Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_be11mf1n _database_code_depnum_ccdc_archive 'CCDC 275611' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H36 N4 Ni2 O8, C29 H34 N4 NI2 O7, 2.5(C2 H3 N), 3.25(H2 O)' _chemical_formula_sum 'C65 H83.50 N10.50 Ni4 O18.25' _chemical_formula_weight 1538.76 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.3067(18) _cell_length_b 16.4584(19) _cell_length_c 18.009(2) _cell_angle_alpha 111.511(2) _cell_angle_beta 93.653(2) _cell_angle_gamma 112.056(2) _cell_volume 3803.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3080 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 28.06 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1610 _exptl_absorpt_coefficient_mu 1.045 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6762 _exptl_absorpt_correction_T_max 0.8182 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_reflns_number 47616 _diffrn_reflns_av_R_equivalents 0.02720 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13372 _reflns_number_gt 10750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0816P)^2^+10.7461P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13372 _refine_ls_number_parameters 919 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1595 _refine_ls_wR_factor_gt 0.1449 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.030 _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 Ni11 Ni 0.05334(4) 0.50100(4) 0.25027(3) 0.01911(14) Uani 1 1 d . . . Ni12 Ni 0.08171(4) 0.35818(4) 0.09180(3) 0.01683(13) Uani 1 1 d . . . O101 O 0.1790(2) 0.5683(2) 0.33241(17) 0.0263(7) Uani 1 1 d . . . O102 O 0.21735(19) 0.36498(19) 0.11281(17) 0.0196(6) Uani 1 1 d . . . O103 O 0.06179(19) 0.36967(19) 0.20725(16) 0.0190(6) Uani 1 1 d . . . N101 N -0.0192(3) 0.4944(2) 0.3389(2) 0.0234(8) Uani 1 1 d . . . N102 N 0.0273(2) 0.2129(2) 0.0375(2) 0.0198(7) Uani 1 1 d . . . N103 N -0.0900(2) 0.4299(2) 0.1719(2) 0.0205(7) Uani 1 1 d . . . N104 N -0.0665(2) 0.3293(2) 0.0549(2) 0.0192(7) Uani 1 1 d . . . O11W O 0.0475(2) 0.6365(2) 0.27565(18) 0.0270(7) Uani 1 1 d . . . H11W H -0.0061 0.6460 0.2725 0.040 Uiso 1 1 d R . . H11X H 0.0849 0.6936 0.3217 0.040 Uiso 1 1 d R . . O12W O 0.1013(2) 0.3784(2) -0.01526(16) 0.0213(6) Uani 1 1 d . . . H12A H 0.1053 0.3277 -0.0618 0.032 Uiso 1 1 d R . . H12B H 0.1387 0.4215 -0.0144 0.032 Uiso 1 1 d R . . O11 O 0.1257(2) 0.5074(2) 0.15568(17) 0.0201(6) Uani 1 1 d . . . O12 O 0.2251(2) 0.5594(2) 0.08217(18) 0.0253(6) Uani 1 1 d . . . C10 C 0.1912(3) 0.5752(3) 0.1443(3) 0.0206(9) Uani 1 1 d . . . C11 C 0.2268(3) 0.6771(3) 0.2077(3) 0.0277(10) Uani 1 1 d . . . H11A H 0.2863 0.7184 0.1984 0.041 Uiso 1 1 calc R . . H11B H 0.2402 0.6791 0.2625 0.041 Uiso 1 1 calc R . . H11C H 0.1771 0.7003 0.2039 0.041 Uiso 1 1 calc R . . C100 C 0.1942(3) 0.6064(3) 0.4129(3) 0.0271(10) Uani 1 1 d . . . C101 C 0.2896(4) 0.6541(4) 0.4604(3) 0.0374(11) Uani 1 1 d . . . H101 H 0.3410 0.6545 0.4334 0.045 Uiso 1 1 calc R . . C102 C 0.3115(4) 0.7003(4) 0.5448(3) 0.0460(14) Uani 1 1 d . . . H102 H 0.3770 0.7322 0.5749 0.055 Uiso 1 1 calc R . . C103 C 0.2380(4) 0.7006(4) 0.5861(3) 0.0438(13) Uani 1 1 d . . . H103 H 0.2529 0.7339 0.6442 0.053 Uiso 1 1 calc R . . C104 C 0.1432(4) 0.6520(3) 0.5419(3) 0.0340(11) Uani 1 1 d . . . H104 H 0.0929 0.6517 0.5702 0.041 Uiso 1 1 calc R . . C105 C 0.1189(3) 0.6026(3) 0.4555(3) 0.0265(9) Uani 1 1 d . . . C106 C 0.0168(3) 0.5464(3) 0.4160(3) 0.0264(9) Uani 1 1 d . . . H106 H -0.0277 0.5482 0.4504 0.032 Uiso 1 1 calc R . . C107 C -0.1239(3) 0.4395(3) 0.3081(3) 0.0264(9) Uani 1 1 d . . . H10A H -0.1569 0.4662 0.3495 0.032 Uiso 1 1 calc R . . H10B H -0.1427 0.3711 0.2980 0.032 Uiso 1 1 calc R . . C108 C -0.1551(3) 0.4449(3) 0.2283(3) 0.0248(9) Uani 1 1 d . . . H10C H -0.2222 0.3950 0.2005 0.030 Uiso 1 1 calc R . . H10D H -0.1546 0.5089 0.2413 0.030 Uiso 1 1 calc R . . C109 C -0.0960(3) 0.4706(3) 0.1107(3) 0.0237(9) Uani 1 1 d . . . H10E H -0.0459 0.5380 0.1311 0.028 Uiso 1 1 calc R . . H10F H -0.1606 0.4697 0.0994 0.028 Uiso 1 1 calc R . . C110 C -0.0787(3) 0.4043(3) 0.0336(3) 0.0244(9) Uani 1 1 d . . . H11D H -0.1348 0.3742 -0.0135 0.029 Uiso 1 1 calc R . . H11E H -0.0198 0.4410 0.0192 0.029 Uiso 1 1 calc R . . C111 C -0.1054(3) 0.2354(3) -0.0195(2) 0.0238(9) Uani 1 1 d . . . H11F H -0.0814 0.2468 -0.0661 0.029 Uiso 1 1 calc R . . H11G H -0.1771 0.2083 -0.0339 0.029 Uiso 1 1 calc R . . C112 C -0.0757(3) 0.1631(3) -0.0059(3) 0.0235(9) Uani 1 1 d . . . H11H H -0.1160 0.1351 0.0271 0.028 Uiso 1 1 calc R . . H11J H -0.0855 0.1099 -0.0593 0.028 Uiso 1 1 calc R . . C113 C 0.0689(3) 0.1624(3) 0.0469(3) 0.0233(9) Uani 1 1 d . . . H113 H 0.0306 0.0945 0.0249 0.028 Uiso 1 1 calc R . . C114 C 0.1683(3) 0.1974(3) 0.0875(2) 0.0217(9) Uani 1 1 d . . . C115 C 0.1988(4) 0.1287(3) 0.0950(3) 0.0298(10) Uani 1 1 d . . . H115 H 0.1525 0.0632 0.0750 0.036 Uiso 1 1 calc R . . C116 C 0.2927(4) 0.1532(4) 0.1299(3) 0.0332(11) Uani 1 1 d . . . H116 H 0.3110 0.1059 0.1347 0.040 Uiso 1 1 calc R . . C117 C 0.3599(3) 0.2484(4) 0.1577(3) 0.0323(10) Uani 1 1 d . . . H117 H 0.4252 0.2662 0.1819 0.039 Uiso 1 1 calc R . . C118 C 0.3346(3) 0.3183(3) 0.1513(3) 0.0273(10) Uani 1 1 d . . . H118 H 0.3829 0.3827 0.1700 0.033 Uiso 1 1 calc R . . C119 C 0.2378(3) 0.2957(3) 0.1173(2) 0.0209(9) Uani 1 1 d . . . C120 C -0.1228(3) 0.3257(3) 0.1185(2) 0.0190(8) Uani 1 1 d . . . H120 H -0.1933 0.2971 0.0921 0.023 Uiso 1 1 calc R . . C121 C -0.1088(3) 0.2696(3) 0.1641(2) 0.0203(8) Uani 1 1 d . . . C122 C -0.1891(3) 0.1942(3) 0.1664(3) 0.0238(9) Uani 1 1 d . . . H122 H -0.2516 0.1762 0.1362 0.029 Uiso 1 1 calc R . . C123 C -0.1786(3) 0.1456(3) 0.2122(3) 0.0276(10) Uani 1 1 d . . . H123 H -0.2334 0.0941 0.2133 0.033 Uiso 1 1 calc R . . C124 C -0.0876(3) 0.1727(3) 0.2565(3) 0.0289(10) Uani 1 1 d . . . H124 H -0.0801 0.1403 0.2888 0.035 Uiso 1 1 calc R . . C125 C -0.0070(3) 0.2468(3) 0.2542(3) 0.0247(9) Uani 1 1 d . . . H125 H 0.0551 0.2636 0.2844 0.030 Uiso 1 1 calc R . . C126 C -0.0152(3) 0.2974(3) 0.2085(2) 0.0192(8) Uani 1 1 d . . . Ni21 Ni 0.72709(4) 0.72227(4) 0.13843(3) 0.01847(14) Uani 1 1 d . . . Ni22 Ni 0.65379(4) 0.68943(4) 0.28816(3) 0.01991(14) Uani 1 1 d . . . O201 O 0.86695(19) 0.7416(2) 0.14998(16) 0.0202(6) Uani 1 1 d . . . O202 O 0.7559(2) 0.6734(2) 0.34768(17) 0.0238(6) Uani 1 1 d . . . O203 O 0.74967(19) 0.7988(2) 0.26289(16) 0.0199(6) Uani 1 1 d . . . N201 N 0.7639(2) 0.8367(2) 0.1100(2) 0.0216(7) Uani 1 1 d . . . N202 N 0.6395(2) 0.7776(2) 0.3927(2) 0.0222(7) Uani 1 1 d . . . N203 N 0.5866(2) 0.7186(3) 0.1188(2) 0.0222(7) Uani 1 1 d . . . N204 N 0.5350(2) 0.7042(3) 0.2331(2) 0.0225(7) Uani 1 1 d . . . O21W O 0.6894(2) 0.6169(2) 0.01578(19) 0.0238(7) Uani 1 1 d . . . O21 O 0.6734(2) 0.60875(19) 0.17652(16) 0.0210(6) Uani 1 1 d . . . O20 O 0.6857(2) 0.4897(2) 0.07509(17) 0.0277(7) Uani 1 1 d . . . C20 C 0.6642(3) 0.5217(3) 0.1417(2) 0.0220(9) Uani 1 1 d . . . C21 C 0.6229(3) 0.4559(3) 0.1830(3) 0.0308(10) Uani 1 1 d . . . H21A H 0.6251 0.3938 0.1527 0.046 Uiso 1 1 calc R . . H21B H 0.5556 0.4451 0.1836 0.046 Uiso 1 1 calc R . . H21C H 0.6612 0.4857 0.2394 0.046 Uiso 1 1 calc R . . O22 O 0.5372(2) 0.5718(2) 0.30181(18) 0.0272(7) Uani 1 1 d . . . O23 O 0.4275(3) 0.5057(3) 0.3612(2) 0.0455(9) Uani 1 1 d . . . H23 H 0.3798 0.5040 0.3211 0.050 Uiso 1 1 d . . . C22 C 0.5166(4) 0.5408(4) 0.3536(3) 0.0355(11) Uani 1 1 d . . . C23 C 0.5870(4) 0.5376(5) 0.4132(4) 0.0560(16) Uani 1 1 d . . . H23A H 0.5634 0.4719 0.4100 0.084 Uiso 1 1 calc R . . H23B H 0.5929 0.5827 0.4690 0.084 Uiso 1 1 calc R . . H23C H 0.6504 0.5559 0.3995 0.084 Uiso 1 1 calc R . . C200 C 0.9424(3) 0.8258(3) 0.1737(2) 0.0218(9) Uani 1 1 d . . . C201 C 1.0349(3) 0.8377(3) 0.2074(2) 0.0238(9) Uani 1 1 d . . . H201 H 1.0408 0.7848 0.2134 0.029 Uiso 1 1 calc R . . C202 C 1.1168(3) 0.9236(3) 0.2317(3) 0.0296(10) Uani 1 1 d . . . H202 H 1.1773 0.9291 0.2550 0.035 Uiso 1 1 calc R . . C203 C 1.1119(3) 1.0025(3) 0.2226(3) 0.0302(10) Uani 1 1 d . . . H203 H 1.1683 1.0614 0.2388 0.036 Uiso 1 1 calc R . . C204 C 1.0222(3) 0.9926(3) 0.1891(3) 0.0277(10) Uani 1 1 d . . . H204 H 1.0181 1.0458 0.1825 0.033 Uiso 1 1 calc R . . C205 C 0.9376(3) 0.9069(3) 0.1647(2) 0.0225(9) Uani 1 1 d . . . C206 C 0.8484(3) 0.9049(3) 0.1295(2) 0.0245(9) Uani 1 1 d . . . H206 H 0.8536 0.9595 0.1202 0.029 Uiso 1 1 calc R . . C207 C 0.6810(3) 0.8489(3) 0.0778(3) 0.0266(9) Uani 1 1 d . . . H20A H 0.6907 0.8614 0.0285 0.032 Uiso 1 1 calc R . . H20B H 0.6754 0.9048 0.1197 0.032 Uiso 1 1 calc R . . C208 C 0.5887(3) 0.7567(3) 0.0557(3) 0.0278(10) Uani 1 1 d . . . H20C H 0.5316 0.7705 0.0502 0.033 Uiso 1 1 calc R . . H20D H 0.5846 0.7070 0.0021 0.033 Uiso 1 1 calc R . . C209 C 0.5050(3) 0.6187(3) 0.0879(3) 0.0264(9) Uani 1 1 d . . . H20E H 0.5290 0.5687 0.0648 0.032 Uiso 1 1 calc R . . H20F H 0.4537 0.6089 0.0448 0.032 Uiso 1 1 calc R . . C210 C 0.4661(3) 0.6135(3) 0.1628(3) 0.0265(9) Uani 1 1 d . . . H21D H 0.3998 0.6099 0.1573 0.032 Uiso 1 1 calc R . . H21E H 0.4645 0.5562 0.1700 0.032 Uiso 1 1 calc R . . C211 C 0.4876(3) 0.7336(3) 0.3015(3) 0.0272(10) Uani 1 1 d . . . H21F H 0.4444 0.6753 0.3077 0.033 Uiso 1 1 calc R . . H21G H 0.4469 0.7629 0.2874 0.033 Uiso 1 1 calc R . . C212 C 0.5607(3) 0.8060(3) 0.3835(3) 0.0269(9) Uani 1 1 d . . . H21H H 0.5875 0.8716 0.3851 0.032 Uiso 1 1 calc R . . H21I H 0.5280 0.8072 0.4293 0.032 Uiso 1 1 calc R . . C213 C 0.6962(3) 0.8150(3) 0.4637(3) 0.0256(9) Uani 1 1 d . . . H213 H 0.6831 0.8587 0.5081 0.031 Uiso 1 1 calc R . . C214 C 0.7783(3) 0.7965(3) 0.4821(3) 0.0238(9) Uani 1 1 d . . . C215 C 0.8369(3) 0.8522(3) 0.5630(3) 0.0306(10) Uani 1 1 d . . . H215 H 0.8208 0.8991 0.6010 0.037 Uiso 1 1 calc R . . C216 C 0.9164(4) 0.8407(4) 0.5885(3) 0.0350(11) Uani 1 1 d . . . H216 H 0.9559 0.8809 0.6425 0.042 Uiso 1 1 calc R . . C217 C 0.9382(4) 0.7690(3) 0.5339(3) 0.0321(10) Uani 1 1 d . . . H217 H 0.9917 0.7589 0.5511 0.039 Uiso 1 1 calc R . . C218 C 0.8816(3) 0.7128(3) 0.4545(3) 0.0274(10) Uani 1 1 d . . . H218 H 0.8967 0.6637 0.4186 0.033 Uiso 1 1 calc R . . C219 C 0.8024(3) 0.7256(3) 0.4248(2) 0.0229(9) Uani 1 1 d . . . C220 C 0.5635(3) 0.7736(3) 0.1943(3) 0.0230(9) Uani 1 1 d . . . H220 H 0.5053 0.7827 0.1781 0.028 Uiso 1 1 calc R . . C221 C 0.6426(3) 0.8710(3) 0.2519(2) 0.0222(9) Uani 1 1 d . . . C222 C 0.6236(3) 0.9517(3) 0.2774(3) 0.0282(10) Uani 1 1 d . . . H222 H 0.5637 0.9464 0.2531 0.034 Uiso 1 1 calc R . . C223 C 0.6900(3) 1.0396(3) 0.3373(3) 0.0297(10) Uani 1 1 d . . . H223 H 0.6759 1.0943 0.3547 0.036 Uiso 1 1 calc R . . C224 C 0.7776(3) 1.0467(3) 0.3718(3) 0.0310(10) Uani 1 1 d . . . H224 H 0.8236 1.1066 0.4136 0.037 Uiso 1 1 calc R . . C225 C 0.7992(3) 0.9670(3) 0.3460(3) 0.0253(9) Uani 1 1 d . . . H225 H 0.8602 0.9734 0.3691 0.030 Uiso 1 1 calc R . . C226 C 0.7311(3) 0.8774(3) 0.2859(2) 0.0202(8) Uani 1 1 d . . . H21W H 0.690(4) 0.568(4) 0.020(3) 0.033(15) Uiso 1 1 d . . . H21X H 0.724(5) 0.623(5) -0.013(4) 0.06(2) Uiso 1 1 d . . . O1W O 0.3083(2) 0.5144(2) 0.26554(19) 0.0319(7) Uani 1 1 d . . . H1WA H 0.2641 0.5367 0.2893 0.048 Uiso 1 1 d R . . H1WB H 0.2725 0.4655 0.2095 0.048 Uiso 1 1 d R . . O2W O 0.8902(2) 0.6663(2) 0.25781(18) 0.0274(7) Uani 1 1 d . . . H2WA H 0.8808 0.6842 0.2214 0.041 Uiso 1 1 d R . . H2WB H 0.8420 0.6617 0.2839 0.041 Uiso 1 1 d R . . O3W O 0.3347(3) 0.6986(3) 0.0281(3) 0.0590(12) Uani 1 1 d . . . H3WA H 0.2990 0.6625 0.0575 0.089 Uiso 1 1 d R . . H3WB H 0.3221 0.6423 -0.0219 0.089 Uiso 1 1 d R . . N1S N 1.1265(4) 0.8367(4) 0.4055(3) 0.0506(12) Uani 1 1 d . . . C10S C 1.0691(4) 0.8652(4) 0.4046(3) 0.0365(11) Uani 1 1 d . . . C11S C 0.9955(4) 0.8999(3) 0.4023(3) 0.0372(11) Uani 1 1 d . . . H11I H 1.0228 0.9608 0.3965 0.056 Uiso 1 1 calc R . . H11K H 0.9731 0.9106 0.4534 0.056 Uiso 1 1 calc R . . H11L H 0.9407 0.8518 0.3556 0.056 Uiso 1 1 calc R . . N2S N 0.3976(8) 0.2650(8) 0.3740(7) 0.056(3) Uiso 0.50 1 d P . . C20S C 0.3422(6) 0.2830(6) 0.3610(5) 0.031(18) Uiso 0.50 1 d P . . C21S C 0.2679(7) 0.3082(7) 0.3472(6) 0.035(2) Uiso 0.50 1 d P . . H21J H 0.2125 0.2744 0.3658 0.052 Uiso 0.50 1 calc PR . . H21K H 0.2481 0.2898 0.2884 0.052 Uiso 0.50 1 calc PR . . H21L H 0.2905 0.3782 0.3776 0.052 Uiso 0.50 1 calc PR . . N3S N 0.3730(14) -0.0753(14) 0.3202(12) 0.046(5) Uiso 0.25 1 d PD A 1 C30S C 0.3696(14) -0.0782(14) 0.3880(13) 0.025(4) Uiso 0.25 1 d PD A 1 C31S C 0.3608(12) -0.0999(14) 0.4508(9) 0.031(4) Uiso 0.25 1 d PD A 1 H31A H 0.3273 -0.1702 0.4313 0.025 Uiso 0.25 1 calc PR A 1 H31B H 0.3233 -0.0698 0.4832 0.025 Uiso 0.25 1 calc PR A 1 H31C H 0.4253 -0.0758 0.4850 0.025 Uiso 0.25 1 calc PR A 1 N4S N 0.5648(19) 0.1744(19) 0.1244(16) 0.075(7) Uiso 0.25 1 d P B 2 C40S C 0.5626(15) 0.1552(15) 0.0583(13) 0.068(5) Uiso 0.25 1 d P B 2 C41S C 0.601(2) 0.127(2) -0.0203(19) 0.075(8) Uiso 0.25 1 d P B 2 H41A H 0.6593 0.1827 -0.0160 0.112 Uiso 0.25 1 calc PR B 2 H41B H 0.5514 0.1070 -0.0683 0.112 Uiso 0.25 1 calc PR B 2 H41C H 0.6182 0.0733 -0.0263 0.112 Uiso 0.25 1 calc PR B 2 N5S N 0.395(2) -0.041(3) 0.370(2) 0.04(8) Uiso 0.25 1 d PD C 3 C50S C 0.3830(13) -0.0631(13) 0.4219(14) 0.022(4) Uiso 0.25 1 d PD C 3 C51S C 0.3520(12) -0.1270(13) 0.4563(10) 0.022(4) Uiso 0.25 1 d PD C 3 H51A H 0.2851 -0.1401 0.4609 0.033 Uiso 0.25 1 calc PR C 3 H51B H 0.3939 -0.0995 0.5110 0.033 Uiso 0.25 1 calc PR C 3 H51C H 0.3548 -0.1874 0.4216 0.033 Uiso 0.25 1 calc PR C 3 N6S N 0.4693(17) 0.1025(18) 0.2662(15) 0.069(6) Uiso 0.25 1 d PD D 4 C60S C 0.5157(18) 0.1348(18) 0.2392(15) 0.052(6) Uiso 0.25 1 d PD D 4 C61S C 0.575(2) 0.203(2) 0.215(2) 0.086(9) Uiso 0.25 1 d PD D 4 H61A H 0.5718 0.2643 0.2445 0.128 Uiso 0.25 1 calc PR D 4 H61B H 0.5534 0.1805 0.1560 0.128 Uiso 0.25 1 calc PR D 4 H61C H 0.6418 0.2110 0.2281 0.128 Uiso 0.25 1 calc PR D 4 O4W O 0.4058(19) 0.011(2) 0.4035(17) 0.06(7) Uiso 0.25 1 d P E 4 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 Ni11 0.0212(3) 0.0204(3) 0.0163(3) 0.0068(2) 0.0060(2) 0.0103(2) Ni12 0.0173(3) 0.0177(3) 0.0149(3) 0.0059(2) 0.0042(2) 0.0078(2) O101 0.0288(16) 0.0311(16) 0.0153(14) 0.0053(13) 0.0032(12) 0.0138(14) O102 0.0184(14) 0.0184(14) 0.0208(14) 0.0071(12) 0.0033(11) 0.0081(12) O103 0.0192(14) 0.0216(14) 0.0162(14) 0.0075(12) 0.0034(11) 0.0093(12) N101 0.0284(19) 0.0222(18) 0.0220(19) 0.0091(15) 0.0089(15) 0.0131(16) N102 0.0193(17) 0.0194(17) 0.0174(17) 0.0047(14) 0.0058(14) 0.0074(14) N103 0.0208(18) 0.0250(18) 0.0237(18) 0.0135(15) 0.0081(14) 0.0145(15) N104 0.0200(17) 0.0205(17) 0.0170(17) 0.0085(14) 0.0033(14) 0.0081(14) O11W 0.0247(16) 0.0235(15) 0.0297(16) 0.0064(13) 0.0054(13) 0.0121(13) O12W 0.0226(15) 0.0222(15) 0.0180(14) 0.0082(12) 0.0077(12) 0.0085(12) O11 0.0200(14) 0.0208(14) 0.0197(14) 0.0085(12) 0.0061(11) 0.0088(12) O12 0.0237(15) 0.0283(16) 0.0226(15) 0.0109(13) 0.0076(12) 0.0092(13) C10 0.017(2) 0.024(2) 0.024(2) 0.0125(18) 0.0033(17) 0.0094(17) C11 0.025(2) 0.020(2) 0.029(2) 0.0074(19) 0.0062(19) 0.0043(18) C100 0.037(3) 0.021(2) 0.020(2) 0.0069(18) 0.0058(19) 0.0106(19) C101 0.034(3) 0.038(3) 0.026(2) 0.008(2) 0.004(2) 0.006(2) C102 0.046(3) 0.041(3) 0.025(3) 0.006(2) -0.002(2) 0.002(3) C103 0.059(4) 0.030(3) 0.018(2) 0.003(2) 0.004(2) 0.002(2) C104 0.050(3) 0.021(2) 0.021(2) 0.0073(19) 0.010(2) 0.007(2) C105 0.042(3) 0.020(2) 0.017(2) 0.0082(17) 0.0061(19) 0.013(2) C106 0.039(3) 0.022(2) 0.024(2) 0.0119(19) 0.015(2) 0.016(2) C107 0.029(2) 0.028(2) 0.027(2) 0.0125(19) 0.0150(19) 0.0151(19) C108 0.024(2) 0.027(2) 0.027(2) 0.0102(19) 0.0110(18) 0.0150(19) C109 0.024(2) 0.028(2) 0.023(2) 0.0146(18) 0.0047(17) 0.0128(18) C110 0.025(2) 0.033(2) 0.026(2) 0.0185(19) 0.0078(18) 0.0163(19) C111 0.021(2) 0.028(2) 0.015(2) 0.0039(17) 0.0009(16) 0.0078(18) C112 0.019(2) 0.022(2) 0.019(2) 0.0019(17) 0.0017(16) 0.0056(17) C113 0.027(2) 0.019(2) 0.021(2) 0.0075(17) 0.0070(17) 0.0080(18) C114 0.025(2) 0.024(2) 0.019(2) 0.0099(17) 0.0070(17) 0.0120(18) C115 0.038(3) 0.028(2) 0.030(2) 0.016(2) 0.010(2) 0.017(2) C116 0.040(3) 0.041(3) 0.038(3) 0.025(2) 0.013(2) 0.028(2) C117 0.028(2) 0.044(3) 0.034(3) 0.020(2) 0.007(2) 0.021(2) C118 0.023(2) 0.035(2) 0.028(2) 0.015(2) 0.0077(18) 0.013(2) C119 0.023(2) 0.027(2) 0.0148(19) 0.0086(17) 0.0090(16) 0.0128(18) C120 0.0152(19) 0.023(2) 0.020(2) 0.0085(17) 0.0051(16) 0.0089(16) C121 0.023(2) 0.022(2) 0.019(2) 0.0078(17) 0.0076(17) 0.0129(17) C122 0.022(2) 0.025(2) 0.020(2) 0.0063(18) 0.0058(17) 0.0080(18) C123 0.029(2) 0.023(2) 0.029(2) 0.0111(19) 0.0111(19) 0.0088(19) C124 0.038(3) 0.030(2) 0.027(2) 0.018(2) 0.011(2) 0.016(2) C125 0.026(2) 0.028(2) 0.023(2) 0.0127(19) 0.0057(18) 0.0135(19) C126 0.022(2) 0.019(2) 0.018(2) 0.0073(16) 0.0085(16) 0.0106(17) Ni21 0.0164(3) 0.0203(3) 0.0145(3) 0.0047(2) 0.0033(2) 0.0063(2) Ni22 0.0194(3) 0.0198(3) 0.0155(3) 0.0040(2) 0.0049(2) 0.0065(2) O201 0.0189(14) 0.0214(14) 0.0159(14) 0.0055(12) 0.0043(11) 0.0063(12) O202 0.0282(16) 0.0247(15) 0.0149(14) 0.0050(12) 0.0042(12) 0.0111(13) O203 0.0181(14) 0.0216(14) 0.0165(14) 0.0052(12) 0.0037(11) 0.0076(12) N201 0.0222(19) 0.0240(18) 0.0179(17) 0.0081(15) 0.0050(14) 0.0100(16) N202 0.0203(18) 0.0238(18) 0.0193(18) 0.0077(15) 0.0068(14) 0.0071(15) N203 0.0189(17) 0.0250(18) 0.0160(17) 0.0040(15) 0.0011(14) 0.0075(15) N204 0.0174(17) 0.0241(18) 0.0190(17) 0.0040(15) 0.0052(14) 0.0067(15) O21W 0.0238(16) 0.0268(17) 0.0178(15) 0.0076(13) 0.0081(13) 0.0092(14) O21 0.0191(14) 0.0188(14) 0.0171(14) 0.0030(12) 0.0024(11) 0.0048(12) O20 0.0312(17) 0.0284(16) 0.0185(15) 0.0024(13) 0.0044(13) 0.0154(14) C20 0.0143(19) 0.022(2) 0.020(2) 0.0006(17) -0.0031(16) 0.0066(17) C21 0.028(2) 0.026(2) 0.036(3) 0.011(2) 0.011(2) 0.012(2) O22 0.0268(16) 0.0254(16) 0.0241(16) 0.0092(13) 0.0073(13) 0.0070(13) O23 0.0300(19) 0.058(2) 0.045(2) 0.0265(19) 0.0096(16) 0.0106(18) C22 0.030(3) 0.032(3) 0.037(3) 0.013(2) 0.005(2) 0.007(2) C23 0.037(3) 0.072(4) 0.061(4) 0.042(4) 0.008(3) 0.014(3) C200 0.022(2) 0.026(2) 0.0117(19) 0.0026(16) 0.0060(16) 0.0097(18) C201 0.023(2) 0.030(2) 0.0146(19) 0.0069(17) 0.0056(17) 0.0104(19) C202 0.021(2) 0.038(3) 0.017(2) 0.0045(19) 0.0035(17) 0.007(2) C203 0.023(2) 0.029(2) 0.020(2) 0.0003(18) 0.0052(18) 0.0016(19) C204 0.032(2) 0.022(2) 0.019(2) 0.0034(18) 0.0076(18) 0.0073(19) C205 0.023(2) 0.023(2) 0.0150(19) 0.0030(17) 0.0054(16) 0.0084(18) C206 0.032(2) 0.023(2) 0.018(2) 0.0065(17) 0.0100(18) 0.0122(19) C207 0.027(2) 0.033(2) 0.024(2) 0.0143(19) 0.0049(18) 0.015(2) C208 0.026(2) 0.036(3) 0.021(2) 0.0106(19) 0.0035(18) 0.014(2) C209 0.019(2) 0.026(2) 0.021(2) 0.0027(18) -0.0009(17) 0.0041(18) C210 0.019(2) 0.025(2) 0.023(2) 0.0034(18) 0.0032(17) 0.0033(18) C211 0.019(2) 0.034(2) 0.023(2) 0.0074(19) 0.0082(18) 0.0097(19) C212 0.024(2) 0.032(2) 0.020(2) 0.0050(19) 0.0096(18) 0.0124(19) C213 0.029(2) 0.024(2) 0.019(2) 0.0060(18) 0.0106(18) 0.0077(19) C214 0.024(2) 0.027(2) 0.020(2) 0.0113(18) 0.0069(17) 0.0098(18) C215 0.038(3) 0.029(2) 0.019(2) 0.0060(19) 0.0041(19) 0.013(2) C216 0.043(3) 0.034(3) 0.019(2) 0.007(2) 0.000(2) 0.014(2) C217 0.037(3) 0.036(3) 0.025(2) 0.013(2) 0.002(2) 0.018(2) C218 0.035(3) 0.025(2) 0.024(2) 0.0100(19) 0.0062(19) 0.015(2) C219 0.027(2) 0.020(2) 0.018(2) 0.0091(17) 0.0065(17) 0.0050(18) C220 0.017(2) 0.026(2) 0.021(2) 0.0058(18) 0.0041(17) 0.0092(18) C221 0.021(2) 0.023(2) 0.018(2) 0.0055(17) 0.0056(17) 0.0091(18) C222 0.029(2) 0.031(2) 0.026(2) 0.011(2) 0.0072(19) 0.015(2) C223 0.036(3) 0.027(2) 0.030(2) 0.012(2) 0.012(2) 0.017(2) C224 0.036(3) 0.024(2) 0.022(2) 0.0037(19) 0.0055(19) 0.007(2) C225 0.025(2) 0.025(2) 0.020(2) 0.0067(18) 0.0037(17) 0.0071(18) C226 0.021(2) 0.020(2) 0.0156(19) 0.0064(16) 0.0066(16) 0.0060(17) O1W 0.0243(16) 0.0335(18) 0.0269(17) 0.0038(14) 0.0022(13) 0.0104(14) O2W 0.0323(17) 0.0341(17) 0.0260(16) 0.0158(14) 0.0116(13) 0.0207(14) O3W 0.040(2) 0.040(2) 0.081(3) 0.012(2) 0.012(2) 0.0139(18) N1S 0.050(3) 0.044(3) 0.039(3) 0.003(2) -0.003(2) 0.018(2) C10S 0.041(3) 0.031(3) 0.024(2) 0.003(2) 0.003(2) 0.011(2) C11S 0.047(3) 0.024(2) 0.037(3) 0.009(2) 0.018(2) 0.015(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni11 O101 1.988(3) . ? Ni11 N101 2.013(4) . ? Ni11 O103 2.070(3) . ? Ni11 O11 2.103(3) . ? Ni11 O11W 2.144(3) . ? Ni11 N103 2.155(3) . ? Ni12 N102 2.013(3) . ? Ni12 O102 2.040(3) . ? Ni12 O103 2.071(3) . ? Ni12 O12W 2.094(3) . ? Ni12 O11 2.097(3) . ? Ni12 N104 2.140(3) . ? O101 C100 1.315(5) . ? O102 C119 1.318(5) . ? O103 C126 1.332(5) . ? N101 C106 1.282(6) . ? N101 C107 1.458(6) . ? N102 C113 1.271(5) . ? N102 C112 1.473(5) . ? N103 C120 1.483(5) . ? N103 C108 1.488(5) . ? N103 C109 1.498(5) . ? N104 C120 1.483(5) . ? N104 C110 1.489(5) . ? N104 C111 1.491(5) . ? O11W H11W 0.8943 . ? O11W H11X 0.9286 . ? O12W H12A 0.9666 . ? O12W H12B 0.7199 . ? O11 C10 1.283(5) . ? O12 C10 1.245(5) . ? C10 C11 1.498(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C100 C101 1.403(7) . ? C100 C105 1.420(6) . ? C101 C102 1.378(7) . ? C101 H101 0.9500 . ? C102 C103 1.388(8) . ? C102 H102 0.9500 . ? C103 C104 1.376(8) . ? C103 H103 0.9500 . ? C104 C105 1.410(6) . ? C104 H104 0.9500 . ? C105 C106 1.448(7) . ? C106 H106 0.9500 . ? C107 C108 1.530(6) . ? C107 H10A 0.9900 . ? C107 H10B 0.9900 . ? C108 H10C 0.9900 . ? C108 H10D 0.9900 . ? C109 C110 1.531(6) . ? C109 H10E 0.9900 . ? C109 H10F 0.9900 . ? C110 H11D 0.9900 . ? C110 H11E 0.9900 . ? C111 C112 1.513(6) . ? C111 H11F 0.9900 . ? C111 H11G 0.9900 . ? C112 H11H 0.9900 . ? C112 H11J 0.9900 . ? C113 C114 1.439(6) . ? C113 H113 0.9500 . ? C114 C115 1.419(6) . ? C114 C119 1.427(6) . ? C115 C116 1.374(7) . ? C115 H115 0.9500 . ? C116 C117 1.382(7) . ? C116 H116 0.9500 . ? C117 C118 1.384(6) . ? C117 H117 0.9500 . ? C118 C119 1.418(6) . ? C118 H118 0.9500 . ? C120 C121 1.502(6) . ? C120 H120 1.0000 . ? C121 C122 1.397(6) . ? C121 C126 1.412(6) . ? C122 C123 1.382(6) . ? C122 H122 0.9500 . ? C123 C124 1.380(7) . ? C123 H123 0.9500 . ? C124 C125 1.387(6) . ? C124 H124 0.9500 . ? C125 C126 1.398(6) . ? C125 H125 0.9500 . ? Ni21 N201 2.018(3) . ? Ni21 O201 2.027(3) . ? Ni21 O203 2.058(3) . ? Ni21 O21W 2.120(3) . ? Ni21 O21 2.120(3) . ? Ni21 N203 2.132(3) . ? Ni22 O202 1.991(3) . ? Ni22 N202 1.996(3) . ? Ni22 O203 2.075(3) . ? Ni22 O21 2.077(3) . ? Ni22 N204 2.151(4) . ? Ni22 O22 2.192(3) . ? O201 C200 1.319(5) . ? O202 C219 1.309(5) . ? O203 C226 1.350(5) . ? N201 C206 1.272(6) . ? N201 C207 1.474(5) . ? N202 C213 1.284(5) . ? N202 C212 1.468(6) . ? N203 C220 1.481(5) . ? N203 C208 1.482(6) . ? N203 C209 1.507(5) . ? N204 C210 1.485(5) . ? N204 C211 1.489(5) . ? N204 C220 1.495(6) . ? O21W H21W 0.85(6) . ? O21W H21X 0.77(7) . ? O21 C20 1.282(5) . ? O20 C20 1.242(5) . ? C20 C21 1.505(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O22 C22 1.222(6) . ? O23 C22 1.304(6) . ? O23 H23 0.9791 . ? C22 C23 1.502(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C200 C201 1.416(6) . ? C200 C205 1.429(6) . ? C201 C202 1.381(6) . ? C201 H201 0.9500 . ? C202 C203 1.395(7) . ? C202 H202 0.9500 . ? C203 C204 1.389(7) . ? C203 H203 0.9500 . ? C204 C205 1.400(6) . ? C204 H204 0.9500 . ? C205 C206 1.452(6) . ? C206 H206 0.9500 . ? C207 C208 1.527(6) . ? C207 H20A 0.9900 . ? C207 H20B 0.9900 . ? C208 H20C 0.9900 . ? C208 H20D 0.9900 . ? C209 C210 1.528(6) . ? C209 H20E 0.9900 . ? C209 H20F 0.9900 . ? C210 H21D 0.9900 . ? C210 H21E 0.9900 . ? C211 C212 1.533(6) . ? C211 H21F 0.9900 . ? C211 H21G 0.9900 . ? C212 H21H 0.9900 . ? C212 H21I 0.9900 . ? C213 C214 1.446(6) . ? C213 H213 0.9500 . ? C214 C215 1.416(6) . ? C214 C219 1.432(6) . ? C215 C216 1.374(7) . ? C215 H215 0.9500 . ? C216 C217 1.400(7) . ? C216 H216 0.9500 . ? C217 C218 1.386(6) . ? C217 H217 0.9500 . ? C218 C219 1.410(6) . ? C218 H218 0.9500 . ? C220 C221 1.508(6) . ? C220 H220 1.0000 . ? C221 C222 1.386(6) . ? C221 C226 1.400(6) . ? C222 C223 1.379(7) . ? C222 H222 0.9500 . ? C223 C224 1.387(7) . ? C223 H223 0.9500 . ? C224 C225 1.394(6) . ? C224 H224 0.9500 . ? C225 C226 1.401(6) . ? C225 H225 0.9500 . ? O1W H1WA 0.9414 . ? O1W H1WB 0.9840 . ? O2W H2WA 0.8358 . ? O2W H2WB 0.8927 . ? O3W H3WA 0.9787 . ? O3W H3WB 0.9678 . ? N1S C10S 1.143(7) . ? C10S C11S 1.447(7) . ? C11S H11I 0.9800 . ? C11S H11K 0.9800 . ? C11S H11L 0.9800 . ? N2S C20S 1.036(12) . ? C20S C21S 1.387(13) . ? C21S H21J 0.9800 . ? C21S H21K 0.9800 . ? C21S H21L 0.9800 . ? N3S C30S 1.24(3) . ? C30S C31S 1.30(2) . ? C31S H31A 0.9800 . ? C31S H31B 0.9800 . ? C31S H31C 0.9800 . ? N4S C40S 1.11(3) . ? C40S C41S 1.55(4) . ? C41S H41A 0.9800 . ? C41S H41B 0.9800 . ? C41S H41C 0.9800 . ? N5S C50S 1.12(3) . ? C50S C51S 1.36(2) . ? C51S H51A 0.9800 . ? C51S H51B 0.9800 . ? C51S H51C 0.9800 . ? N6S C60S 0.99(2) . ? C60S C61S 1.38(3) . ? C61S H61A 0.9800 . ? C61S H61B 0.9800 . ? C61S H61C 0.9800 . ? 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 O101 Ni11 N101 90.49(13) . . ? O101 Ni11 O103 92.96(12) . . ? N101 Ni11 O103 102.11(12) . . ? O101 Ni11 O11 90.97(11) . . ? N101 Ni11 O11 178.43(13) . . ? O103 Ni11 O11 78.38(11) . . ? O101 Ni11 O11W 90.58(12) . . ? N101 Ni11 O11W 86.47(13) . . ? O103 Ni11 O11W 170.68(11) . . ? O11 Ni11 O11W 92.95(11) . . ? O101 Ni11 N103 174.02(12) . . ? N101 Ni11 N103 83.59(14) . . ? O103 Ni11 N103 89.13(12) . . ? O11 Ni11 N103 94.94(12) . . ? O11W Ni11 N103 88.21(12) . . ? N102 Ni12 O102 89.27(12) . . ? N102 Ni12 O103 96.39(12) . . ? O102 Ni12 O103 94.60(11) . . ? N102 Ni12 O12W 95.99(12) . . ? O102 Ni12 O12W 90.82(11) . . ? O103 Ni12 O12W 166.54(11) . . ? N102 Ni12 O11 173.42(12) . . ? O102 Ni12 O11 95.25(11) . . ? O103 Ni12 O11 78.51(11) . . ? O12W Ni12 O11 88.74(11) . . ? N102 Ni12 N104 82.49(13) . . ? O102 Ni12 N104 171.08(12) . . ? O103 Ni12 N104 89.72(12) . . ? O12W Ni12 N104 86.67(12) . . ? O11 Ni12 N104 93.25(12) . . ? C100 O101 Ni11 128.0(3) . . ? C119 O102 Ni12 125.6(2) . . ? C126 O103 Ni11 114.1(2) . . ? C126 O103 Ni12 115.6(2) . . ? Ni11 O103 Ni12 98.67(11) . . ? C106 N101 C107 119.7(4) . . ? C106 N101 Ni11 125.3(3) . . ? C107 N101 Ni11 113.8(3) . . ? C113 N102 C112 118.4(3) . . ? C113 N102 Ni12 126.0(3) . . ? C112 N102 Ni12 114.9(3) . . ? C120 N103 C108 111.2(3) . . ? C120 N103 C109 102.3(3) . . ? C108 N103 C109 111.5(3) . . ? C120 N103 Ni11 115.0(2) . . ? C108 N103 Ni11 105.3(2) . . ? C109 N103 Ni11 111.7(3) . . ? C120 N104 C110 102.8(3) . . ? C120 N104 C111 112.7(3) . . ? C110 N104 C111 109.9(3) . . ? C120 N104 Ni12 114.8(2) . . ? C110 N104 Ni12 113.7(3) . . ? C111 N104 Ni12 103.2(2) . . ? Ni11 O11W H11W 126.2 . . ? Ni11 O11W H11X 124.6 . . ? H11W O11W H11X 96.7 . . ? Ni12 O12W H12A 119.0 . . ? Ni12 O12W H12B 121.9 . . ? H12A O12W H12B 102.8 . . ? C10 O11 Ni12 127.0(3) . . ? C10 O11 Ni11 134.9(3) . . ? Ni12 O11 Ni11 96.77(11) . . ? O12 C10 O11 122.5(4) . . ? O12 C10 C11 119.1(4) . . ? O11 C10 C11 118.4(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O101 C100 C101 119.1(4) . . ? O101 C100 C105 123.7(4) . . ? C101 C100 C105 117.2(4) . . ? C102 C101 C100 122.4(5) . . ? C102 C101 H101 118.8 . . ? C100 C101 H101 118.8 . . ? C101 C102 C103 120.2(5) . . ? C101 C102 H102 119.9 . . ? C103 C102 H102 119.9 . . ? C104 C103 C102 119.2(5) . . ? C104 C103 H103 120.4 . . ? C102 C103 H103 120.4 . . ? C103 C104 C105 121.6(5) . . ? C103 C104 H104 119.2 . . ? C105 C104 H104 119.2 . . ? C104 C105 C100 119.2(4) . . ? C104 C105 C106 116.8(4) . . ? C100 C105 C106 123.8(4) . . ? N101 C106 C105 125.9(4) . . ? N101 C106 H106 117.0 . . ? C105 C106 H106 117.0 . . ? N101 C107 C108 109.7(3) . . ? N101 C107 H10A 109.7 . . ? C108 C107 H10A 109.7 . . ? N101 C107 H10B 109.7 . . ? C108 C107 H10B 109.7 . . ? H10A C107 H10B 108.2 . . ? N103 C108 C107 111.9(3) . . ? N103 C108 H10C 109.2 . . ? C107 C108 H10C 109.2 . . ? N103 C108 H10D 109.2 . . ? C107 C108 H10D 109.2 . . ? H10C C108 H10D 107.9 . . ? N103 C109 C110 104.7(3) . . ? N103 C109 H10E 110.8 . . ? C110 C109 H10E 110.8 . . ? N103 C109 H10F 110.8 . . ? C110 C109 H10F 110.8 . . ? H10E C109 H10F 108.9 . . ? N104 C110 C109 105.2(3) . . ? N104 C110 H11D 110.7 . . ? C109 C110 H11D 110.7 . . ? N104 C110 H11E 110.7 . . ? C109 C110 H11E 110.7 . . ? H11D C110 H11E 108.8 . . ? N104 C111 C112 111.9(3) . . ? N104 C111 H11F 109.2 . . ? C112 C111 H11F 109.2 . . ? N104 C111 H11G 109.2 . . ? C112 C111 H11G 109.2 . . ? H11F C111 H11G 107.9 . . ? N102 C112 C111 108.8(3) . . ? N102 C112 H11H 109.9 . . ? C111 C112 H11H 109.9 . . ? N102 C112 H11J 109.9 . . ? C111 C112 H11J 109.9 . . ? H11H C112 H11J 108.3 . . ? N102 C113 C114 126.7(4) . . ? N102 C113 H113 116.6 . . ? C114 C113 H113 116.6 . . ? C115 C114 C119 118.8(4) . . ? C115 C114 C113 117.4(4) . . ? C119 C114 C113 123.7(4) . . ? C116 C115 C114 122.5(4) . . ? C116 C115 H115 118.7 . . ? C114 C115 H115 118.7 . . ? C115 C116 C117 118.4(4) . . ? C115 C116 H116 120.8 . . ? C117 C116 H116 120.8 . . ? C116 C117 C118 121.6(4) . . ? C116 C117 H117 119.2 . . ? C118 C117 H117 119.2 . . ? C117 C118 C119 121.4(4) . . ? C117 C118 H118 119.3 . . ? C119 C118 H118 119.3 . . ? O102 C119 C118 118.9(4) . . ? O102 C119 C114 123.7(4) . . ? C118 C119 C114 117.3(4) . . ? N104 C120 N103 101.8(3) . . ? N104 C120 C121 115.3(3) . . ? N103 C120 C121 113.3(3) . . ? N104 C120 H120 108.7 . . ? N103 C120 H120 108.7 . . ? C121 C120 H120 108.7 . . ? C122 C121 C126 120.5(4) . . ? C122 C121 C120 119.7(4) . . ? C126 C121 C120 119.6(4) . . ? C123 C122 C121 120.7(4) . . ? C123 C122 H122 119.6 . . ? C121 C122 H122 119.6 . . ? C124 C123 C122 119.3(4) . . ? C124 C123 H123 120.4 . . ? C122 C123 H123 120.4 . . ? C123 C124 C125 120.7(4) . . ? C123 C124 H124 119.6 . . ? C125 C124 H124 119.6 . . ? C124 C125 C126 121.4(4) . . ? C124 C125 H125 119.3 . . ? C126 C125 H125 119.3 . . ? O103 C126 C125 121.6(4) . . ? O103 C126 C121 121.0(4) . . ? C125 C126 C121 117.3(4) . . ? N201 Ni21 O201 88.64(13) . . ? N201 Ni21 O203 96.50(12) . . ? O201 Ni21 O203 91.58(11) . . ? N201 Ni21 O21W 95.71(14) . . ? O201 Ni21 O21W 91.12(12) . . ? O203 Ni21 O21W 167.55(13) . . ? N201 Ni21 O21 171.52(12) . . ? O201 Ni21 O21 98.44(11) . . ? O203 Ni21 O21 78.75(11) . . ? O21W Ni21 O21 88.84(12) . . ? N201 Ni21 N203 82.48(14) . . ? O201 Ni21 N203 171.03(13) . . ? O203 Ni21 N203 90.76(12) . . ? O21W Ni21 N203 88.44(13) . . ? O21 Ni21 N203 90.51(12) . . ? O202 Ni22 N202 92.01(13) . . ? O202 Ni22 O203 95.39(12) . . ? N202 Ni22 O203 95.55(13) . . ? O202 Ni22 O21 90.28(11) . . ? N202 Ni22 O21 174.60(13) . . ? O203 Ni22 O21 79.36(11) . . ? O202 Ni22 N204 174.00(12) . . ? N202 Ni22 N204 83.88(14) . . ? O203 Ni22 N204 89.37(12) . . ? O21 Ni22 N204 94.20(12) . . ? O202 Ni22 O22 92.28(12) . . ? N202 Ni22 O22 86.31(13) . . ? O203 Ni22 O22 172.03(11) . . ? O21 Ni22 O22 98.50(11) . . ? N204 Ni22 O22 83.12(13) . . ? C200 O201 Ni21 124.7(3) . . ? C219 O202 Ni22 126.5(3) . . ? C226 O203 Ni21 115.7(2) . . ? C226 O203 Ni22 113.0(2) . . ? Ni21 O203 Ni22 98.63(11) . . ? C206 N201 C207 118.5(4) . . ? C206 N201 Ni21 126.0(3) . . ? C207 N201 Ni21 114.5(3) . . ? C213 N202 C212 119.2(4) . . ? C213 N202 Ni22 125.8(3) . . ? C212 N202 Ni22 114.9(3) . . ? C220 N203 C208 113.6(3) . . ? C220 N203 C209 102.9(3) . . ? C208 N203 C209 110.2(3) . . ? C220 N203 Ni21 113.8(2) . . ? C208 N203 Ni21 102.8(3) . . ? C209 N203 Ni21 113.8(3) . . ? C210 N204 C211 111.4(3) . . ? C210 N204 C220 101.6(3) . . ? C211 N204 C220 112.5(3) . . ? C210 N204 Ni22 112.9(3) . . ? C211 N204 Ni22 104.0(3) . . ? C220 N204 Ni22 114.6(2) . . ? Ni21 O21W H21W 104(4) . . ? Ni21 O21W H21X 121(5) . . ? H21W O21W H21X 100(6) . . ? C20 O21 Ni22 133.9(3) . . ? C20 O21 Ni21 129.4(3) . . ? Ni22 O21 Ni21 96.60(11) . . ? O20 C20 O21 122.8(4) . . ? O20 C20 C21 119.3(4) . . ? O21 C20 C21 117.8(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 O22 Ni22 139.2(3) . . ? C22 O23 H23 114.6 . . ? O22 C22 O23 121.4(5) . . ? O22 C22 C23 125.5(5) . . ? O23 C22 C23 113.1(4) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O201 C200 C201 119.5(4) . . ? O201 C200 C205 123.6(4) . . ? C201 C200 C205 116.9(4) . . ? C202 C201 C200 122.0(4) . . ? C202 C201 H201 119.0 . . ? C200 C201 H201 119.0 . . ? C201 C202 C203 121.0(4) . . ? C201 C202 H202 119.5 . . ? C203 C202 H202 119.5 . . ? C204 C203 C202 118.2(4) . . ? C204 C203 H203 120.9 . . ? C202 C203 H203 120.9 . . ? C203 C204 C205 122.3(4) . . ? C203 C204 H204 118.8 . . ? C205 C204 H204 118.8 . . ? C204 C205 C200 119.7(4) . . ? C204 C205 C206 117.2(4) . . ? C200 C205 C206 123.1(4) . . ? N201 C206 C205 126.0(4) . . ? N201 C206 H206 117.0 . . ? C205 C206 H206 117.0 . . ? N201 C207 C208 108.8(3) . . ? N201 C207 H20A 109.9 . . ? C208 C207 H20A 109.9 . . ? N201 C207 H20B 109.9 . . ? C208 C207 H20B 109.9 . . ? H20A C207 H20B 108.3 . . ? N203 C208 C207 111.7(3) . . ? N203 C208 H20C 109.3 . . ? C207 C208 H20C 109.3 . . ? N203 C208 H20D 109.3 . . ? C207 C208 H20D 109.3 . . ? H20C C208 H20D 107.9 . . ? N203 C209 C210 105.3(3) . . ? N203 C209 H20E 110.7 . . ? C210 C209 H20E 110.7 . . ? N203 C209 H20F 110.7 . . ? C210 C209 H20F 110.7 . . ? H20E C209 H20F 108.8 . . ? N204 C210 C209 104.8(3) . . ? N204 C210 H21D 110.8 . . ? C209 C210 H21D 110.8 . . ? N204 C210 H21E 110.8 . . ? C209 C210 H21E 110.8 . . ? H21D C210 H21E 108.9 . . ? N204 C211 C212 112.8(3) . . ? N204 C211 H21F 109.0 . . ? C212 C211 H21F 109.0 . . ? N204 C211 H21G 109.0 . . ? C212 C211 H21G 109.0 . . ? H21F C211 H21G 107.8 . . ? N202 C212 C211 109.5(3) . . ? N202 C212 H21H 109.8 . . ? C211 C212 H21H 109.8 . . ? N202 C212 H21I 109.8 . . ? C211 C212 H21I 109.8 . . ? H21H C212 H21I 108.2 . . ? N202 C213 C214 125.6(4) . . ? N202 C213 H213 117.2 . . ? C214 C213 H213 117.2 . . ? C215 C214 C219 118.9(4) . . ? C215 C214 C213 116.6(4) . . ? C219 C214 C213 124.5(4) . . ? C216 C215 C214 122.3(4) . . ? C216 C215 H215 118.9 . . ? C214 C215 H215 118.9 . . ? C215 C216 C217 119.2(4) . . ? C215 C216 H216 120.4 . . ? C217 C216 H216 120.4 . . ? C218 C217 C216 119.7(4) . . ? C218 C217 H217 120.1 . . ? C216 C217 H217 120.1 . . ? C217 C218 C219 122.8(4) . . ? C217 C218 H218 118.6 . . ? C219 C218 H218 118.6 . . ? O202 C219 C218 119.1(4) . . ? O202 C219 C214 123.9(4) . . ? C218 C219 C214 117.0(4) . . ? N203 C220 N204 101.9(3) . . ? N203 C220 C221 116.9(3) . . ? N204 C220 C221 112.3(3) . . ? N203 C220 H220 108.5 . . ? N204 C220 H220 108.5 . . ? C221 C220 H220 108.5 . . ? C222 C221 C226 120.4(4) . . ? C222 C221 C220 119.6(4) . . ? C226 C221 C220 119.7(4) . . ? C223 C222 C221 121.4(4) . . ? C223 C222 H222 119.3 . . ? C221 C222 H222 119.3 . . ? C222 C223 C224 118.8(4) . . ? C222 C223 H223 120.6 . . ? C224 C223 H223 120.6 . . ? C223 C224 C225 120.9(4) . . ? C223 C224 H224 119.5 . . ? C225 C224 H224 119.5 . . ? C224 C225 C226 120.2(4) . . ? C224 C225 H225 119.9 . . ? C226 C225 H225 119.9 . . ? O203 C226 C221 121.0(4) . . ? O203 C226 C225 120.7(4) . . ? C221 C226 C225 118.3(4) . . ? H1WA O1W H1WB 105.7 . . ? H2WA O2W H2WB 109.0 . . ? H3WA O3W H3WB 95.7 . . ? N1S C10S C11S 179.1(6) . . ? C10S C11S H11I 109.5 . . ? C10S C11S H11K 109.5 . . ? H11I C11S H11K 109.5 . . ? C10S C11S H11L 109.5 . . ? H11I C11S H11L 109.5 . . ? H11K C11S H11L 109.5 . . ? N2S C20S C21S 177.5(11) . . ? C20S C21S H21J 109.5 . . ? C20S C21S H21K 109.5 . . ? H21J C21S H21K 109.5 . . ? C20S C21S H21L 109.5 . . ? H21J C21S H21L 109.5 . . ? H21K C21S H21L 109.5 . . ? C31S C30S N3S 168(2) . . ? N4S C40S C41S 155(3) . . ? C40S C41S H41A 109.5 . . ? C40S C41S H41B 109.5 . . ? H41A C41S H41B 109.5 . . ? C40S C41S H41C 109.5 . . ? H41A C41S H41C 109.5 . . ? H41B C41S H41C 109.5 . . ? N5S C50S C51S 155(3) . . ? N6S C60S C61S 163(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N101 Ni11 O101 C100 -12.0(4) . . . . ? O103 Ni11 O101 C100 -114.2(3) . . . . ? O11 Ni11 O101 C100 167.4(3) . . . . ? O11W Ni11 O101 C100 74.5(3) . . . . ? N102 Ni12 O102 C119 -23.6(3) . . . . ? O103 Ni12 O102 C119 72.8(3) . . . . ? O12W Ni12 O102 C119 -119.5(3) . . . . ? O11 Ni12 O102 C119 151.7(3) . . . . ? O101 Ni11 O103 C126 125.5(3) . . . . ? N101 Ni11 O103 C126 34.3(3) . . . . ? O11 Ni11 O103 C126 -144.2(3) . . . . ? N103 Ni11 O103 C126 -48.9(3) . . . . ? O101 Ni11 O103 Ni12 -111.42(12) . . . . ? N101 Ni11 O103 Ni12 157.44(13) . . . . ? O11 Ni11 O103 Ni12 -21.04(11) . . . . ? N103 Ni11 O103 Ni12 74.18(12) . . . . ? N102 Ni12 O103 C126 -32.7(3) . . . . ? O102 Ni12 O103 C126 -122.4(3) . . . . ? O12W Ni12 O103 C126 124.1(5) . . . . ? O11 Ni12 O103 C126 143.1(3) . . . . ? N104 Ni12 O103 C126 49.8(3) . . . . ? N102 Ni12 O103 Ni11 -154.68(13) . . . . ? O102 Ni12 O103 Ni11 115.53(11) . . . . ? O12W Ni12 O103 Ni11 2.1(5) . . . . ? O11 Ni12 O103 Ni11 21.10(11) . . . . ? N104 Ni12 O103 Ni11 -72.27(12) . . . . ? O101 Ni11 N101 C106 18.2(4) . . . . ? O103 Ni11 N101 C106 111.3(3) . . . . ? O11W Ni11 N101 C106 -72.4(4) . . . . ? N103 Ni11 N101 C106 -161.0(4) . . . . ? O101 Ni11 N101 C107 -174.6(3) . . . . ? O103 Ni11 N101 C107 -81.4(3) . . . . ? O11W Ni11 N101 C107 94.9(3) . . . . ? N103 Ni11 N101 C107 6.3(3) . . . . ? O102 Ni12 N102 C113 20.3(3) . . . . ? O103 Ni12 N102 C113 -74.3(4) . . . . ? O12W Ni12 N102 C113 111.0(3) . . . . ? N104 Ni12 N102 C113 -163.1(4) . . . . ? O102 Ni12 N102 C112 -169.9(3) . . . . ? O103 Ni12 N102 C112 95.5(3) . . . . ? O12W Ni12 N102 C112 -79.2(3) . . . . ? N104 Ni12 N102 C112 6.7(3) . . . . ? N101 Ni11 N103 C120 -105.5(3) . . . . ? O103 Ni11 N103 C120 -3.2(3) . . . . ? O11 Ni11 N103 C120 75.1(3) . . . . ? O11W Ni11 N103 C120 167.9(3) . . . . ? N101 Ni11 N103 C108 17.2(2) . . . . ? O103 Ni11 N103 C108 119.5(2) . . . . ? O11 Ni11 N103 C108 -162.2(2) . . . . ? O11W Ni11 N103 C108 -69.4(2) . . . . ? N101 Ni11 N103 C109 138.4(3) . . . . ? O103 Ni11 N103 C109 -119.3(3) . . . . ? O11 Ni11 N103 C109 -41.0(3) . . . . ? O11W Ni11 N103 C109 51.8(3) . . . . ? N102 Ni12 N104 C120 94.8(3) . . . . ? O103 Ni12 N104 C120 -1.6(3) . . . . ? O12W Ni12 N104 C120 -168.7(3) . . . . ? O11 Ni12 N104 C120 -80.1(3) . . . . ? N102 Ni12 N104 C110 -147.1(3) . . . . ? O103 Ni12 N104 C110 116.4(3) . . . . ? O12W Ni12 N104 C110 -50.6(3) . . . . ? O11 Ni12 N104 C110 37.9(3) . . . . ? N102 Ni12 N104 C111 -28.1(2) . . . . ? O103 Ni12 N104 C111 -124.6(2) . . . . ? O12W Ni12 N104 C111 68.4(2) . . . . ? O11 Ni12 N104 C111 156.9(2) . . . . ? O102 Ni12 O11 C10 54.1(3) . . . . ? O103 Ni12 O11 C10 147.7(3) . . . . ? O12W Ni12 O11 C10 -36.6(3) . . . . ? N104 Ni12 O11 C10 -123.2(3) . . . . ? O102 Ni12 O11 Ni11 -114.29(11) . . . . ? O103 Ni12 O11 Ni11 -20.65(10) . . . . ? O12W Ni12 O11 Ni11 155.01(12) . . . . ? N104 Ni12 O11 Ni11 68.41(12) . . . . ? O101 Ni11 O11 C10 -53.4(4) . . . . ? O103 Ni11 O11 C10 -146.2(4) . . . . ? O11W Ni11 O11 C10 37.2(4) . . . . ? N103 Ni11 O11 C10 125.7(4) . . . . ? O101 Ni11 O11 Ni12 113.49(12) . . . . ? O103 Ni11 O11 Ni12 20.66(10) . . . . ? O11W Ni11 O11 Ni12 -155.88(11) . . . . ? N103 Ni11 O11 Ni12 -67.43(12) . . . . ? Ni12 O11 C10 O12 14.1(5) . . . . ? Ni11 O11 C10 O12 177.7(3) . . . . ? Ni12 O11 C10 C11 -166.9(3) . . . . ? Ni11 O11 C10 C11 -3.3(6) . . . . ? Ni11 O101 C100 C101 -177.7(3) . . . . ? Ni11 O101 C100 C105 2.0(6) . . . . ? O101 C100 C101 C102 176.3(5) . . . . ? C105 C100 C101 C102 -3.4(7) . . . . ? C100 C101 C102 C103 0.3(9) . . . . ? C101 C102 C103 C104 1.7(8) . . . . ? C102 C103 C104 C105 -0.5(8) . . . . ? C103 C104 C105 C100 -2.7(7) . . . . ? C103 C104 C105 C106 174.3(4) . . . . ? O101 C100 C105 C104 -175.3(4) . . . . ? C101 C100 C105 C104 4.5(6) . . . . ? O101 C100 C105 C106 8.0(7) . . . . ? C101 C100 C105 C106 -172.2(4) . . . . ? C107 N101 C106 C105 178.3(4) . . . . ? Ni11 N101 C106 C105 -15.1(6) . . . . ? C104 C105 C106 N101 -177.6(4) . . . . ? C100 C105 C106 N101 -0.8(7) . . . . ? C106 N101 C107 C108 139.7(4) . . . . ? Ni11 N101 C107 C108 -28.3(4) . . . . ? C120 N103 C108 C107 87.8(4) . . . . ? C109 N103 C108 C107 -158.7(4) . . . . ? Ni11 N103 C108 C107 -37.4(4) . . . . ? N101 C107 C108 N103 44.6(5) . . . . ? C120 N103 C109 C110 -29.1(4) . . . . ? C108 N103 C109 C110 -148.0(3) . . . . ? Ni11 N103 C109 C110 94.5(3) . . . . ? C120 N104 C110 C109 27.0(4) . . . . ? C111 N104 C110 C109 147.2(3) . . . . ? Ni12 N104 C110 C109 -97.8(3) . . . . ? N103 C109 C110 N104 1.3(4) . . . . ? C120 N104 C111 C112 -78.3(4) . . . . ? C110 N104 C111 C112 167.7(3) . . . . ? Ni12 N104 C111 C112 46.1(4) . . . . ? C113 N102 C112 C111 -172.6(4) . . . . ? Ni12 N102 C112 C111 16.8(4) . . . . ? N104 C111 C112 N102 -43.1(4) . . . . ? C112 N102 C113 C114 -179.8(4) . . . . ? Ni12 N102 C113 C114 -10.3(6) . . . . ? N102 C113 C114 C115 176.8(4) . . . . ? N102 C113 C114 C119 -5.9(7) . . . . ? C119 C114 C115 C116 0.1(7) . . . . ? C113 C114 C115 C116 177.6(4) . . . . ? C114 C115 C116 C117 -0.8(7) . . . . ? C115 C116 C117 C118 0.1(7) . . . . ? C116 C117 C118 C119 1.3(7) . . . . ? Ni12 O102 C119 C118 -165.0(3) . . . . ? Ni12 O102 C119 C114 16.8(5) . . . . ? C117 C118 C119 O102 179.7(4) . . . . ? C117 C118 C119 C114 -2.0(6) . . . . ? C115 C114 C119 O102 179.4(4) . . . . ? C113 C114 C119 O102 2.2(6) . . . . ? C115 C114 C119 C118 1.2(6) . . . . ? C113 C114 C119 C118 -176.0(4) . . . . ? C110 N104 C120 N103 -45.7(4) . . . . ? C111 N104 C120 N103 -163.9(3) . . . . ? Ni12 N104 C120 N103 78.3(3) . . . . ? C110 N104 C120 C121 -168.8(3) . . . . ? C111 N104 C120 C121 73.0(4) . . . . ? Ni12 N104 C120 C121 -44.7(4) . . . . ? C108 N103 C120 N104 165.6(3) . . . . ? C109 N103 C120 N104 46.4(3) . . . . ? Ni11 N103 C120 N104 -74.9(3) . . . . ? C108 N103 C120 C121 -70.0(4) . . . . ? C109 N103 C120 C121 170.8(3) . . . . ? Ni11 N103 C120 C121 49.5(4) . . . . ? N104 C120 C121 C122 -124.8(4) . . . . ? N103 C120 C121 C122 118.4(4) . . . . ? N104 C120 C121 C126 59.2(5) . . . . ? N103 C120 C121 C126 -57.6(5) . . . . ? C126 C121 C122 C123 0.1(6) . . . . ? C120 C121 C122 C123 -175.9(4) . . . . ? C121 C122 C123 C124 0.5(6) . . . . ? C122 C123 C124 C125 -1.0(7) . . . . ? C123 C124 C125 C126 1.1(7) . . . . ? Ni11 O103 C126 C125 -119.8(4) . . . . ? Ni12 O103 C126 C125 126.8(3) . . . . ? Ni11 O103 C126 C121 59.6(4) . . . . ? Ni12 O103 C126 C121 -53.8(4) . . . . ? C124 C125 C126 O103 178.9(4) . . . . ? C124 C125 C126 C121 -0.5(6) . . . . ? C122 C121 C126 O103 -179.5(4) . . . . ? C120 C121 C126 O103 -3.5(6) . . . . ? C122 C121 C126 C125 -0.1(6) . . . . ? C120 C121 C126 C125 175.9(4) . . . . ? N201 Ni21 O201 C200 30.5(3) . . . . ? O203 Ni21 O201 C200 -66.0(3) . . . . ? O21W Ni21 O201 C200 126.2(3) . . . . ? O21 Ni21 O201 C200 -144.8(3) . . . . ? N202 Ni22 O202 C219 -13.0(3) . . . . ? O203 Ni22 O202 C219 82.7(3) . . . . ? O21 Ni22 O202 C219 162.1(3) . . . . ? O22 Ni22 O202 C219 -99.4(3) . . . . ? N201 Ni21 O203 C226 32.6(3) . . . . ? O201 Ni21 O203 C226 121.4(3) . . . . ? O21W Ni21 O203 C226 -136.2(5) . . . . ? O21 Ni21 O203 C226 -140.3(3) . . . . ? N203 Ni21 O203 C226 -50.0(3) . . . . ? N201 Ni21 O203 Ni22 153.40(13) . . . . ? O201 Ni21 O203 Ni22 -117.78(12) . . . . ? O21W Ni21 O203 Ni22 -15.3(6) . . . . ? O21 Ni21 O203 Ni22 -19.49(11) . . . . ? N203 Ni21 O203 Ni22 70.88(13) . . . . ? O202 Ni22 O203 C226 -128.1(3) . . . . ? N202 Ni22 O203 C226 -35.5(3) . . . . ? O21 Ni22 O203 C226 142.6(3) . . . . ? N204 Ni22 O203 C226 48.2(3) . . . . ? O202 Ni22 O203 Ni21 109.14(12) . . . . ? N202 Ni22 O203 Ni21 -158.31(13) . . . . ? O21 Ni22 O203 Ni21 19.87(11) . . . . ? N204 Ni22 O203 Ni21 -74.53(13) . . . . ? O201 Ni21 N201 C206 -23.4(3) . . . . ? O203 Ni21 N201 C206 68.0(4) . . . . ? O21W Ni21 N201 C206 -114.4(3) . . . . ? N203 Ni21 N201 C206 157.9(4) . . . . ? O201 Ni21 N201 C207 168.6(3) . . . . ? O203 Ni21 N201 C207 -99.9(3) . . . . ? O21W Ni21 N201 C207 77.7(3) . . . . ? N203 Ni21 N201 C207 -10.0(3) . . . . ? O202 Ni22 N202 C213 10.7(4) . . . . ? O203 Ni22 N202 C213 -85.0(4) . . . . ? N204 Ni22 N202 C213 -173.7(4) . . . . ? O22 Ni22 N202 C213 102.8(4) . . . . ? O202 Ni22 N202 C212 -174.3(3) . . . . ? O203 Ni22 N202 C212 90.0(3) . . . . ? N204 Ni22 N202 C212 1.3(3) . . . . ? O22 Ni22 N202 C212 -82.2(3) . . . . ? N201 Ni21 N203 C220 -92.5(3) . . . . ? O203 Ni21 N203 C220 4.0(3) . . . . ? O21W Ni21 N203 C220 171.5(3) . . . . ? O21 Ni21 N203 C220 82.7(3) . . . . ? N201 Ni21 N203 C208 30.8(3) . . . . ? O203 Ni21 N203 C208 127.3(3) . . . . ? O21W Ni21 N203 C208 -65.1(3) . . . . ? O21 Ni21 N203 C208 -154.0(3) . . . . ? N201 Ni21 N203 C209 150.0(3) . . . . ? O203 Ni21 N203 C209 -113.5(3) . . . . ? O21W Ni21 N203 C209 54.1(3) . . . . ? O21 Ni21 N203 C209 -34.8(3) . . . . ? N202 Ni22 N204 C210 -143.3(3) . . . . ? O203 Ni22 N204 C210 121.0(3) . . . . ? O21 Ni22 N204 C210 41.7(3) . . . . ? O22 Ni22 N204 C210 -56.3(3) . . . . ? N202 Ni22 N204 C211 -22.3(3) . . . . ? O203 Ni22 N204 C211 -118.0(3) . . . . ? O21 Ni22 N204 C211 162.7(3) . . . . ? O22 Ni22 N204 C211 64.7(3) . . . . ? N202 Ni22 N204 C220 100.9(3) . . . . ? O203 Ni22 N204 C220 5.2(3) . . . . ? O21 Ni22 N204 C220 -74.0(3) . . . . ? O22 Ni22 N204 C220 -172.1(3) . . . . ? O202 Ni22 O21 C20 60.9(3) . . . . ? O203 Ni22 O21 C20 156.4(4) . . . . ? N204 Ni22 O21 C20 -115.1(4) . . . . ? O22 Ni22 O21 C20 -31.4(4) . . . . ? O202 Ni22 O21 Ni21 -114.60(12) . . . . ? O203 Ni22 O21 Ni21 -19.17(10) . . . . ? N204 Ni22 O21 Ni21 69.40(13) . . . . ? O22 Ni22 O21 Ni21 153.05(11) . . . . ? O201 Ni21 O21 C20 -66.5(3) . . . . ? O203 Ni21 O21 C20 -156.5(3) . . . . ? O21W Ni21 O21 C20 24.4(3) . . . . ? N203 Ni21 O21 C20 112.9(3) . . . . ? O201 Ni21 O21 Ni22 109.31(11) . . . . ? O203 Ni21 O21 Ni22 19.37(11) . . . . ? O21W Ni21 O21 Ni22 -159.73(12) . . . . ? N203 Ni21 O21 Ni22 -71.30(12) . . . . ? Ni22 O21 C20 O20 -175.6(3) . . . . ? Ni21 O21 C20 O20 -1.3(6) . . . . ? Ni22 O21 C20 C21 6.0(6) . . . . ? Ni21 O21 C20 C21 -179.7(3) . . . . ? O202 Ni22 O22 C22 40.9(5) . . . . ? N202 Ni22 O22 C22 -51.0(5) . . . . ? O21 Ni22 O22 C22 131.5(5) . . . . ? N204 Ni22 O22 C22 -135.3(5) . . . . ? Ni22 O22 C22 O23 142.6(4) . . . . ? Ni22 O22 C22 C23 -37.9(8) . . . . ? Ni21 O201 C200 C201 157.6(3) . . . . ? Ni21 O201 C200 C205 -24.8(5) . . . . ? O201 C200 C201 C202 178.7(4) . . . . ? C205 C200 C201 C202 0.9(6) . . . . ? C200 C201 C202 C203 -1.2(6) . . . . ? C201 C202 C203 C204 0.6(6) . . . . ? C202 C203 C204 C205 0.2(6) . . . . ? C203 C204 C205 C200 -0.4(6) . . . . ? C203 C204 C205 C206 -179.2(4) . . . . ? O201 C200 C205 C204 -177.8(4) . . . . ? C201 C200 C205 C204 -0.1(6) . . . . ? O201 C200 C205 C206 0.9(6) . . . . ? C201 C200 C205 C206 178.6(4) . . . . ? C207 N201 C206 C205 177.7(4) . . . . ? Ni21 N201 C206 C205 10.2(6) . . . . ? C204 C205 C206 N201 -174.1(4) . . . . ? C200 C205 C206 N201 7.1(7) . . . . ? C206 N201 C207 C208 177.7(4) . . . . ? Ni21 N201 C207 C208 -13.3(4) . . . . ? C220 N203 C208 C207 75.9(4) . . . . ? C209 N203 C208 C207 -169.3(3) . . . . ? Ni21 N203 C208 C207 -47.6(4) . . . . ? N201 C207 C208 N203 42.0(5) . . . . ? C220 N203 C209 C210 -22.2(4) . . . . ? C208 N203 C209 C210 -143.7(4) . . . . ? Ni21 N203 C209 C210 101.4(3) . . . . ? C211 N204 C210 C209 153.6(4) . . . . ? C220 N204 C210 C209 33.6(4) . . . . ? Ni22 N204 C210 C209 -89.7(3) . . . . ? N203 C209 C210 N204 -7.3(4) . . . . ? C210 N204 C211 C212 161.8(4) . . . . ? C220 N204 C211 C212 -84.8(4) . . . . ? Ni22 N204 C211 C212 39.8(4) . . . . ? C213 N202 C212 C211 -164.6(4) . . . . ? Ni22 N202 C212 C211 20.1(4) . . . . ? N204 C211 C212 N202 -41.2(5) . . . . ? C212 N202 C213 C214 -178.2(4) . . . . ? Ni22 N202 C213 C214 -3.4(6) . . . . ? N202 C213 C214 C215 174.2(4) . . . . ? N202 C213 C214 C219 -6.7(7) . . . . ? C219 C214 C215 C216 0.1(7) . . . . ? C213 C214 C215 C216 179.2(4) . . . . ? C214 C215 C216 C217 -2.6(7) . . . . ? C215 C216 C217 C218 1.9(7) . . . . ? C216 C217 C218 C219 1.2(7) . . . . ? Ni22 O202 C219 C218 -171.7(3) . . . . ? Ni22 O202 C219 C214 8.0(6) . . . . ? C217 C218 C219 O202 176.1(4) . . . . ? C217 C218 C219 C214 -3.6(6) . . . . ? C215 C214 C219 O202 -176.8(4) . . . . ? C213 C214 C219 O202 4.2(7) . . . . ? C215 C214 C219 C218 2.9(6) . . . . ? C213 C214 C219 C218 -176.1(4) . . . . ? C208 N203 C220 N204 162.5(3) . . . . ? C209 N203 C220 N204 43.4(4) . . . . ? Ni21 N203 C220 N204 -80.2(3) . . . . ? C208 N203 C220 C221 -74.7(5) . . . . ? C209 N203 C220 C221 166.2(4) . . . . ? Ni21 N203 C220 C221 42.5(4) . . . . ? C210 N204 C220 N203 -48.2(4) . . . . ? C211 N204 C220 N203 -167.5(3) . . . . ? Ni22 N204 C220 N203 74.0(3) . . . . ? C210 N204 C220 C221 -174.1(3) . . . . ? C211 N204 C220 C221 66.7(4) . . . . ? Ni22 N204 C220 C221 -51.9(4) . . . . ? N203 C220 C221 C222 127.5(4) . . . . ? N204 C220 C221 C222 -115.3(4) . . . . ? N203 C220 C221 C226 -59.3(5) . . . . ? N204 C220 C221 C226 57.9(5) . . . . ? C226 C221 C222 C223 -1.0(7) . . . . ? C220 C221 C222 C223 172.2(4) . . . . ? C221 C222 C223 C224 0.6(7) . . . . ? C222 C223 C224 C225 0.8(7) . . . . ? C223 C224 C225 C226 -1.7(7) . . . . ? Ni21 O203 C226 C221 51.5(4) . . . . ? Ni22 O203 C226 C221 -61.2(4) . . . . ? Ni21 O203 C226 C225 -130.0(3) . . . . ? Ni22 O203 C226 C225 117.3(3) . . . . ? C222 C221 C226 O203 178.6(4) . . . . ? C220 C221 C226 O203 5.4(6) . . . . ? C222 C221 C226 C225 0.0(6) . . . . ? C220 C221 C226 C225 -173.1(4) . . . . ? C224 C225 C226 O203 -177.3(4) . . . . ? C224 C225 C226 C221 1.3(6) . . . . ? 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 O11W H11W O2W 0.89 1.76 2.656(4) 174.6 1_455 O11W H11X N1S 0.93 2.09 2.964(6) 156.0 1_455 O12W H12A O201 0.97 1.77 2.716(4) 166.4 2_665 O12W H12B O12 0.72 2.12 2.655(4) 132.3 . O23 H23 O1W 0.98 1.53 2.509(5) 172.9 . O21W H21W O20 0.85(6) 1.87(6) 2.662(5) 155(5) . O21W H21X O102 0.77(7) 2.10(7) 2.845(4) 163(6) 2_665 O1W H1WA O101 0.94 1.70 2.644(4) 175.4 . O1W H1WB O102 0.98 1.77 2.744(4) 169.7 . O2W H2WA O201 0.84 1.90 2.727(4) 172.4 . O2W H2WB O202 0.89 1.82 2.706(4) 170.6 . O3W H3WA O12 0.98 1.88 2.823(5) 161.4 . O3W H3WB O20 0.97 1.98 2.851(5) 148.8 2_665 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.688 _refine_diff_density_min -0.881 _refine_diff_density_rms 0.127 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_be21mf2n _database_code_depnum_ccdc_archive 'CCDC 275612' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C61 H76 N8 Ni5 O17, 1.5 (C H4 O), 2.70(H2 O)' _chemical_formula_sum 'C62.50 H85.50 N8 Ni5 O21.20' _chemical_formula_weight 1581.64 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_h-m 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0930(10) _cell_length_b 26.699(2) _cell_length_c 22.9070(19) _cell_angle_alpha 90.00 _cell_angle_beta 104.105(2) _cell_angle_gamma 90.00 _cell_volume 7173.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120.0(1) _cell_measurement_reflns_used 2734 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 24.92 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3304 _exptl_absorpt_coefficient_mu 1.364 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_t_min 0.7602 _exptl_absorpt_correction_t_max 0.8534 _exptl_absorpt_process_details SADABS _exptl_special_details ; 'additional spherical absorption correction applied with mu*r = 0.1134' ; _diffrn_ambient_temperature 120(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART-CCD-1000 Bruker' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15837 _diffrn_reflns_av_r_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0892 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 24.71 _reflns_number_total 12225 _reflns_number_gt 7416 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'DIRDIF99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1028P)^2^+11.6736P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00102(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12225 _refine_ls_number_parameters 890 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1245 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1955 _refine_ls_wR_factor_gt 0.1590 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Ni11 Ni 0.13629(7) 0.36229(3) 0.60231(4) 0.0231(2) Uani 1 1 d . . . Ni12 Ni 0.09820(7) 0.33364(3) 0.72773(4) 0.0227(2) Uani 1 1 d . . . O101 O 0.2938(4) 0.39128(18) 0.6166(2) 0.0268(11) Uani 1 1 d . . . O102 O 0.2413(4) 0.35322(18) 0.79130(19) 0.0248(11) Uani 1 1 d . . . O103 O 0.1027(4) 0.39622(17) 0.6769(2) 0.0243(11) Uani 1 1 d . . . N101 N 0.0789(5) 0.4158(2) 0.5401(3) 0.0296(14) Uani 1 1 d . . . N102 N 0.0023(5) 0.3610(2) 0.7807(3) 0.0257(13) Uani 1 1 d . . . N103 N -0.0381(5) 0.3357(2) 0.5781(3) 0.0262(13) Uani 1 1 d . . . N104 N -0.0659(5) 0.3136(2) 0.6699(3) 0.0251(13) Uani 1 1 d . . . O11S O 0.1702(4) 0.3129(2) 0.5355(2) 0.0299(12) Uani 1 1 d . . . H11S H 0.222(9) 0.298(4) 0.559(5) 0.080 Uiso 1 1 d . . . C11S C 0.2275(7) 0.3286(3) 0.4913(3) 0.040(2) Uani 1 1 d . . . H11A H 0.1778 0.3495 0.4623 0.061 Uiso 1 1 calc R . . H11B H 0.2486 0.2997 0.4714 0.061 Uiso 1 1 calc R . . H11C H 0.2948 0.3470 0.5104 0.061 Uiso 1 1 calc R . . O12S O 0.1098(4) 0.2609(2) 0.7642(2) 0.0297(12) Uani 1 1 d . . . H12S H 0.167(9) 0.248(4) 0.749(5) 0.080 Uiso 1 1 d . . . C12S C 0.1187(7) 0.2512(3) 0.8268(3) 0.038(2) Uani 1 1 d . . . H12A H 0.1579 0.2785 0.8504 0.056 Uiso 1 1 calc R . . H12B H 0.1605 0.2207 0.8383 0.056 Uiso 1 1 calc R . . H12C H 0.0437 0.2480 0.8336 0.056 Uiso 1 1 calc R . . O10 O 0.2798(5) 0.2556(2) 0.6190(2) 0.0430(15) Uani 1 1 d . . . O11 O 0.1837(4) 0.30648(18) 0.6657(2) 0.0245(11) Uani 1 1 d . . . O12 O 0.2729(4) 0.2407(2) 0.7138(2) 0.0331(12) Uani 1 1 d . . . C10 C 0.2470(6) 0.2675(3) 0.6659(3) 0.0274(16) Uani 1 1 d . . . C100 C 0.3257(6) 0.4317(3) 0.5944(3) 0.0237(15) Uani 1 1 d . . . C101 C 0.4395(6) 0.4487(3) 0.6167(3) 0.0289(17) Uani 1 1 d . . . H101 H 0.4879 0.4303 0.6468 0.035 Uiso 1 1 calc R . . C102 C 0.4807(7) 0.4908(3) 0.5960(4) 0.040(2) Uani 1 1 d . . . H102 H 0.5551 0.5010 0.6128 0.048 Uiso 1 1 calc R . . C103 C 0.4116(7) 0.5187(3) 0.5494(4) 0.047(2) Uani 1 1 d . . . H103 H 0.4397 0.5471 0.5344 0.056 Uiso 1 1 calc R . . C104 C 0.3018(7) 0.5033(3) 0.5263(4) 0.043(2) Uani 1 1 d . . . H104 H 0.2560 0.5216 0.4950 0.051 Uiso 1 1 calc R . . C105 C 0.2558(6) 0.4611(3) 0.5482(3) 0.0298(17) Uani 1 1 d . . . C106 C 0.1371(6) 0.4498(3) 0.5231(3) 0.0303(17) Uani 1 1 d . . . H106 H 0.0993 0.4695 0.4909 0.036 Uiso 1 1 calc R . . C107 C -0.0438(6) 0.4115(3) 0.5130(3) 0.0332(18) Uani 1 1 d . . . H10A H -0.0604 0.4222 0.4713 0.040 Uiso 1 1 calc R . . H10B H -0.0856 0.4329 0.5343 0.040 Uiso 1 1 calc R . . C108 C -0.0799(6) 0.3580(3) 0.5165(3) 0.0307(17) Uani 1 1 d . . . H10C H -0.0512 0.3382 0.4879 0.037 Uiso 1 1 calc R . . H10D H -0.1625 0.3563 0.5051 0.037 Uiso 1 1 calc R . . C109 C -0.0479(6) 0.2805(3) 0.5759(3) 0.0298(17) Uani 1 1 d . . . H10E H 0.0213 0.2655 0.5697 0.036 Uiso 1 1 calc R . . H10F H -0.1116 0.2701 0.5436 0.036 Uiso 1 1 calc R . . C110 C -0.0668(6) 0.2656(3) 0.6364(3) 0.0266(16) Uani 1 1 d . . . H11D H -0.1393 0.2486 0.6316 0.032 Uiso 1 1 calc R . . H11E H -0.0064 0.2436 0.6575 0.032 Uiso 1 1 calc R . . C111 C -0.1415(6) 0.3106(3) 0.7125(3) 0.0313(17) Uani 1 1 d . . . H11F H -0.1281 0.2790 0.7340 0.038 Uiso 1 1 calc R . . H11G H -0.2204 0.3111 0.6897 0.038 Uiso 1 1 calc R . . C112 C -0.1217(6) 0.3536(3) 0.7579(4) 0.0356(19) Uani 1 1 d . . . H12H H -0.1568 0.3840 0.7388 0.043 Uiso 1 1 calc R . . H12I H -0.1558 0.3456 0.7910 0.043 Uiso 1 1 calc R . . C113 C 0.0350(7) 0.3868(3) 0.8292(4) 0.0345(18) Uani 1 1 d . . . H113 H -0.0209 0.3975 0.8479 0.041 Uiso 1 1 calc R . . C114 C 0.1507(6) 0.4005(3) 0.8569(3) 0.0288(17) Uani 1 1 d . . . C115 C 0.1700(8) 0.4324(3) 0.9085(4) 0.043(2) Uani 1 1 d . . . H115 H 0.1078 0.4423 0.9229 0.051 Uiso 1 1 calc R . . C116 C 0.2766(8) 0.4493(3) 0.9378(4) 0.044(2) Uani 1 1 d . . . H116 H 0.2860 0.4703 0.9710 0.053 Uiso 1 1 calc R . . C117 C 0.3696(7) 0.4345(3) 0.9167(3) 0.038(2) Uani 1 1 d . . . H117 H 0.4423 0.4457 0.9355 0.046 Uiso 1 1 calc R . . C118 C 0.3538(6) 0.4029(3) 0.8675(3) 0.0292(17) Uani 1 1 d . . . H118 H 0.4174 0.3932 0.8543 0.035 Uiso 1 1 calc R . . C119 C 0.2489(6) 0.3850(3) 0.8372(3) 0.0258(16) Uani 1 1 d . . . C120 C -0.1079(6) 0.3508(3) 0.6204(3) 0.0252(16) Uani 1 1 d . . . H120 H -0.1880 0.3434 0.6016 0.030 Uiso 1 1 calc R . . C121 C -0.0982(6) 0.4043(3) 0.6383(3) 0.0248(16) Uani 1 1 d . . . C122 C -0.1931(6) 0.4350(3) 0.6265(3) 0.0344(19) Uani 1 1 d . . . H122 H -0.2647 0.4213 0.6101 0.041 Uiso 1 1 calc R . . C123 C -0.1829(7) 0.4853(3) 0.6386(4) 0.047(2) Uani 1 1 d . . . H123 H -0.2469 0.5059 0.6292 0.056 Uiso 1 1 calc R . . C124 C -0.0777(7) 0.5053(3) 0.6647(4) 0.042(2) Uani 1 1 d . . . H124 H -0.0711 0.5394 0.6729 0.051 Uiso 1 1 calc R . . C125 C 0.0175(6) 0.4757(3) 0.6788(3) 0.0318(18) Uani 1 1 d . . . H125 H 0.0875 0.4898 0.6975 0.038 Uiso 1 1 calc R . . C126 C 0.0108(6) 0.4250(3) 0.6656(3) 0.0243(16) Uani 1 1 d . . . Ni21 Ni 0.59767(8) 0.14545(4) 0.77471(4) 0.0269(2) Uani 1 1 d . . . Ni22 Ni 0.56244(8) 0.17505(4) 0.64394(4) 0.0286(3) Uani 1 1 d . . . O201 O 0.5987(4) 0.21123(19) 0.8167(2) 0.0274(11) Uani 1 1 d . . . O202 O 0.5681(4) 0.25026(18) 0.6360(2) 0.0313(12) Uani 1 1 d . . . O203 O 0.6976(4) 0.17169(18) 0.7178(2) 0.0265(11) Uani 1 1 d . . . N201 N 0.6396(6) 0.1692(2) 0.5743(3) 0.0350(15) Uani 1 1 d . . . N202 N 0.7377(6) 0.1251(2) 0.8361(3) 0.0317(15) Uani 1 1 d . . . N203 N 0.5671(6) 0.0921(2) 0.6388(3) 0.0337(15) Uani 1 1 d . . . N204 N 0.6056(5) 0.0720(2) 0.7395(3) 0.0306(14) Uani 1 1 d . . . O21 O 0.4866(4) 0.11720(19) 0.8223(2) 0.0350(13) Uani 1 1 d . . . O22 O 0.3634(4) 0.18138(19) 0.8106(2) 0.0328(12) Uani 1 1 d . . . C20 C 0.3995(6) 0.1389(3) 0.8307(3) 0.0272(16) Uani 1 1 d . . . C21 C 0.3311(8) 0.1118(3) 0.8663(5) 0.051(2) Uani 1 1 d . . . H21A H 0.2537 0.1089 0.8431 0.077 Uiso 1 1 calc R . . H21B H 0.3327 0.1300 0.9027 0.077 Uiso 1 1 calc R . . H21C H 0.3626 0.0790 0.8763 0.077 Uiso 1 1 calc R . . O22S O 0.3929(5) 0.1785(2) 0.5867(2) 0.0361(14) Uani 1 1 d . . . H22S H 0.374(10) 0.204(4) 0.593(5) 0.080 Uiso 1 1 d . . . C22S C 0.3587(7) 0.1873(3) 0.5222(3) 0.0370(19) Uani 1 1 d . . . H22A H 0.3895 0.2187 0.5131 0.055 Uiso 1 1 calc R . . H22B H 0.2771 0.1883 0.5093 0.055 Uiso 1 1 calc R . . H22C H 0.3871 0.1608 0.5015 0.055 Uiso 1 1 calc R . . C200 C 0.6904(6) 0.2350(3) 0.8468(3) 0.0260(16) Uani 1 1 d . . . C201 C 0.6870(6) 0.2864(3) 0.8593(3) 0.0292(17) Uani 1 1 d . . . H201 H 0.6194 0.3039 0.8449 0.035 Uiso 1 1 calc R . . C202 C 0.7815(7) 0.3117(3) 0.8923(3) 0.0373(19) Uani 1 1 d . . . H202 H 0.7764 0.3456 0.9003 0.045 Uiso 1 1 calc R . . C203 C 0.8842(7) 0.2866(3) 0.9137(4) 0.041(2) Uani 1 1 d . . . H203 H 0.9481 0.3037 0.9354 0.049 Uiso 1 1 calc R . . C204 C 0.8899(7) 0.2370(3) 0.9023(3) 0.0357(19) Uani 1 1 d . . . H204 H 0.9588 0.2204 0.9166 0.043 Uiso 1 1 calc R . . C205 C 0.7948(6) 0.2092(3) 0.8694(3) 0.0305(17) Uani 1 1 d . . . C206 C 0.8128(7) 0.1562(3) 0.8630(3) 0.0331(19) Uani 1 1 d . . . H206 H 0.8853 0.1438 0.8801 0.040 Uiso 1 1 calc R . . C207 C 0.7694(7) 0.0720(3) 0.8314(3) 0.0354(19) Uani 1 1 d . . . H20A H 0.7927 0.0573 0.8712 0.043 Uiso 1 1 calc R . . H20B H 0.8327 0.0697 0.8124 0.043 Uiso 1 1 calc R . . C208 C 0.6663(7) 0.0438(3) 0.7938(3) 0.0368(19) Uani 1 1 d . . . H20C H 0.6915 0.0119 0.7814 0.044 Uiso 1 1 calc R . . H20D H 0.6135 0.0370 0.8186 0.044 Uiso 1 1 calc R . . C209 C 0.4915(7) 0.0505(3) 0.7139(4) 0.042(2) Uani 1 1 d . . . H20E H 0.4358 0.0640 0.7339 0.051 Uiso 1 1 calc R . . H20F H 0.4928 0.0143 0.7177 0.051 Uiso 1 1 calc R . . C210 C 0.4642(7) 0.0665(3) 0.6473(4) 0.039(2) Uani 1 1 d . . . H21D H 0.4471 0.0374 0.6212 0.047 Uiso 1 1 calc R . . H21E H 0.3992 0.0889 0.6381 0.047 Uiso 1 1 calc R . . C211 C 0.5830(8) 0.0828(3) 0.5778(3) 0.045(2) Uani 1 1 d . . . H21F H 0.5104 0.0868 0.5487 0.053 Uiso 1 1 calc R . . H21G H 0.6080 0.0486 0.5754 0.053 Uiso 1 1 calc R . . C212 C 0.6684(8) 0.1176(3) 0.5621(4) 0.048(2) Uani 1 1 d . . . H21H H 0.7442 0.1095 0.5858 0.057 Uiso 1 1 calc R . . H21I H 0.6677 0.1140 0.5199 0.057 Uiso 1 1 calc R . . C213 C 0.6540(6) 0.2045(3) 0.5393(3) 0.0281(17) Uani 1 1 d . . . H213 H 0.6873 0.1956 0.5082 0.034 Uiso 1 1 calc R . . C214 C 0.6248(6) 0.2560(3) 0.5424(3) 0.0239(16) Uani 1 1 d . . . C215 C 0.6350(6) 0.2871(3) 0.4942(3) 0.0275(17) Uani 1 1 d . . . H215 H 0.6674 0.2742 0.4645 0.033 Uiso 1 1 calc R . . C216 C 0.5978(6) 0.3365(3) 0.4900(3) 0.0306(17) Uani 1 1 d . . . H216 H 0.6035 0.3563 0.4575 0.037 Uiso 1 1 calc R . . C217 C 0.5520(6) 0.3554(3) 0.5351(3) 0.0289(17) Uani 1 1 d . . . H217 H 0.5274 0.3885 0.5328 0.035 Uiso 1 1 calc R . . C218 C 0.5418(6) 0.3269(3) 0.5833(3) 0.0263(16) Uani 1 1 d . . . H218 H 0.5104 0.3409 0.6128 0.032 Uiso 1 1 calc R . . C219 C 0.5784(6) 0.2765(3) 0.5888(3) 0.0233(15) Uani 1 1 d . . . C220 C 0.6595(7) 0.0693(3) 0.6867(3) 0.0335(18) Uani 1 1 d . . . H220 H 0.6668 0.0340 0.6766 0.040 Uiso 1 1 calc R . . C221 C 0.7727(7) 0.0925(3) 0.6984(3) 0.0311(18) Uani 1 1 d . . . C222 C 0.8672(7) 0.0640(3) 0.6952(4) 0.041(2) Uani 1 1 d . . . H222 H 0.8574 0.0308 0.6826 0.049 Uiso 1 1 calc R . . C223 C 0.9759(8) 0.0843(4) 0.7105(4) 0.049(2) Uani 1 1 d . . . H223 H 1.0386 0.0648 0.7085 0.058 Uiso 1 1 calc R . . C224 C 0.9903(8) 0.1336(3) 0.7287(4) 0.045(2) Uani 1 1 d . . . H224 H 1.0631 0.1474 0.7392 0.054 Uiso 1 1 calc R . . C225 C 0.8975(6) 0.1625(3) 0.7315(4) 0.0339(18) Uani 1 1 d . . . H225 H 0.9088 0.1955 0.7446 0.041 Uiso 1 1 calc R . . C226 C 0.7871(6) 0.1435(3) 0.7151(3) 0.0283(17) Uani 1 1 d . . . Ni5 Ni 0.43950(8) 0.23109(4) 0.76640(4) 0.0264(2) Uani 1 1 d . . . O5W O 0.5079(4) 0.28789(19) 0.7276(2) 0.0316(12) Uani 1 1 d . . . H5W1 H 0.5389 0.2715 0.6971 0.080 Uiso 1 1 d . . . H5W2 H 0.4625 0.3167 0.7257 0.080 Uiso 1 1 d . . . O5 O 0.4749(4) 0.17682(18) 0.7099(2) 0.0292(11) Uani 1 1 d . . . H5 H 0.4131 0.1661 0.7021 0.080 Uiso 1 1 d . . . O5S O 0.4065(4) 0.28491(19) 0.8259(2) 0.0322(12) Uani 1 1 d . . . H5S H 0.3411 0.3048 0.8096 0.080 Uiso 1 1 d . . . C5S C 0.4217(7) 0.2752(3) 0.8883(3) 0.0344(19) Uani 1 1 d . . . H5S1 H 0.4678 0.2458 0.8992 0.052 Uiso 1 1 calc R . . H5S2 H 0.3487 0.2700 0.8969 0.052 Uiso 1 1 calc R . . H5S3 H 0.4588 0.3033 0.9111 0.052 Uiso 1 1 calc R . . O1W O 0.3972(4) 0.3778(2) 0.7283(2) 0.0311(12) Uani 1 1 d . . . H1W1 H 0.3310 0.3680 0.7417 0.080 Uiso 1 1 d . . . H1W2 H 0.3698 0.3818 0.6882 0.080 Uiso 1 1 d . . . O2W O 0.6238(8) 0.3946(4) 0.7703(5) 0.076(3) Uiso 0.75 1 d P A 1 H2W1 H 0.5981 0.3963 0.7967 0.080 Uiso 0.75 1 d P B 1 H2W2 H 0.5950 0.3745 0.7425 0.080 Uiso 0.75 1 d P C 1 O2W' O 0.5693(18) 0.4288(8) 0.7985(10) 0.039(5) Uiso 0.25 1 d P D 2 O3W O 0.7579(18) 0.4557(8) 0.9607(10) 0.057(6) Uiso 0.30 1 d P E 3 O3W' O 0.870(3) 0.4473(13) 0.9867(16) 0.065(9) Uiso 0.20 1 d P F 4 O3W" O 0.651(2) 0.4437(10) 0.9224(13) 0.041(7) Uiso 0.20 1 d P G 5 O1S O 0.2397(5) 0.1364(3) 0.6829(3) 0.0609(18) Uani 1 1 d . . . H1S H 0.2402 0.1640 0.6988 0.091 Uiso 1 1 calc R . . C1S C 0.1621(10) 0.1373(5) 0.6233(6) 0.087(4) Uani 1 1 d . . . H1S1 H 0.0865 0.1292 0.6265 0.130 Uiso 1 1 calc R . . H1S2 H 0.1866 0.1133 0.5979 0.130 Uiso 1 1 calc R . . H1S3 H 0.1621 0.1702 0.6062 0.130 Uiso 1 1 calc R . . O2S O 0.7629(11) 0.4502(5) 0.8438(7) 0.064(4) Uiso 0.50 1 d P H 3 H2S H 0.7664 0.4595 0.8783 0.096 Uiso 0.50 1 calc PR H 3 C2S C 0.8031(16) 0.4871(7) 0.8133(9) 0.054(5) Uiso 0.50 1 d P H 3 H2S1 H 0.8221 0.5160 0.8387 0.081 Uiso 0.50 1 calc PR H 3 H2S2 H 0.7457 0.4958 0.7778 0.081 Uiso 0.50 1 calc PR H 3 H2S3 H 0.8700 0.4754 0.8019 0.081 Uiso 0.50 1 calc PR H 3 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 Ni11 0.0259(5) 0.0268(5) 0.0149(5) 0.0020(4) 0.0017(4) 0.0015(4) Ni12 0.0255(5) 0.0268(5) 0.0147(5) 0.0019(4) 0.0031(3) 0.0031(4) O101 0.030(3) 0.026(3) 0.022(3) 0.005(2) 0.002(2) -0.001(2) O102 0.030(3) 0.032(3) 0.011(2) -0.001(2) 0.0010(19) 0.006(2) O103 0.025(2) 0.026(3) 0.020(3) 0.000(2) 0.001(2) 0.003(2) N101 0.034(3) 0.037(4) 0.015(3) -0.003(3) 0.000(3) 0.001(3) N102 0.031(3) 0.027(3) 0.018(3) 0.003(3) 0.006(3) 0.005(3) N103 0.033(3) 0.025(3) 0.017(3) -0.002(3) -0.001(2) 0.003(3) N104 0.027(3) 0.027(3) 0.020(3) 0.004(3) 0.006(2) -0.001(3) O11S 0.033(3) 0.035(3) 0.020(3) 0.004(2) 0.002(2) 0.005(2) C11S 0.047(5) 0.060(6) 0.017(4) 0.007(4) 0.012(3) 0.007(4) O12S 0.037(3) 0.036(3) 0.016(3) 0.004(2) 0.006(2) 0.005(2) C12S 0.045(5) 0.050(5) 0.019(4) 0.015(4) 0.010(3) 0.003(4) O10 0.058(4) 0.051(4) 0.023(3) 0.004(3) 0.015(3) 0.024(3) O11 0.022(2) 0.030(3) 0.021(3) 0.003(2) 0.005(2) 0.005(2) O12 0.042(3) 0.041(3) 0.016(3) 0.009(2) 0.006(2) 0.015(3) C10 0.029(4) 0.031(4) 0.022(4) 0.003(3) 0.006(3) 0.006(3) C100 0.032(4) 0.026(4) 0.015(3) 0.001(3) 0.009(3) -0.002(3) C101 0.028(4) 0.027(4) 0.034(4) 0.001(3) 0.012(3) 0.005(3) C102 0.036(4) 0.043(5) 0.046(5) 0.004(4) 0.018(4) -0.003(4) C103 0.044(5) 0.042(5) 0.062(6) 0.012(4) 0.030(5) -0.002(4) C104 0.044(5) 0.041(5) 0.049(5) 0.021(4) 0.023(4) 0.012(4) C105 0.029(4) 0.033(4) 0.030(4) 0.003(3) 0.013(3) 0.005(3) C106 0.042(4) 0.030(4) 0.020(4) 0.005(3) 0.009(3) 0.008(4) C107 0.032(4) 0.046(5) 0.017(4) 0.006(3) -0.003(3) 0.006(4) C108 0.036(4) 0.038(5) 0.013(4) -0.001(3) -0.002(3) -0.003(4) C109 0.037(4) 0.025(4) 0.025(4) -0.001(3) 0.001(3) 0.001(3) C110 0.033(4) 0.018(4) 0.026(4) -0.002(3) 0.003(3) -0.004(3) C111 0.027(4) 0.036(5) 0.030(4) 0.008(3) 0.005(3) -0.001(3) C112 0.032(4) 0.040(5) 0.039(5) 0.006(4) 0.018(4) 0.004(4) C113 0.044(5) 0.031(5) 0.031(5) 0.001(4) 0.014(4) 0.006(4) C114 0.045(5) 0.027(4) 0.015(4) -0.002(3) 0.010(3) -0.002(3) C115 0.061(6) 0.042(5) 0.029(5) -0.005(4) 0.016(4) 0.001(4) C116 0.066(6) 0.043(5) 0.024(4) -0.011(4) 0.011(4) -0.005(5) C117 0.057(5) 0.029(5) 0.023(4) 0.002(3) -0.003(4) -0.008(4) C118 0.035(4) 0.030(4) 0.020(4) -0.001(3) 0.001(3) 0.003(3) C119 0.032(4) 0.028(4) 0.016(4) 0.000(3) 0.003(3) 0.003(3) C120 0.022(3) 0.032(4) 0.019(4) 0.005(3) 0.000(3) -0.005(3) C121 0.032(4) 0.021(4) 0.019(4) 0.000(3) 0.002(3) -0.001(3) C122 0.027(4) 0.038(5) 0.031(4) -0.004(4) -0.007(3) 0.006(3) C123 0.031(4) 0.040(5) 0.061(6) -0.006(4) -0.006(4) 0.019(4) C124 0.040(5) 0.023(4) 0.057(6) -0.009(4) -0.002(4) 0.006(4) C125 0.027(4) 0.034(5) 0.028(4) 0.000(3) -0.004(3) 0.000(3) C126 0.028(4) 0.028(4) 0.014(4) 0.004(3) 0.000(3) 0.005(3) Ni21 0.0369(5) 0.0269(5) 0.0183(5) 0.0048(4) 0.0092(4) 0.0077(4) Ni22 0.0428(6) 0.0285(6) 0.0158(5) 0.0024(4) 0.0095(4) 0.0100(4) O201 0.032(3) 0.033(3) 0.018(3) 0.003(2) 0.007(2) 0.008(2) O202 0.054(3) 0.025(3) 0.019(3) 0.003(2) 0.016(2) 0.009(2) O203 0.039(3) 0.027(3) 0.015(2) 0.006(2) 0.008(2) 0.011(2) N201 0.050(4) 0.031(4) 0.025(4) 0.000(3) 0.012(3) 0.011(3) N202 0.048(4) 0.030(4) 0.020(3) 0.003(3) 0.014(3) 0.014(3) N203 0.052(4) 0.026(4) 0.023(3) -0.001(3) 0.010(3) 0.009(3) N204 0.045(4) 0.026(3) 0.022(3) 0.001(3) 0.010(3) 0.007(3) O21 0.043(3) 0.031(3) 0.032(3) 0.011(2) 0.011(2) 0.008(3) O22 0.039(3) 0.034(3) 0.026(3) 0.007(2) 0.009(2) 0.009(2) C20 0.032(4) 0.026(4) 0.024(4) 0.000(3) 0.010(3) 0.003(3) C21 0.058(6) 0.036(5) 0.067(7) 0.016(5) 0.028(5) 0.003(4) O22S 0.054(3) 0.039(3) 0.015(3) 0.001(2) 0.008(2) 0.012(3) C22S 0.054(5) 0.042(5) 0.015(4) 0.001(3) 0.007(3) 0.005(4) C200 0.041(4) 0.026(4) 0.013(3) 0.005(3) 0.010(3) 0.004(3) C201 0.038(4) 0.029(4) 0.023(4) 0.008(3) 0.013(3) 0.006(3) C202 0.049(5) 0.044(5) 0.024(4) 0.005(4) 0.017(4) -0.002(4) C203 0.051(5) 0.041(5) 0.033(5) 0.005(4) 0.017(4) -0.011(4) C204 0.036(4) 0.043(5) 0.028(4) 0.005(4) 0.009(4) -0.001(4) C205 0.035(4) 0.034(5) 0.026(4) 0.008(3) 0.014(3) 0.006(4) C206 0.035(4) 0.051(5) 0.014(4) 0.010(3) 0.006(3) 0.011(4) C207 0.047(5) 0.035(5) 0.023(4) 0.010(3) 0.004(4) 0.013(4) C208 0.056(5) 0.031(5) 0.026(4) 0.013(3) 0.016(4) 0.014(4) C209 0.053(5) 0.032(5) 0.041(5) 0.001(4) 0.012(4) -0.001(4) C210 0.052(5) 0.028(5) 0.035(5) -0.006(4) 0.008(4) 0.007(4) C211 0.077(6) 0.038(5) 0.016(4) -0.002(3) 0.006(4) 0.019(5) C212 0.083(7) 0.044(5) 0.021(4) 0.001(4) 0.021(4) 0.028(5) C213 0.032(4) 0.040(5) 0.014(4) 0.001(3) 0.010(3) 0.005(3) C214 0.024(4) 0.032(4) 0.015(3) 0.000(3) 0.002(3) -0.002(3) C215 0.027(4) 0.045(5) 0.010(3) -0.002(3) 0.003(3) -0.009(3) C216 0.037(4) 0.035(5) 0.018(4) 0.003(3) 0.005(3) -0.007(4) C217 0.028(4) 0.024(4) 0.032(4) 0.003(3) 0.003(3) -0.005(3) C218 0.033(4) 0.033(4) 0.013(3) 0.002(3) 0.008(3) 0.001(3) C219 0.026(4) 0.031(4) 0.011(3) 0.001(3) 0.003(3) 0.001(3) C220 0.053(5) 0.022(4) 0.028(4) 0.003(3) 0.014(4) 0.011(4) C221 0.042(4) 0.033(5) 0.021(4) 0.008(3) 0.012(3) 0.009(4) C222 0.060(6) 0.034(5) 0.034(5) 0.015(4) 0.022(4) 0.024(4) C223 0.050(5) 0.057(6) 0.048(6) 0.024(5) 0.028(4) 0.031(5) C224 0.055(5) 0.040(5) 0.044(5) 0.013(4) 0.020(4) 0.010(4) C225 0.039(4) 0.031(4) 0.035(5) 0.010(4) 0.014(4) 0.012(4) C226 0.042(4) 0.027(4) 0.019(4) 0.013(3) 0.014(3) 0.016(4) Ni5 0.0378(5) 0.0281(5) 0.0144(5) 0.0047(4) 0.0084(4) 0.0099(4) O5W 0.051(3) 0.029(3) 0.018(3) 0.004(2) 0.014(2) 0.009(2) O5 0.039(3) 0.029(3) 0.020(3) 0.000(2) 0.008(2) 0.006(2) O5S 0.047(3) 0.038(3) 0.010(2) 0.003(2) 0.004(2) 0.015(3) C5S 0.046(5) 0.049(5) 0.008(3) 0.005(3) 0.006(3) 0.005(4) O1W 0.035(3) 0.039(3) 0.017(3) 0.005(2) 0.001(2) 0.003(2) O1S 0.057(4) 0.054(4) 0.079(5) -0.012(4) 0.029(4) -0.003(3) C1S 0.067(7) 0.110(11) 0.083(10) 0.019(8) 0.018(7) -0.006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni11 O101 2.007(5) . ? Ni11 N101 2.017(6) . ? Ni11 O103 2.060(5) . ? Ni11 O11 2.062(5) . ? Ni11 O11S 2.134(5) . ? Ni11 N103 2.165(6) . ? Ni12 N102 2.010(6) . ? Ni12 O102 2.040(5) . ? Ni12 O103 2.045(5) . ? Ni12 O11 2.081(5) . ? Ni12 O12S 2.106(5) . ? Ni12 N104 2.167(6) . ? O101 C100 1.290(8) . ? O102 C119 1.337(8) . ? O103 C126 1.325(8) . ? N101 C106 1.267(9) . ? N101 C107 1.466(9) . ? N102 C113 1.283(10) . ? N102 C112 1.477(9) . ? N103 C109 1.477(9) . ? N103 C120 1.488(9) . ? N103 C108 1.501(9) . ? N104 C110 1.491(9) . ? N104 C111 1.492(9) . ? N104 C120 1.500(9) . ? O11S C11S 1.423(9) . ? O11S H11S 0.82(11) . ? C11S H11A 0.9600 . ? C11S H11B 0.9600 . ? C11S H11C 0.9600 . ? O12S C12S 1.435(8) . ? O12S H12S 0.91(11) . ? C12S H12A 0.9600 . ? C12S H12B 0.9600 . ? C12S H12C 0.9600 . ? O10 C10 1.271(9) . ? O11 C10 1.291(8) . ? O12 C10 1.283(9) . ? O12 Ni5 2.097(5) . ? C100 C101 1.420(10) . ? C100 C105 1.420(10) . ? C101 C102 1.360(11) . ? C101 H101 0.9300 . ? C102 C103 1.400(12) . ? C102 H102 0.9300 . ? C103 C104 1.367(12) . ? C103 H103 0.9300 . ? C104 C105 1.404(11) . ? C104 H104 0.9300 . ? C105 C106 1.443(10) . ? C106 H106 0.9300 . ? C107 C108 1.501(11) . ? C107 H10A 0.9700 . ? C107 H10B 0.9700 . ? C108 H10C 0.9700 . ? C108 H10D 0.9700 . ? C109 C110 1.511(10) . ? C109 H10E 0.9700 . ? C109 H10F 0.9700 . ? C110 H11D 0.9700 . ? C110 H11E 0.9700 . ? C111 C112 1.529(11) . ? C111 H11F 0.9700 . ? C111 H11G 0.9700 . ? C112 H12H 0.9700 . ? C112 H12I 0.9700 . ? C113 C114 1.436(11) . ? C113 H113 0.9300 . ? C114 C115 1.430(11) . ? C114 C119 1.430(10) . ? C115 C116 1.376(12) . ? C115 H115 0.9300 . ? C116 C117 1.386(12) . ? C116 H116 0.9300 . ? C117 C118 1.383(11) . ? C117 H117 0.9300 . ? C118 C119 1.375(10) . ? C118 H118 0.9300 . ? C120 C121 1.482(10) . ? C120 H120 0.9800 . ? C121 C122 1.383(10) . ? C121 C126 1.426(10) . ? C122 C123 1.373(12) . ? C122 H122 0.9300 . ? C123 C124 1.375(11) . ? C123 H123 0.9300 . ? C124 C125 1.368(10) . ? C124 H124 0.9300 . ? C125 C126 1.384(10) . ? C125 H125 0.9300 . ? Ni21 N202 1.995(6) . ? Ni21 O201 2.001(5) . ? Ni21 O5 2.009(5) . ? Ni21 O21 2.068(5) . ? Ni21 O203 2.102(5) . ? Ni21 N204 2.131(6) . ? Ni21 Ni5 2.9572(13) . ? Ni22 O202 2.019(5) . ? Ni22 N201 2.041(6) . ? Ni22 O5 2.045(5) . ? Ni22 O203 2.047(5) . ? Ni22 O22S 2.149(6) . ? Ni22 N203 2.218(6) . ? O201 C200 1.318(9) . ? O201 Ni5 2.058(5) . ? O202 C219 1.318(8) . ? O203 C226 1.333(8) . ? N201 C213 1.276(9) . ? N201 C212 1.464(10) . ? N202 C206 1.274(10) . ? N202 C207 1.479(10) . ? N203 C210 1.474(10) . ? N203 C211 1.477(9) . ? N203 C220 1.491(10) . ? N204 C209 1.478(10) . ? N204 C208 1.487(9) . ? N204 C220 1.508(9) . ? O21 C20 1.257(8) . ? O22 C20 1.261(9) . ? O22 Ni5 2.021(5) . ? C20 C21 1.484(10) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? O22S C22S 1.454(9) . ? O22S H22S 0.75(11) . ? C22S H22A 0.9600 . ? C22S H22B 0.9600 . ? C22S H22C 0.9600 . ? C200 C201 1.402(10) . ? C200 C205 1.421(10) . ? C201 C202 1.384(11) . ? C201 H201 0.9300 . ? C202 C203 1.389(12) . ? C202 H202 0.9300 . ? C203 C204 1.357(12) . ? C203 H203 0.9300 . ? C204 C205 1.420(11) . ? C204 H204 0.9300 . ? C205 C206 1.444(11) . ? C206 H206 0.9300 . ? C207 C208 1.530(11) . ? C207 H20A 0.9700 . ? C207 H20B 0.9700 . ? C208 H20C 0.9700 . ? C208 H20D 0.9700 . ? C209 C210 1.542(11) . ? C209 H20E 0.9700 . ? C209 H20F 0.9700 . ? C210 H21D 0.9700 . ? C210 H21E 0.9700 . ? C211 C212 1.497(13) . ? C211 H21F 0.9700 . ? C211 H21G 0.9700 . ? C212 H21H 0.9700 . ? C212 H21I 0.9700 . ? C213 C214 1.426(10) . ? C213 H213 0.9300 . ? C214 C215 1.412(10) . ? C214 C219 1.426(9) . ? C215 C216 1.388(11) . ? C215 H215 0.9300 . ? C216 C217 1.382(10) . ? C216 H216 0.9300 . ? C217 C218 1.372(10) . ? C217 H217 0.9300 . ? C218 C219 1.412(10) . ? C218 H218 0.9300 . ? C220 C221 1.467(11) . ? C220 H220 0.9800 . ? C221 C222 1.390(10) . ? C221 C226 1.412(11) . ? C222 C223 1.385(13) . ? C222 H222 0.9300 . ? C223 C224 1.380(13) . ? C223 H223 0.9300 . ? C224 C225 1.375(11) . ? C224 H224 0.9300 . ? C225 C226 1.392(11) . ? C225 H225 0.9300 . ? Ni5 O5W 2.033(5) . ? Ni5 O5 2.057(5) . ? Ni5 O5S 2.085(5) . ? O5W H5W1 0.9736 . ? O5W H5W2 0.9402 . ? O5 H5 0.7794 . ? O5S C5S 1.421(8) . ? O5S H5S 0.9491 . ? C5S H5S1 0.9600 . ? C5S H5S2 0.9600 . ? C5S H5S3 0.9600 . ? O1W H1W1 0.9605 . ? O1W H1W2 0.9041 . ? O2W H2W1 0.7448 . ? O2W H2W2 0.8419 . ? O2W' H2W1 0.9405 . ? O1S C1S 1.457(14) . ? O1S H1S 0.8200 . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? O2S C2S 1.36(2) . ? O2S H2S 0.8200 . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 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 O101 Ni11 N101 89.5(2) . . ? O101 Ni11 O103 93.81(19) . . ? N101 Ni11 O103 99.8(2) . . ? O101 Ni11 O11 94.26(18) . . ? N101 Ni11 O11 176.1(2) . . ? O103 Ni11 O11 79.09(18) . . ? O101 Ni11 O11S 90.8(2) . . ? N101 Ni11 O11S 91.4(2) . . ? O103 Ni11 O11S 167.8(2) . . ? O11 Ni11 O11S 89.36(19) . . ? O101 Ni11 N103 173.8(2) . . ? N101 Ni11 N103 84.6(2) . . ? O103 Ni11 N103 88.9(2) . . ? O11 Ni11 N103 91.7(2) . . ? O11S Ni11 N103 87.6(2) . . ? N102 Ni12 O102 89.4(2) . . ? N102 Ni12 O103 98.4(2) . . ? O102 Ni12 O103 93.50(19) . . ? N102 Ni12 O11 174.3(2) . . ? O102 Ni12 O11 95.78(18) . . ? O103 Ni12 O11 79.01(19) . . ? N102 Ni12 O12S 95.1(2) . . ? O102 Ni12 O12S 89.44(19) . . ? O103 Ni12 O12S 166.24(19) . . ? O11 Ni12 O12S 87.33(19) . . ? N102 Ni12 N104 83.2(2) . . ? O102 Ni12 N104 172.2(2) . . ? O103 Ni12 N104 90.1(2) . . ? O11 Ni12 N104 91.7(2) . . ? O12S Ni12 N104 88.7(2) . . ? C100 O101 Ni11 128.4(4) . . ? C119 O102 Ni12 127.4(4) . . ? C126 O103 Ni12 116.6(4) . . ? C126 O103 Ni11 114.8(4) . . ? Ni12 O103 Ni11 98.7(2) . . ? C106 N101 C107 120.4(6) . . ? C106 N101 Ni11 127.1(5) . . ? C107 N101 Ni11 112.5(5) . . ? C113 N102 C112 116.8(6) . . ? C113 N102 Ni12 128.0(5) . . ? C112 N102 Ni12 115.0(5) . . ? C109 N103 C120 103.8(6) . . ? C109 N103 C108 111.0(5) . . ? C120 N103 C108 112.9(5) . . ? C109 N103 Ni11 113.6(4) . . ? C120 N103 Ni11 114.6(4) . . ? C108 N103 Ni11 101.2(4) . . ? C110 N104 C111 111.3(6) . . ? C110 N104 C120 102.8(5) . . ? C111 N104 C120 112.4(5) . . ? C110 N104 Ni12 114.7(4) . . ? C111 N104 Ni12 103.2(4) . . ? C120 N104 Ni12 112.9(4) . . ? C11S O11S Ni11 122.7(5) . . ? C11S O11S H11S 100(8) . . ? Ni11 O11S H11S 95(8) . . ? O11S C11S H11A 109.5 . . ? O11S C11S H11B 109.5 . . ? H11A C11S H11B 109.5 . . ? O11S C11S H11C 109.5 . . ? H11A C11S H11C 109.5 . . ? H11B C11S H11C 109.5 . . ? C12S O12S Ni12 123.0(5) . . ? C12S O12S H12S 115(7) . . ? Ni12 O12S H12S 101(7) . . ? O12S C12S H12A 109.5 . . ? O12S C12S H12B 109.5 . . ? H12A C12S H12B 109.5 . . ? O12S C12S H12C 109.5 . . ? H12A C12S H12C 109.5 . . ? H12B C12S H12C 109.5 . . ? C10 O11 Ni11 130.3(4) . . ? C10 O11 Ni12 132.2(4) . . ? Ni11 O11 Ni12 97.48(19) . . ? C10 O12 Ni5 124.0(5) . . ? O10 C10 O12 121.4(7) . . ? O10 C10 O11 120.4(6) . . ? O12 C10 O11 118.2(6) . . ? O101 C100 C101 118.9(6) . . ? O101 C100 C105 125.1(6) . . ? C101 C100 C105 116.0(6) . . ? C102 C101 C100 123.0(7) . . ? C102 C101 H101 118.5 . . ? C100 C101 H101 118.5 . . ? C101 C102 C103 120.3(8) . . ? C101 C102 H102 119.9 . . ? C103 C102 H102 119.9 . . ? C104 C103 C102 118.6(8) . . ? C104 C103 H103 120.7 . . ? C102 C103 H103 120.7 . . ? C103 C104 C105 122.4(8) . . ? C103 C104 H104 118.8 . . ? C105 C104 H104 118.8 . . ? C104 C105 C100 119.7(7) . . ? C104 C105 C106 117.9(7) . . ? C100 C105 C106 122.3(7) . . ? N101 C106 C105 126.9(7) . . ? N101 C106 H106 116.5 . . ? C105 C106 H106 116.5 . . ? N101 C107 C108 109.3(6) . . ? N101 C107 H10A 109.8 . . ? C108 C107 H10A 109.8 . . ? N101 C107 H10B 109.8 . . ? C108 C107 H10B 109.8 . . ? H10A C107 H10B 108.3 . . ? C107 C108 N103 113.1(6) . . ? C107 C108 H10C 109.0 . . ? N103 C108 H10C 109.0 . . ? C107 C108 H10D 109.0 . . ? N103 C108 H10D 109.0 . . ? H10C C108 H10D 107.8 . . ? N103 C109 C110 105.1(6) . . ? N103 C109 H10E 110.7 . . ? C110 C109 H10E 110.7 . . ? N103 C109 H10F 110.7 . . ? C110 C109 H10F 110.7 . . ? H10E C109 H10F 108.8 . . ? N104 C110 C109 105.2(6) . . ? N104 C110 H11D 110.7 . . ? C109 C110 H11D 110.7 . . ? N104 C110 H11E 110.7 . . ? C109 C110 H11E 110.7 . . ? H11D C110 H11E 108.8 . . ? N104 C111 C112 112.7(6) . . ? N104 C111 H11F 109.0 . . ? C112 C111 H11F 109.0 . . ? N104 C111 H11G 109.0 . . ? C112 C111 H11G 109.0 . . ? H11F C111 H11G 107.8 . . ? N102 C112 C111 108.6(6) . . ? N102 C112 H12H 110.0 . . ? C111 C112 H12H 110.0 . . ? N102 C112 H12I 110.0 . . ? C111 C112 H12I 110.0 . . ? H12H C112 H12I 108.4 . . ? N102 C113 C114 125.5(7) . . ? N102 C113 H113 117.2 . . ? C114 C113 H113 117.2 . . ? C115 C114 C119 116.9(7) . . ? C115 C114 C113 117.6(7) . . ? C119 C114 C113 125.5(7) . . ? C116 C115 C114 122.9(8) . . ? C116 C115 H115 118.6 . . ? C114 C115 H115 118.6 . . ? C115 C116 C117 118.7(8) . . ? C115 C116 H116 120.7 . . ? C117 C116 H116 120.7 . . ? C118 C117 C116 119.7(8) . . ? C118 C117 H117 120.1 . . ? C116 C117 H117 120.1 . . ? C119 C118 C117 123.4(7) . . ? C119 C118 H118 118.3 . . ? C117 C118 H118 118.3 . . ? O102 C119 C118 119.7(6) . . ? O102 C119 C114 121.9(6) . . ? C118 C119 C114 118.3(7) . . ? C121 C120 N103 114.9(6) . . ? C121 C120 N104 116.1(6) . . ? N103 C120 N104 99.9(5) . . ? C121 C120 H120 108.5 . . ? N103 C120 H120 108.5 . . ? N104 C120 H120 108.5 . . ? C122 C121 C126 119.3(7) . . ? C122 C121 C120 120.8(6) . . ? C126 C121 C120 119.9(6) . . ? C123 C122 C121 120.8(7) . . ? C123 C122 H122 119.6 . . ? C121 C122 H122 119.6 . . ? C122 C123 C124 119.7(7) . . ? C122 C123 H123 120.1 . . ? C124 C123 H123 120.1 . . ? C125 C124 C123 121.0(8) . . ? C125 C124 H124 119.5 . . ? C123 C124 H124 119.5 . . ? C124 C125 C126 120.8(7) . . ? C124 C125 H125 119.6 . . ? C126 C125 H125 119.6 . . ? O103 C126 C125 121.6(6) . . ? O103 C126 C121 120.1(6) . . ? C125 C126 C121 118.3(6) . . ? N202 Ni21 O201 89.7(2) . . ? N202 Ni21 O5 169.1(2) . . ? O201 Ni21 O5 84.64(19) . . ? N202 Ni21 O21 94.5(2) . . ? O201 Ni21 O21 89.7(2) . . ? O5 Ni21 O21 94.8(2) . . ? N202 Ni21 O203 90.6(2) . . ? O201 Ni21 O203 93.92(19) . . ? O5 Ni21 O203 80.50(19) . . ? O21 Ni21 O203 173.8(2) . . ? N202 Ni21 N204 84.7(2) . . ? O201 Ni21 N204 173.7(2) . . ? O5 Ni21 N204 101.3(2) . . ? O21 Ni21 N204 87.7(2) . . ? O203 Ni21 N204 89.2(2) . . ? N202 Ni21 Ni5 132.90(18) . . ? O201 Ni21 Ni5 43.99(14) . . ? O5 Ni21 Ni5 43.98(14) . . ? O21 Ni21 Ni5 79.79(14) . . ? O203 Ni21 Ni5 99.37(13) . . ? N204 Ni21 Ni5 140.81(18) . . ? O202 Ni22 N201 88.5(2) . . ? O202 Ni22 O5 94.51(19) . . ? N201 Ni22 O5 175.2(2) . . ? O202 Ni22 O203 94.6(2) . . ? N201 Ni22 O203 102.6(2) . . ? O5 Ni22 O203 81.00(19) . . ? O202 Ni22 O22S 87.2(2) . . ? N201 Ni22 O22S 94.4(2) . . ? O5 Ni22 O22S 82.0(2) . . ? O203 Ni22 O22S 163.01(19) . . ? O202 Ni22 N203 170.4(2) . . ? N201 Ni22 N203 82.0(2) . . ? O5 Ni22 N203 95.0(2) . . ? O203 Ni22 N203 88.5(2) . . ? O22S Ni22 N203 92.5(2) . . ? C200 O201 Ni21 125.5(4) . . ? C200 O201 Ni5 136.2(5) . . ? Ni21 O201 Ni5 93.5(2) . . ? C219 O202 Ni22 127.9(4) . . ? C226 O203 Ni22 118.7(4) . . ? C226 O203 Ni21 115.9(4) . . ? Ni22 O203 Ni21 93.6(2) . . ? C213 N201 C212 120.0(6) . . ? C213 N201 Ni22 126.4(5) . . ? C212 N201 Ni22 113.3(5) . . ? C206 N202 C207 119.6(7) . . ? C206 N202 Ni21 123.1(5) . . ? C207 N202 Ni21 113.6(5) . . ? C210 N203 C211 110.8(6) . . ? C210 N203 C220 102.6(6) . . ? C211 N203 C220 112.3(6) . . ? C210 N203 Ni22 115.1(5) . . ? C211 N203 Ni22 103.2(5) . . ? C220 N203 Ni22 113.2(5) . . ? C209 N204 C208 110.9(6) . . ? C209 N204 C220 102.0(6) . . ? C208 N204 C220 115.2(6) . . ? C209 N204 Ni21 112.5(5) . . ? C208 N204 Ni21 102.0(5) . . ? C220 N204 Ni21 114.6(5) . . ? C20 O21 Ni21 126.0(5) . . ? C20 O22 Ni5 127.9(5) . . ? O21 C20 O22 125.9(7) . . ? O21 C20 C21 117.3(7) . . ? O22 C20 C21 116.7(6) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22S O22S Ni22 128.3(5) . . ? C22S O22S H22S 91(9) . . ? Ni22 O22S H22S 102(9) . . ? O22S C22S H22A 109.5 . . ? O22S C22S H22B 109.5 . . ? H22A C22S H22B 109.5 . . ? O22S C22S H22C 109.5 . . ? H22A C22S H22C 109.5 . . ? H22B C22S H22C 109.5 . . ? O201 C200 C201 121.0(7) . . ? O201 C200 C205 121.1(7) . . ? C201 C200 C205 117.9(7) . . ? C202 C201 C200 121.8(7) . . ? C202 C201 H201 119.1 . . ? C200 C201 H201 119.1 . . ? C201 C202 C203 120.3(8) . . ? C201 C202 H202 119.8 . . ? C203 C202 H202 119.8 . . ? C204 C203 C202 119.1(8) . . ? C204 C203 H203 120.5 . . ? C202 C203 H203 120.5 . . ? C203 C204 C205 122.7(8) . . ? C203 C204 H204 118.7 . . ? C205 C204 H204 118.7 . . ? C204 C205 C200 118.2(7) . . ? C204 C205 C206 116.3(7) . . ? C200 C205 C206 125.5(7) . . ? N202 C206 C205 125.6(7) . . ? N202 C206 H206 117.2 . . ? C205 C206 H206 117.2 . . ? N202 C207 C208 108.8(6) . . ? N202 C207 H20A 109.9 . . ? C208 C207 H20A 109.9 . . ? N202 C207 H20B 109.9 . . ? C208 C207 H20B 109.9 . . ? H20A C207 H20B 108.3 . . ? N204 C208 C207 112.9(6) . . ? N204 C208 H20C 109.0 . . ? C207 C208 H20C 109.0 . . ? N204 C208 H20D 109.0 . . ? C207 C208 H20D 109.0 . . ? H20C C208 H20D 107.8 . . ? N204 C209 C210 103.8(6) . . ? N204 C209 H20E 111.0 . . ? C210 C209 H20E 111.0 . . ? N204 C209 H20F 111.0 . . ? C210 C209 H20F 111.0 . . ? H20E C209 H20F 109.0 . . ? N203 C210 C209 105.9(6) . . ? N203 C210 H21D 110.5 . . ? C209 C210 H21D 110.5 . . ? N203 C210 H21E 110.5 . . ? C209 C210 H21E 110.5 . . ? H21D C210 H21E 108.7 . . ? N203 C211 C212 112.3(7) . . ? N203 C211 H21F 109.1 . . ? C212 C211 H21F 109.1 . . ? N203 C211 H21G 109.1 . . ? C212 C211 H21G 109.1 . . ? H21F C211 H21G 107.9 . . ? N201 C212 C211 109.1(7) . . ? N201 C212 H21H 109.9 . . ? C211 C212 H21H 109.9 . . ? N201 C212 H21I 109.9 . . ? C211 C212 H21I 109.9 . . ? H21H C212 H21I 108.3 . . ? N201 C213 C214 127.4(6) . . ? N201 C213 H213 116.3 . . ? C214 C213 H213 116.3 . . ? C215 C214 C219 118.9(7) . . ? C215 C214 C213 117.2(6) . . ? C219 C214 C213 123.7(6) . . ? C216 C215 C214 121.6(6) . . ? C216 C215 H215 119.2 . . ? C214 C215 H215 119.2 . . ? C217 C216 C215 118.5(7) . . ? C217 C216 H216 120.7 . . ? C215 C216 H216 120.7 . . ? C218 C217 C216 122.0(7) . . ? C218 C217 H217 119.0 . . ? C216 C217 H217 119.0 . . ? C217 C218 C219 120.9(6) . . ? C217 C218 H218 119.5 . . ? C219 C218 H218 119.5 . . ? O202 C219 C218 119.3(6) . . ? O202 C219 C214 122.7(6) . . ? C218 C219 C214 118.0(6) . . ? C221 C220 N203 117.4(6) . . ? C221 C220 N204 113.5(6) . . ? N203 C220 N204 100.2(6) . . ? C221 C220 H220 108.4 . . ? N203 C220 H220 108.4 . . ? N204 C220 H220 108.4 . . ? C222 C221 C226 119.6(8) . . ? C222 C221 C220 120.1(7) . . ? C226 C221 C220 120.3(7) . . ? C223 C222 C221 120.9(8) . . ? C223 C222 H222 119.5 . . ? C221 C222 H222 119.5 . . ? C224 C223 C222 119.5(8) . . ? C224 C223 H223 120.3 . . ? C222 C223 H223 120.3 . . ? C225 C224 C223 120.3(9) . . ? C225 C224 H224 119.9 . . ? C223 C224 H224 119.9 . . ? C224 C225 C226 121.6(8) . . ? C224 C225 H225 119.2 . . ? C226 C225 H225 119.2 . . ? O203 C226 C225 121.2(7) . . ? O203 C226 C221 120.6(7) . . ? C225 C226 C221 118.1(7) . . ? O22 Ni5 O5W 172.8(2) . . ? O22 Ni5 O5 92.5(2) . . ? O5W Ni5 O5 94.62(19) . . ? O22 Ni5 O201 91.6(2) . . ? O5W Ni5 O201 90.7(2) . . ? O5 Ni5 O201 82.01(19) . . ? O22 Ni5 O5S 86.7(2) . . ? O5W Ni5 O5S 86.3(2) . . ? O5 Ni5 O5S 178.30(19) . . ? O201 Ni5 O5S 96.52(19) . . ? O22 Ni5 O12 83.0(2) . . ? O5W Ni5 O12 95.4(2) . . ? O5 Ni5 O12 92.4(2) . . ? O201 Ni5 O12 172.1(2) . . ? O5S Ni5 O12 88.9(2) . . ? O22 Ni5 Ni21 80.00(14) . . ? O5W Ni5 Ni21 106.20(14) . . ? O5 Ni5 Ni21 42.71(14) . . ? O201 Ni5 Ni21 42.49(14) . . ? O5S Ni5 Ni21 135.62(14) . . ? O12 Ni5 Ni21 130.36(15) . . ? Ni5 O5W H5W1 104.3 . . ? Ni5 O5W H5W2 109.6 . . ? H5W1 O5W H5W2 131.1 . . ? Ni21 O5 Ni22 96.6(2) . . ? Ni21 O5 Ni5 93.3(2) . . ? Ni22 O5 Ni5 134.9(3) . . ? Ni21 O5 H5 120.6 . . ? Ni22 O5 H5 117.7 . . ? Ni5 O5 H5 93.8 . . ? C5S O5S Ni5 122.3(5) . . ? C5S O5S H5S 112.8 . . ? Ni5 O5S H5S 113.7 . . ? O5S C5S H5S1 109.5 . . ? O5S C5S H5S2 109.5 . . ? H5S1 C5S H5S2 109.5 . . ? O5S C5S H5S3 109.5 . . ? H5S1 C5S H5S3 109.5 . . ? H5S2 C5S H5S3 109.5 . . ? H1W1 O1W H1W2 103.2 . . ? H2W1 O2W H2W2 118.3 . . ? C1S O1S H1S 109.5 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C2S O2S H2S 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N101 Ni11 O101 C100 5.7(6) . . . . ? O103 Ni11 O101 C100 -94.1(6) . . . . ? O11 Ni11 O101 C100 -173.4(5) . . . . ? O11S Ni11 O101 C100 97.1(6) . . . . ? N102 Ni12 O102 C119 -16.6(6) . . . . ? O103 Ni12 O102 C119 81.7(5) . . . . ? O11 Ni12 O102 C119 161.0(5) . . . . ? O12S Ni12 O102 C119 -111.7(5) . . . . ? N102 Ni12 O103 C126 -33.3(5) . . . . ? O102 Ni12 O103 C126 -123.2(5) . . . . ? O11 Ni12 O103 C126 141.6(5) . . . . ? O12S Ni12 O103 C126 134.7(8) . . . . ? N104 Ni12 O103 C126 49.9(5) . . . . ? N102 Ni12 O103 Ni11 -156.7(2) . . . . ? O102 Ni12 O103 Ni11 113.36(19) . . . . ? O11 Ni12 O103 Ni11 18.15(18) . . . . ? O12S Ni12 O103 Ni11 11.3(9) . . . . ? N104 Ni12 O103 Ni11 -73.6(2) . . . . ? O101 Ni11 O103 C126 123.3(5) . . . . ? N101 Ni11 O103 C126 33.2(5) . . . . ? O11 Ni11 O103 C126 -143.0(5) . . . . ? O11S Ni11 O103 C126 -124.5(9) . . . . ? N103 Ni11 O103 C126 -51.1(5) . . . . ? O101 Ni11 O103 Ni12 -111.9(2) . . . . ? N101 Ni11 O103 Ni12 157.9(2) . . . . ? O11 Ni11 O103 Ni12 -18.32(18) . . . . ? N103 Ni11 O103 Ni12 73.6(2) . . . . ? O101 Ni11 N101 C106 1.7(6) . . . . ? O103 Ni11 N101 C106 95.5(6) . . . . ? O11S Ni11 N101 C106 -89.1(6) . . . . ? N103 Ni11 N101 C106 -176.6(6) . . . . ? O101 Ni11 N101 C107 -179.8(5) . . . . ? O103 Ni11 N101 C107 -86.0(5) . . . . ? O11S Ni11 N101 C107 89.4(5) . . . . ? N103 Ni11 N101 C107 1.9(5) . . . . ? O102 Ni12 N102 C113 9.4(7) . . . . ? O103 Ni12 N102 C113 -84.1(7) . . . . ? O12S Ni12 N102 C113 98.8(7) . . . . ? N104 Ni12 N102 C113 -173.2(7) . . . . ? O102 Ni12 N102 C112 -175.7(5) . . . . ? O103 Ni12 N102 C112 90.8(5) . . . . ? O12S Ni12 N102 C112 -86.3(5) . . . . ? N104 Ni12 N102 C112 1.7(5) . . . . ? N101 Ni11 N103 C109 141.0(5) . . . . ? O103 Ni11 N103 C109 -119.0(5) . . . . ? O11 Ni11 N103 C109 -39.9(5) . . . . ? O11S Ni11 N103 C109 49.4(5) . . . . ? N101 Ni11 N103 C120 -99.9(5) . . . . ? O103 Ni11 N103 C120 0.1(5) . . . . ? O11 Ni11 N103 C120 79.1(5) . . . . ? O11S Ni11 N103 C120 168.4(5) . . . . ? N101 Ni11 N103 C108 22.0(4) . . . . ? O103 Ni11 N103 C108 122.0(4) . . . . ? O11 Ni11 N103 C108 -159.0(4) . . . . ? O11S Ni11 N103 C108 -69.7(4) . . . . ? N102 Ni12 N104 C110 -145.1(5) . . . . ? O103 Ni12 N104 C110 116.5(4) . . . . ? O11 Ni12 N104 C110 37.5(5) . . . . ? O12S Ni12 N104 C110 -49.8(5) . . . . ? N102 Ni12 N104 C111 -23.9(4) . . . . ? O103 Ni12 N104 C111 -122.3(4) . . . . ? O11 Ni12 N104 C111 158.7(4) . . . . ? O12S Ni12 N104 C111 71.4(4) . . . . ? N102 Ni12 N104 C120 97.7(5) . . . . ? O103 Ni12 N104 C120 -0.7(4) . . . . ? O11 Ni12 N104 C120 -79.7(4) . . . . ? O12S Ni12 N104 C120 -167.0(4) . . . . ? O101 Ni11 O11S C11S -43.3(5) . . . . ? N101 Ni11 O11S C11S 46.3(5) . . . . ? O103 Ni11 O11S C11S -155.7(8) . . . . ? O11 Ni11 O11S C11S -137.5(5) . . . . ? N103 Ni11 O11S C11S 130.8(5) . . . . ? N102 Ni12 O12S C12S -36.4(5) . . . . ? O102 Ni12 O12S C12S 52.9(5) . . . . ? O103 Ni12 O12S C12S 155.4(7) . . . . ? O11 Ni12 O12S C12S 148.7(5) . . . . ? N104 Ni12 O12S C12S -119.5(5) . . . . ? O101 Ni11 O11 C10 -68.6(6) . . . . ? O103 Ni11 O11 C10 -161.7(6) . . . . ? O11S Ni11 O11 C10 22.2(6) . . . . ? N103 Ni11 O11 C10 109.8(6) . . . . ? O101 Ni11 O11 Ni12 111.0(2) . . . . ? O103 Ni11 O11 Ni12 17.94(18) . . . . ? O11S Ni11 O11 Ni12 -158.2(2) . . . . ? N103 Ni11 O11 Ni12 -70.6(2) . . . . ? O102 Ni12 O11 C10 69.1(6) . . . . ? O103 Ni12 O11 C10 161.5(6) . . . . ? O12S Ni12 O11 C10 -20.1(6) . . . . ? N104 Ni12 O11 C10 -108.7(6) . . . . ? O102 Ni12 O11 Ni11 -110.5(2) . . . . ? O103 Ni12 O11 Ni11 -18.08(18) . . . . ? O12S Ni12 O11 Ni11 160.3(2) . . . . ? N104 Ni12 O11 Ni11 71.7(2) . . . . ? Ni5 O12 C10 O10 65.8(9) . . . . ? Ni5 O12 C10 O11 -116.2(6) . . . . ? Ni12 O11 C10 O10 171.9(5) . . . . ? Ni11 O11 C10 O12 173.4(5) . . . . ? Ni11 O101 C100 C101 171.9(5) . . . . ? O101 C100 C101 C102 179.9(7) . . . . ? C103 C104 C105 C106 176.4(8) . . . . ? O101 C100 C105 C104 -177.7(7) . . . . ? C101 C100 C105 C106 -177.1(6) . . . . ? C107 N101 C106 C105 175.2(7) . . . . ? C104 C105 C106 N101 -174.2(8) . . . . ? C106 N101 C107 C108 152.4(7) . . . . ? Ni11 N101 C107 C108 -26.2(7) . . . . ? N101 C107 C108 N103 48.9(8) . . . . ? C109 N103 C108 C107 -164.6(6) . . . . ? C120 N103 C108 C107 79.4(8) . . . . ? Ni11 N103 C108 C107 -43.6(7) . . . . ? C120 N103 C109 C110 -28.4(7) . . . . ? C108 N103 C109 C110 -150.0(6) . . . . ? Ni11 N103 C109 C110 96.6(6) . . . . ? C111 N104 C110 C109 149.0(6) . . . . ? C120 N104 C110 C109 28.6(7) . . . . ? Ni12 N104 C110 C109 -94.3(6) . . . . ? N103 C109 C110 N104 -0.3(7) . . . . ? C110 N104 C111 C112 166.3(6) . . . . ? C120 N104 C111 C112 -79.1(7) . . . . ? Ni12 N104 C111 C112 42.8(7) . . . . ? C113 N102 C112 C111 -163.6(7) . . . . ? Ni12 N102 C112 C111 20.9(7) . . . . ? N104 C111 C112 N102 -43.9(8) . . . . ? C112 N102 C113 C114 -176.6(7) . . . . ? N102 C113 C114 C115 175.5(8) . . . . ? C113 C114 C115 C116 -177.9(8) . . . . ? Ni12 O102 C119 C118 -165.1(5) . . . . ? Ni12 O102 C119 C114 16.2(9) . . . . ? C117 C118 C119 O102 -177.8(7) . . . . ? C115 C114 C119 O102 176.8(7) . . . . ? C113 C114 C119 C118 177.7(7) . . . . ? C109 N103 C120 C121 170.9(6) . . . . ? C108 N103 C120 C121 -68.8(7) . . . . ? Ni11 N103 C120 C121 46.4(7) . . . . ? C109 N103 C120 N104 45.9(6) . . . . ? C108 N103 C120 N104 166.2(5) . . . . ? Ni11 N103 C120 N104 -78.6(5) . . . . ? C110 N104 C120 C121 -169.8(6) . . . . ? C111 N104 C120 C121 70.5(8) . . . . ? Ni12 N104 C120 C121 -45.8(7) . . . . ? C110 N104 C120 N103 -45.6(6) . . . . ? C111 N104 C120 N103 -165.3(5) . . . . ? Ni12 N104 C120 N103 78.4(5) . . . . ? N103 C120 C121 C122 120.3(7) . . . . ? N104 C120 C121 C122 -123.6(7) . . . . ? N103 C120 C121 C126 -57.0(8) . . . . ? N104 C120 C121 C126 59.0(9) . . . . ? C120 C121 C122 C123 -174.8(8) . . . . ? Ni12 O103 C126 C125 126.0(6) . . . . ? Ni11 O103 C126 C125 -119.3(6) . . . . ? Ni12 O103 C126 C121 -55.1(7) . . . . ? Ni11 O103 C126 C121 59.6(7) . . . . ? C124 C125 C126 O103 177.4(7) . . . . ? C122 C121 C126 O103 -179.6(6) . . . . ? C120 C121 C126 C125 176.7(6) . . . . ? N202 Ni21 O201 C200 31.2(5) . . . . ? O5 Ni21 O201 C200 -139.5(5) . . . . ? O21 Ni21 O201 C200 125.6(5) . . . . ? O203 Ni21 O201 C200 -59.4(5) . . . . ? Ni5 Ni21 O201 C200 -158.9(6) . . . . ? N202 Ni21 O201 Ni5 -170.0(2) . . . . ? O5 Ni21 O201 Ni5 19.38(19) . . . . ? O21 Ni21 O201 Ni5 -75.5(2) . . . . ? O203 Ni21 O201 Ni5 99.44(19) . . . . ? N201 Ni22 O202 C219 21.1(6) . . . . ? O5 Ni22 O202 C219 -155.1(6) . . . . ? O203 Ni22 O202 C219 123.6(6) . . . . ? O22S Ni22 O202 C219 -73.4(6) . . . . ? O202 Ni22 O203 C226 -122.8(5) . . . . ? N201 Ni22 O203 C226 -33.4(5) . . . . ? O5 Ni22 O203 C226 143.3(5) . . . . ? O22S Ni22 O203 C226 141.7(7) . . . . ? N203 Ni22 O203 C226 48.1(5) . . . . ? O202 Ni22 O203 Ni21 114.95(19) . . . . ? N201 Ni22 O203 Ni21 -155.6(2) . . . . ? O5 Ni22 O203 Ni21 21.10(19) . . . . ? O22S Ni22 O203 Ni21 19.5(8) . . . . ? N203 Ni22 O203 Ni21 -74.2(2) . . . . ? N202 Ni21 O203 C226 40.3(5) . . . . ? O201 Ni21 O203 C226 130.1(5) . . . . ? O5 Ni21 O203 C226 -146.0(5) . . . . ? N204 Ni21 O203 C226 -44.3(5) . . . . ? Ni5 Ni21 O203 C226 174.1(5) . . . . ? N202 Ni21 O203 Ni22 164.8(2) . . . . ? O201 Ni21 O203 Ni22 -105.4(2) . . . . ? O5 Ni21 O203 Ni22 -21.53(19) . . . . ? N204 Ni21 O203 Ni22 80.1(2) . . . . ? Ni5 Ni21 O203 Ni22 -61.43(16) . . . . ? O202 Ni22 N201 C213 -11.8(7) . . . . ? O203 Ni22 N201 C213 -106.1(7) . . . . ? O22S Ni22 N201 C213 75.3(7) . . . . ? N203 Ni22 N201 C213 167.2(7) . . . . ? O202 Ni22 N201 C212 174.8(6) . . . . ? O203 Ni22 N201 C212 80.4(6) . . . . ? O22S Ni22 N201 C212 -98.1(6) . . . . ? N203 Ni22 N201 C212 -6.2(6) . . . . ? O201 Ni21 N202 C206 -30.3(6) . . . . ? O21 Ni21 N202 C206 -120.0(6) . . . . ? O203 Ni21 N202 C206 63.7(6) . . . . ? N204 Ni21 N202 C206 152.8(6) . . . . ? Ni5 Ni21 N202 C206 -39.8(7) . . . . ? O201 Ni21 N202 C207 171.6(5) . . . . ? O21 Ni21 N202 C207 81.9(5) . . . . ? O203 Ni21 N202 C207 -94.5(5) . . . . ? N204 Ni21 N202 C207 -5.4(5) . . . . ? Ni5 Ni21 N202 C207 162.1(4) . . . . ? N201 Ni22 N203 C210 -140.1(5) . . . . ? O5 Ni22 N203 C210 36.2(5) . . . . ? O203 Ni22 N203 C210 117.0(5) . . . . ? O22S Ni22 N203 C210 -46.0(5) . . . . ? N201 Ni22 N203 C211 -19.3(5) . . . . ? O5 Ni22 N203 C211 157.0(5) . . . . ? O203 Ni22 N203 C211 -122.2(5) . . . . ? O22S Ni22 N203 C211 74.8(5) . . . . ? N201 Ni22 N203 C220 102.4(5) . . . . ? O5 Ni22 N203 C220 -81.4(5) . . . . ? O203 Ni22 N203 C220 -0.5(5) . . . . ? O22S Ni22 N203 C220 -163.5(5) . . . . ? N202 Ni21 N204 C209 145.6(5) . . . . ? O5 Ni21 N204 C209 -43.6(5) . . . . ? O21 Ni21 N204 C209 50.9(5) . . . . ? O203 Ni21 N204 C209 -123.7(5) . . . . ? Ni5 Ni21 N204 C209 -19.8(6) . . . . ? N202 Ni21 N204 C208 26.8(5) . . . . ? O5 Ni21 N204 C208 -162.4(4) . . . . ? O21 Ni21 N204 C208 -67.9(5) . . . . ? O203 Ni21 N204 C208 117.4(5) . . . . ? Ni5 Ni21 N204 C208 -138.7(4) . . . . ? N202 Ni21 N204 C220 -98.4(5) . . . . ? O5 Ni21 N204 C220 72.4(5) . . . . ? O21 Ni21 N204 C220 166.9(5) . . . . ? O203 Ni21 N204 C220 -7.7(5) . . . . ? Ni5 Ni21 N204 C220 96.2(5) . . . . ? N202 Ni21 O21 C20 135.1(6) . . . . ? O201 Ni21 O21 C20 45.4(6) . . . . ? O5 Ni21 O21 C20 -39.2(6) . . . . ? N204 Ni21 O21 C20 -140.4(6) . . . . ? Ni5 Ni21 O21 C20 2.3(6) . . . . ? Ni21 O21 C20 C21 179.9(6) . . . . ? Ni5 O22 C20 C21 174.7(6) . . . . ? O202 Ni22 O22S C22S 74.0(6) . . . . ? N201 Ni22 O22S C22S -14.3(6) . . . . ? O5 Ni22 O22S C22S 168.9(6) . . . . ? O203 Ni22 O22S C22S 170.6(7) . . . . ? N203 Ni22 O22S C22S -96.4(6) . . . . ? Ni21 O201 C200 C201 160.8(5) . . . . ? Ni21 O201 C200 C205 -21.2(8) . . . . ? Ni5 O201 C200 C205 -169.9(5) . . . . ? O201 C200 C201 C202 178.1(6) . . . . ? C203 C204 C205 C206 -177.6(7) . . . . ? O201 C200 C205 C204 -179.0(6) . . . . ? C201 C200 C205 C206 177.5(6) . . . . ? C207 N202 C206 C205 178.0(7) . . . . ? C204 C205 C206 N202 178.8(7) . . . . ? C206 N202 C207 C208 -176.5(6) . . . . ? Ni21 N202 C207 C208 -17.5(7) . . . . ? C209 N204 C208 C207 -164.7(6) . . . . ? C220 N204 C208 C207 80.1(8) . . . . ? Ni21 N204 C208 C207 -44.6(7) . . . . ? N202 C207 C208 N204 43.3(8) . . . . ? C208 N204 C209 C210 -155.8(6) . . . . ? C220 N204 C209 C210 -32.6(7) . . . . ? Ni21 N204 C209 C210 90.7(6) . . . . ? C211 N203 C210 C209 146.2(7) . . . . ? C220 N203 C210 C209 26.1(7) . . . . ? Ni22 N203 C210 C209 -97.2(6) . . . . ? N204 C209 C210 N203 4.2(8) . . . . ? C210 N203 C211 C212 166.0(7) . . . . ? C220 N203 C211 C212 -79.8(8) . . . . ? Ni22 N203 C211 C212 42.4(7) . . . . ? C213 N201 C212 C211 -143.0(7) . . . . ? Ni22 N201 C212 C211 30.9(8) . . . . ? N203 C211 C212 N201 -50.6(9) . . . . ? C212 N201 C213 C214 176.2(7) . . . . ? N201 C213 C214 C215 -171.9(7) . . . . ? C213 C214 C215 C216 173.3(6) . . . . ? Ni22 O202 C219 C218 158.1(5) . . . . ? Ni22 O202 C219 C214 -21.6(9) . . . . ? C217 C218 C219 O202 179.5(6) . . . . ? C215 C214 C219 O202 -178.6(6) . . . . ? C213 C214 C219 C218 -173.4(7) . . . . ? C210 N203 C220 C221 -169.6(6) . . . . ? C211 N203 C220 C221 71.4(9) . . . . ? Ni22 N203 C220 C221 -45.0(8) . . . . ? C210 N203 C220 N204 -46.2(7) . . . . ? C211 N203 C220 N204 -165.2(6) . . . . ? Ni22 N203 C220 N204 78.4(6) . . . . ? C209 N204 C220 C221 175.3(6) . . . . ? C208 N204 C220 C221 -64.5(9) . . . . ? Ni21 N204 C220 C221 53.4(7) . . . . ? C209 N204 C220 N203 49.2(7) . . . . ? C208 N204 C220 N203 169.4(6) . . . . ? Ni21 N204 C220 N203 -72.7(6) . . . . ? N203 C220 C221 C222 -124.2(8) . . . . ? N204 C220 C221 C222 119.4(7) . . . . ? N203 C220 C221 C226 58.0(9) . . . . ? N204 C220 C221 C226 -58.3(9) . . . . ? C220 C221 C222 C223 -175.1(7) . . . . ? Ni22 O203 C226 C225 129.6(6) . . . . ? Ni21 O203 C226 C225 -120.2(6) . . . . ? Ni22 O203 C226 C221 -53.7(7) . . . . ? Ni21 O203 C226 C221 56.6(7) . . . . ? C224 C225 C226 O203 -179.9(7) . . . . ? C222 C221 C226 O203 179.2(6) . . . . ? C220 C221 C226 C225 173.8(7) . . . . ? C20 O22 Ni5 O5 47.2(6) . . . . ? C20 O22 Ni5 O201 -34.9(6) . . . . ? C20 O22 Ni5 O5S -131.3(6) . . . . ? C20 O22 Ni5 O12 139.3(6) . . . . ? C20 O22 Ni5 Ni21 6.2(6) . . . . ? C200 O201 Ni5 O22 -131.9(6) . . . . ? Ni21 O201 Ni5 O22 73.2(2) . . . . ? C200 O201 Ni5 O5W 41.3(6) . . . . ? Ni21 O201 Ni5 O5W -113.6(2) . . . . ? C200 O201 Ni5 O5 135.9(6) . . . . ? Ni21 O201 Ni5 O5 -19.02(19) . . . . ? C200 O201 Ni5 O5S -45.0(6) . . . . ? Ni21 O201 Ni5 O5S 160.1(2) . . . . ? C200 O201 Ni5 Ni21 154.9(7) . . . . ? C10 O12 Ni5 O22 -173.6(6) . . . . ? C10 O12 Ni5 O5W 13.5(6) . . . . ? C10 O12 Ni5 O5 -81.4(6) . . . . ? C10 O12 Ni5 O5S 99.6(6) . . . . ? C10 O12 Ni5 Ni21 -103.1(6) . . . . ? N202 Ni21 Ni5 O22 -89.9(3) . . . . ? O201 Ni21 Ni5 O22 -103.6(2) . . . . ? O5 Ni21 Ni5 O22 104.8(3) . . . . ? O21 Ni21 Ni5 O22 -3.3(2) . . . . ? O203 Ni21 Ni5 O22 170.5(2) . . . . ? N204 Ni21 Ni5 O22 70.1(3) . . . . ? N202 Ni21 Ni5 O5W 86.4(3) . . . . ? O201 Ni21 Ni5 O5W 72.6(2) . . . . ? O5 Ni21 Ni5 O5W -79.0(3) . . . . ? O21 Ni21 Ni5 O5W 172.9(2) . . . . ? O203 Ni21 Ni5 O5W -13.3(2) . . . . ? N204 Ni21 Ni5 O5W -113.6(3) . . . . ? N202 Ni21 Ni5 O5 165.3(3) . . . . ? O201 Ni21 Ni5 O5 151.6(3) . . . . ? O21 Ni21 Ni5 O5 -108.1(3) . . . . ? O203 Ni21 Ni5 O5 65.7(2) . . . . ? N204 Ni21 Ni5 O5 -34.7(3) . . . . ? N202 Ni21 Ni5 O201 13.7(3) . . . . ? O5 Ni21 Ni5 O201 -151.6(3) . . . . ? O21 Ni21 Ni5 O201 100.3(2) . . . . ? O203 Ni21 Ni5 O201 -85.9(2) . . . . ? N204 Ni21 Ni5 O201 173.7(3) . . . . ? N202 Ni21 Ni5 O5S -15.2(3) . . . . ? O201 Ni21 Ni5 O5S -28.9(3) . . . . ? O5 Ni21 Ni5 O5S 179.5(3) . . . . ? O21 Ni21 Ni5 O5S 71.4(3) . . . . ? O203 Ni21 Ni5 O5S -114.8(3) . . . . ? N204 Ni21 Ni5 O5S 144.8(3) . . . . ? N202 Ni21 Ni5 O12 -161.6(3) . . . . ? O201 Ni21 Ni5 O12 -175.4(3) . . . . ? O5 Ni21 Ni5 O12 33.1(3) . . . . ? O21 Ni21 Ni5 O12 -75.0(2) . . . . ? O203 Ni21 Ni5 O12 98.7(2) . . . . ? N204 Ni21 Ni5 O12 -1.6(3) . . . . ? O201 Ni21 O5 Ni22 116.6(2) . . . . ? O21 Ni21 O5 Ni22 -154.2(2) . . . . ? O203 Ni21 O5 Ni22 21.66(19) . . . . ? N204 Ni21 O5 Ni22 -65.6(2) . . . . ? Ni5 Ni21 O5 Ni22 135.9(3) . . . . ? O201 Ni21 O5 Ni5 -19.39(19) . . . . ? O21 Ni21 O5 Ni5 69.9(2) . . . . ? O203 Ni21 O5 Ni5 -114.3(2) . . . . ? N204 Ni21 O5 Ni5 158.5(2) . . . . ? O202 Ni22 O5 Ni21 -116.2(2) . . . . ? O203 Ni22 O5 Ni21 -22.2(2) . . . . ? O22S Ni22 O5 Ni21 157.3(2) . . . . ? N203 Ni22 O5 Ni21 65.5(2) . . . . ? O202 Ni22 O5 Ni5 -14.8(4) . . . . ? O203 Ni22 O5 Ni5 79.1(4) . . . . ? O22S Ni22 O5 Ni5 -101.4(4) . . . . ? N203 Ni22 O5 Ni5 166.8(4) . . . . ? O22 Ni5 O5 Ni21 -72.4(2) . . . . ? O5W Ni5 O5 Ni21 109.0(2) . . . . ? O201 Ni5 O5 Ni21 18.93(19) . . . . ? O12 Ni5 O5 Ni21 -155.4(2) . . . . ? O22 Ni5 O5 Ni22 -175.1(4) . . . . ? O5W Ni5 O5 Ni22 6.3(4) . . . . ? O201 Ni5 O5 Ni22 -83.8(4) . . . . ? O12 Ni5 O5 Ni22 101.9(4) . . . . ? Ni21 Ni5 O5 Ni22 -102.7(4) . . . . ? O22 Ni5 O5S C5S 41.7(5) . . . . ? O5W Ni5 O5S C5S -139.8(6) . . . . ? O201 Ni5 O5S C5S -49.5(6) . . . . ? O12 Ni5 O5S C5S 124.7(5) . . . . ? Ni21 Ni5 O5S C5S -30.4(6) . . . . ? 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 O11S H11S O10 0.82(11) 1.79(11) 2.552(7) 154(11) . O12S H12S O12 0.91(11) 1.69(11) 2.574(7) 163(10) . O22S H22S O10 0.75(11) 1.96(11) 2.676(7) 158(12) . O5W H5W1 O202 0.97 1.63 2.586(6) 167.5 . O5W H5W2 O1W 0.94 1.82 2.751(7) 170.2 . O5 H5 O1S 0.78 2.18 2.963(8) 178.5 . O5S H5S O102 0.95 1.75 2.678(7) 165.3 . O1W H1W2 O101 0.90 1.69 2.586(7) 168.8 . O1W H1W1 O102 0.96 1.80 2.719(7) 160.1 . O2W H2W2 O5W 0.84 2.53 3.221(12) 140.1 . O1S H1S O12 0.82 2.10 2.876(9) 158.4 . O2S H2S O3W 0.82 1.92 2.70(3) 158.4 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.127 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.157 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_be66no1n _database_code_depnum_ccdc_archive 'CCDC 616419' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H44 N4 Ni3 O11, 0.5(C H4 O), 3(H2 O)' _chemical_formula_sum 'C33.50 H50 N4 Ni3 O14.50' _chemical_formula_weight 916.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9790(14) _cell_length_b 21.449(3) _cell_length_c 19.317(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.998(2) _cell_angle_gamma 90.00 _cell_volume 4071.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1899 _cell_measurement_theta_min 2.3425 _cell_measurement_theta_max 27.7345 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1916 _exptl_absorpt_coefficient_mu 1.442 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.57642 _exptl_absorpt_correction_T_max 0.8021 _exptl_absorpt_process_details SADABS-2004/1 _exptl_special_details ; Additional spherical absorption correction applied with mu*r = 0.2124 ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38231 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7579 _reflns_number_gt 6059 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'SIR-92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0540P)^2^+4.9002P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7579 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.012 _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 Ni11 Ni 0.03914(4) 0.010486(18) 0.733878(19) 0.01827(11) Uani 1 1 d . . . Ni12 Ni 0.08506(4) 0.140301(18) 0.799505(19) 0.01838(11) Uani 1 1 d . . . Ni3 Ni 0.22815(4) -0.018031(18) 0.867747(19) 0.01937(11) Uani 1 1 d . . . O101 O 0.2171(2) -0.03382(10) 0.76223(10) 0.0222(5) Uani 1 1 d . . . O102 O 0.2801(2) 0.15029(10) 0.84638(11) 0.0228(5) Uani 1 1 d . . . O103 O 0.1271(2) 0.09581(10) 0.70923(10) 0.0198(4) Uani 1 1 d . . . N101 N 0.0239(3) -0.02425(12) 0.63680(13) 0.0216(6) Uani 1 1 d . . . N102 N 0.0857(3) 0.22820(12) 0.76411(13) 0.0220(6) Uani 1 1 d . . . N103 N -0.1575(2) 0.04730(12) 0.69675(13) 0.0215(6) Uani 1 1 d . . . N104 N -0.1297(3) 0.14314(12) 0.74903(13) 0.0217(6) Uani 1 1 d . . . O1H O 0.0829(2) 0.04950(10) 0.83156(11) 0.0186(5) Uani 1 1 d . . . O11 O -0.0567(2) -0.06771(10) 0.76951(11) 0.0252(5) Uani 1 1 d . . . O13 O 0.0721(2) -0.07831(10) 0.87583(11) 0.0267(5) Uani 1 1 d . . . O12S O 0.0190(3) 0.17379(12) 0.89332(13) 0.0283(5) Uani 1 1 d . . . O30 O 0.2207(2) 0.00880(11) 0.96992(11) 0.0258(5) Uani 1 1 d . . . O31 O 0.3968(2) -0.04336(12) 1.02934(12) 0.0359(6) Uani 1 1 d . . . O3W O 0.3877(2) 0.04126(11) 0.86495(11) 0.0230(5) Uani 1 1 d . . . O3S O 0.3700(2) -0.08794(11) 0.90400(12) 0.0286(5) Uani 1 1 d . . . C10 C -0.0226(3) -0.09472(15) 0.82713(17) 0.0250(7) Uani 1 1 d . . . C11 C -0.1004(4) -0.15285(18) 0.8400(2) 0.0410(9) Uani 1 1 d . . . H11A H -0.0642 -0.1694 0.8868 0.062 Uiso 0.52(4) 1 calc PR . . H11B H -0.0904 -0.1842 0.8043 0.062 Uiso 0.52(4) 1 calc PR . . H11C H -0.1969 -0.1426 0.8372 0.062 Uiso 0.52(4) 1 calc PR . . H11D H -0.1701 -0.1614 0.7987 0.062 Uiso 0.48(4) 1 calc PR . . H11E H -0.1439 -0.1466 0.8812 0.062 Uiso 0.48(4) 1 calc PR . . H11F H -0.0375 -0.1882 0.8483 0.062 Uiso 0.48(4) 1 calc PR . . C12S C 0.0980(6) 0.2213(2) 0.9378(2) 0.0582(13) Uani 1 1 d . . . H12A H 0.0532 0.2307 0.9779 0.087 Uiso 1 1 calc R . . H12B H 0.1035 0.2593 0.9103 0.087 Uiso 1 1 calc R . . H12C H 0.1900 0.2055 0.9549 0.087 Uiso 1 1 calc R . . C3S C 0.3364(5) -0.15233(18) 0.9039(2) 0.0455(10) Uani 1 1 d . . . H3S1 H 0.4178 -0.1765 0.9231 0.068 Uiso 1 1 calc R . . H3S2 H 0.3020 -0.1659 0.8556 0.068 Uiso 1 1 calc R . . H3S3 H 0.2663 -0.1590 0.9329 0.068 Uiso 1 1 calc R . . C30 C 0.3044(3) -0.00302(16) 1.02525(16) 0.0262(7) Uani 1 1 d . . . C31 C 0.2917(4) 0.0341(2) 1.08927(18) 0.0425(10) Uani 1 1 d . . . H31A H 0.1973 0.0327 1.0971 0.064 Uiso 1 1 calc R . . H31B H 0.3177 0.0775 1.0825 0.064 Uiso 1 1 calc R . . H31C H 0.3517 0.0165 1.1301 0.064 Uiso 1 1 calc R . . C100 C 0.2984(3) -0.05530(14) 0.72121(16) 0.0196(6) Uani 1 1 d . . . C101 C 0.4351(3) -0.06925(14) 0.74841(17) 0.0238(7) Uani 1 1 d . . . H101 H 0.4679 -0.0626 0.7970 0.029 Uiso 1 1 calc R . . C102 C 0.5230(3) -0.09228(15) 0.70694(18) 0.0282(7) Uani 1 1 d . . . H102 H 0.6156 -0.0996 0.7268 0.034 Uiso 1 1 calc R . . C103 C 0.4769(4) -0.10497(18) 0.63585(19) 0.0351(8) Uani 1 1 d . . . H103 H 0.5362 -0.1223 0.6074 0.042 Uiso 1 1 calc R . . C104 C 0.3439(4) -0.09179(17) 0.60816(18) 0.0340(8) Uani 1 1 d . . . H104 H 0.3122 -0.1003 0.5598 0.041 Uiso 1 1 calc R . . C105 C 0.2527(3) -0.06634(15) 0.64795(16) 0.0232(7) Uani 1 1 d . . . C106 C 0.1169(3) -0.05250(15) 0.61168(16) 0.0242(7) Uani 1 1 d . . . H106 H 0.0947 -0.0659 0.5642 0.029 Uiso 1 1 calc R . . C107 C -0.1061(3) -0.00985(16) 0.59126(17) 0.0277(7) Uani 1 1 d . . . H10A H -0.1365 -0.0460 0.5606 0.033 Uiso 1 1 calc R . . H10B H -0.0950 0.0264 0.5610 0.033 Uiso 1 1 calc R . . C108 C -0.2118(3) 0.00496(16) 0.63737(17) 0.0271(7) Uani 1 1 d . . . H10C H -0.2919 0.0247 0.6082 0.032 Uiso 1 1 calc R . . H10D H -0.2424 -0.0344 0.6564 0.032 Uiso 1 1 calc R . . C109 C -0.2481(3) 0.04581(15) 0.75025(17) 0.0257(7) Uani 1 1 d . . . H10E H -0.2233 0.0110 0.7836 0.031 Uiso 1 1 calc R . . H10F H -0.3444 0.0411 0.7276 0.031 Uiso 1 1 calc R . . C110 C -0.2245(3) 0.10871(16) 0.78780(17) 0.0262(7) Uani 1 1 d . . . H11G H -0.3113 0.1316 0.7854 0.031 Uiso 1 1 calc R . . H11H H -0.1830 0.1029 0.8378 0.031 Uiso 1 1 calc R . . C111 C -0.1593(3) 0.21125(15) 0.74814(18) 0.0273(7) Uani 1 1 d . . . H11I H -0.1708 0.2247 0.7958 0.033 Uiso 1 1 calc R . . H11J H -0.2458 0.2194 0.7157 0.033 Uiso 1 1 calc R . . C112 C -0.0463(3) 0.24934(15) 0.72491(18) 0.0268(7) Uani 1 1 d . . . H11K H -0.0486 0.2439 0.6738 0.032 Uiso 1 1 calc R . . H11L H -0.0593 0.2941 0.7342 0.032 Uiso 1 1 calc R . . C113 C 0.1849(3) 0.26666(15) 0.77295(16) 0.0240(7) Uani 1 1 d . . . H113 H 0.1667 0.3074 0.7545 0.029 Uiso 1 1 calc R . . C114 C 0.3221(3) 0.25417(14) 0.80832(16) 0.0226(7) Uani 1 1 d . . . C115 C 0.4191(3) 0.30204(15) 0.80742(17) 0.0271(7) Uani 1 1 d . . . H115 H 0.3912 0.3400 0.7840 0.033 Uiso 1 1 calc R . . C116 C 0.5528(3) 0.29534(16) 0.83940(17) 0.0292(8) Uani 1 1 d . . . H116 H 0.6167 0.3279 0.8376 0.035 Uiso 1 1 calc R . . C117 C 0.5924(3) 0.23985(16) 0.87452(17) 0.0271(7) Uani 1 1 d . . . H117 H 0.6841 0.2349 0.8974 0.033 Uiso 1 1 calc R . . C118 C 0.5009(3) 0.19184(16) 0.87679(16) 0.0251(7) Uani 1 1 d . . . H118 H 0.5309 0.1546 0.9013 0.030 Uiso 1 1 calc R . . C119 C 0.3629(3) 0.19712(15) 0.84316(15) 0.0211(6) Uani 1 1 d . . . C120 C -0.1607(3) 0.11427(15) 0.67794(16) 0.0225(7) Uani 1 1 d . . . H120 H -0.2558 0.1257 0.6560 0.027 Uiso 1 1 calc R . . C121 C -0.0668(3) 0.13277(15) 0.62905(16) 0.0225(7) Uani 1 1 d . . . C122 C -0.1207(3) 0.16118(16) 0.56497(17) 0.0276(7) Uani 1 1 d . . . H122 H -0.2162 0.1674 0.5530 0.033 Uiso 1 1 calc R . . C123 C -0.0374(4) 0.18029(18) 0.51890(18) 0.0352(8) Uani 1 1 d . . . H123 H -0.0746 0.1993 0.4754 0.042 Uiso 1 1 calc R . . C124 C 0.1015(4) 0.1712(2) 0.53745(19) 0.0441(10) Uani 1 1 d . . . H124 H 0.1600 0.1843 0.5063 0.053 Uiso 1 1 calc R . . C125 C 0.1570(4) 0.1430(2) 0.60093(19) 0.0391(9) Uani 1 1 d . . . H125 H 0.2527 0.1374 0.6126 0.047 Uiso 1 1 calc R . . C126 C 0.0738(3) 0.12300(15) 0.64774(16) 0.0226(7) Uani 1 1 d . . . H3W1 H 0.463(5) 0.042(2) 0.899(2) 0.058(14) Uiso 1 1 d . . . H3W2 H 0.345(5) 0.075(2) 0.864(2) 0.067(16) Uiso 1 1 d . . . H12S H 0.016(4) 0.1464(18) 0.916(2) 0.047(11) Uiso 1 1 d . . . H3S H 0.409(4) -0.081(2) 0.955(2) 0.055(13) Uiso 1 1 d . . . H1H H 0.036(4) 0.0420(16) 0.8540(18) 0.047(10) Uiso 1 1 d . . . O1W O 0.4053(2) 0.08553(11) 0.72300(11) 0.0285(5) Uani 1 1 d . . . H1W1 H 0.4238 0.0686 0.7749 0.050(14) Uiso 1 1 d . . . H1W2 H 0.3047 0.0837 0.7192 0.051(15) Uiso 1 1 d . . . O2W O -0.0108(3) 0.07599(12) 0.97446(13) 0.0325(6) Uani 1 1 d . . . H2W1 H 0.071(5) 0.052(2) 0.982(2) 0.060(14) Uiso 1 1 d . . . H2W2 H -0.036(5) 0.075(2) 1.015(3) 0.066(15) Uiso 1 1 d . . . O4W O 0.5000(8) 0.1896(4) 0.6827(5) 0.0186(19) Uiso 0.25 1 d P A 1 O4W' O 0.4971(16) 0.1791(8) 0.6530(9) 0.027(4) Uiso 0.15 1 d P B 2 O5W O 0.5146(13) 0.1484(7) 0.5453(7) 0.013(3) Uiso 0.15 1 d P C 3 O6W O 0.4330(12) 0.0595(7) 0.5473(6) 0.022(3) Uiso 0.20 1 d P D 4 O7W O 0.540(3) 0.1998(13) 0.5571(14) 0.032(7) Uiso 0.15 1 d P E 5 O8W O 0.417(4) 0.240(2) 0.534(2) 0.033(12) Uiso 0.10 1 d P F 6 O1S O 0.5032(9) 0.0992(5) 0.5986(5) 0.032(2) Uiso 0.30 1 d P G 7 H1S H 0.4512 0.0913 0.6274 0.048 Uiso 0.30 1 calc PR G 7 C1S C 0.4504(13) 0.0850(7) 0.5425(6) 0.028(3) Uiso 0.30 1 d P G 7 H1S1 H 0.4769 0.1142 0.5082 0.042 Uiso 0.30 1 calc PR G 7 H1S2 H 0.3514 0.0863 0.5398 0.042 Uiso 0.30 1 calc PR G 7 H1S3 H 0.4782 0.0427 0.5322 0.042 Uiso 0.30 1 calc PR G 7 O2S O 0.5103(15) 0.1261(8) 0.6052(8) 0.043(4) Uiso 0.20 1 d P H 8 H2S H 0.4542 0.1019 0.6190 0.064 Uiso 0.20 1 calc PR H 8 C2S C 0.5144(17) 0.1151(10) 0.5410(8) 0.024(3) Uiso 0.20 1 d P H 8 H2S1 H 0.4773 0.1509 0.5124 0.036 Uiso 0.20 1 calc PR H 8 H2S2 H 0.4602 0.0779 0.5258 0.036 Uiso 0.20 1 calc PR H 8 H2S3 H 0.6089 0.1081 0.5353 0.036 Uiso 0.20 1 calc PR H 8 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 Ni11 0.0189(2) 0.0198(2) 0.01596(19) 0.00051(15) 0.00276(15) 0.00150(15) Ni12 0.0196(2) 0.0172(2) 0.0184(2) 0.00257(15) 0.00376(15) 0.00187(15) Ni3 0.0208(2) 0.0204(2) 0.0167(2) 0.00256(15) 0.00264(15) 0.00242(16) O101 0.0228(11) 0.0267(12) 0.0170(10) -0.0018(9) 0.0035(9) 0.0057(9) O102 0.0221(11) 0.0202(11) 0.0248(11) 0.0019(9) 0.0007(9) -0.0022(9) O103 0.0185(11) 0.0244(12) 0.0164(10) 0.0041(8) 0.0031(8) 0.0022(9) N101 0.0222(14) 0.0225(14) 0.0195(13) -0.0007(10) 0.0022(11) -0.0006(11) N102 0.0239(14) 0.0193(14) 0.0228(13) 0.0016(11) 0.0037(11) 0.0019(11) N103 0.0186(13) 0.0228(14) 0.0235(13) 0.0026(11) 0.0049(10) -0.0005(11) N104 0.0181(13) 0.0229(14) 0.0249(14) 0.0019(11) 0.0061(11) 0.0027(11) O1H 0.0198(11) 0.0199(12) 0.0174(11) 0.0044(9) 0.0066(9) 0.0011(9) O11 0.0279(12) 0.0237(12) 0.0244(11) -0.0003(9) 0.0058(9) -0.0019(9) O13 0.0276(12) 0.0266(12) 0.0255(12) 0.0051(10) 0.0035(10) -0.0013(10) O12S 0.0399(14) 0.0207(13) 0.0266(13) 0.0019(11) 0.0118(11) 0.0012(11) O30 0.0259(12) 0.0344(13) 0.0167(11) 0.0028(9) 0.0027(9) 0.0051(10) O31 0.0334(14) 0.0400(15) 0.0298(13) 0.0037(11) -0.0071(11) 0.0053(12) O3W 0.0228(12) 0.0238(13) 0.0211(11) 0.0022(9) 0.0004(10) 0.0036(10) O3S 0.0325(13) 0.0255(13) 0.0274(12) 0.0060(10) 0.0038(10) 0.0082(10) C10 0.0285(17) 0.0210(17) 0.0267(17) -0.0025(13) 0.0081(14) -0.0020(13) C11 0.053(2) 0.032(2) 0.039(2) -0.0007(16) 0.0121(18) -0.0161(18) C12S 0.096(4) 0.041(3) 0.044(2) -0.009(2) 0.030(3) -0.012(2) C3S 0.061(3) 0.028(2) 0.046(2) -0.0022(17) 0.004(2) 0.0116(19) C30 0.0237(17) 0.0341(19) 0.0212(16) 0.0058(14) 0.0053(13) -0.0057(14) C31 0.032(2) 0.068(3) 0.0263(18) -0.0077(18) 0.0030(16) 0.0029(19) C100 0.0224(15) 0.0152(15) 0.0224(15) 0.0015(12) 0.0072(12) -0.0006(12) C101 0.0258(17) 0.0186(16) 0.0272(16) 0.0012(13) 0.0055(13) -0.0001(13) C102 0.0227(17) 0.0251(18) 0.0381(19) 0.0058(14) 0.0090(14) 0.0005(14) C103 0.0299(19) 0.043(2) 0.036(2) -0.0042(16) 0.0162(16) 0.0038(16) C104 0.036(2) 0.041(2) 0.0260(17) -0.0053(15) 0.0104(15) 0.0001(16) C105 0.0249(17) 0.0226(17) 0.0231(16) 0.0006(13) 0.0070(13) -0.0019(13) C106 0.0290(17) 0.0245(17) 0.0190(15) -0.0025(13) 0.0038(13) -0.0032(14) C107 0.0257(17) 0.0321(19) 0.0226(16) -0.0024(14) -0.0035(13) 0.0012(14) C108 0.0206(16) 0.0293(18) 0.0287(17) -0.0022(14) -0.0027(13) -0.0024(13) C109 0.0204(16) 0.0272(18) 0.0309(17) 0.0033(14) 0.0089(13) 0.0020(13) C110 0.0201(16) 0.0292(18) 0.0313(17) 0.0025(14) 0.0106(14) 0.0011(14) C111 0.0251(17) 0.0229(17) 0.0333(18) 0.0031(14) 0.0038(14) 0.0065(13) C112 0.0271(17) 0.0194(16) 0.0319(18) 0.0040(13) -0.0005(14) 0.0035(13) C113 0.0297(17) 0.0194(16) 0.0240(16) 0.0019(13) 0.0077(13) 0.0023(14) C114 0.0268(17) 0.0202(16) 0.0224(15) -0.0018(12) 0.0091(13) 0.0001(13) C115 0.0367(19) 0.0205(17) 0.0266(17) -0.0014(13) 0.0123(15) 0.0002(14) C116 0.0292(18) 0.0282(18) 0.0330(18) -0.0066(15) 0.0128(15) -0.0066(14) C117 0.0247(17) 0.0334(19) 0.0237(16) -0.0087(14) 0.0052(13) -0.0015(14) C118 0.0252(17) 0.0258(17) 0.0241(16) -0.0031(13) 0.0038(13) 0.0015(13) C119 0.0244(16) 0.0223(16) 0.0179(15) -0.0029(12) 0.0073(12) 0.0001(13) C120 0.0172(15) 0.0257(17) 0.0240(16) 0.0040(13) 0.0017(12) 0.0025(13) C121 0.0227(16) 0.0240(17) 0.0208(15) 0.0008(13) 0.0034(12) -0.0004(13) C122 0.0273(17) 0.0282(18) 0.0246(17) 0.0034(14) -0.0027(14) 0.0014(14) C123 0.035(2) 0.046(2) 0.0224(17) 0.0107(16) 0.0002(15) 0.0016(17) C124 0.037(2) 0.069(3) 0.0291(19) 0.0214(19) 0.0129(16) 0.000(2) C125 0.0242(18) 0.063(3) 0.0316(19) 0.0193(18) 0.0081(15) 0.0054(17) C126 0.0223(16) 0.0256(17) 0.0195(15) 0.0038(13) 0.0025(13) 0.0004(13) O1W 0.0225(12) 0.0380(14) 0.0262(12) 0.0025(10) 0.0071(9) 0.0023(10) O2W 0.0330(14) 0.0359(15) 0.0305(14) 0.0090(11) 0.0107(11) 0.0052(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni11 N101 1.999(3) . ? Ni11 O101 2.005(2) . ? Ni11 O1H 2.041(2) . ? Ni11 O11 2.105(2) . ? Ni11 O103 2.119(2) . ? Ni11 N103 2.121(3) . ? Ni11 Ni3 2.9875(6) . ? Ni12 N102 2.006(3) . ? Ni12 O102 2.011(2) . ? Ni12 O1H 2.045(2) . ? Ni12 O103 2.093(2) . ? Ni12 O12S 2.156(2) . ? Ni12 N104 2.196(3) . ? Ni3 O3W 2.046(2) . ? Ni3 O101 2.050(2) . ? Ni3 O13 2.051(2) . ? Ni3 O30 2.070(2) . ? Ni3 O1H 2.082(2) . ? Ni3 O3S 2.097(2) . ? O101 C100 1.312(4) . ? O102 C119 1.309(4) . ? O103 C126 1.347(4) . ? N101 C106 1.273(4) . ? N101 C107 1.468(4) . ? N102 C113 1.277(4) . ? N102 C112 1.472(4) . ? N103 C120 1.481(4) . ? N103 C109 1.486(4) . ? N103 C108 1.489(4) . ? N104 C120 1.489(4) . ? N104 C111 1.490(4) . ? N104 C110 1.499(4) . ? O1H H1H 0.71(4) . ? O11 C10 1.249(4) . ? O13 C10 1.262(4) . ? O12S C12S 1.471(5) . ? O12S H12S 0.73(4) . ? O30 C30 1.262(4) . ? O31 C30 1.257(4) . ? O3W H3W1 0.90(5) . ? O3W H3W2 0.85(5) . ? O3S C3S 1.421(5) . ? O3S H3S 1.00(4) . ? C10 C11 1.512(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 H11D 0.9800 . ? C11 H11E 0.9800 . ? C11 H11F 0.9800 . ? C12S H12A 0.9800 . ? C12S H12B 0.9800 . ? C12S H12C 0.9800 . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? C30 C31 1.495(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C100 C101 1.406(4) . ? C100 C105 1.429(4) . ? C101 C102 1.378(4) . ? C101 H101 0.9500 . ? C102 C103 1.397(5) . ? C102 H102 0.9500 . ? C103 C104 1.372(5) . ? C103 H103 0.9500 . ? C104 C105 1.400(5) . ? C104 H104 0.9500 . ? C105 C106 1.444(4) . ? C106 H106 0.9500 . ? C107 C108 1.528(5) . ? C107 H10A 0.9900 . ? C107 H10B 0.9900 . ? C108 H10C 0.9900 . ? C108 H10D 0.9900 . ? C109 C110 1.530(5) . ? C109 H10E 0.9900 . ? C109 H10F 0.9900 . ? C110 H11G 0.9900 . ? C110 H11H 0.9900 . ? C111 C112 1.522(5) . ? C111 H11I 0.9900 . ? C111 H11J 0.9900 . ? C112 H11K 0.9900 . ? C112 H11L 0.9900 . ? C113 C114 1.446(4) . ? C113 H113 0.9500 . ? C114 C115 1.413(5) . ? C114 C119 1.422(4) . ? C115 C116 1.377(5) . ? C115 H115 0.9500 . ? C116 C117 1.393(5) . ? C116 H116 0.9500 . ? C117 C118 1.382(5) . ? C117 H117 0.9500 . ? C118 C119 1.421(4) . ? C118 H118 0.9500 . ? C120 C121 1.494(4) . ? C120 H120 1.0000 . ? C121 C122 1.401(4) . ? C121 C126 1.403(4) . ? C122 C123 1.382(5) . ? C122 H122 0.9500 . ? C123 C124 1.383(5) . ? C123 H123 0.9500 . ? C124 C125 1.392(5) . ? C124 H124 0.9500 . ? C125 C126 1.397(5) . ? C125 H125 0.9500 . ? O1W H1W1 1.0520 . ? O1W H1W2 0.9943 . ? O2W H2W1 0.96(5) . ? O2W H2W2 0.86(5) . ? O1S C1S 1.160(14) . ? O1S H1S 0.8400 . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? O2S C2S 1.27(2) . ? O2S H2S 0.8400 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? 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 N101 Ni11 O101 89.95(9) . . ? N101 Ni11 O1H 171.63(10) . . ? O101 Ni11 O1H 84.51(8) . . ? N101 Ni11 O11 92.57(10) . . ? O101 Ni11 O11 87.93(9) . . ? O1H Ni11 O11 93.50(9) . . ? N101 Ni11 O103 94.48(9) . . ? O101 Ni11 O103 95.10(8) . . ? O1H Ni11 O103 79.81(8) . . ? O11 Ni11 O103 172.32(8) . . ? N101 Ni11 N103 84.63(10) . . ? O101 Ni11 N103 172.92(10) . . ? O1H Ni11 N103 101.36(9) . . ? O11 Ni11 N103 87.77(9) . . ? O103 Ni11 N103 89.87(9) . . ? N101 Ni11 Ni3 132.03(8) . . ? O101 Ni11 Ni3 43.13(6) . . ? O1H Ni11 Ni3 44.11(6) . . ? O11 Ni11 Ni3 78.94(6) . . ? O103 Ni11 Ni3 98.47(5) . . ? N103 Ni11 Ni3 140.97(7) . . ? N102 Ni12 O102 89.62(10) . . ? N102 Ni12 O1H 177.74(10) . . ? O102 Ni12 O1H 91.45(9) . . ? N102 Ni12 O103 97.57(9) . . ? O102 Ni12 O103 96.05(8) . . ? O1H Ni12 O103 80.34(9) . . ? N102 Ni12 O12S 89.59(10) . . ? O102 Ni12 O12S 89.96(9) . . ? O1H Ni12 O12S 92.41(9) . . ? O103 Ni12 O12S 170.67(9) . . ? N102 Ni12 N104 83.29(10) . . ? O102 Ni12 N104 172.28(9) . . ? O1H Ni12 N104 95.75(9) . . ? O103 Ni12 N104 87.94(9) . . ? O12S Ni12 N104 86.95(10) . . ? O3W Ni3 O101 89.10(9) . . ? O3W Ni3 O13 177.09(9) . . ? O101 Ni3 O13 93.49(9) . . ? O3W Ni3 O30 90.53(9) . . ? O101 Ni3 O30 171.66(9) . . ? O13 Ni3 O30 87.10(9) . . ? O3W Ni3 O1H 93.33(10) . . ? O101 Ni3 O1H 82.35(8) . . ? O13 Ni3 O1H 88.32(9) . . ? O30 Ni3 O1H 89.35(9) . . ? O3W Ni3 O3S 88.28(10) . . ? O101 Ni3 O3S 97.51(9) . . ? O13 Ni3 O3S 90.08(9) . . ? O30 Ni3 O3S 90.81(9) . . ? O1H Ni3 O3S 178.38(9) . . ? O3W Ni3 Ni11 103.13(7) . . ? O101 Ni3 Ni11 41.95(6) . . ? O13 Ni3 Ni11 79.70(6) . . ? O30 Ni3 Ni11 130.30(6) . . ? O1H Ni3 Ni11 43.02(6) . . ? O3S Ni3 Ni11 136.35(7) . . ? C100 O101 Ni11 127.78(19) . . ? C100 O101 Ni3 136.57(19) . . ? Ni11 O101 Ni3 94.91(8) . . ? C119 O102 Ni12 129.06(19) . . ? C126 O103 Ni12 115.57(18) . . ? C126 O103 Ni11 117.15(18) . . ? Ni12 O103 Ni11 93.20(8) . . ? C106 N101 C107 119.9(3) . . ? C106 N101 Ni11 126.4(2) . . ? C107 N101 Ni11 113.5(2) . . ? C113 N102 C112 118.2(3) . . ? C113 N102 Ni12 127.6(2) . . ? C112 N102 Ni12 114.2(2) . . ? C120 N103 C109 101.6(2) . . ? C120 N103 C108 114.4(2) . . ? C109 N103 C108 109.8(2) . . ? C120 N103 Ni11 115.02(18) . . ? C109 N103 Ni11 113.28(19) . . ? C108 N103 Ni11 103.00(18) . . ? C120 N104 C111 112.8(2) . . ? C120 N104 C110 102.0(2) . . ? C111 N104 C110 110.3(2) . . ? C120 N104 Ni12 115.37(18) . . ? C111 N104 Ni12 102.04(19) . . ? C110 N104 Ni12 114.63(19) . . ? Ni11 O1H Ni12 97.03(9) . . ? Ni11 O1H Ni3 92.87(9) . . ? Ni12 O1H Ni3 136.15(12) . . ? Ni11 O1H H1H 114(3) . . ? Ni12 O1H H1H 116(3) . . ? Ni3 O1H H1H 97(3) . . ? C10 O11 Ni11 126.3(2) . . ? C10 O13 Ni3 126.8(2) . . ? C12S O12S Ni12 120.7(2) . . ? C12S O12S H12S 106(3) . . ? Ni12 O12S H12S 106(3) . . ? C30 O30 Ni3 128.6(2) . . ? Ni3 O3W H3W1 123(3) . . ? Ni3 O3W H3W2 98(3) . . ? H3W1 O3W H3W2 110(4) . . ? C3S O3S Ni3 123.3(2) . . ? C3S O3S H3S 102(3) . . ? Ni3 O3S H3S 110(2) . . ? O11 C10 O13 126.0(3) . . ? O11 C10 C11 117.4(3) . . ? O13 C10 C11 116.5(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C11 H11D 109.5 . . ? H11A C11 H11D 141.1 . . ? H11B C11 H11D 56.3 . . ? H11C C11 H11D 56.3 . . ? C10 C11 H11E 109.5 . . ? H11A C11 H11E 56.3 . . ? H11B C11 H11E 141.1 . . ? H11C C11 H11E 56.3 . . ? H11D C11 H11E 109.5 . . ? C10 C11 H11F 109.5 . . ? H11A C11 H11F 56.3 . . ? H11B C11 H11F 56.3 . . ? H11C C11 H11F 141.1 . . ? H11D C11 H11F 109.5 . . ? H11E C11 H11F 109.5 . . ? O12S C12S H12A 109.5 . . ? O12S C12S H12B 109.5 . . ? H12A C12S H12B 109.5 . . ? O12S C12S H12C 109.5 . . ? H12A C12S H12C 109.5 . . ? H12B C12S H12C 109.5 . . ? O3S C3S H3S1 109.5 . . ? O3S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? O3S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? O31 C30 O30 124.2(3) . . ? O31 C30 C31 118.8(3) . . ? O30 C30 C31 117.0(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O101 C100 C101 120.7(3) . . ? O101 C100 C105 122.1(3) . . ? C101 C100 C105 117.2(3) . . ? C102 C101 C100 122.2(3) . . ? C102 C101 H101 118.9 . . ? C100 C101 H101 118.9 . . ? C101 C102 C103 120.5(3) . . ? C101 C102 H102 119.8 . . ? C103 C102 H102 119.8 . . ? C104 C103 C102 118.3(3) . . ? C104 C103 H103 120.8 . . ? C102 C103 H103 120.8 . . ? C103 C104 C105 122.9(3) . . ? C103 C104 H104 118.5 . . ? C105 C104 H104 118.5 . . ? C104 C105 C100 118.8(3) . . ? C104 C105 C106 117.3(3) . . ? C100 C105 C106 123.9(3) . . ? N101 C106 C105 126.7(3) . . ? N101 C106 H106 116.6 . . ? C105 C106 H106 116.6 . . ? N101 C107 C108 108.8(3) . . ? N101 C107 H10A 109.9 . . ? C108 C107 H10A 109.9 . . ? N101 C107 H10B 109.9 . . ? C108 C107 H10B 109.9 . . ? H10A C107 H10B 108.3 . . ? N103 C108 C107 112.3(3) . . ? N103 C108 H10C 109.1 . . ? C107 C108 H10C 109.1 . . ? N103 C108 H10D 109.1 . . ? C107 C108 H10D 109.1 . . ? H10C C108 H10D 107.9 . . ? N103 C109 C110 104.4(2) . . ? N103 C109 H10E 110.9 . . ? C110 C109 H10E 110.9 . . ? N103 C109 H10F 110.9 . . ? C110 C109 H10F 110.9 . . ? H10E C109 H10F 108.9 . . ? N104 C110 C109 104.8(2) . . ? N104 C110 H11G 110.8 . . ? C109 C110 H11G 110.8 . . ? N104 C110 H11H 110.8 . . ? C109 C110 H11H 110.8 . . ? H11G C110 H11H 108.9 . . ? N104 C111 C112 112.0(3) . . ? N104 C111 H11I 109.2 . . ? C112 C111 H11I 109.2 . . ? N104 C111 H11J 109.2 . . ? C112 C111 H11J 109.2 . . ? H11I C111 H11J 107.9 . . ? N102 C112 C111 109.0(3) . . ? N102 C112 H11K 109.9 . . ? C111 C112 H11K 109.9 . . ? N102 C112 H11L 109.9 . . ? C111 C112 H11L 109.9 . . ? H11K C112 H11L 108.3 . . ? N102 C113 C114 126.3(3) . . ? N102 C113 H113 116.8 . . ? C114 C113 H113 116.8 . . ? C115 C114 C119 119.4(3) . . ? C115 C114 C113 117.0(3) . . ? C119 C114 C113 123.6(3) . . ? C116 C115 C114 122.1(3) . . ? C116 C115 H115 119.0 . . ? C114 C115 H115 119.0 . . ? C115 C116 C117 118.6(3) . . ? C115 C116 H116 120.7 . . ? C117 C116 H116 120.7 . . ? C118 C117 C116 121.3(3) . . ? C118 C117 H117 119.4 . . ? C116 C117 H117 119.4 . . ? C117 C118 C119 121.3(3) . . ? C117 C118 H118 119.4 . . ? C119 C118 H118 119.4 . . ? O102 C119 C118 119.1(3) . . ? O102 C119 C114 123.5(3) . . ? C118 C119 C114 117.4(3) . . ? N103 C120 N104 100.7(2) . . ? N103 C120 C121 115.1(3) . . ? N104 C120 C121 114.8(3) . . ? N103 C120 H120 108.6 . . ? N104 C120 H120 108.6 . . ? C121 C120 H120 108.6 . . ? C122 C121 C126 120.4(3) . . ? C122 C121 C120 119.2(3) . . ? C126 C121 C120 120.4(3) . . ? C123 C122 C121 121.1(3) . . ? C123 C122 H122 119.5 . . ? C121 C122 H122 119.5 . . ? C122 C123 C124 118.6(3) . . ? C122 C123 H123 120.7 . . ? C124 C123 H123 120.7 . . ? C123 C124 C125 121.1(3) . . ? C123 C124 H124 119.4 . . ? C125 C124 H124 119.4 . . ? C124 C125 C126 120.9(3) . . ? C124 C125 H125 119.6 . . ? C126 C125 H125 119.6 . . ? O103 C126 C125 121.1(3) . . ? O103 C126 C121 121.0(3) . . ? C125 C126 C121 117.9(3) . . ? H1W1 O1W H1W2 93.7 . . ? H2W1 O2W H2W2 102(4) . . ? C1S O1S H1S 109.5 . . ? C2S O2S H2S 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N101 Ni11 Ni3 O3W 89.02(12) . . . . ? O101 Ni11 Ni3 O3W 73.53(12) . . . . ? O1H Ni11 Ni3 O3W -80.65(12) . . . . ? O11 Ni11 Ni3 O3W 172.44(9) . . . . ? O103 Ni11 Ni3 O3W -14.90(9) . . . . ? N103 Ni11 Ni3 O3W -115.27(13) . . . . ? N101 Ni11 Ni3 O101 15.49(14) . . . . ? O1H Ni11 Ni3 O101 -154.18(13) . . . . ? O11 Ni11 Ni3 O101 98.91(11) . . . . ? O103 Ni11 Ni3 O101 -88.43(11) . . . . ? N103 Ni11 Ni3 O101 171.20(15) . . . . ? N101 Ni11 Ni3 O13 -91.65(12) . . . . ? O101 Ni11 Ni3 O13 -107.14(11) . . . . ? O1H Ni11 Ni3 O13 98.68(11) . . . . ? O11 Ni11 Ni3 O13 -8.23(9) . . . . ? O103 Ni11 Ni3 O13 164.43(9) . . . . ? N103 Ni11 Ni3 O13 64.06(13) . . . . ? N101 Ni11 Ni3 O30 -168.85(13) . . . . ? O101 Ni11 Ni3 O30 175.66(13) . . . . ? O1H Ni11 Ni3 O30 21.48(13) . . . . ? O11 Ni11 Ni3 O30 -85.43(11) . . . . ? O103 Ni11 Ni3 O30 87.23(10) . . . . ? N103 Ni11 Ni3 O30 -13.14(15) . . . . ? N101 Ni11 Ni3 O1H 169.67(14) . . . . ? O101 Ni11 Ni3 O1H 154.18(13) . . . . ? O11 Ni11 Ni3 O1H -106.91(11) . . . . ? O103 Ni11 Ni3 O1H 65.75(11) . . . . ? N103 Ni11 Ni3 O1H -34.62(15) . . . . ? N101 Ni11 Ni3 O3S -12.51(14) . . . . ? O101 Ni11 Ni3 O3S -28.00(13) . . . . ? O1H Ni11 Ni3 O3S 177.82(13) . . . . ? O11 Ni11 Ni3 O3S 70.91(12) . . . . ? O103 Ni11 Ni3 O3S -116.43(11) . . . . ? N103 Ni11 Ni3 O3S 143.20(15) . . . . ? N101 Ni11 O101 C100 20.0(2) . . . . ? O1H Ni11 O101 C100 -153.7(2) . . . . ? O11 Ni11 O101 C100 112.6(2) . . . . ? O103 Ni11 O101 C100 -74.5(2) . . . . ? Ni3 Ni11 O101 C100 -171.4(3) . . . . ? N101 Ni11 O101 Ni3 -168.55(10) . . . . ? O1H Ni11 O101 Ni3 17.73(9) . . . . ? O11 Ni11 O101 Ni3 -75.98(9) . . . . ? O103 Ni11 O101 Ni3 96.95(9) . . . . ? O3W Ni3 O101 C100 59.2(3) . . . . ? O13 Ni3 O101 C100 -119.5(3) . . . . ? O30 Ni3 O101 C100 146.7(6) . . . . ? O1H Ni3 O101 C100 152.7(3) . . . . ? O3S Ni3 O101 C100 -28.9(3) . . . . ? Ni11 Ni3 O101 C100 170.1(3) . . . . ? O3W Ni3 O101 Ni11 -110.93(10) . . . . ? O13 Ni3 O101 Ni11 70.38(10) . . . . ? O1H Ni3 O101 Ni11 -17.45(9) . . . . ? O3S Ni3 O101 Ni11 160.92(9) . . . . ? N102 Ni12 O102 C119 -5.8(2) . . . . ? O1H Ni12 O102 C119 172.2(2) . . . . ? O103 Ni12 O102 C119 91.8(2) . . . . ? O12S Ni12 O102 C119 -95.3(2) . . . . ? N102 Ni12 O103 C126 -34.1(2) . . . . ? O102 Ni12 O103 C126 -124.5(2) . . . . ? O1H Ni12 O103 C126 145.0(2) . . . . ? N104 Ni12 O103 C126 48.8(2) . . . . ? N102 Ni12 O103 Ni11 -156.37(9) . . . . ? O102 Ni12 O103 Ni11 113.21(8) . . . . ? O1H Ni12 O103 Ni11 22.77(8) . . . . ? O12S Ni12 O103 Ni11 -16.6(6) . . . . ? N104 Ni12 O103 Ni11 -73.42(9) . . . . ? N101 Ni11 O103 C126 42.4(2) . . . . ? O101 Ni11 O103 C126 132.7(2) . . . . ? O1H Ni11 O103 C126 -143.8(2) . . . . ? N103 Ni11 O103 C126 -42.2(2) . . . . ? Ni3 Ni11 O103 C126 176.03(19) . . . . ? N101 Ni11 O103 Ni12 163.31(9) . . . . ? O101 Ni11 O103 Ni12 -106.34(8) . . . . ? O1H Ni11 O103 Ni12 -22.86(8) . . . . ? O11 Ni11 O103 Ni12 6.7(6) . . . . ? N103 Ni11 O103 Ni12 78.71(9) . . . . ? Ni3 Ni11 O103 Ni12 -63.01(6) . . . . ? O101 Ni11 N101 C106 -10.7(3) . . . . ? O11 Ni11 N101 C106 -98.7(3) . . . . ? O103 Ni11 N101 C106 84.4(3) . . . . ? N103 Ni11 N101 C106 173.8(3) . . . . ? Ni3 Ni11 N101 C106 -21.3(3) . . . . ? O101 Ni11 N101 C107 174.3(2) . . . . ? O11 Ni11 N101 C107 86.3(2) . . . . ? O103 Ni11 N101 C107 -90.6(2) . . . . ? N103 Ni11 N101 C107 -1.2(2) . . . . ? Ni3 Ni11 N101 C107 163.73(17) . . . . ? O102 Ni12 N102 C113 1.5(3) . . . . ? O103 Ni12 N102 C113 -94.6(3) . . . . ? O12S Ni12 N102 C113 91.4(3) . . . . ? N104 Ni12 N102 C113 178.4(3) . . . . ? O102 Ni12 N102 C112 -177.2(2) . . . . ? O1H Ni12 N102 C112 65(3) . . . . ? O103 Ni12 N102 C112 86.8(2) . . . . ? O12S Ni12 N102 C112 -87.2(2) . . . . ? N104 Ni12 N102 C112 -0.3(2) . . . . ? N101 Ni11 N103 C120 -101.3(2) . . . . ? O1H Ni11 N103 C120 72.8(2) . . . . ? O11 Ni11 N103 C120 166.0(2) . . . . ? O103 Ni11 N103 C120 -6.7(2) . . . . ? Ni3 Ni11 N103 C120 96.6(2) . . . . ? N101 Ni11 N103 C109 142.4(2) . . . . ? O1H Ni11 N103 C109 -43.5(2) . . . . ? O11 Ni11 N103 C109 49.6(2) . . . . ? O103 Ni11 N103 C109 -123.1(2) . . . . ? Ni3 Ni11 N103 C109 -19.7(3) . . . . ? N101 Ni11 N103 C108 23.89(19) . . . . ? O1H Ni11 N103 C108 -162.02(18) . . . . ? O11 Ni11 N103 C108 -68.90(19) . . . . ? O103 Ni11 N103 C108 118.41(19) . . . . ? Ni3 Ni11 N103 C108 -138.23(16) . . . . ? N102 Ni12 N104 C120 98.9(2) . . . . ? O1H Ni12 N104 C120 -79.0(2) . . . . ? O103 Ni12 N104 C120 1.0(2) . . . . ? O12S Ni12 N104 C120 -171.1(2) . . . . ? N102 Ni12 N104 C111 -23.78(19) . . . . ? O1H Ni12 N104 C111 158.28(19) . . . . ? O103 Ni12 N104 C111 -121.65(19) . . . . ? O12S Ni12 N104 C111 66.16(19) . . . . ? N102 Ni12 N104 C110 -143.0(2) . . . . ? O1H Ni12 N104 C110 39.0(2) . . . . ? O103 Ni12 N104 C110 119.1(2) . . . . ? O12S Ni12 N104 C110 -53.1(2) . . . . ? O101 Ni11 O1H Ni12 119.78(10) . . . . ? O11 Ni11 O1H Ni12 -152.63(9) . . . . ? O103 Ni11 O1H Ni12 23.58(8) . . . . ? N103 Ni11 O1H Ni12 -64.21(11) . . . . ? Ni3 Ni11 O1H Ni12 137.19(13) . . . . ? O101 Ni11 O1H Ni3 -17.41(9) . . . . ? O11 Ni11 O1H Ni3 70.17(9) . . . . ? O103 Ni11 O1H Ni3 -113.61(9) . . . . ? N103 Ni11 O1H Ni3 158.60(9) . . . . ? O102 Ni12 O1H Ni11 -119.74(9) . . . . ? O103 Ni12 O1H Ni11 -23.85(8) . . . . ? O12S Ni12 O1H Ni11 150.24(10) . . . . ? N104 Ni12 O1H Ni11 63.07(10) . . . . ? O102 Ni12 O1H Ni3 -18.14(17) . . . . ? O103 Ni12 O1H Ni3 77.74(16) . . . . ? O12S Ni12 O1H Ni3 -108.16(16) . . . . ? N104 Ni12 O1H Ni3 164.66(16) . . . . ? O3W Ni3 O1H Ni11 105.73(9) . . . . ? O101 Ni3 O1H Ni11 17.09(9) . . . . ? O13 Ni3 O1H Ni11 -76.67(9) . . . . ? O30 Ni3 O1H Ni11 -163.78(9) . . . . ? O3W Ni3 O1H Ni12 2.50(17) . . . . ? O101 Ni3 O1H Ni12 -86.15(16) . . . . ? O13 Ni3 O1H Ni12 -179.90(16) . . . . ? O30 Ni3 O1H Ni12 92.98(17) . . . . ? Ni11 Ni3 O1H Ni12 -103.23(18) . . . . ? N101 Ni11 O11 C10 138.4(3) . . . . ? O101 Ni11 O11 C10 48.5(3) . . . . ? O1H Ni11 O11 C10 -35.9(3) . . . . ? N103 Ni11 O11 C10 -137.1(3) . . . . ? Ni3 Ni11 O11 C10 6.0(2) . . . . ? O101 Ni3 O13 C10 -24.4(3) . . . . ? O30 Ni3 O13 C10 147.3(3) . . . . ? O1H Ni3 O13 C10 57.9(3) . . . . ? O3S Ni3 O13 C10 -121.9(3) . . . . ? Ni11 Ni3 O13 C10 15.4(2) . . . . ? N102 Ni12 O12S C12S -56.0(3) . . . . ? O102 Ni12 O12S C12S 33.7(3) . . . . ? O1H Ni12 O12S C12S 125.1(3) . . . . ? N104 Ni12 O12S C12S -139.3(3) . . . . ? O3W Ni3 O30 C30 -70.4(3) . . . . ? O13 Ni3 O30 C30 107.9(3) . . . . ? O1H Ni3 O30 C30 -163.8(3) . . . . ? O3S Ni3 O30 C30 17.9(3) . . . . ? Ni11 Ni3 O30 C30 -178.2(2) . . . . ? O3W Ni3 O3S C3S -164.5(3) . . . . ? O101 Ni3 O3S C3S -75.6(3) . . . . ? O13 Ni3 O3S C3S 17.9(3) . . . . ? O30 Ni3 O3S C3S 105.0(3) . . . . ? Ni11 Ni3 O3S C3S -57.2(3) . . . . ? Ni11 O11 C10 O13 3.3(5) . . . . ? Ni11 O11 C10 C11 -176.0(2) . . . . ? Ni3 O13 C10 O11 -16.9(5) . . . . ? Ni3 O13 C10 C11 162.5(2) . . . . ? Ni3 O30 C30 O31 -13.5(5) . . . . ? Ni3 O30 C30 C31 166.1(2) . . . . ? Ni11 O101 C100 C101 161.9(2) . . . . ? Ni3 O101 C100 C101 -5.6(5) . . . . ? Ni11 O101 C100 C105 -19.0(4) . . . . ? Ni3 O101 C100 C105 173.5(2) . . . . ? O101 C100 C101 C102 179.5(3) . . . . ? C105 C100 C101 C102 0.4(5) . . . . ? C100 C101 C102 C103 -2.5(5) . . . . ? C101 C102 C103 C104 2.3(5) . . . . ? C102 C103 C104 C105 -0.1(6) . . . . ? C103 C104 C105 C100 -2.0(5) . . . . ? C103 C104 C105 C106 177.7(3) . . . . ? O101 C100 C105 C104 -177.3(3) . . . . ? C101 C100 C105 C104 1.8(4) . . . . ? O101 C100 C105 C106 3.0(5) . . . . ? C101 C100 C105 C106 -177.9(3) . . . . ? C107 N101 C106 C105 175.6(3) . . . . ? Ni11 N101 C106 C105 0.9(5) . . . . ? C104 C105 C106 N101 -173.1(3) . . . . ? C100 C105 C106 N101 6.6(5) . . . . ? C106 N101 C107 C108 162.7(3) . . . . ? Ni11 N101 C107 C108 -21.9(3) . . . . ? C120 N103 C108 C107 82.4(3) . . . . ? C109 N103 C108 C107 -164.1(3) . . . . ? Ni11 N103 C108 C107 -43.1(3) . . . . ? N101 C107 C108 N103 44.8(4) . . . . ? C120 N103 C109 C110 -33.2(3) . . . . ? C108 N103 C109 C110 -154.7(3) . . . . ? Ni11 N103 C109 C110 90.8(2) . . . . ? C120 N104 C110 C109 26.4(3) . . . . ? C111 N104 C110 C109 146.5(3) . . . . ? Ni12 N104 C110 C109 -99.0(2) . . . . ? N103 C109 C110 N104 4.0(3) . . . . ? C120 N104 C111 C112 -80.0(3) . . . . ? C110 N104 C111 C112 166.6(3) . . . . ? Ni12 N104 C111 C112 44.4(3) . . . . ? C113 N102 C112 C111 -154.2(3) . . . . ? Ni12 N102 C112 C111 24.6(3) . . . . ? N104 C111 C112 N102 -47.9(4) . . . . ? C112 N102 C113 C114 -178.4(3) . . . . ? Ni12 N102 C113 C114 2.9(5) . . . . ? N102 C113 C114 C115 175.2(3) . . . . ? N102 C113 C114 C119 -4.8(5) . . . . ? C119 C114 C115 C116 -0.1(5) . . . . ? C113 C114 C115 C116 180.0(3) . . . . ? C114 C115 C116 C117 -1.0(5) . . . . ? C115 C116 C117 C118 0.9(5) . . . . ? C116 C117 C118 C119 0.2(5) . . . . ? Ni12 O102 C119 C118 -175.2(2) . . . . ? Ni12 O102 C119 C114 5.7(4) . . . . ? C117 C118 C119 O102 179.6(3) . . . . ? C117 C118 C119 C114 -1.2(4) . . . . ? C115 C114 C119 O102 -179.8(3) . . . . ? C113 C114 C119 O102 0.2(5) . . . . ? C115 C114 C119 C118 1.1(4) . . . . ? C113 C114 C119 C118 -178.9(3) . . . . ? C109 N103 C120 N104 50.2(3) . . . . ? C108 N103 C120 N104 168.5(2) . . . . ? Ni11 N103 C120 N104 -72.5(2) . . . . ? C109 N103 C120 C121 174.3(3) . . . . ? C108 N103 C120 C121 -67.5(3) . . . . ? Ni11 N103 C120 C121 51.5(3) . . . . ? C111 N104 C120 N103 -165.8(2) . . . . ? C110 N104 C120 N103 -47.4(3) . . . . ? Ni12 N104 C120 N103 77.5(2) . . . . ? C111 N104 C120 C121 70.0(3) . . . . ? C110 N104 C120 C121 -171.6(3) . . . . ? Ni12 N104 C120 C121 -46.7(3) . . . . ? N103 C120 C121 C122 122.2(3) . . . . ? N104 C120 C121 C122 -121.7(3) . . . . ? N103 C120 C121 C126 -59.2(4) . . . . ? N104 C120 C121 C126 57.0(4) . . . . ? C126 C121 C122 C123 -0.1(5) . . . . ? C120 C121 C122 C123 178.5(3) . . . . ? C121 C122 C123 C124 -0.4(6) . . . . ? C122 C123 C124 C125 0.3(6) . . . . ? C123 C124 C125 C126 0.2(7) . . . . ? Ni12 O103 C126 C125 121.5(3) . . . . ? Ni11 O103 C126 C125 -130.2(3) . . . . ? Ni12 O103 C126 C121 -57.7(3) . . . . ? Ni11 O103 C126 C121 50.6(4) . . . . ? C124 C125 C126 O103 -180.0(4) . . . . ? C124 C125 C126 C121 -0.7(6) . . . . ? C122 C121 C126 O103 179.9(3) . . . . ? C120 C121 C126 O103 1.3(5) . . . . ? C122 C121 C126 C125 0.7(5) . . . . ? C120 C121 C126 C125 -178.0(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 O1H H1H O2W 0.71(4) 2.56(4) 3.117(3) 137(3) . O3W H3W1 O31 0.90(5) 1.80(5) 2.697(3) 176(4) 3_657 O3W H3W2 O102 0.85(5) 1.74(5) 2.572(3) 165(5) . O12S H12S O2W 0.73(4) 1.94(4) 2.666(4) 174(4) . O3S H3S O31 1.00(4) 1.67(4) 2.573(3) 148(4) . O1W H1W2 O103 0.99 1.77 2.751(3) 169.2 . O1W H1W1 O3W 1.05 1.93 2.935(3) 159.3 . O2W H2W1 O30 0.96(5) 1.80(5) 2.737(3) 163(4) . O2W H2W2 O13 0.86(5) 2.20(5) 3.058(3) 172(5) 3_557 O1S H1S O1W 0.84 1.98 2.762(9) 153.9 . O1S H1S O1W 0.84 1.98 2.762(9) 153.9 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.065 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.086