2_565 . ? N11' Ni1' N31' 90.3(4) . . ? N31' Ni1' N31' 180.0(8) 2_565 . ? N32' Ni2' N612 172.7(6) . . ? N32' Ni2' N12' 91.5(5) . . ? N612 Ni2' N12' 93.4(5) . . ? N32' Ni2' N601 95.7(6) . . ? N612 Ni2' N601 78.5(6) . . ? N12' Ni2' N601 94.3(5) . . ? N32' Ni2' N22' 92.0(5) . 2_565 ? N612 Ni2' N22' 93.2(5) . 2_565 ? N12' Ni2' N22' 92.3(5) . 2_565 ? N601 Ni2' N22' 169.7(5) . 2_565 ? N32' Ni2' O615 88.7(5) . . ? N612 Ni2' O615 86.4(5) . . ? N12' Ni2' O615 179.8(5) . . ? N601 Ni2' O615 85.7(5) . . ? N22' Ni2' O615 87.7(5) 2_565 . ? N23' Ni3' N33' 91.5(6) . 2_565 ? N23' Ni3' N712 90.8(7) . . ? N33' Ni3' N712 90.1(6) 2_565 . ? N23' Ni3' N701 173.8(5) . . ? N33' Ni3' N701 91.0(5) 2_565 . ? N712 Ni3' N701 83.5(6) . . ? N23' Ni3' N13' 93.1(5) . . ? N33' Ni3' N13' 93.8(5) 2_565 . ? N712 Ni3' N13' 174.4(6) . . ? N701 Ni3' N13' 92.3(5) . . ? N23' Ni3' N724 92.4(6) . . ? N33' Ni3' N724 173.0(6) 2_565 . ? N712 Ni3' N724 84.1(6) . . ? N701 Ni3' N724 84.6(6) . . ? N13' Ni3' N724 91.8(5) . . ? N812 Ni4' N34' 95.5(5) . . ? N812 Ni4' N14' 173.3(5) . 2_565 ? N34' Ni4' N14' 89.8(5) . 2_565 ? N812 Ni4' N801 78.5(5) . . ? N34' Ni4' N801 173.2(5) . . ? N14' Ni4' N801 96.0(5) 2_565 . ? N812 Ni4' N24' 92.0(5) . . ? N34' Ni4' N24' 91.6(5) . . ? N14' Ni4' N24' 91.9(5) 2_565 . ? N801 Ni4' N24' 91.7(5) . . ? N812 Ni4' O815 86.6(5) . . ? N34' Ni4' O815 88.8(5) . . ? N14' Ni4' O815 89.4(5) 2_565 . ? N801 Ni4' O815 87.7(5) . . ? N24' Ni4' O815 178.6(5) . . ? N15' Ni5' N25' 90.9(5) . . ? N15' Ni5' N912 94.7(6) . . ? N25' Ni5' N912 174.3(6) . . ? N15' Ni5' N35' 92.0(5) . . ? N25' Ni5' N35' 91.4(5) . . ? N912 Ni5' N35' 89.3(6) . . ? N15' Ni5' N901 173.2(6) . . ? N25' Ni5' N901 94.6(5) . . ? N912 Ni5' N901 79.8(6) . . ? N35' Ni5' N901 91.8(5) . . ? N15' Ni5' O915 88.5(5) . . ? N25' Ni5' O915 90.4(5) . . ? N912 Ni5' O915 88.9(6) . . ? N35' Ni5' O915 178.1(5) . . ? N901 Ni5' O915 87.5(5) . . ? N11' C11' W1' 177.0(12) . . ? C11' N11' Ni1' 174.8(11) . . ? N12' C12' W1' 174.9(13) . . ? C12' N12' Ni2' 171.3(13) . . ? N13' C13' W1' 175.6(13) . . ? C13' N13' Ni3' 176.5(13) . . ? N14' C14' W1' 176.9(13) . . ? C14' N14' Ni4' 172.5(13) . 2_565 ? N15' C15' W1' 179.4(17) . . ? C15' N15' Ni5' 174.4(14) . . ? N16' C16' W1' 177.9(17) . . ? N17' C17' W1' 178(2) . . ? N18' C18' W1' 178(2) . . ? N21' C21' W2' 176.6(12) . . ? C21' N21' Ni1' 172.1(11) . . ? N22' C22' W2' 179.1(14) . . ? C22' N22' Ni2' 175.1(13) . 2_565 ? N23' C23' W2' 177.1(14) . . ? C23' N23' Ni3' 173.1(13) . . ? N24' C24' W2' 175.1(14) . . ? C24' N24' Ni4' 175.9(13) . . ? N25' C25' W2' 176.1(14) . . ? C25' N25' Ni5' 175.1(13) . . ? N26' C26' W2' 176.5(17) . . ? N27' C27' W2' 174.0(19) . . ? N28' C28' W2' 178(2) . . ? N31' C31' W3' 177.6(12) . . ? C31' N31' Ni1' 177.6(11) . . ? N32' C32' W3' 177.5(15) . . ? C32' N32' Ni2' 177.9(15) . . ? N33' C33' W3' 176.7(15) . . ? C33' N33' Ni3' 178.5(15) . 2_565 ? N34' C34' W3' 177.1(14) . . ? C34' N34' Ni4' 179.3(16) . . ? N35' C35' W3' 174.9(15) . . ? C35' N35' Ni5' 175.5(14) . . ? N36' C36' W3' 166(4) . . ? N37' C37' W3' 174(3) . . ? N38' C38' W3' 170(6) . . ? C602 N601 C606 121.7(18) . . ? C602 N601 Ni2' 125.2(14) . . ? C606 N601 Ni2' 112.5(13) . . ? N601 C602 C603 123(2) . . ? N601 C602 H602 118.6 . . ? C603 C602 H602 118.6 . . ? C604 C603 C602 114(2) . . ? C604 C603 C613 129(3) . . ? C602 C603 C613 116(2) . . ? C605 C604 C603 124(3) . . ? C605 C604 H604 117.8 . . ? C603 C604 H604 117.8 . . ? C604 C605 C606 122(3) . . ? C604 C605 H605 119.1 . . ? C606 C605 H605 119.1 . . ? N601 C606 C605 115(2) . . ? N601 C606 C607 117.5(19) . . ? C605 C606 C607 128(2) . . ? N612 C607 C608 120(2) . . ? N612 C607 C606 115.1(18) . . ? C608 C607 C606 125(2) . . ? C609 C608 C607 120(3) . . ? C609 C608 H608 120.1 . . ? C607 C608 H608 120.1 . . ? C608 C609 C610 124(3) . . ? C608 C609 H609 118.0 . . ? C610 C609 H609 118.0 . . ? C609 C610 C611 113(2) . . ? C609 C610 C614 129(2) . . ? C611 C610 C614 117(2) . . ? N612 C611 C610 124(2) . . ? N612 C611 H611 118.2 . . ? C610 C611 H611 118.2 . . ? C611 N612 C607 118.7(16) . . ? C611 N612 Ni2' 125.3(13) . . ? C607 N612 Ni2' 115.8(12) . . ? C603 C613 H61A 109.5 . . ? C603 C613 H61B 109.5 . . ? H61A C613 H61B 109.5 . . ? C603 C613 H61C 109.5 . . ? H61A C613 H61C 109.5 . . ? H61B C613 H61C 109.5 . . ? C610 C614 H61D 109.5 . . ? C610 C614 H61E 109.5 . . ? H61D C614 H61E 109.5 . . ? C610 C614 H61F 109.5 . . ? H61D C614 H61F 109.5 . . ? H61E C614 H61F 109.5 . . ? C802 N801 C806 121.9(15) . . ? C802 N801 Ni4' 126.0(11) . . ? C806 N801 Ni4' 112.0(11) . . ? N801 C802 C803 124.7(17) . . ? N801 C802 H802 117.7 . . ? C803 C802 H802 117.7 . . ? C804 C803 C802 113.1(19) . . ? C804 C803 C813 123(2) . . ? C802 C803 C813 124.1(18) . . ? C803 C804 C805 124(2) . . ? C803 C804 H804 118.0 . . ? C805 C804 H804 118.0 . . ? C804 C805 C806 119(2) . . ? C804 C805 H805 120.7 . . ? C806 C805 H805 120.7 . . ? N801 C806 C807 117.5(16) . . ? N801 C806 C805 117.6(17) . . ? C807 C806 C805 125.0(18) . . ? N812 C807 C806 117.6(17) . . ? N812 C807 C808 116.7(19) . . ? C806 C807 C808 125.7(19) . . ? C809 C808 C807 124(3) . . ? C809 C808 H808 118.2 . . ? C807 C808 H808 118.2 . . ? C808 C809 C810 122(3) . . ? C808 C809 H809 119.2 . . ? C810 C809 H809 119.2 . . ? C809 C810 C811 112(2) . . ? C809 C810 C814 125(2) . . ? C811 C810 C814 123(2) . . ? N812 C811 C810 124.7(19) . . ? N812 C811 H811 117.6 . . ? C810 C811 H811 117.6 . . ? C807 N812 C811 121.1(16) . . ? C807 N812 Ni4' 114.4(12) . . ? C811 N812 Ni4' 124.5(12) . . ? C803 C813 H81A 109.5 . . ? C803 C813 H81B 109.5 . . ? H81A C813 H81B 109.5 . . ? C803 C813 H81C 109.5 . . ? H81A C813 H81C 109.5 . . ? H81B C813 H81C 109.5 . . ? C810 C814 H81D 109.5 . . ? C810 C814 H81E 109.5 . . ? H81D C814 H81E 109.5 . . ? C810 C814 H81F 109.5 . . ? H81D C814 H81F 109.5 . . ? H81E C814 H81F 109.5 . . ? C902 N901 C906 121.4(16) . . ? C902 N901 Ni5' 126.2(12) . . ? C906 N901 Ni5' 112.3(12) . . ? N901 C902 C903 123.8(18) . . ? N901 C902 H902 118.1 . . ? C903 C902 H902 118.1 . . ? C904 C903 C902 113(2) . . ? C904 C903 C913 129(2) . . ? C902 C903 C913 118.1(19) . . ? C903 C904 C905 128(3) . . ? C903 C904 H904 115.8 . . ? C905 C904 H904 115.8 . . ? C904 C905 C906 115(2) . . ? C904 C905 H905 122.5 . . ? C906 C905 H905 122.5 . . ? N901 C906 C905 118.7(19) . . ? N901 C906 C907 118.3(19) . . ? C905 C906 C907 123(2) . . ? N912 C907 C908 120(2) . . ? N912 C907 C906 114.9(19) . . ? C908 C907 C906 125(2) . . ? C909 C908 C907 118(3) . . ? C909 C908 H908 121.1 . . ? C907 C908 H908 121.1 . . ? C910 C909 C908 123(3) . . ? C910 C909 H909 118.3 . . ? C908 C909 H909 118.3 . . ? C909 C910 C914 125(3) . . ? C909 C910 C911 116(2) . . ? C914 C910 C911 118(2) . . ? N912 C911 C910 121(2) . . ? N912 C911 H911 119.5 . . ? C910 C911 H911 119.5 . . ? C911 N912 C907 121.1(18) . . ? C911 N912 Ni5' 124.2(14) . . ? C907 N912 Ni5' 114.7(13) . . ? C903 C913 H91A 109.5 . . ? C903 C913 H91B 109.5 . . ? H91A C913 H91B 109.5 . . ? C903 C913 H91C 109.5 . . ? H91A C913 H91C 109.5 . . ? H91B C913 H91C 109.5 . . ? C910 C914 H91D 109.5 . . ? C910 C914 H91E 109.5 . . ? H91D C914 H91E 109.5 . . ? C910 C914 H91F 109.5 . . ? H91D C914 H91F 109.5 . . ? H91E C914 H91F 109.5 . . ? C706 N701 C715 83.5(13) . . ? C706 N701 C718 65.0(11) . . ? C715 N701 C718 121.8(16) . . ? C706 N701 C702 120.6(16) . . ? C715 N701 C702 67.1(11) . . ? C718 N701 C702 88.0(12) . . ? C706 N701 Ni3' 114.4(12) . . ? C715 N701 Ni3' 124.3(14) . . ? C718 N701 Ni3' 113.3(11) . . ? C702 N701 Ni3' 124.8(13) . . ? C711 N712 C707 123(2) . . ? C711 N712 Ni3' 132(2) . . ? C707 N712 Ni3' 104.0(16) . . ? C723 N724 C719 122(2) . . ? C723 N724 Ni3' 128.1(17) . . ? C719 N724 Ni3' 103.8(14) . . ? C705 C704 C716 84.9(13) . . ? C705 C704 C717 65.9(12) . . ? C716 C704 C717 120.6(18) . . ? C705 C704 C703 121.5(18) . . ? C716 C704 C703 66.0(12) . . ? C717 C704 C703 86.3(13) . . ? N701 C702 C703 120(2) . . ? C704 C703 C702 117(2) . . ? C704 C703 C713 134(4) . . ? C702 C703 C713 108(4) . . ? C704 C705 C706 117(2) . . ? N701 C706 C705 123.8(19) . . ? N701 C706 C707 111(2) . . ? C705 C706 C707 125(2) . . ? N712 C707 C708 122.0(19) . . ? N712 C707 C706 127(2) . . ? C708 C707 C706 111(2) . . ? C709 C708 C707 114(2) . . ? C708 C709 C710 122(2) . . ? C709 C710 C711 119(2) . . ? C709 C710 C714 138(5) . . ? C711 C710 C714 99(5) . . ? N712 C711 C710 117(2) . . ? N701 C715 C716 122(2) . . ? C704 C716 C715 118(2) . . ? C704 C716 C725 108(4) . . ? C715 C716 C725 133(4) . . ? C718 C717 C704 119.0(19) . . ? N701 C718 C717 118.8(17) . . ? N701 C718 C719 110.9(19) . . ? C717 C718 C719 130.2(19) . . ? N724 C719 C720 117.2(18) . . ? N724 C719 C718 126(2) . . ? C720 C719 C718 116(2) . . ? C721 C720 C719 117(2) . . ? C720 C721 C722 123(2) . . ? C721 C722 C723 114(2) . . ? C721 C722 C726 119(3) . . ? C723 C722 C726 116(2) . . ? N724 C723 C722 117(2) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.384 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.188 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 876833' #TrackingRef '- clusters1-4_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; {Ni[Ni(4,4'dtbpy)(H2O)]8[W(CN)8]6}*17H2O ; _chemical_name_common (Ni(Ni(4,4'dtbpy)(H2O))8(W(CN)8)6)*17H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C208 H232 N64 Ni9 O23 W6' _chemical_formula_weight 5627.84 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' _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 20.2904(2) _cell_length_b 20.3359(2) _cell_length_c 21.3903(3) _cell_angle_alpha 105.60 _cell_angle_beta 111.6140(10) _cell_angle_gamma 98.0810(10) _cell_volume 7615.02(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2820 _exptl_absorpt_coefficient_mu 2.853 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4350 _exptl_absorpt_correction_T_max 0.6742 _exptl_absorpt_process_details 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 KappaCCD _diffrn_measurement_method '\f and \o scans to fill Ewald sphere' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 54204 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0786 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 27.50 _reflns_number_total 33881 _reflns_number_gt 21982 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (ALTOMARE et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+20.7765P] 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 33881 _refine_ls_number_parameters 1402 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1534 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.017 _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 W1 W 0.718278(14) 0.600284(13) 0.441211(16) 0.03650(7) Uani 1 1 d . . . W2 W 0.301214(15) 0.470198(14) 0.241920(16) 0.04017(8) Uani 1 1 d . . . W3 W 0.503157(14) 0.233553(12) 0.389339(16) 0.03633(7) Uani 1 1 d . . . Ni1 Ni 0.5000 0.5000 0.5000 0.0295(2) Uani 1 2 d S . . Ni2 Ni 0.49831(5) 0.72099(4) 0.35189(6) 0.0438(2) Uani 1 1 d . . . Ni3 Ni 0.22656(5) 0.23803(4) 0.29532(5) 0.0423(2) Uani 1 1 d . . . Ni4 Ni 0.52660(5) 0.37490(5) 0.21792(5) 0.0442(2) Uani 1 1 d . . . Ni5 Ni 0.77827(5) 0.39808(5) 0.55448(6) 0.0442(2) Uani 1 1 d . . . C11 C 0.6328(3) 0.5607(3) 0.4688(4) 0.0370(15) Uani 1 1 d . . . N11 N 0.5869(3) 0.5384(3) 0.4819(3) 0.0392(13) Uani 1 1 d . . . C12 C 0.6288(4) 0.6470(4) 0.4020(5) 0.0476(18) Uani 1 1 d . . . N12 N 0.5819(4) 0.6735(3) 0.3825(4) 0.0511(16) Uani 1 1 d . . . C13 C 0.7534(4) 0.6601(4) 0.5538(4) 0.0438(17) Uani 1 1 d . . . N13 N 0.7695(3) 0.6964(3) 0.6113(4) 0.0466(15) Uani 1 1 d . . . C14 C 0.6460(4) 0.5048(4) 0.3533(4) 0.0445(16) Uani 1 1 d . . . N14 N 0.6046(4) 0.4553(3) 0.3068(4) 0.0507(15) Uani 1 1 d . . . C15 C 0.7445(4) 0.5155(4) 0.4811(4) 0.0435(17) Uani 1 1 d . . . N15 N 0.7554(3) 0.4701(3) 0.5021(4) 0.0516(16) Uani 1 1 d . . . C16 C 0.7690(5) 0.7100(4) 0.4594(5) 0.056(2) Uani 1 1 d . . . N16 N 0.7941(4) 0.7673(4) 0.4694(5) 0.072(2) Uani 1 1 d . . . C17 C 0.8322(5) 0.6069(5) 0.4687(6) 0.064(2) Uani 1 1 d . . . N17 N 0.8947(4) 0.6113(5) 0.4849(7) 0.106(4) Uani 1 1 d . . . C18 C 0.7272(5) 0.6037(5) 0.3445(6) 0.070(3) Uani 1 1 d . . . N18 N 0.7302(6) 0.6079(6) 0.2924(5) 0.094(3) Uani 1 1 d . . . C21 C 0.3851(4) 0.4842(3) 0.3456(4) 0.0401(15) Uani 1 1 d . . . N21 N 0.4283(3) 0.4928(3) 0.4004(3) 0.0381(12) Uani 1 1 d . . . C22 C 0.3788(4) 0.5727(4) 0.2800(4) 0.0452(17) Uani 1 1 d . . . N22 N 0.4208(4) 0.6257(3) 0.3026(4) 0.0535(17) Uani 1 1 d . . . C23 C 0.2833(4) 0.3723(4) 0.2612(4) 0.0489(18) Uani 1 1 d . . . N23 N 0.2700(4) 0.3221(4) 0.2735(4) 0.0619(19) Uani 1 1 d . . . C24 C 0.3932(4) 0.4404(4) 0.2257(4) 0.0486(18) Uani 1 1 d . . . N24 N 0.4427(4) 0.4226(4) 0.2203(4) 0.0553(17) Uani 1 1 d . . . C25 C 0.2673(4) 0.5227(4) 0.3222(4) 0.0478(18) Uani 1 1 d . . . N25 N 0.2497(4) 0.5484(4) 0.3664(4) 0.0554(17) Uani 1 1 d . . . C26 C 0.1835(5) 0.4273(7) 0.2000(6) 0.086(4) Uani 1 1 d . . . N26 N 0.1231(5) 0.4013(8) 0.1821(7) 0.150(6) Uani 1 1 d . . . C27 C 0.2637(7) 0.4021(8) 0.1317(6) 0.100(4) Uani 1 1 d . . . N27 N 0.2425(8) 0.3644(10) 0.0744(7) 0.178(8) Uani 1 1 d . . . C28 C 0.2533(9) 0.5323(7) 0.1809(8) 0.152(8) Uani 1 1 d . . . N28 N 0.2280(11) 0.5683(8) 0.1527(11) 0.277(16) Uani 1 1 d . . . C31 C 0.5005(3) 0.3410(3) 0.4337(4) 0.0336(14) Uani 1 1 d . . . N31 N 0.5020(3) 0.3982(3) 0.4577(3) 0.0399(13) Uani 1 1 d . . . C32 C 0.5091(4) 0.2499(4) 0.4968(5) 0.0472(18) Uani 1 1 d . . . N32 N 0.5117(4) 0.2622(3) 0.5531(4) 0.0483(15) Uani 1 1 d . . . C33 C 0.3891(4) 0.2277(3) 0.3661(4) 0.0432(16) Uani 1 1 d . . . N33 N 0.3284(3) 0.2274(3) 0.3490(4) 0.0539(17) Uani 1 1 d . . . C34 C 0.5078(4) 0.2892(4) 0.3179(4) 0.0443(17) Uani 1 1 d . . . N34 N 0.5098(4) 0.3182(3) 0.2793(3) 0.0489(15) Uani 1 1 d . . . C35 C 0.6159(4) 0.2943(4) 0.4596(4) 0.0417(16) Uani 1 1 d . . . N35 N 0.6744(3) 0.3293(3) 0.4958(4) 0.0536(17) Uani 1 1 d . . . C36 C 0.4881(5) 0.1317(3) 0.4029(5) 0.056(2) Uani 1 1 d . . . N36 N 0.4778(5) 0.0771(4) 0.4060(5) 0.081(3) Uani 1 1 d . . . C37 C 0.4341(5) 0.1593(4) 0.2811(5) 0.056(2) Uani 1 1 d . . . N37 N 0.3980(5) 0.1229(4) 0.2228(4) 0.077(2) Uani 1 1 d . . . C38 C 0.5751(5) 0.1858(4) 0.3490(5) 0.057(2) Uani 1 1 d . . . N38 N 0.6119(5) 0.1620(4) 0.3248(5) 0.074(2) Uani 1 1 d . . . N201 N 0.5665(3) 0.8218(3) 0.3970(4) 0.0483(15) Uani 1 1 d . . . C202 C 0.6367(4) 0.8404(4) 0.4400(5) 0.062(2) Uani 1 1 d . . . H202 H 0.6603 0.8053 0.4477 0.074 Uiso 1 1 calc R . . C203 C 0.6770(5) 0.9110(5) 0.4744(6) 0.075(3) Uani 1 1 d . . . H203 H 0.7267 0.9224 0.5049 0.091 Uiso 1 1 calc R . . C204 C 0.6439(5) 0.9645(5) 0.4639(6) 0.074(3) Uani 1 1 d . . . C205 C 0.5703(5) 0.9434(4) 0.4177(5) 0.064(3) Uani 1 1 d . . . H205 H 0.5456 0.9775 0.4087 0.077 Uiso 1 1 calc R . . C206 C 0.5333(4) 0.8741(4) 0.3854(5) 0.0510(19) Uani 1 1 d . . . C207 C 0.4534(4) 0.8473(4) 0.3341(4) 0.0497(18) Uani 1 1 d . . . C208 C 0.4121(5) 0.8900(5) 0.3060(6) 0.071(3) Uani 1 1 d . . . H208 H 0.4337 0.9382 0.3207 0.085 Uiso 1 1 calc R . . C209 C 0.3391(5) 0.8615(5) 0.2562(6) 0.077(3) Uani 1 1 d . . . C210 C 0.3110(5) 0.7906(5) 0.2390(7) 0.086(4) Uani 1 1 d . . . H210 H 0.2623 0.7690 0.2063 0.104 Uiso 1 1 calc R . . C211 C 0.3535(5) 0.7504(5) 0.2691(6) 0.076(3) Uani 1 1 d . . . H211 H 0.3320 0.7025 0.2564 0.091 Uiso 1 1 calc R . . N212 N 0.4235(3) 0.7770(3) 0.3153(4) 0.0501(16) Uani 1 1 d . . . C213 C 0.6835(7) 1.0426(5) 0.5016(9) 0.120(6) Uani 1 1 d . . . C214 C 0.7643(8) 1.0542(7) 0.5516(10) 0.162(9) Uani 1 1 d . . . H21G H 0.7881 1.0301 0.5247 0.244 Uiso 1 1 calc R . . H21H H 0.7669 1.0357 0.5890 0.244 Uiso 1 1 calc R . . H21I H 0.7887 1.1040 0.5724 0.244 Uiso 1 1 calc R . . C215 C 0.6442(10) 1.0802(7) 0.5435(9) 0.159(9) Uani 1 1 d . . . H21A H 0.6699 1.1296 0.5671 0.239 Uiso 1 1 calc R . . H21B H 0.6436 1.0595 0.5787 0.239 Uiso 1 1 calc R . . H21C H 0.5947 1.0751 0.5111 0.239 Uiso 1 1 calc R . . C216 C 0.6788(9) 1.0781(7) 0.4464(10) 0.166(9) Uani 1 1 d . . . H21D H 0.7027 1.0574 0.4179 0.248 Uiso 1 1 calc R . . H21E H 0.7026 1.1279 0.4705 0.248 Uiso 1 1 calc R . . H21F H 0.6281 1.0715 0.4158 0.248 Uiso 1 1 calc R . . C217 C 0.2961(6) 0.9086(6) 0.2237(9) 0.113(6) Uani 1 1 d . . . C218 C 0.3348(10) 0.9401(11) 0.1844(12) 0.178(10) Uani 1 1 d . . . H21M H 0.3849 0.9652 0.2173 0.267 Uiso 1 1 calc R . . H21N H 0.3097 0.9721 0.1661 0.267 Uiso 1 1 calc R . . H21O H 0.3340 0.9026 0.1454 0.267 Uiso 1 1 calc R . . C219 C 0.2976(10) 0.9729(9) 0.2820(11) 0.189(11) Uani 1 1 d . . . H21J H 0.3477 0.9985 0.3141 0.284 Uiso 1 1 calc R . . H21K H 0.2731 0.9572 0.3082 0.284 Uiso 1 1 calc R . . H21L H 0.2730 1.0033 0.2600 0.284 Uiso 1 1 calc R . . C220 C 0.2176(8) 0.8675(9) 0.1709(13) 0.233(15) Uani 1 1 d . . . H22F H 0.2180 0.8272 0.1354 0.350 Uiso 1 1 calc R . . H22G H 0.1936 0.8976 0.1479 0.350 Uiso 1 1 calc R . . H22H H 0.1916 0.8519 0.1960 0.350 Uiso 1 1 calc R . . O221 O 0.5128(4) 0.7089(4) 0.2555(4) 0.0786(19) Uani 1 1 d . . . C222 C 0.4565(16) 0.6757(12) 0.1798(11) 0.197(10) Uani 1 1 d . . . H22A H 0.4091 0.6597 0.1799 0.237 Uiso 1 1 calc R . . H22B H 0.4685 0.6342 0.1567 0.237 Uiso 1 1 calc R . . C223 C 0.4491(19) 0.7237(17) 0.1354(14) 0.30(2) Uani 1 1 d . . . H22C H 0.4110 0.6986 0.0879 0.457 Uiso 1 1 calc R . . H22D H 0.4949 0.7379 0.1328 0.457 Uiso 1 1 calc R . . H22E H 0.4367 0.7649 0.1575 0.457 Uiso 1 1 calc R . . N301 N 0.1703(3) 0.1460(3) 0.2976(3) 0.0456(14) Uani 1 1 d . . . C302 C 0.1533(5) 0.1399(4) 0.3497(5) 0.062(2) Uani 1 1 d . . . H302 H 0.1703 0.1792 0.3913 0.074 Uiso 1 1 calc R . . C303 C 0.1109(5) 0.0773(5) 0.3456(5) 0.068(3) Uani 1 1 d . . . H303 H 0.1024 0.0747 0.3847 0.082 Uiso 1 1 calc R . . C304 C 0.0822(5) 0.0203(4) 0.2839(5) 0.062(2) Uani 1 1 d . . . C305 C 0.1001(4) 0.0267(4) 0.2292(5) 0.055(2) Uani 1 1 d . . . H305 H 0.0826 -0.0119 0.1869 0.066 Uiso 1 1 calc R . . C306 C 0.1440(4) 0.0899(3) 0.2361(4) 0.0446(17) Uani 1 1 d . . . C307 C 0.1674(4) 0.1003(4) 0.1810(4) 0.0460(17) Uani 1 1 d . . . C308 C 0.1478(4) 0.0486(4) 0.1145(5) 0.056(2) Uani 1 1 d . . . H308 H 0.1168 0.0045 0.1022 0.067 Uiso 1 1 calc R . . C309 C 0.1735(5) 0.0619(6) 0.0669(5) 0.067(3) Uani 1 1 d . . . C310 C 0.2201(6) 0.1272(5) 0.0874(5) 0.069(2) Uani 1 1 d . . . H310 H 0.2398 0.1379 0.0572 0.083 Uiso 1 1 calc R . . C311 C 0.2375(5) 0.1773(5) 0.1538(5) 0.069(3) Uani 1 1 d . . . H311 H 0.2686 0.2217 0.1671 0.083 Uiso 1 1 calc R . . N312 N 0.2114(3) 0.1644(3) 0.1991(4) 0.0504(15) Uani 1 1 d . . . C313 C 0.0296(6) -0.0479(5) 0.2730(7) 0.082(3) Uani 1 1 d . . . C314 C -0.0444(8) -0.0508(12) 0.2258(13) 0.221(14) Uani 1 1 d . . . H31J H -0.0450 -0.0466 0.1820 0.331 Uiso 1 1 calc R . . H31K H -0.0598 -0.0125 0.2489 0.331 Uiso 1 1 calc R . . H31L H -0.0773 -0.0951 0.2155 0.331 Uiso 1 1 calc R . . C315 C 0.0342(11) -0.0532(10) 0.3434(10) 0.192(11) Uani 1 1 d . . . H31M H 0.0843 -0.0489 0.3740 0.288 Uiso 1 1 calc R . . H31N H 0.0037 -0.0982 0.3349 0.288 Uiso 1 1 calc R . . H31O H 0.0176 -0.0158 0.3662 0.288 Uiso 1 1 calc R . . C316 C 0.0538(15) -0.1113(7) 0.2430(18) 0.268(18) Uani 1 1 d . . . H31G H 0.1023 -0.1083 0.2762 0.402 Uiso 1 1 calc R . . H31H H 0.0542 -0.1121 0.1981 0.402 Uiso 1 1 calc R . . H31I H 0.0202 -0.1539 0.2357 0.402 Uiso 1 1 calc R . . C317 C 0.1489(7) 0.0035(7) -0.0072(5) 0.084(3) Uani 1 1 d . . . C318 C 0.0649(7) -0.0127(8) -0.0488(6) 0.115(5) Uani 1 1 d . . . H31D H 0.0521 0.0297 -0.0544 0.173 Uiso 1 1 calc R . . H31E H 0.0411 -0.0299 -0.0227 0.173 Uiso 1 1 calc R . . H31F H 0.0490 -0.0480 -0.0952 0.173 Uiso 1 1 calc R . . C319 C 0.1686(11) -0.0620(8) 0.0009(7) 0.152(8) Uani 1 1 d . . . H31A H 0.2210 -0.0518 0.0269 0.228 Uiso 1 1 calc R . . H31B H 0.1529 -0.0971 -0.0456 0.228 Uiso 1 1 calc R . . H31C H 0.1449 -0.0796 0.0268 0.228 Uiso 1 1 calc R . . C320 C 0.1865(11) 0.0303(10) -0.0503(7) 0.156(8) Uani 1 1 d . . . H32F H 0.1738 0.0727 -0.0562 0.234 Uiso 1 1 calc R . . H32G H 0.1702 -0.0054 -0.0965 0.234 Uiso 1 1 calc R . . H32H H 0.2389 0.0404 -0.0247 0.234 Uiso 1 1 calc R . . O321 O 0.1215(3) 0.2529(4) 0.2338(4) 0.0763(19) Uani 1 1 d . . . C322 C 0.0666(7) 0.2632(9) 0.2559(8) 0.122(5) Uani 1 1 d . . . H32A H 0.0735 0.3136 0.2774 0.147 Uiso 1 1 calc R . . H32B H 0.0701 0.2419 0.2921 0.147 Uiso 1 1 calc R . . C323 C -0.0071(8) 0.2319(17) 0.1954(13) 0.29(2) Uani 1 1 d . . . H32C H -0.0439 0.2396 0.2125 0.439 Uiso 1 1 calc R . . H32D H -0.0142 0.1819 0.1742 0.439 Uiso 1 1 calc R . . H32E H -0.0111 0.2538 0.1600 0.439 Uiso 1 1 calc R . . N401 N 0.6005(4) 0.3205(3) 0.1963(4) 0.0534(16) Uani 1 1 d . . . C402 C 0.6169(6) 0.2656(5) 0.2150(6) 0.073(3) Uani 1 1 d . . . H402 H 0.6046 0.2560 0.2501 0.087 Uiso 1 1 calc R . . C403 C 0.6517(6) 0.2220(6) 0.1840(6) 0.079(3) Uani 1 1 d . . . H403 H 0.6633 0.1847 0.1994 0.095 Uiso 1 1 calc R . . C404 C 0.6690(6) 0.2336(6) 0.1309(7) 0.084(3) Uani 1 1 d . . . C405 C 0.6537(6) 0.2930(5) 0.1130(5) 0.073(3) Uani 1 1 d . . . H405 H 0.6656 0.3038 0.0782 0.087 Uiso 1 1 calc R . . C406 C 0.6210(5) 0.3354(5) 0.1476(5) 0.058(2) Uani 1 1 d . . . C407 C 0.6048(5) 0.3999(5) 0.1325(5) 0.061(2) Uani 1 1 d . . . C408 C 0.6383(6) 0.4342(6) 0.0996(6) 0.076(3) Uani 1 1 d . . . H408 H 0.6700 0.4149 0.0826 0.091 Uiso 1 1 calc R . . C409 C 0.6250(7) 0.4959(7) 0.0922(6) 0.087(3) Uani 1 1 d . . . C410 C 0.5764(7) 0.5209(6) 0.1162(6) 0.086(3) Uani 1 1 d . . . H410 H 0.5646 0.5619 0.1100 0.104 Uiso 1 1 calc R . . C411 C 0.5444(6) 0.4859(6) 0.1495(6) 0.077(3) Uani 1 1 d . . . H411 H 0.5128 0.5050 0.1667 0.092 Uiso 1 1 calc R . . N412 N 0.5576(4) 0.4261(4) 0.1574(4) 0.0563(17) Uani 1 1 d . . . C413 C 0.7022(8) 0.1822(8) 0.0931(9) 0.124(6) Uani 1 1 d . . . C414 C 0.6506(13) 0.1214(12) 0.0471(18) 0.35(3) Uani 1 1 d . . . H41M H 0.6127 0.1313 0.0109 0.527 Uiso 1 1 calc R . . H41N H 0.6297 0.0999 0.0728 0.527 Uiso 1 1 calc R . . H41O H 0.6728 0.0895 0.0248 0.527 Uiso 1 1 calc R . . C415 C 0.7604(16) 0.1626(16) 0.1479(14) 0.264(17) Uani 1 1 d . . . H41G H 0.7979 0.2048 0.1826 0.395 Uiso 1 1 calc R . . H41H H 0.7820 0.1313 0.1242 0.395 Uiso 1 1 calc R . . H41I H 0.7384 0.1394 0.1718 0.395 Uiso 1 1 calc R . . C416 C 0.7534(15) 0.2214(11) 0.0683(17) 0.240(16) Uani 1 1 d . . . H41J H 0.7867 0.2635 0.1073 0.360 Uiso 1 1 calc R . . H41K H 0.7243 0.2343 0.0289 0.360 Uiso 1 1 calc R . . H41L H 0.7809 0.1910 0.0533 0.360 Uiso 1 1 calc R . . C417 C 0.6605(10) 0.5368(10) 0.0567(9) 0.125(6) Uani 1 1 d . . . C418 C 0.6402(12) 0.4893(12) -0.0173(10) 0.176(9) Uani 1 1 d . . . H41D H 0.5876 0.4739 -0.0432 0.264 Uiso 1 1 calc R . . H41E H 0.6593 0.4489 -0.0157 0.264 Uiso 1 1 calc R . . H41F H 0.6606 0.5144 -0.0410 0.264 Uiso 1 1 calc R . . C419 C 0.7396(12) 0.5621(19) 0.1047(14) 0.32(3) Uani 1 1 d . . . H41A H 0.7467 0.5916 0.1513 0.486 Uiso 1 1 calc R . . H41B H 0.7646 0.5890 0.0855 0.486 Uiso 1 1 calc R . . H41C H 0.7591 0.5223 0.1086 0.486 Uiso 1 1 calc R . . C420 C 0.6349(19) 0.6021(15) 0.0506(17) 0.272(17) Uani 1 1 d . . . H42A H 0.5832 0.5883 0.0196 0.408 Uiso 1 1 calc R . . H42B H 0.6616 0.6267 0.0311 0.408 Uiso 1 1 calc R . . H42C H 0.6434 0.6327 0.0973 0.408 Uiso 1 1 calc R . . O421 O 0.4460(4) 0.2917(3) 0.1223(3) 0.0746(19) Uani 1 1 d . . . N501 N 0.8196(3) 0.3391(3) 0.4895(4) 0.0506(16) Uani 1 1 d . . . C502 C 0.7824(5) 0.2780(5) 0.4353(5) 0.068(3) Uani 1 1 d . . . H502 H 0.7313 0.2658 0.4166 0.082 Uiso 1 1 calc R . . C503 C 0.8148(5) 0.2319(6) 0.4053(6) 0.083(4) Uani 1 1 d . . . H503 H 0.7864 0.1895 0.3680 0.100 Uiso 1 1 calc R . . C504 C 0.8906(5) 0.2500(5) 0.4319(6) 0.077(3) Uani 1 1 d . . . C505 C 0.9302(5) 0.3139(5) 0.4870(6) 0.069(3) Uani 1 1 d . . . H505 H 0.9813 0.3273 0.5058 0.082 Uiso 1 1 calc R . . C506 C 0.8936(4) 0.3581(4) 0.5145(5) 0.0511(19) Uani 1 1 d . . . C507 C 0.9308(4) 0.4257(4) 0.5749(5) 0.0507(19) Uani 1 1 d . . . C508 C 1.0050(4) 0.4603(4) 0.6009(5) 0.061(2) Uani 1 1 d . . . H508 H 1.0337 0.4404 0.5800 0.073 Uiso 1 1 calc R . . C509 C 1.0364(4) 0.5245(5) 0.6579(6) 0.070(3) Uani 1 1 d . . . C510 C 0.9915(5) 0.5509(5) 0.6860(7) 0.089(4) Uani 1 1 d . . . H510 H 1.0103 0.5932 0.7248 0.107 Uiso 1 1 calc R . . C511 C 0.9173(5) 0.5146(5) 0.6569(6) 0.077(3) Uani 1 1 d . . . H511 H 0.8876 0.5344 0.6765 0.093 Uiso 1 1 calc R . . N512 N 0.8874(3) 0.4542(3) 0.6034(4) 0.0515(16) Uani 1 1 d . . . C513 C 0.9300(7) 0.1944(8) 0.4067(10) 0.149(9) Uani 1 1 d . . . C514 C 0.958(3) 0.227(2) 0.358(3) 0.45(4) Uani 1 1 d . . . H51A H 0.9158 0.2269 0.3175 0.674 Uiso 1 1 calc R . . H51B H 0.9863 0.1994 0.3415 0.674 Uiso 1 1 calc R . . H51C H 0.9871 0.2750 0.3857 0.674 Uiso 1 1 calc R . . C515 C 0.8840(12) 0.1346(12) 0.351(2) 0.38(3) Uani 1 1 d . . . H51G H 0.8363 0.1421 0.3296 0.569 Uiso 1 1 calc R . . H51H H 0.8797 0.0961 0.3687 0.569 Uiso 1 1 calc R . . H51I H 0.9034 0.1232 0.3162 0.569 Uiso 1 1 calc R . . C516 C 0.9996(13) 0.2027(16) 0.453(2) 0.34(3) Uani 1 1 d . . . H51D H 1.0203 0.2510 0.4855 0.513 Uiso 1 1 calc R . . H51E H 1.0287 0.1913 0.4273 0.513 Uiso 1 1 calc R . . H51F H 0.9995 0.1719 0.4802 0.513 Uiso 1 1 calc R . . C517 C 1.1173(6) 0.5625(6) 0.6866(9) 0.099(5) Uani 1 1 d . . . C518 C 1.1360(11) 0.5693(12) 0.6258(12) 0.208(12) Uani 1 1 d . . . H51J H 1.1872 0.5933 0.6447 0.311 Uiso 1 1 calc R . . H51K H 1.1068 0.5960 0.6021 0.311 Uiso 1 1 calc R . . H51L H 1.1260 0.5230 0.5921 0.311 Uiso 1 1 calc R . . C519 C 1.1630(8) 0.5138(11) 0.7136(13) 0.211(12) Uani 1 1 d . . . H51M H 1.2144 0.5368 0.7319 0.316 Uiso 1 1 calc R . . H51N H 1.1503 0.4704 0.6747 0.316 Uiso 1 1 calc R . . H51O H 1.1530 0.5037 0.7510 0.316 Uiso 1 1 calc R . . C520 C 1.1393(9) 0.6332(9) 0.7437(16) 0.273(19) Uani 1 1 d . . . H52F H 1.1906 0.6548 0.7599 0.410 Uiso 1 1 calc R . . H52G H 1.1306 0.6272 0.7833 0.410 Uiso 1 1 calc R . . H52H H 1.1109 0.6629 0.7247 0.410 Uiso 1 1 calc R . . O521 O 0.8138(4) 0.3347(4) 0.6200(4) 0.083(2) Uani 1 1 d . . . C522 C 0.7769(13) 0.2817(11) 0.6272(14) 0.212(13) Uani 1 1 d . . . H52A H 0.7517 0.2442 0.5806 0.254 Uiso 1 1 calc R . . H52B H 0.7396 0.2970 0.6409 0.254 Uiso 1 1 calc R . . C523 C 0.8208(17) 0.2500(12) 0.6814(14) 0.244(15) Uani 1 1 d . . . H52C H 0.7880 0.2118 0.6824 0.366 Uiso 1 1 calc R . . H52D H 0.8453 0.2859 0.7282 0.366 Uiso 1 1 calc R . . H52E H 0.8567 0.2324 0.6675 0.366 Uiso 1 1 calc R . . O1E O 0.4122(8) 0.1544(5) 0.1090(6) 0.145(4) Uani 1 1 d . . . C2E C 0.439(2) 0.0954(18) 0.082(2) 0.29(2) Uani 1 1 d . . . H2E1 H 0.4864 0.0978 0.1187 0.352 Uiso 1 1 calc R . . H2E2 H 0.4049 0.0508 0.0710 0.352 Uiso 1 1 calc R . . C3E C 0.446(3) 0.100(4) 0.023(4) 0.62(7) Uani 1 1 d . . . H3E1 H 0.4643 0.0617 0.0043 0.928 Uiso 1 1 calc R . . H3E2 H 0.4794 0.1443 0.0346 0.928 Uiso 1 1 calc R . . H3E3 H 0.3986 0.0965 -0.0130 0.928 Uiso 1 1 calc R . . O2 O 0.3585(8) 0.2933(9) 0.7537(8) 0.182(6) Uani 1 1 d . . . O3 O 0.1347(11) 0.0867(8) 0.5385(17) 0.374(18) Uani 1 1 d . . . O4 O 0.663(2) 0.0590(18) 0.2464(15) 0.42(2) Uani 1 1 d . . . O5 O 0.084(4) 0.298(2) 0.680(2) 0.61(4) Uani 1 1 d . . . O6 O 0.0832(14) 0.2480(18) 0.079(3) 0.59(4) Uani 1 1 d . . . O7 O -0.0061(18) 0.156(2) -0.0368(18) 0.39(2) Uani 1 1 d . . . O8 O 0.9082(17) 0.4216(14) 0.7636(14) 0.193(13) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.03109(13) 0.03043(12) 0.05314(17) 0.01269(11) 0.02444(12) 0.00897(10) W2 0.03550(14) 0.03539(13) 0.04557(16) 0.01436(12) 0.01261(12) 0.00993(10) W3 0.03534(13) 0.02182(11) 0.05208(17) 0.00996(11) 0.01976(12) 0.01095(9) Ni1 0.0260(5) 0.0223(5) 0.0434(6) 0.0110(4) 0.0175(5) 0.0093(4) Ni2 0.0468(5) 0.0326(4) 0.0607(6) 0.0240(4) 0.0249(4) 0.0154(4) Ni3 0.0353(4) 0.0318(4) 0.0521(5) 0.0090(4) 0.0164(4) 0.0036(3) Ni4 0.0506(5) 0.0363(4) 0.0499(5) 0.0105(4) 0.0281(4) 0.0141(4) Ni5 0.0301(4) 0.0400(4) 0.0649(6) 0.0160(4) 0.0218(4) 0.0168(3) C11 0.028(3) 0.031(3) 0.049(4) 0.008(3) 0.016(3) 0.011(2) N11 0.033(3) 0.037(3) 0.052(4) 0.013(3) 0.024(3) 0.012(2) C12 0.052(4) 0.030(3) 0.069(5) 0.017(3) 0.036(4) 0.009(3) N12 0.050(4) 0.040(3) 0.073(5) 0.027(3) 0.029(3) 0.019(3) C13 0.038(4) 0.032(3) 0.062(5) 0.017(3) 0.021(3) 0.012(3) N13 0.041(3) 0.032(3) 0.057(4) 0.010(3) 0.016(3) 0.008(2) C14 0.049(4) 0.040(4) 0.057(5) 0.019(4) 0.035(4) 0.013(3) N14 0.056(4) 0.040(3) 0.054(4) 0.011(3) 0.026(3) 0.010(3) C15 0.029(3) 0.041(4) 0.061(5) 0.013(3) 0.022(3) 0.011(3) N15 0.036(3) 0.043(3) 0.080(5) 0.027(3) 0.025(3) 0.016(3) C16 0.055(5) 0.040(4) 0.075(6) 0.018(4) 0.030(4) 0.009(3) N16 0.072(5) 0.045(4) 0.099(6) 0.025(4) 0.043(5) 0.002(3) C17 0.051(5) 0.058(5) 0.097(7) 0.024(5) 0.047(5) 0.017(4) N17 0.043(4) 0.100(7) 0.190(11) 0.042(7) 0.068(6) 0.026(4) C18 0.059(5) 0.063(5) 0.077(7) 0.005(5) 0.037(5) -0.004(4) N18 0.116(8) 0.103(7) 0.083(6) 0.037(6) 0.066(6) 0.015(6) C21 0.038(3) 0.029(3) 0.053(4) 0.011(3) 0.021(3) 0.010(3) N21 0.033(3) 0.035(3) 0.043(3) 0.013(2) 0.012(3) 0.009(2) C22 0.044(4) 0.041(4) 0.057(5) 0.024(3) 0.019(3) 0.020(3) N22 0.054(4) 0.038(3) 0.077(5) 0.031(3) 0.029(3) 0.015(3) C23 0.047(4) 0.037(4) 0.044(4) 0.008(3) 0.007(3) 0.003(3) N23 0.058(4) 0.049(4) 0.068(5) 0.021(3) 0.020(4) 0.001(3) C24 0.049(4) 0.038(4) 0.049(4) 0.010(3) 0.016(4) 0.011(3) N24 0.060(4) 0.058(4) 0.053(4) 0.018(3) 0.029(3) 0.022(3) C25 0.036(4) 0.045(4) 0.060(5) 0.016(4) 0.017(3) 0.016(3) N25 0.042(3) 0.052(4) 0.070(5) 0.014(3) 0.024(3) 0.017(3) C26 0.034(4) 0.108(9) 0.071(6) -0.006(6) 0.008(4) 0.007(5) N26 0.047(5) 0.201(15) 0.138(11) -0.012(10) 0.033(6) -0.002(7) C27 0.083(8) 0.129(11) 0.060(7) 0.005(7) 0.025(6) 0.016(7) N27 0.123(11) 0.240(19) 0.074(8) -0.037(10) 0.012(7) 0.026(11) C28 0.129(12) 0.085(8) 0.122(11) 0.054(8) -0.065(9) -0.026(8) N28 0.25(2) 0.114(11) 0.242(19) 0.114(13) -0.143(16) -0.035(12) C31 0.035(3) 0.025(3) 0.050(4) 0.017(3) 0.023(3) 0.015(2) N31 0.037(3) 0.033(3) 0.051(3) 0.012(2) 0.021(3) 0.012(2) C32 0.042(4) 0.033(3) 0.069(6) 0.017(4) 0.027(4) 0.012(3) N32 0.052(4) 0.040(3) 0.061(4) 0.021(3) 0.028(3) 0.016(3) C33 0.046(4) 0.028(3) 0.052(4) 0.012(3) 0.019(3) 0.008(3) N33 0.038(3) 0.048(3) 0.067(4) 0.014(3) 0.017(3) 0.009(3) C34 0.044(4) 0.034(3) 0.055(5) 0.005(3) 0.028(3) 0.015(3) N34 0.062(4) 0.045(3) 0.047(4) 0.014(3) 0.031(3) 0.020(3) C35 0.029(3) 0.038(3) 0.057(4) 0.013(3) 0.019(3) 0.013(3) N35 0.042(3) 0.047(3) 0.079(5) 0.019(3) 0.033(3) 0.018(3) C36 0.072(5) 0.023(3) 0.077(6) 0.019(3) 0.030(5) 0.019(3) N36 0.092(6) 0.039(4) 0.109(7) 0.030(4) 0.036(5) 0.018(4) C37 0.068(5) 0.032(3) 0.064(5) 0.009(4) 0.029(4) 0.013(3) N37 0.089(6) 0.057(4) 0.056(5) -0.001(4) 0.016(4) 0.014(4) C38 0.058(5) 0.030(3) 0.081(6) 0.009(4) 0.032(4) 0.017(3) N38 0.078(5) 0.060(4) 0.093(6) 0.013(4) 0.050(5) 0.034(4) N201 0.048(3) 0.038(3) 0.064(4) 0.026(3) 0.022(3) 0.017(3) C202 0.044(4) 0.048(4) 0.079(6) 0.026(4) 0.008(4) 0.012(3) C203 0.056(5) 0.052(5) 0.091(7) 0.027(5) 0.001(5) 0.012(4) C204 0.054(5) 0.044(4) 0.096(7) 0.029(5) 0.002(5) 0.004(4) C205 0.058(5) 0.040(4) 0.076(6) 0.023(4) 0.005(4) 0.018(4) C206 0.052(4) 0.045(4) 0.065(5) 0.033(4) 0.023(4) 0.019(3) C207 0.057(4) 0.034(3) 0.060(5) 0.023(3) 0.023(4) 0.015(3) C208 0.065(5) 0.044(4) 0.091(7) 0.032(5) 0.013(5) 0.019(4) C209 0.062(6) 0.065(6) 0.088(7) 0.036(5) 0.006(5) 0.023(5) C210 0.055(5) 0.062(5) 0.115(9) 0.042(6) 0.001(5) 0.009(4) C211 0.055(5) 0.051(5) 0.102(8) 0.031(5) 0.013(5) 0.007(4) N212 0.045(3) 0.040(3) 0.069(4) 0.027(3) 0.021(3) 0.011(3) C213 0.079(7) 0.044(5) 0.154(13) 0.024(7) -0.025(8) -0.005(5) C214 0.107(11) 0.061(7) 0.201(18) 0.022(9) -0.034(11) -0.002(7) C215 0.166(16) 0.071(8) 0.146(14) -0.009(9) -0.009(12) 0.053(10) C216 0.139(13) 0.078(8) 0.212(19) 0.088(11) -0.003(12) -0.024(9) C217 0.060(6) 0.081(7) 0.174(13) 0.084(9) -0.003(7) 0.020(5) C218 0.150(16) 0.169(17) 0.22(2) 0.152(18) 0.024(15) 0.038(14) C219 0.158(16) 0.110(12) 0.22(2) 0.034(13) -0.014(14) 0.093(12) C220 0.088(10) 0.126(13) 0.36(3) 0.147(18) -0.070(14) 0.005(9) O221 0.088(5) 0.089(5) 0.063(4) 0.031(4) 0.035(4) 0.019(4) C222 0.30(3) 0.16(2) 0.140(18) 0.055(16) 0.11(2) 0.04(2) C223 0.40(5) 0.26(4) 0.16(2) 0.12(2) 0.04(3) -0.06(3) N301 0.041(3) 0.036(3) 0.052(4) 0.008(3) 0.020(3) 0.001(2) C302 0.080(6) 0.040(4) 0.068(6) 0.013(4) 0.043(5) 0.003(4) C303 0.075(6) 0.062(5) 0.075(6) 0.026(5) 0.043(5) 0.002(5) C304 0.059(5) 0.044(4) 0.072(6) 0.021(4) 0.022(4) -0.001(4) C305 0.054(4) 0.042(4) 0.059(5) 0.013(4) 0.020(4) 0.002(3) C306 0.031(3) 0.030(3) 0.061(5) 0.012(3) 0.010(3) 0.008(3) C307 0.046(4) 0.039(3) 0.050(4) 0.013(3) 0.018(3) 0.012(3) C308 0.048(4) 0.052(4) 0.057(5) 0.006(4) 0.019(4) 0.013(3) C309 0.056(5) 0.087(7) 0.053(5) 0.015(5) 0.020(4) 0.035(5) C310 0.074(6) 0.076(6) 0.059(6) 0.020(5) 0.036(5) 0.016(5) C311 0.060(5) 0.071(6) 0.071(6) 0.017(5) 0.032(5) 0.001(4) N312 0.046(3) 0.048(3) 0.055(4) 0.013(3) 0.023(3) 0.010(3) C313 0.063(6) 0.060(5) 0.108(9) 0.041(6) 0.022(6) -0.009(5) C314 0.078(10) 0.21(2) 0.29(3) 0.17(2) -0.037(13) -0.059(12) C315 0.201(19) 0.160(16) 0.141(15) 0.089(13) 0.017(13) -0.088(15) C316 0.32(3) 0.050(7) 0.52(5) 0.056(16) 0.32(4) 0.003(13) C317 0.092(8) 0.102(8) 0.050(5) 0.005(5) 0.031(5) 0.040(6) C318 0.105(10) 0.132(12) 0.067(7) -0.005(7) 0.014(7) 0.049(9) C319 0.219(19) 0.119(12) 0.075(9) -0.005(8) 0.028(10) 0.094(13) C320 0.203(18) 0.163(16) 0.072(9) -0.013(9) 0.082(11) 0.003(14) O321 0.049(3) 0.092(5) 0.081(5) 0.022(4) 0.021(3) 0.032(3) C322 0.069(7) 0.162(14) 0.135(12) 0.035(11) 0.044(8) 0.057(8) C323 0.053(9) 0.44(4) 0.20(2) -0.09(3) 0.022(11) 0.013(16) N401 0.059(4) 0.050(4) 0.063(4) 0.016(3) 0.037(3) 0.022(3) C402 0.089(7) 0.052(5) 0.100(8) 0.027(5) 0.060(6) 0.029(5) C403 0.084(7) 0.076(6) 0.104(8) 0.035(6) 0.055(7) 0.047(6) C404 0.085(7) 0.070(6) 0.105(9) 0.010(6) 0.060(7) 0.031(5) C405 0.083(7) 0.077(6) 0.067(6) 0.009(5) 0.052(5) 0.024(5) C406 0.059(5) 0.057(5) 0.062(5) 0.014(4) 0.037(4) 0.014(4) C407 0.064(5) 0.069(5) 0.052(5) 0.014(4) 0.032(4) 0.015(4) C408 0.087(7) 0.082(7) 0.076(7) 0.032(6) 0.052(6) 0.016(6) C409 0.102(9) 0.089(8) 0.072(7) 0.030(6) 0.045(6) 0.006(7) C410 0.113(9) 0.073(7) 0.085(8) 0.046(6) 0.045(7) 0.019(6) C411 0.091(7) 0.072(6) 0.077(7) 0.035(5) 0.040(6) 0.021(5) N412 0.066(4) 0.055(4) 0.053(4) 0.020(3) 0.029(3) 0.017(3) C413 0.104(10) 0.114(11) 0.149(13) -0.003(10) 0.077(10) 0.048(9) C414 0.18(2) 0.20(2) 0.47(5) -0.22(3) 0.19(3) -0.027(17) C415 0.30(3) 0.36(4) 0.24(3) 0.10(3) 0.17(3) 0.28(3) C416 0.31(3) 0.143(17) 0.44(4) 0.10(2) 0.32(4) 0.12(2) C417 0.140(13) 0.146(14) 0.116(12) 0.074(11) 0.073(11) 0.012(11) C418 0.22(2) 0.20(2) 0.143(16) 0.091(15) 0.122(16) 0.002(17) C419 0.142(18) 0.53(6) 0.26(3) 0.26(4) 0.040(18) -0.12(3) C420 0.44(5) 0.24(3) 0.34(4) 0.24(3) 0.27(4) 0.11(3) O421 0.088(5) 0.054(3) 0.061(4) 0.002(3) 0.026(3) 0.006(3) N501 0.035(3) 0.053(4) 0.066(4) 0.016(3) 0.024(3) 0.018(3) C502 0.038(4) 0.072(6) 0.081(6) 0.004(5) 0.030(4) 0.008(4) C503 0.044(5) 0.073(6) 0.102(8) -0.012(6) 0.029(5) 0.014(4) C504 0.054(5) 0.061(5) 0.114(8) 0.006(5) 0.050(6) 0.021(4) C505 0.045(4) 0.061(5) 0.097(7) 0.010(5) 0.038(5) 0.018(4) C506 0.036(4) 0.050(4) 0.073(5) 0.020(4) 0.029(4) 0.017(3) C507 0.035(4) 0.048(4) 0.073(5) 0.020(4) 0.026(4) 0.020(3) C508 0.036(4) 0.046(4) 0.096(7) 0.011(4) 0.030(4) 0.012(3) C509 0.036(4) 0.050(4) 0.102(8) 0.009(5) 0.022(4) 0.007(3) C510 0.044(5) 0.052(5) 0.137(10) -0.008(6) 0.032(6) 0.009(4) C511 0.055(5) 0.056(5) 0.100(8) -0.007(5) 0.035(5) 0.014(4) N512 0.033(3) 0.042(3) 0.075(5) 0.012(3) 0.024(3) 0.014(2) C513 0.069(7) 0.125(12) 0.174(15) -0.070(11) 0.055(9) 0.019(7) C514 0.83(10) 0.43(6) 0.62(8) 0.32(6) 0.67(9) 0.48(7) C515 0.143(17) 0.135(17) 0.67(7) -0.17(3) 0.20(3) 0.011(14) C516 0.16(2) 0.25(3) 0.40(5) -0.12(3) 0.01(2) 0.16(2) C517 0.048(5) 0.065(6) 0.152(12) 0.002(7) 0.038(7) 0.002(5) C518 0.135(16) 0.22(2) 0.21(2) 0.064(19) 0.067(16) -0.078(15) C519 0.060(9) 0.18(2) 0.28(3) 0.05(2) -0.012(12) 0.008(11) C520 0.085(10) 0.130(14) 0.43(4) -0.14(2) 0.121(17) -0.056(10) O521 0.086(5) 0.077(5) 0.115(6) 0.058(4) 0.050(5) 0.041(4) C522 0.18(2) 0.136(16) 0.24(3) 0.113(18) -0.009(18) 0.010(15) C523 0.34(4) 0.144(19) 0.20(2) 0.090(18) 0.06(2) 0.00(2) O1E 0.217(12) 0.085(6) 0.133(9) 0.015(6) 0.096(9) 0.028(7) C2E 0.36(5) 0.25(3) 0.34(5) 0.03(3) 0.26(4) 0.12(3) C3E 0.50(8) 0.77(13) 0.57(11) -0.07(9) 0.39(8) 0.29(8) O2 0.212(14) 0.274(18) 0.187(13) 0.151(13) 0.138(11) 0.152(13) O3 0.207(18) 0.093(10) 0.59(4) -0.039(17) 0.05(2) 0.003(11) O4 0.69(6) 0.51(4) 0.32(3) 0.19(3) 0.35(4) 0.44(5) O5 1.14(12) 0.40(5) 0.38(5) 0.20(4) 0.35(6) 0.27(7) O6 0.21(2) 0.33(4) 1.07(10) 0.43(5) 0.01(4) 0.00(2) O7 0.43(4) 0.63(6) 0.44(4) 0.37(4) 0.31(4) 0.36(4) O8 0.21(3) 0.126(19) 0.13(2) 0.038(16) -0.021(18) 0.009(18) _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 W1 C17 2.139(8) . ? W1 C11 2.150(7) . ? W1 C14 2.159(8) . ? W1 C18 2.159(11) . ? W1 C12 2.167(8) . ? W1 C15 2.168(8) . ? W1 C13 2.169(8) . ? W1 C16 2.186(8) . ? W2 C28 2.130(13) . ? W2 C23 2.148(8) . ? W2 C21 2.154(8) . ? W2 C25 2.157(8) . ? W2 C24 2.159(8) . ? W2 C27 2.164(12) . ? W2 C26 2.164(9) . ? W2 C22 2.170(7) . ? W3 C34 2.151(9) . ? W3 C31 2.151(6) . ? W3 C33 2.159(7) . ? W3 C36 2.163(7) . ? W3 C38 2.166(8) . ? W3 C35 2.167(7) . ? W3 C37 2.177(9) . ? W3 C32 2.186(9) . ? Ni1 N11 2.037(6) . ? Ni1 N11 2.037(6) 2_666 ? Ni1 N31 2.038(5) . ? Ni1 N31 2.038(5) 2_666 ? Ni1 N21 2.040(6) . ? Ni1 N21 2.040(6) 2_666 ? Ni2 N22 2.040(6) . ? Ni2 N201 2.051(6) . ? Ni2 N12 2.056(6) . ? Ni2 N32 2.059(7) 2_666 ? Ni2 N212 2.074(6) . ? Ni2 O221 2.142(7) . ? Ni3 N33 2.037(7) . ? Ni3 N13 2.049(7) 2_666 ? Ni3 N23 2.056(7) . ? Ni3 N301 2.072(6) . ? Ni3 N312 2.078(7) . ? Ni3 O321 2.167(6) . ? Ni4 N14 2.043(6) . ? Ni4 N34 2.050(7) . ? Ni4 N412 2.072(7) . ? Ni4 N24 2.083(7) . ? Ni4 N401 2.095(6) . ? Ni4 O421 2.149(6) . ? Ni5 N512 2.060(6) . ? Ni5 N35 2.061(7) . ? Ni5 N25 2.064(7) 2_666 ? Ni5 N15 2.076(7) . ? Ni5 N501 2.078(6) . ? Ni5 O521 2.153(7) . ? C11 N11 1.136(8) . ? C12 N12 1.157(10) . ? C13 N13 1.145(10) . ? N13 Ni3 2.049(7) 2_666 ? C14 N14 1.147(9) . ? C15 N15 1.144(10) . ? C16 N16 1.133(10) . ? C17 N17 1.168(11) . ? C18 N18 1.163(13) . ? C21 N21 1.125(9) . ? C22 N22 1.131(9) . ? C23 N23 1.142(10) . ? C24 N24 1.147(10) . ? C25 N25 1.154(10) . ? N25 Ni5 2.064(7) 2_666 ? C26 N26 1.137(13) . ? C27 N27 1.135(15) . ? C28 N28 1.131(17) . ? C31 N31 1.130(8) . ? C32 N32 1.141(10) . ? N32 Ni2 2.059(7) 2_666 ? C33 N33 1.146(9) . ? C34 N34 1.146(10) . ? C35 N35 1.142(9) . ? C36 N36 1.125(10) . ? C37 N37 1.148(11) . ? C38 N38 1.144(11) . ? N201 C202 1.310(10) . ? N201 C206 1.367(9) . ? C202 C203 1.389(12) . ? C203 C204 1.384(12) . ? C204 C205 1.377(12) . ? C204 C213 1.514(12) . ? C205 C206 1.351(11) . ? C206 C207 1.499(11) . ? C207 N212 1.358(9) . ? C207 C208 1.389(11) . ? C208 C209 1.389(13) . ? C209 C210 1.366(13) . ? C209 C217 1.520(13) . ? C210 C211 1.377(13) . ? C211 N212 1.323(11) . ? C213 C216 1.52(2) . ? C213 C215 1.53(2) . ? C213 C214 1.535(17) . ? C217 C220 1.517(17) . ? C217 C219 1.53(2) . ? C217 C218 1.54(2) . ? O221 C222 1.49(2) . ? C222 C223 1.52(3) . ? N301 C302 1.313(11) . ? N301 C306 1.350(9) . ? C302 C303 1.393(12) . ? C303 C304 1.358(13) . ? C304 C305 1.379(13) . ? C304 C313 1.530(11) . ? C305 C306 1.393(10) . ? C306 C307 1.477(11) . ? C307 N312 1.340(9) . ? C307 C308 1.395(11) . ? C308 C309 1.372(13) . ? C309 C310 1.371(14) . ? C309 C317 1.552(13) . ? C310 C311 1.391(13) . ? C311 N312 1.327(11) . ? C313 C314 1.450(18) . ? C313 C316 1.51(2) . ? C313 C315 1.51(2) . ? C317 C319 1.481(18) . ? C317 C318 1.540(16) . ? C317 C320 1.549(19) . ? O321 C322 1.380(14) . ? C322 C323 1.48(2) . ? N401 C402 1.330(12) . ? N401 C406 1.342(11) . ? C402 C403 1.389(13) . ? C403 C404 1.373(16) . ? C404 C405 1.405(16) . ? C404 C413 1.530(14) . ? C405 C406 1.383(12) . ? C406 C407 1.483(13) . ? C407 N412 1.360(11) . ? C407 C408 1.390(13) . ? C408 C409 1.356(16) . ? C409 C410 1.367(17) . ? C409 C417 1.537(17) . ? C410 C411 1.384(15) . ? C411 N412 1.323(12) . ? C413 C414 1.35(2) . ? C413 C415 1.51(3) . ? C413 C416 1.55(3) . ? C417 C419 1.47(3) . ? C417 C418 1.48(2) . ? C417 C420 1.51(3) . ? N501 C502 1.333(11) . ? N501 C506 1.350(9) . ? C502 C503 1.372(12) . ? C503 C504 1.382(12) . ? C504 C505 1.382(13) . ? C504 C513 1.565(14) . ? C505 C506 1.389(11) . ? C506 C507 1.471(11) . ? C507 N512 1.354(9) . ? C507 C508 1.395(10) . ? C508 C509 1.391(12) . ? C509 C510 1.359(13) . ? C509 C517 1.522(12) . ? C510 C511 1.397(12) . ? C511 N512 1.307(11) . ? C513 C516 1.35(3) . ? C513 C515 1.36(2) . ? C513 C514 1.59(4) . ? C517 C520 1.493(18) . ? C517 C518 1.52(2) . ? C517 C519 1.53(2) . ? O521 C522 1.30(2) . ? C522 C523 1.53(3) . ? O1E C2E 1.45(3) . ? C2E C3E 1.36(7) . ? 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 C17 W1 C11 139.4(3) . . ? C17 W1 C14 113.0(3) . . ? C11 W1 C14 72.7(3) . . ? C17 W1 C18 77.9(4) . . ? C11 W1 C18 136.6(3) . . ? C14 W1 C18 71.0(3) . . ? C17 W1 C12 146.2(3) . . ? C11 W1 C12 72.0(3) . . ? C14 W1 C12 84.8(3) . . ? C18 W1 C12 81.6(4) . . ? C17 W1 C15 71.8(3) . . ? C11 W1 C15 71.2(2) . . ? C14 W1 C15 75.7(3) . . ? C18 W1 C15 120.5(3) . . ? C12 W1 C15 142.1(3) . . ? C17 W1 C13 85.9(3) . . ? C11 W1 C13 73.9(3) . . ? C14 W1 C13 144.7(3) . . ? C18 W1 C13 144.1(3) . . ? C12 W1 C13 95.5(3) . . ? C15 W1 C13 83.2(3) . . ? C17 W1 C16 74.6(3) . . ? C11 W1 C16 128.7(3) . . ? C14 W1 C16 139.3(3) . . ? C18 W1 C16 72.0(3) . . ? C12 W1 C16 73.6(3) . . ? C15 W1 C16 139.7(3) . . ? C13 W1 C16 72.9(3) . . ? C28 W2 C23 145.5(4) . . ? C28 W2 C21 139.6(4) . . ? C23 W2 C21 72.2(3) . . ? C28 W2 C25 88.5(7) . . ? C23 W2 C25 92.1(3) . . ? C21 W2 C25 72.1(3) . . ? C28 W2 C24 113.9(7) . . ? C23 W2 C24 84.7(3) . . ? C21 W2 C24 72.7(3) . . ? C25 W2 C24 143.8(3) . . ? C28 W2 C27 75.9(6) . . ? C23 W2 C27 84.2(5) . . ? C21 W2 C27 137.8(4) . . ? C25 W2 C27 145.0(4) . . ? C24 W2 C27 70.7(4) . . ? C28 W2 C26 74.6(6) . . ? C23 W2 C26 72.7(4) . . ? C21 W2 C26 128.4(4) . . ? C25 W2 C26 72.7(3) . . ? C24 W2 C26 138.7(3) . . ? C27 W2 C26 73.0(4) . . ? C28 W2 C22 70.4(4) . . ? C23 W2 C22 143.9(3) . . ? C21 W2 C22 72.4(3) . . ? C25 W2 C22 83.6(3) . . ? C24 W2 C22 78.3(3) . . ? C27 W2 C22 118.7(5) . . ? C26 W2 C22 137.9(4) . . ? C34 W3 C31 70.5(3) . . ? C34 W3 C33 95.0(3) . . ? C31 W3 C33 74.7(2) . . ? C34 W3 C36 146.1(3) . . ? C31 W3 C36 142.3(3) . . ? C33 W3 C36 89.3(3) . . ? C34 W3 C38 79.5(3) . . ? C31 W3 C38 134.1(3) . . ? C33 W3 C38 143.3(3) . . ? C36 W3 C38 77.2(3) . . ? C34 W3 C35 87.3(3) . . ? C31 W3 C35 73.3(2) . . ? C33 W3 C35 145.1(3) . . ? C36 W3 C35 107.9(3) . . ? C38 W3 C35 71.4(3) . . ? C34 W3 C37 73.7(3) . . ? C31 W3 C37 126.9(3) . . ? C33 W3 C37 70.7(3) . . ? C36 W3 C37 76.1(3) . . ? C38 W3 C37 72.9(3) . . ? C35 W3 C37 141.9(3) . . ? C34 W3 C32 142.3(2) . . ? C31 W3 C32 72.3(3) . . ? C33 W3 C32 80.9(3) . . ? C36 W3 C32 71.6(3) . . ? C38 W3 C32 124.8(3) . . ? C35 W3 C32 76.5(3) . . ? C37 W3 C32 136.8(3) . . ? N11 Ni1 N11 180.00(16) . 2_666 ? N11 Ni1 N31 91.7(2) . . ? N11 Ni1 N31 88.3(2) 2_666 . ? N11 Ni1 N31 88.3(2) . 2_666 ? N11 Ni1 N31 91.7(2) 2_666 2_666 ? N31 Ni1 N31 180.000(1) . 2_666 ? N11 Ni1 N21 90.7(2) . . ? N11 Ni1 N21 89.3(2) 2_666 . ? N31 Ni1 N21 89.0(2) . . ? N31 Ni1 N21 91.0(2) 2_666 . ? N11 Ni1 N21 89.3(2) . 2_666 ? N11 Ni1 N21 90.7(2) 2_666 2_666 ? N31 Ni1 N21 91.0(2) . 2_666 ? N31 Ni1 N21 89.0(2) 2_666 2_666 ? N21 Ni1 N21 180.000(1) . 2_666 ? N22 Ni2 N201 173.4(3) . . ? N22 Ni2 N12 91.8(3) . . ? N201 Ni2 N12 94.8(2) . . ? N22 Ni2 N32 92.9(3) . 2_666 ? N201 Ni2 N32 87.3(3) . 2_666 ? N12 Ni2 N32 92.8(3) . 2_666 ? N22 Ni2 N212 93.8(2) . . ? N201 Ni2 N212 79.6(2) . . ? N12 Ni2 N212 171.3(3) . . ? N32 Ni2 N212 93.5(3) 2_666 . ? N22 Ni2 O221 90.1(3) . . ? N201 Ni2 O221 89.7(3) . . ? N12 Ni2 O221 87.2(3) . . ? N32 Ni2 O221 177.0(3) 2_666 . ? N212 Ni2 O221 86.2(3) . . ? N33 Ni3 N13 90.9(3) . 2_666 ? N33 Ni3 N23 91.7(3) . . ? N13 Ni3 N23 92.1(3) 2_666 . ? N33 Ni3 N301 94.9(3) . . ? N13 Ni3 N301 95.8(2) 2_666 . ? N23 Ni3 N301 169.6(3) . . ? N33 Ni3 N312 92.8(3) . . ? N13 Ni3 N312 173.5(2) 2_666 . ? N23 Ni3 N312 93.2(3) . . ? N301 Ni3 N312 78.6(3) . . ? N33 Ni3 O321 175.8(3) . . ? N13 Ni3 O321 91.0(3) 2_666 . ? N23 Ni3 O321 84.5(3) . . ? N301 Ni3 O321 88.6(3) . . ? N312 Ni3 O321 85.6(3) . . ? N14 Ni4 N34 91.5(3) . . ? N14 Ni4 N412 87.1(3) . . ? N34 Ni4 N412 171.1(3) . . ? N14 Ni4 N24 92.6(3) . . ? N34 Ni4 N24 92.7(3) . . ? N412 Ni4 N24 96.2(3) . . ? N14 Ni4 N401 95.7(3) . . ? N34 Ni4 N401 92.5(3) . . ? N412 Ni4 N401 78.9(3) . . ? N24 Ni4 N401 170.1(3) . . ? N14 Ni4 O421 178.1(3) . . ? N34 Ni4 O421 90.3(3) . . ? N412 Ni4 O421 91.0(3) . . ? N24 Ni4 O421 87.9(3) . . ? N401 Ni4 O421 83.6(3) . . ? N512 Ni5 N35 170.5(2) . . ? N512 Ni5 N25 96.5(3) . 2_666 ? N35 Ni5 N25 92.5(3) . 2_666 ? N512 Ni5 N15 88.5(3) . . ? N35 Ni5 N15 94.5(3) . . ? N25 Ni5 N15 91.8(3) 2_666 . ? N512 Ni5 N501 78.6(2) . . ? N35 Ni5 N501 92.1(3) . . ? N25 Ni5 N501 169.5(3) 2_666 . ? N15 Ni5 N501 97.2(3) . . ? N512 Ni5 O521 85.0(3) . . ? N35 Ni5 O521 92.6(3) . . ? N25 Ni5 O521 85.3(3) 2_666 . ? N15 Ni5 O521 172.4(3) . . ? N501 Ni5 O521 85.1(3) . . ? N11 C11 W1 178.4(6) . . ? C11 N11 Ni1 176.3(6) . . ? N12 C12 W1 178.3(7) . . ? C12 N12 Ni2 177.6(7) . . ? N13 C13 W1 173.8(6) . . ? C13 N13 Ni3 166.7(6) . 2_666 ? N14 C14 W1 176.6(6) . . ? C14 N14 Ni4 173.4(7) . . ? N15 C15 W1 177.1(6) . . ? C15 N15 Ni5 171.7(7) . . ? N16 C16 W1 178.4(8) . . ? N17 C17 W1 178.9(11) . . ? N18 C18 W1 176.8(11) . . ? N21 C21 W2 178.4(6) . . ? C21 N21 Ni1 174.3(6) . . ? N22 C22 W2 177.0(7) . . ? C22 N22 Ni2 175.1(7) . . ? N23 C23 W2 174.5(8) . . ? C23 N23 Ni3 168.0(8) . . ? N24 C24 W2 175.6(7) . . ? C24 N24 Ni4 168.8(7) . . ? N25 C25 W2 176.9(7) . . ? C25 N25 Ni5 175.6(7) . 2_666 ? N26 C26 W2 173.7(15) . . ? N27 C27 W2 177.2(17) . . ? N28 C28 W2 175(2) . . ? N31 C31 W3 177.3(6) . . ? C31 N31 Ni1 177.5(5) . . ? N32 C32 W3 176.1(6) . . ? C32 N32 Ni2 172.5(6) . 2_666 ? N33 C33 W3 173.6(7) . . ? C33 N33 Ni3 161.8(7) . . ? N34 C34 W3 179.3(7) . . ? C34 N34 Ni4 173.2(7) . . ? N35 C35 W3 176.5(6) . . ? C35 N35 Ni5 174.3(7) . . ? N36 C36 W3 176.1(9) . . ? N37 C37 W3 176.5(8) . . ? N38 C38 W3 176.3(9) . . ? C202 N201 C206 118.2(7) . . ? C202 N201 Ni2 125.7(5) . . ? C206 N201 Ni2 115.9(5) . . ? N201 C202 C203 121.8(8) . . ? C204 C203 C202 120.6(8) . . ? C205 C204 C203 116.2(8) . . ? C205 C204 C213 120.1(9) . . ? C203 C204 C213 123.7(9) . . ? C206 C205 C204 121.1(8) . . ? C205 C206 N201 122.0(7) . . ? C205 C206 C207 124.0(7) . . ? N201 C206 C207 114.0(7) . . ? N212 C207 C208 121.4(7) . . ? N212 C207 C206 115.2(6) . . ? C208 C207 C206 123.5(7) . . ? C207 C208 C209 120.8(8) . . ? C210 C209 C208 115.9(8) . . ? C210 C209 C217 124.2(9) . . ? C208 C209 C217 119.9(9) . . ? C209 C210 C211 121.4(9) . . ? N212 C211 C210 122.9(8) . . ? C211 N212 C207 117.5(7) . . ? C211 N212 Ni2 127.1(6) . . ? C207 N212 Ni2 114.8(5) . . ? C204 C213 C216 109.8(12) . . ? C204 C213 C215 110.5(13) . . ? C216 C213 C215 104.6(13) . . ? C204 C213 C214 111.4(10) . . ? C216 C213 C214 109.9(14) . . ? C215 C213 C214 110.4(14) . . ? C220 C217 C209 111.7(10) . . ? C220 C217 C219 111.0(15) . . ? C209 C217 C219 111.4(12) . . ? C220 C217 C218 109.0(16) . . ? C209 C217 C218 108.8(12) . . ? C219 C217 C218 104.7(14) . . ? C222 O221 Ni2 128.4(11) . . ? O221 C222 C223 115.0(19) . . ? C302 N301 C306 118.8(7) . . ? C302 N301 Ni3 126.2(5) . . ? C306 N301 Ni3 114.7(5) . . ? N301 C302 C303 123.2(8) . . ? C304 C303 C302 119.6(9) . . ? C303 C304 C305 117.2(8) . . ? C303 C304 C313 122.6(10) . . ? C305 C304 C313 120.2(9) . . ? C304 C305 C306 121.4(8) . . ? N301 C306 C305 119.8(8) . . ? N301 C306 C307 115.5(6) . . ? C305 C306 C307 124.6(7) . . ? N312 C307 C308 120.2(8) . . ? N312 C307 C306 115.2(6) . . ? C308 C307 C306 124.6(7) . . ? C309 C308 C307 121.1(8) . . ? C310 C309 C308 117.6(8) . . ? C310 C309 C317 122.9(10) . . ? C308 C309 C317 119.5(10) . . ? C309 C310 C311 119.2(9) . . ? N312 C311 C310 122.7(9) . . ? C311 N312 C307 119.1(7) . . ? C311 N312 Ni3 125.6(6) . . ? C307 N312 Ni3 115.1(5) . . ? C314 C313 C316 111.8(18) . . ? C314 C313 C315 111.8(15) . . ? C316 C313 C315 102.8(17) . . ? C314 C313 C304 108.7(10) . . ? C316 C313 C304 110.0(11) . . ? C315 C313 C304 111.7(10) . . ? C319 C317 C318 109.5(13) . . ? C319 C317 C320 108.7(13) . . ? C318 C317 C320 109.0(12) . . ? C319 C317 C309 111.2(10) . . ? C318 C317 C309 108.6(9) . . ? C320 C317 C309 109.7(11) . . ? C322 O321 Ni3 126.8(8) . . ? O321 C322 C323 111.5(14) . . ? C402 N401 C406 118.4(7) . . ? C402 N401 Ni4 126.3(6) . . ? C406 N401 Ni4 114.0(6) . . ? N401 C402 C403 122.2(10) . . ? C404 C403 C402 120.4(10) . . ? C403 C404 C405 117.0(9) . . ? C403 C404 C413 120.2(13) . . ? C405 C404 C413 122.8(13) . . ? C406 C405 C404 119.4(10) . . ? N401 C406 C405 122.4(9) . . ? N401 C406 C407 115.3(7) . . ? C405 C406 C407 122.4(9) . . ? N412 C407 C408 121.6(10) . . ? N412 C407 C406 115.0(8) . . ? C408 C407 C406 123.2(9) . . ? C409 C408 C407 120.2(11) . . ? C408 C409 C410 117.5(10) . . ? C408 C409 C417 122.9(13) . . ? C410 C409 C417 119.5(13) . . ? C409 C410 C411 121.0(11) . . ? N412 C411 C410 121.7(11) . . ? C411 N412 C407 117.9(8) . . ? C411 N412 Ni4 126.6(7) . . ? C407 N412 Ni4 114.8(6) . . ? C414 C413 C415 107(2) . . ? C414 C413 C404 110.9(13) . . ? C415 C413 C404 109.6(14) . . ? C414 C413 C416 120(2) . . ? C415 C413 C416 97.6(18) . . ? C404 C413 C416 110.7(13) . . ? C419 C417 C418 116(2) . . ? C419 C417 C420 106(2) . . ? C418 C417 C420 106.8(18) . . ? C419 C417 C409 105.8(14) . . ? C418 C417 C409 108.2(13) . . ? C420 C417 C409 114.0(16) . . ? C502 N501 C506 117.9(7) . . ? C502 N501 Ni5 125.8(5) . . ? C506 N501 Ni5 114.9(5) . . ? N501 C502 C503 124.0(8) . . ? C502 C503 C504 118.4(9) . . ? C505 C504 C503 118.5(8) . . ? C505 C504 C513 121.3(9) . . ? C503 C504 C513 119.8(9) . . ? C504 C505 C506 119.9(8) . . ? N501 C506 C505 121.2(7) . . ? N501 C506 C507 114.7(6) . . ? C505 C506 C507 124.0(7) . . ? N512 C507 C508 121.1(7) . . ? N512 C507 C506 115.3(6) . . ? C508 C507 C506 123.7(7) . . ? C509 C508 C507 120.5(8) . . ? C510 C509 C508 116.9(8) . . ? C510 C509 C517 122.4(9) . . ? C508 C509 C517 120.7(9) . . ? C509 C510 C511 120.2(9) . . ? N512 C511 C510 123.3(9) . . ? C511 N512 C507 118.1(7) . . ? C511 N512 Ni5 126.4(6) . . ? C507 N512 Ni5 115.5(5) . . ? C516 C513 C515 127(2) . . ? C516 C513 C504 115.9(13) . . ? C515 C513 C504 114.6(12) . . ? C516 C513 C514 92(3) . . ? C515 C513 C514 94(3) . . ? C504 C513 C514 100.8(17) . . ? C520 C517 C518 110.8(17) . . ? C520 C517 C509 112.8(10) . . ? C518 C517 C509 110.5(13) . . ? C520 C517 C519 111.5(17) . . ? C518 C517 C519 102.5(16) . . ? C509 C517 C519 108.1(11) . . ? C522 O521 Ni5 131.2(11) . . ? O521 C522 C523 116.9(19) . . ? C3E C2E O1E 108(4) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 2.417 _refine_diff_density_min -1.105 _refine_diff_density_rms 0.140 #===END