data_am _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66.67 H60 Cl2.67 N8 Ni2.67 O13.33' _chemical_formula_weight 1437.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' _cell_length_a 10.2115(4) _cell_length_b 10.2115(4) _cell_length_c 43.848(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4572.3(4) _cell_formula_units_Z 3 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8145 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 27.48 _exptl_crystal_description Diamond _exptl_crystal_colour Dark brown _exptl_crystal_size_max 0.84 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2228 _exptl_absorpt_coefficient_mu 1.010 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4860 _exptl_absorpt_correction_T_max 0.8077 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38628 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0837 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 27.52 _reflns_number_total 10482 _reflns_number_gt 9782 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0569P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.026(19) _refine_ls_number_reflns 10482 _refine_ls_number_parameters 636 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.12509(7) 0.83006(7) 0.234438(15) 0.01662(15) Uani 1 1 d . . . Ni2 Ni 0.23925(7) 0.79125(7) 0.292207(15) 0.01424(14) Uani 1 1 d . . . N1 N 0.1434(5) 0.7563(5) 0.19653(10) 0.0156(10) Uani 1 1 d . . . N2 N 0.0026(5) 0.9415(4) 0.21869(9) 0.0124(9) Uani 1 1 d . . . N3 N 0.2087(4) 0.8532(4) 0.33059(9) 0.0113(9) Uani 1 1 d . . . N4 N 0.3721(4) 0.6906(4) 0.30738(9) 0.0118(9) Uani 1 1 d . . . O1 O 0.2565(4) 0.7332(4) 0.25260(8) 0.0170(8) Uani 1 1 d . . . O2 O 0.1104(4) 0.8909(4) 0.27373(8) 0.0166(8) Uani 1 1 d . . . C1 C 0.0456(5) 0.8030(5) 0.17444(11) 0.0135(11) Uani 1 1 d . . . H1 H -0.0306 0.7414 0.1750 0.016 Uiso 1 1 calc R . . C2 C 0.0964(5) 0.8085(5) 0.14155(12) 0.0147(11) Uani 1 1 d . . . C3 C 0.0367(6) 0.7381(6) 0.11850(12) 0.0170(11) Uani 1 1 d . . . H3 H -0.0363 0.6836 0.1229 0.020 Uiso 1 1 calc R . . C4 C 0.0836(6) 0.7473(6) 0.08899(13) 0.0236(14) Uani 1 1 d . . . H4 H 0.0418 0.6990 0.0732 0.028 Uiso 1 1 calc R . . C5 C 0.1915(6) 0.8264(6) 0.08188(12) 0.0235(13) Uani 1 1 d . . . H5 H 0.2227 0.8325 0.0615 0.028 Uiso 1 1 calc R . . C6 C 0.2524(6) 0.8964(5) 0.10547(13) 0.0204(12) Uani 1 1 d . . . H6 H 0.3263 0.9498 0.1012 0.024 Uiso 1 1 calc R . . C7 C 0.2052(6) 0.8876(5) 0.13482(13) 0.0193(12) Uani 1 1 d . . . H7 H 0.2467 0.9356 0.1507 0.023 Uiso 1 1 calc R . . C8 C -0.0025(5) 0.9379(5) 0.18482(12) 0.0143(11) Uani 1 1 d . . . H8 H 0.0604 1.0048 0.1769 0.017 Uiso 1 1 calc R . . C9 C -0.2449(6) 0.8917(6) 0.17820(13) 0.0209(12) Uani 1 1 d . . . H9 H -0.2341 0.8128 0.1894 0.025 Uiso 1 1 calc R . . C10 C -0.3665(7) 0.9263(6) 0.16754(14) 0.0266(14) Uani 1 1 d . . . H10 H -0.4406 0.8742 0.1725 0.032 Uiso 1 1 calc R . . C11 C -0.3813(7) 1.0369(7) 0.14960(14) 0.0284(15) Uani 1 1 d . . . H11 H -0.4640 1.0559 0.1407 0.034 Uiso 1 1 calc R . . C12 C -0.2781(7) 1.1186(7) 0.14467(14) 0.0287(15) Uani 1 1 d . . . H12 H -0.2901 1.1974 0.1335 0.034 Uiso 1 1 calc R . . C13 C -0.1536(6) 1.0865(5) 0.15614(12) 0.0202(12) Uani 1 1 d . . . H13 H -0.0810 1.1427 0.1526 0.024 Uiso 1 1 calc R . . C14 C -0.1378(6) 0.9717(6) 0.17266(12) 0.0163(12) Uani 1 1 d . . . C15 C -0.0604(5) 1.0275(5) 0.23366(12) 0.0128(10) Uani 1 1 d . . . H15 H -0.1211 1.0793 0.2225 0.015 Uiso 1 1 calc R . . C16 C -0.0493(5) 1.0546(5) 0.26593(12) 0.0121(11) Uani 1 1 d . . . C17 C -0.1260(5) 1.1547(5) 0.27887(11) 0.0159(11) Uani 1 1 d . . . H17 H -0.1878 1.1982 0.2663 0.019 Uiso 1 1 calc R . . C18 C -0.1158(5) 1.1929(6) 0.30908(11) 0.0154(11) Uani 1 1 d . . . C19 C -0.0249(5) 1.1244(5) 0.32743(11) 0.0127(11) Uani 1 1 d . . . H19 H -0.0149 1.1496 0.3482 0.015 Uiso 1 1 calc R . . C20 C 0.0512(5) 1.0205(5) 0.31617(11) 0.0119(10) Uani 1 1 d . . . C21 C 0.0398(5) 0.9864(5) 0.28503(11) 0.0133(10) Uani 1 1 d . . . C22 C -0.1996(6) 1.2998(6) 0.32261(12) 0.0190(12) Uani 1 1 d . . . H22A H -0.1963 1.3773 0.3095 0.028 Uiso 1 1 calc R . . H22B H -0.1666 1.3224 0.3429 0.028 Uiso 1 1 calc R . . H22C H -0.2902 1.2692 0.3242 0.028 Uiso 1 1 calc R . . C23 C 0.1316(5) 0.9496(6) 0.33732(12) 0.0128(11) Uani 1 1 d . . . H23 H 0.1279 0.9757 0.3581 0.015 Uiso 1 1 calc R . . C24 C 0.2754(5) 0.7705(5) 0.35449(11) 0.0136(10) Uani 1 1 d . . . H24 H 0.2185 0.6926 0.3584 0.016 Uiso 1 1 calc R . . C25 C 0.2999(5) 0.8363(5) 0.38460(11) 0.0142(11) Uani 1 1 d . . . H25 H 0.2231 0.8951 0.3810 0.017 Uiso 1 1 calc R . . C26 C 0.3828(5) 0.9467(6) 0.38656(12) 0.0156(11) Uani 1 1 d . . . H26 H 0.4216 0.9817 0.3686 0.019 Uiso 1 1 calc R . . C27 C 0.4077(6) 1.0040(6) 0.41469(13) 0.0204(13) Uani 1 1 d . . . H27 H 0.4645 1.0775 0.4160 0.024 Uiso 1 1 calc R . . C28 C 0.3500(6) 0.9543(6) 0.44107(12) 0.0229(14) Uani 1 1 d . . . H28 H 0.3683 0.9932 0.4603 0.028 Uiso 1 1 calc R . . C29 C 0.2653(6) 0.8475(6) 0.43929(12) 0.0208(13) Uani 1 1 d . . . H29 H 0.2241 0.8141 0.4571 0.025 Uiso 1 1 calc R . . C30 C 0.2423(6) 0.7904(6) 0.41077(12) 0.0185(11) Uani 1 1 d . . . H30 H 0.1848 0.7175 0.4095 0.022 Uiso 1 1 calc R . . C31 C 0.4030(5) 0.7213(5) 0.34016(11) 0.0126(11) Uani 1 1 d . . . H31 H 0.4668 0.7956 0.3403 0.015 Uiso 1 1 calc R . . C32 C 0.4644(5) 0.6094(5) 0.35722(11) 0.0121(11) Uani 1 1 d . . . C33 C 0.5915(5) 0.6229(6) 0.36725(12) 0.0176(11) Uani 1 1 d . . . H33 H 0.6363 0.7032 0.3639 0.021 Uiso 1 1 calc R . . C34 C 0.6550(6) 0.5218(6) 0.38206(14) 0.0232(13) Uani 1 1 d . . . H34 H 0.7435 0.5318 0.3883 0.028 Uiso 1 1 calc R . . C35 C 0.5890(6) 0.4056(6) 0.38772(13) 0.0224(13) Uani 1 1 d . . . H35 H 0.6312 0.3364 0.3984 0.027 Uiso 1 1 calc R . . C36 C 0.4632(6) 0.3914(6) 0.37784(13) 0.0230(13) Uani 1 1 d . . . H36 H 0.4184 0.3112 0.3813 0.028 Uiso 1 1 calc R . . C37 C 0.4000(5) 0.4924(6) 0.36282(13) 0.0205(13) Uani 1 1 d . . . H37 H 0.3120 0.4815 0.3563 0.025 Uiso 1 1 calc R . . C38 C 0.4383(5) 0.6050(5) 0.29226(12) 0.0132(10) Uani 1 1 d . . . H38 H 0.5048 0.5593 0.3031 0.016 Uiso 1 1 calc R . . C39 C 0.4212(5) 0.5717(5) 0.26038(12) 0.0125(11) Uani 1 1 d . . . C40 C 0.4958(6) 0.4718(6) 0.24753(13) 0.0176(11) Uani 1 1 d . . . H40 H 0.5571 0.4277 0.2602 0.021 Uiso 1 1 calc R . . C41 C 0.4857(6) 0.4334(6) 0.21768(12) 0.0183(12) Uani 1 1 d . . . C42 C 0.3943(6) 0.4972(6) 0.19982(14) 0.0196(13) Uani 1 1 d . . . H42 H 0.3843 0.4705 0.1792 0.023 Uiso 1 1 calc R . . C43 C 0.3160(6) 0.5992(5) 0.21075(12) 0.0146(11) Uani 1 1 d . . . C44 C 0.3301(5) 0.6376(5) 0.24168(11) 0.0119(10) Uani 1 1 d . . . C45 C 0.5672(7) 0.3233(7) 0.20525(14) 0.0290(15) Uani 1 1 d . . . H45A H 0.5616 0.2479 0.2190 0.043 Uiso 1 1 calc R . . H45B H 0.6586 0.3517 0.2036 0.043 Uiso 1 1 calc R . . H45C H 0.5345 0.2985 0.1850 0.043 Uiso 1 1 calc R . . C46 C 0.2223(5) 0.6604(6) 0.19046(11) 0.0153(11) Uani 1 1 d . . . H46 H 0.2182 0.6263 0.1703 0.018 Uiso 1 1 calc R . . Cl1 Cl 0.83750(15) 0.59344(15) 0.24261(3) 0.0256(3) Uani 1 1 d . . . O3 O 0.7491(5) 0.6775(6) 0.25759(12) 0.0480(14) Uani 1 1 d . . . O4 O 0.8186(4) 0.4596(4) 0.25174(10) 0.0323(11) Uani 1 1 d . . . O5 O 0.9684(5) 0.6296(5) 0.24893(17) 0.0653(19) Uani 1 1 d . . . O6 O 0.8149(7) 0.6016(5) 0.21056(10) 0.0548(18) Uani 1 1 d . . . Cl2 Cl 0.39451(15) 0.15956(17) 0.30961(4) 0.0297(3) Uani 1 1 d . . . O7 O 0.3050(4) 0.1867(5) 0.33410(11) 0.0346(11) Uani 1 1 d . . . O8 O 0.4546(6) 0.2761(6) 0.30047(13) 0.0623(18) Uani 1 1 d . . . O9 O 0.3242(5) 0.1034(5) 0.28451(11) 0.0426(13) Uani 1 1 d . . . O10 O 0.4910(6) 0.0672(6) 0.32002(12) 0.0570(18) Uani 1 1 d . . . C60 C 0.1349(7) 0.3769(6) 0.27578(14) 0.0279(14) Uani 1 1 d . . . H60A H 0.0622 0.3931 0.2617 0.042 Uiso 1 1 calc R . . H60B H 0.1375 0.2837 0.2811 0.042 Uiso 1 1 calc R . . H60C H 0.2175 0.4020 0.2660 0.042 Uiso 1 1 calc R . . C61 C 0.1164(6) 0.4541(7) 0.30333(15) 0.0258(14) Uani 1 1 d . . . N62 N 0.1029(5) 0.5089(6) 0.32538(13) 0.0310(13) Uani 1 1 d . . . C71 C 0.4319(7) 0.9739(7) 0.22482(15) 0.0306(15) Uani 1 1 d . . . C70 C 0.5332(8) 0.9423(8) 0.24621(17) 0.0421(19) Uani 1 1 d . . . H70A H 0.5720 0.8576 0.2408 0.063 Uiso 1 1 calc R . . H70B H 0.4959 0.9374 0.2668 0.063 Uiso 1 1 calc R . . H70C H 0.6009 1.0103 0.2456 0.063 Uiso 1 1 calc R . . N72 N 0.3490(7) 0.9989(6) 0.20775(13) 0.0380(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0171(4) 0.0177(4) 0.0151(3) -0.0013(3) -0.0027(3) 0.0035(3) Ni2 0.0133(4) 0.0163(4) 0.0132(3) 0.0003(3) -0.0022(3) 0.0026(3) N1 0.016(2) 0.016(2) 0.014(2) -0.0005(19) 0.0009(18) -0.0040(19) N2 0.015(2) 0.011(2) 0.010(2) 0.0001(17) -0.0023(18) 0.0018(18) N3 0.013(2) 0.010(2) 0.012(2) 0.0024(17) -0.0055(17) -0.0019(18) N4 0.012(2) 0.009(2) 0.014(2) 0.0035(17) -0.0055(17) -0.0050(18) O1 0.022(2) 0.016(2) 0.0134(17) -0.0027(15) -0.0043(16) 0.0052(17) O2 0.019(2) 0.022(2) 0.0081(16) -0.0030(16) -0.0053(15) 0.0065(17) C1 0.014(3) 0.017(3) 0.009(2) 0.001(2) 0.001(2) 0.003(2) C2 0.017(3) 0.014(3) 0.013(2) 0.002(2) -0.001(2) 0.004(2) C3 0.019(3) 0.016(3) 0.015(2) -0.002(2) -0.002(2) 0.004(2) C4 0.030(3) 0.019(3) 0.021(3) -0.002(3) -0.010(3) 0.014(3) C5 0.035(4) 0.023(3) 0.013(2) 0.007(2) 0.001(2) 0.013(3) C6 0.020(3) 0.018(3) 0.023(3) 0.002(2) 0.006(2) 0.002(2) C7 0.026(3) 0.009(3) 0.023(3) 0.000(2) -0.004(2) 0.001(2) C8 0.016(3) 0.012(3) 0.014(2) -0.001(2) 0.003(2) 0.000(2) C9 0.022(3) 0.020(3) 0.021(3) 0.001(2) -0.006(2) 0.000(3) C10 0.027(4) 0.027(3) 0.026(3) -0.012(3) -0.006(3) 0.002(3) C11 0.030(4) 0.034(4) 0.021(3) -0.012(3) -0.016(3) 0.009(3) C12 0.039(4) 0.027(3) 0.020(3) -0.001(3) -0.003(3) 0.020(3) C13 0.030(3) 0.014(3) 0.017(3) -0.003(2) 0.007(2) 0.001(3) C14 0.025(3) 0.016(3) 0.008(2) -0.005(2) 0.000(2) 0.009(2) C15 0.007(2) 0.019(3) 0.013(2) 0.001(2) -0.003(2) 0.000(2) C16 0.012(2) 0.011(3) 0.013(2) -0.003(2) 0.000(2) 0.0005(19) C17 0.013(3) 0.018(3) 0.016(2) 0.000(2) 0.000(2) 0.001(2) C18 0.013(3) 0.018(3) 0.015(2) -0.003(2) -0.003(2) 0.002(2) C19 0.010(2) 0.017(3) 0.011(3) -0.006(2) 0.007(2) -0.002(2) C20 0.014(3) 0.012(3) 0.010(2) 0.001(2) -0.002(2) -0.004(2) C21 0.014(3) 0.014(3) 0.012(2) 0.000(2) -0.001(2) 0.000(2) C22 0.021(3) 0.018(3) 0.019(3) 0.001(2) 0.002(2) 0.004(2) C23 0.008(3) 0.020(3) 0.010(2) 0.002(2) -0.002(2) -0.002(2) C24 0.011(2) 0.014(2) 0.016(2) 0.005(2) -0.003(2) -0.001(2) C25 0.009(2) 0.019(3) 0.015(3) -0.004(2) -0.003(2) 0.007(2) C26 0.010(3) 0.020(3) 0.017(3) 0.000(2) 0.003(2) 0.002(2) C27 0.019(3) 0.019(3) 0.023(3) -0.001(2) -0.005(2) 0.001(2) C28 0.030(3) 0.033(3) 0.006(2) -0.006(2) -0.006(2) 0.009(3) C29 0.027(3) 0.025(3) 0.010(2) 0.000(2) 0.002(2) 0.005(3) C30 0.015(3) 0.021(3) 0.020(3) 0.003(2) 0.000(2) 0.003(2) C31 0.010(3) 0.011(3) 0.017(3) 0.002(2) -0.002(2) 0.000(2) C32 0.012(2) 0.015(3) 0.009(2) 0.002(2) -0.002(2) 0.003(2) C33 0.012(3) 0.019(3) 0.021(3) 0.002(2) -0.001(2) -0.003(2) C34 0.013(3) 0.027(3) 0.029(3) 0.006(3) -0.008(3) 0.001(3) C35 0.020(3) 0.022(3) 0.026(3) 0.005(2) -0.005(2) 0.006(3) C36 0.030(3) 0.016(3) 0.023(3) 0.009(2) -0.001(3) -0.005(3) C37 0.012(3) 0.020(3) 0.030(3) 0.001(2) -0.007(2) -0.003(2) C38 0.009(2) 0.014(3) 0.017(2) 0.001(2) -0.001(2) 0.001(2) C39 0.011(2) 0.014(3) 0.013(2) 0.007(2) -0.003(2) -0.004(2) C40 0.014(3) 0.017(3) 0.022(3) 0.001(2) -0.002(2) 0.005(2) C41 0.022(3) 0.018(3) 0.015(3) 0.000(2) -0.001(2) 0.001(2) C42 0.022(3) 0.015(3) 0.022(3) -0.001(2) 0.003(3) -0.001(2) C43 0.020(3) 0.009(2) 0.015(3) 0.000(2) 0.001(2) 0.000(2) C44 0.010(2) 0.013(3) 0.013(2) -0.001(2) 0.007(2) 0.002(2) C45 0.035(4) 0.029(4) 0.023(3) -0.004(3) 0.003(3) 0.007(3) C46 0.018(3) 0.020(3) 0.008(2) -0.004(2) 0.001(2) -0.001(2) Cl1 0.0241(7) 0.0220(7) 0.0309(8) 0.0067(6) 0.0046(6) 0.0024(6) O3 0.045(3) 0.048(3) 0.051(3) -0.023(3) 0.005(3) 0.017(3) O4 0.025(2) 0.029(2) 0.043(3) 0.018(2) -0.005(2) -0.008(2) O5 0.026(3) 0.032(3) 0.138(6) 0.030(3) -0.008(3) -0.009(2) O6 0.102(5) 0.041(3) 0.021(2) 0.010(2) 0.013(3) 0.018(3) Cl2 0.0212(8) 0.0314(9) 0.0364(8) 0.0138(7) -0.0033(7) -0.0047(6) O7 0.026(2) 0.034(3) 0.044(3) -0.009(2) -0.001(2) -0.004(2) O8 0.064(4) 0.059(4) 0.064(4) 0.032(3) -0.014(3) -0.035(3) O9 0.032(3) 0.052(3) 0.044(3) -0.012(3) -0.004(2) -0.005(3) O10 0.043(3) 0.079(5) 0.049(3) 0.040(3) 0.016(3) 0.026(3) C60 0.028(4) 0.028(3) 0.028(3) -0.003(3) -0.002(3) -0.001(3) C61 0.017(3) 0.025(3) 0.036(4) 0.004(3) -0.004(3) -0.010(3) N62 0.021(3) 0.033(3) 0.039(3) -0.005(3) -0.011(3) 0.001(2) C71 0.032(4) 0.032(4) 0.029(3) 0.000(3) 0.007(3) -0.009(3) C70 0.043(5) 0.047(5) 0.035(4) 0.008(4) 0.001(4) -0.004(4) N72 0.038(4) 0.037(3) 0.040(3) 0.005(3) 0.002(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.826(4) . ? Ni1 N1 1.835(5) . ? Ni1 O2 1.838(4) . ? Ni1 O1 1.848(4) . ? Ni1 Ni2 2.8165(9) . ? Ni2 N3 1.825(4) . ? Ni2 N4 1.828(4) . ? Ni2 O1 1.843(3) . ? Ni2 O2 1.850(4) . ? N1 C46 1.295(7) . ? N1 C1 1.471(7) . ? N2 C15 1.272(7) . ? N2 C8 1.486(6) . ? N3 C23 1.295(7) . ? N3 C24 1.508(6) . ? N4 C38 1.288(7) . ? N4 C31 1.505(6) . ? O1 C44 1.322(6) . ? O2 C21 1.311(7) . ? C1 C8 1.532(7) . ? C1 C2 1.534(7) . ? C2 C3 1.382(7) . ? C2 C7 1.405(8) . ? C3 C4 1.383(8) . ? C4 C5 1.401(9) . ? C5 C6 1.403(8) . ? C6 C7 1.377(8) . ? C8 C14 1.521(8) . ? C9 C10 1.373(8) . ? C9 C14 1.386(8) . ? C10 C11 1.385(9) . ? C11 C12 1.362(10) . ? C12 C13 1.406(9) . ? C13 C14 1.388(8) . ? C15 C16 1.446(7) . ? C16 C17 1.407(7) . ? C16 C21 1.419(7) . ? C17 C18 1.385(7) . ? C18 C19 1.413(8) . ? C18 C22 1.508(8) . ? C19 C20 1.404(7) . ? C20 C21 1.414(7) . ? C20 C23 1.434(7) . ? C24 C25 1.502(7) . ? C24 C31 1.532(7) . ? C25 C30 1.372(7) . ? C25 C26 1.412(8) . ? C26 C27 1.389(7) . ? C27 C28 1.394(8) . ? C28 C29 1.393(9) . ? C29 C30 1.399(7) . ? C31 C32 1.502(7) . ? C32 C33 1.378(7) . ? C32 C37 1.385(8) . ? C33 C34 1.381(8) . ? C34 C35 1.387(9) . ? C35 C36 1.364(8) . ? C36 C37 1.384(8) . ? C38 C39 1.449(7) . ? C39 C40 1.393(8) . ? C39 C44 1.410(7) . ? C40 C41 1.370(7) . ? C41 C42 1.381(8) . ? C41 C45 1.500(8) . ? C42 C43 1.398(8) . ? C43 C44 1.419(7) . ? C43 C46 1.449(7) . ? Cl1 O3 1.408(5) . ? Cl1 O5 1.415(6) . ? Cl1 O6 1.427(5) . ? Cl1 O4 1.438(4) . ? Cl2 O8 1.398(5) . ? Cl2 O9 1.434(5) . ? Cl2 O10 1.438(5) . ? Cl2 O7 1.437(5) . ? C60 C61 1.455(9) . ? C61 N62 1.125(8) . ? C71 N72 1.159(9) . ? C71 C70 1.433(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N1 89.0(2) . . ? N2 Ni1 O2 95.07(17) . . ? N1 Ni1 O2 175.30(19) . . ? N2 Ni1 O1 173.68(19) . . ? N1 Ni1 O1 95.54(18) . . ? O2 Ni1 O1 80.56(15) . . ? N2 Ni1 Ni2 135.34(13) . . ? N1 Ni1 Ni2 135.63(15) . . ? O2 Ni1 Ni2 40.36(12) . . ? O1 Ni1 Ni2 40.21(11) . . ? N3 Ni2 N4 89.21(19) . . ? N3 Ni2 O1 175.31(19) . . ? N4 Ni2 O1 95.22(18) . . ? N3 Ni2 O2 95.26(18) . . ? N4 Ni2 O2 175.35(18) . . ? O1 Ni2 O2 80.35(15) . . ? N3 Ni2 Ni1 135.23(14) . . ? N4 Ni2 Ni1 135.54(13) . . ? O1 Ni2 Ni1 40.32(11) . . ? O2 Ni2 Ni1 40.04(11) . . ? C46 N1 C1 122.1(5) . . ? C46 N1 Ni1 124.1(4) . . ? C1 N1 Ni1 113.2(3) . . ? C15 N2 C8 121.0(4) . . ? C15 N2 Ni1 125.6(4) . . ? C8 N2 Ni1 112.7(3) . . ? C23 N3 C24 122.8(4) . . ? C23 N3 Ni2 125.3(4) . . ? C24 N3 Ni2 111.7(3) . . ? C38 N4 C31 121.5(4) . . ? C38 N4 Ni2 125.7(4) . . ? C31 N4 Ni2 112.7(3) . . ? C44 O1 Ni2 129.3(3) . . ? C44 O1 Ni1 130.7(3) . . ? Ni2 O1 Ni1 99.46(17) . . ? C21 O2 Ni1 130.6(3) . . ? C21 O2 Ni2 129.4(3) . . ? Ni1 O2 Ni2 99.60(17) . . ? N1 C1 C8 108.3(4) . . ? N1 C1 C2 113.7(4) . . ? C8 C1 C2 110.8(4) . . ? C3 C2 C7 119.6(5) . . ? C3 C2 C1 121.3(5) . . ? C7 C2 C1 119.1(5) . . ? C2 C3 C4 119.7(6) . . ? C3 C4 C5 121.3(5) . . ? C6 C5 C4 118.6(5) . . ? C7 C6 C5 120.1(5) . . ? C6 C7 C2 120.7(5) . . ? N2 C8 C14 112.1(4) . . ? N2 C8 C1 107.9(4) . . ? C14 C8 C1 113.0(4) . . ? C10 C9 C14 120.1(6) . . ? C9 C10 C11 120.1(6) . . ? C12 C11 C10 120.3(6) . . ? C11 C12 C13 120.0(6) . . ? C14 C13 C12 119.3(6) . . ? C13 C14 C9 119.8(6) . . ? C13 C14 C8 118.7(5) . . ? C9 C14 C8 121.4(5) . . ? N2 C15 C16 126.7(5) . . ? C17 C16 C21 118.4(5) . . ? C17 C16 C15 119.3(5) . . ? C21 C16 C15 122.3(5) . . ? C18 C17 C16 123.3(5) . . ? C17 C18 C19 117.0(5) . . ? C17 C18 C22 122.5(5) . . ? C19 C18 C22 120.5(4) . . ? C20 C19 C18 122.5(5) . . ? C19 C20 C21 118.7(5) . . ? C19 C20 C23 118.1(5) . . ? C21 C20 C23 123.2(5) . . ? O2 C21 C20 120.2(5) . . ? O2 C21 C16 119.7(4) . . ? C20 C21 C16 120.1(5) . . ? N3 C23 C20 125.8(5) . . ? C25 C24 N3 115.9(4) . . ? C25 C24 C31 111.4(4) . . ? N3 C24 C31 106.4(4) . . ? C30 C25 C26 118.6(5) . . ? C30 C25 C24 120.7(5) . . ? C26 C25 C24 120.7(5) . . ? C27 C26 C25 120.0(5) . . ? C26 C27 C28 120.4(6) . . ? C29 C28 C27 120.1(5) . . ? C28 C29 C30 118.7(5) . . ? C25 C30 C29 122.2(6) . . ? C32 C31 N4 113.9(4) . . ? C32 C31 C24 113.6(4) . . ? N4 C31 C24 106.4(4) . . ? C33 C32 C37 118.4(5) . . ? C33 C32 C31 118.4(5) . . ? C37 C32 C31 123.1(5) . . ? C32 C33 C34 121.2(5) . . ? C33 C34 C35 119.7(5) . . ? C36 C35 C34 119.4(5) . . ? C35 C36 C37 120.8(5) . . ? C36 C37 C32 120.4(5) . . ? N4 C38 C39 126.3(5) . . ? C40 C39 C44 118.4(5) . . ? C40 C39 C38 119.7(5) . . ? C44 C39 C38 121.9(5) . . ? C41 C40 C39 123.7(5) . . ? C40 C41 C42 117.2(5) . . ? C40 C41 C45 121.3(5) . . ? C42 C41 C45 121.4(5) . . ? C41 C42 C43 122.9(5) . . ? C42 C43 C44 118.4(5) . . ? C42 C43 C46 119.3(5) . . ? C44 C43 C46 122.3(5) . . ? O1 C44 C39 121.1(5) . . ? O1 C44 C43 119.5(5) . . ? C39 C44 C43 119.4(5) . . ? N1 C46 C43 127.7(5) . . ? O3 Cl1 O5 110.8(4) . . ? O3 Cl1 O6 108.7(3) . . ? O5 Cl1 O6 109.3(4) . . ? O3 Cl1 O4 111.3(3) . . ? O5 Cl1 O4 108.7(3) . . ? O6 Cl1 O4 108.0(3) . . ? O8 Cl2 O9 109.9(3) . . ? O8 Cl2 O10 110.4(4) . . ? O9 Cl2 O10 108.9(4) . . ? O8 Cl2 O7 109.2(4) . . ? O9 Cl2 O7 109.4(3) . . ? O10 Cl2 O7 109.0(3) . . ? N62 C61 C60 176.9(7) . . ? N72 C71 C70 179.3(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.558 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.181