# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1578 data_global _audit_creation_method 'SHELXL-97' # SUBMISSION DETAILS _publ_contact_author_name 'Song Gao' _publ_contact_author_address ; State Key Laboratory of Rare Earth Materials Chemistry and Applications PKU-HKU Joint Laboratory on Rare Earth Materials and Bioinorganic Chemistry Peking University Beijing 100871 People's Republic of China ; _publ_contact_author_email gaosong@chemms.chem.pku.edu.cn _publ_contact_author_phone '86(10)62756320' _publ_contact_author_fax '86(10)62751708' _publ_requested_journal '' _publ_requested_category ? _publ_contact_letter ; ; # TITLE AND AUTHOR LIST _publ_section_title ; ; loop_ _publ_author_name _publ_author_address ? ; ; data_NiCr _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H98 Cr2 N30 Ni3 O12' _chemical_formula_weight 1471.61 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' 'Cr' 'Cr' 0.3209 0.6236 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.836(5) _cell_length_b 15.369(3) _cell_length_c 19.478(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.15(3) _cell_angle_gamma 90.00 _cell_volume 7466(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 1.31 _exptl_crystal_F_000 3120 _exptl_absorpt_coefficient_mu 1.092 _exptl_absorpt_correction_type 'SORTAV' _exptl_absorpt_correction_T_min 0.759 _exptl_absorpt_correction_T_max 0.880 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS Kappa CCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 0.71 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48195 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 27.88 _reflns_number_total 8871 _reflns_number_gt 6257 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS Kappa CCD' _computing_cell_refinement 'HKL Scalepack' _computing_data_reduction 'HKL Denzo & Maxus' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXL (1990)' _computing_publication_material 'Siemens SHELXL-97' _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^)+(0.1061P)^2^+13.9015P] 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 8871 _refine_ls_number_parameters 518 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0945 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1907 _refine_ls_wR_factor_gt 0.1660 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.5000 0.44006(5) 0.2500 0.03467(18) Uani 1 2 d S . . Ni2 Ni 0.26073(2) 0.71735(3) 0.25963(3) 0.04013(16) Uani 1 1 d . . . Cr Cr 0.29981(2) 0.46701(4) 0.09286(3) 0.03093(16) Uani 1 1 d . . . O1 O 0.3499(2) 0.6082(6) 0.0222(4) 0.183(4) Uani 1 1 d . . . O2 O 0.1548(3) 0.4725(5) 0.1920(5) 0.162(3) Uani 1 1 d . . . O3 O -0.0054(6) 0.6179(11) 0.0085(9) 0.321(8) Uani 1 1 d . . . O4 O -0.1043(4) 0.6464(6) 0.0443(6) 0.204(4) Uani 1 1 d . . . O5 O 0.0746(7) 0.7390(9) -0.0644(7) 0.302(8) Uani 1 1 d . . . O6 O 0.2075(3) 0.7073(4) 0.0171(3) 0.135(2) Uani 1 1 d . . . N1 N 0.3309(2) 0.5529(4) 0.0488(3) 0.0903(19) Uani 1 1 d . . . N2 N 0.27076(16) 0.6111(3) 0.19602(19) 0.0514(9) Uani 1 1 d . . . N3 N 0.41435(12) 0.4425(2) 0.20653(17) 0.0405(7) Uani 1 1 d . . . N4 N 0.1879(2) 0.5023(5) -0.0106(3) 0.108(2) Uani 1 1 d . . . N5 N 0.3355(2) 0.3126(4) 0.0155(3) 0.0974(19) Uani 1 1 d . . . N6 N 0.24998(15) 0.3233(2) 0.1771(2) 0.0499(8) Uani 1 1 d . . . N7 N 0.50910(13) 0.5386(2) 0.18193(17) 0.0390(7) Uani 1 1 d . . . N8 N 0.50972(13) 0.3415(2) 0.18205(17) 0.0400(7) Uani 1 1 d . . . N9 N 0.50055(13) 0.4397(3) 0.08029(17) 0.0449(8) Uani 1 1 d . . . N10 N 0.22258(17) 0.7821(3) 0.1685(2) 0.0533(9) Uani 1 1 d . . . N11 N 0.32998(16) 0.7740(3) 0.2467(2) 0.0554(9) Uani 1 1 d . . . N12 N 0.19132(15) 0.6599(3) 0.2718(2) 0.0498(8) Uani 1 1 d . . . N13 N 0.29904(16) 0.6513(3) 0.3504(2) 0.0490(9) Uani 1 1 d . . . N14 N 0.38884(17) 0.6768(3) 0.3337(2) 0.0695(12) Uani 1 1 d . . . N15 N 0.13209(17) 0.7542(3) 0.1827(2) 0.0637(11) Uani 1 1 d . . . H7 H 0.543(2) 0.553(4) 0.188(3) 0.076 Uiso 1 1 d . . . H7A H 0.312(2) 0.756(4) 0.140(3) 0.076 Uiso 1 1 d . . . H7B H 0.339(2) 0.841(4) 0.168(3) 0.076 Uiso 1 1 d . . . H8 H 0.542(2) 0.332(4) 0.186(3) 0.076 Uiso 1 1 d . . . H8A H 0.267(2) 0.896(4) 0.198(3) 0.076 Uiso 1 1 d . . . H8B H 0.253(4) 0.848(7) 0.172(5) 0.076 Uiso 1 1 d . . . H9A H 0.185(2) 0.869(4) 0.210(3) 0.076 Uiso 1 1 d . . . H9B H 0.155(2) 0.842(4) 0.120(3) 0.076 Uiso 1 1 d . . . H10 H 0.216(2) 0.744(4) 0.136(3) 0.076 Uiso 1 1 d . . . H10A H 0.085(3) 0.668(5) 0.135(4) 0.096 Uiso 1 1 d . . . H10B H 0.143(3) 0.645(5) 0.123(3) 0.096 Uiso 1 1 d . . . H10C H 0.103(3) 0.720(4) 0.081(4) 0.096 Uiso 1 1 d . . . H11 H 0.339(2) 0.823(4) 0.277(3) 0.076 Uiso 1 1 d . . . H11A H 0.114(3) 0.697(4) 0.256(3) 0.076 Uiso 1 1 d . . . H11B H 0.145(2) 0.766(4) 0.298(3) 0.076 Uiso 1 1 d . . . H12 H 0.185(2) 0.616(4) 0.246(3) 0.076 Uiso 1 1 d . . . H12A H 0.181(2) 0.588(4) 0.352(3) 0.076 Uiso 1 1 d . . . H12B H 0.208(2) 0.668(4) 0.377(3) 0.076 Uiso 1 1 d . . . H13 H 0.305(2) 0.685(4) 0.380(3) 0.076 Uiso 1 1 d . . . H13A H 0.272(2) 0.560(4) 0.410(3) 0.076 Uiso 1 1 d . . . H13B H 0.259(2) 0.544(4) 0.323(3) 0.076 Uiso 1 1 d . . . H14A H 0.366(2) 0.592(4) 0.392(3) 0.076 Uiso 1 1 d . . . H14B H 0.344(2) 0.576(4) 0.317(3) 0.076 Uiso 1 1 d . . . H15A H 0.443(3) 0.733(5) 0.402(4) 0.096 Uiso 1 1 d . . . H15B H 0.416(3) 0.695(5) 0.437(4) 0.096 Uiso 1 1 d . . . H15C H 0.385(3) 0.778(5) 0.405(4) 0.096 Uiso 1 1 d . . . H16A H 0.366(2) 0.664(4) 0.226(3) 0.076 Uiso 1 1 d . . . H16B H 0.407(3) 0.731(4) 0.259(3) 0.076 Uiso 1 1 d . . . H17A H 0.450(2) 0.618(4) 0.192(3) 0.076 Uiso 1 1 d . . . H17B H 0.500(2) 0.665(4) 0.183(3) 0.076 Uiso 1 1 d . . . H18A H 0.512(2) 0.197(4) 0.187(3) 0.076 Uiso 1 1 d . . . H18B H 0.449(2) 0.268(4) 0.191(3) 0.076 Uiso 1 1 d . . . H19A H 0.445(2) 0.519(4) 0.101(3) 0.076 Uiso 1 1 d . . . H19B H 0.493(2) 0.570(4) 0.078(3) 0.076 Uiso 1 1 d . . . H20A H 0.488(2) 0.309(4) 0.072(3) 0.076 Uiso 1 1 d . . . H20B H 0.446(2) 0.362(4) 0.099(3) 0.076 Uiso 1 1 d . . . H21A H 0.558(3) 0.485(5) 0.043(4) 0.096 Uiso 1 1 d . . . H21B H 0.561(3) 0.382(5) 0.044(4) 0.096 Uiso 1 1 d . . . H21C H 0.577(3) 0.440(4) 0.122(4) 0.096 Uiso 1 1 d . . . C2 C 0.27964(16) 0.5589(3) 0.1587(2) 0.0383(8) Uani 1 1 d . . . C3 C 0.37201(14) 0.4508(2) 0.17007(19) 0.0335(7) Uani 1 1 d . . . C4 C 0.2291(2) 0.4869(3) 0.0264(2) 0.0575(12) Uani 1 1 d . . . C5 C 0.32090(19) 0.3714(4) 0.0422(2) 0.0597(13) Uani 1 1 d . . . C6 C 0.26618(15) 0.3756(3) 0.1468(2) 0.0399(8) Uani 1 1 d . . . C9 C 0.3158(3) 0.8071(4) 0.1726(3) 0.0705(15) Uani 1 1 d . . . C8 C 0.2621(4) 0.8488(5) 0.1567(5) 0.0718(18) Uani 1 1 d . . . C7 C 0.1694(2) 0.8179(4) 0.1693(3) 0.0631(13) Uani 1 1 d . . . C16 C 0.1152(3) 0.6900(6) 0.1264(4) 0.0873(19) Uani 1 1 d . . . C14 C 0.1432(2) 0.7184(4) 0.2533(3) 0.0612(13) Uani 1 1 d . . . C13 C 0.2053(2) 0.6251(4) 0.3449(3) 0.0618(12) Uani 1 1 d . . . C12 C 0.2601(2) 0.5850(3) 0.3600(3) 0.0615(12) Uani 1 1 d . . . C11 C 0.3520(2) 0.6153(4) 0.3484(3) 0.0643(14) Uani 1 1 d . . . C1 C 0.4083(3) 0.7388(7) 0.3902(4) 0.100(2) Uani 1 1 d . . . C10 C 0.3768(2) 0.7131(4) 0.2638(3) 0.0694(15) Uani 1 1 d . . . C17 C 0.48979(17) 0.6179(3) 0.2097(2) 0.0461(9) Uani 1 1 d . . . C18 C 0.49031(18) 0.2625(3) 0.2094(2) 0.0496(10) Uani 1 1 d . . . C19 C 0.48371(17) 0.5204(3) 0.1055(2) 0.0450(9) Uani 1 1 d . . . C20 C 0.48324(17) 0.3601(3) 0.1057(2) 0.0470(10) Uani 1 1 d . . . C21 C 0.55599(17) 0.4394(4) 0.0767(2) 0.0508(11) Uani 1 1 d . . . H20A H 0.1193(18) 0.487(3) 0.229(2) 0.046(12) Uiso 1 1 d . . . H20B H 0.138(3) 0.430(6) 0.135(5) 0.12(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0285(3) 0.0437(4) 0.0311(3) 0.000 0.0065(2) 0.000 Ni2 0.0454(3) 0.0344(3) 0.0433(3) -0.0015(2) 0.0164(2) 0.0121(2) Cr 0.0329(3) 0.0322(3) 0.0286(3) 0.0003(2) 0.0096(2) 0.0021(2) O1 0.105(4) 0.274(10) 0.193(7) 0.173(7) 0.079(5) 0.041(5) O2 0.167(7) 0.110(5) 0.195(8) 0.009(5) 0.020(6) 0.020(5) O3 0.248(14) 0.322(16) 0.331(18) 0.030(16) -0.035(12) -0.021(13) O4 0.200(9) 0.161(8) 0.262(11) 0.028(7) 0.079(8) 0.042(6) O5 0.44(2) 0.255(14) 0.193(11) 0.055(10) 0.054(13) 0.044(14) O6 0.230(8) 0.106(4) 0.075(3) 0.008(3) 0.049(4) 0.035(4) N1 0.063(3) 0.156(6) 0.061(3) 0.041(3) 0.031(2) 0.034(3) N2 0.063(2) 0.047(2) 0.0455(19) -0.0029(16) 0.0166(17) 0.0179(17) N3 0.0307(15) 0.051(2) 0.0378(17) 0.0006(14) 0.0054(13) -0.0016(13) N4 0.088(4) 0.125(5) 0.082(4) -0.012(4) -0.027(3) 0.020(4) N5 0.106(4) 0.126(5) 0.059(3) -0.033(3) 0.021(3) 0.037(4) N6 0.059(2) 0.041(2) 0.053(2) 0.0064(16) 0.0206(17) -0.0121(17) N7 0.0335(15) 0.049(2) 0.0338(16) 0.0027(14) 0.0085(13) 0.0022(14) N8 0.0345(15) 0.047(2) 0.0383(17) -0.0012(14) 0.0100(13) 0.0007(14) N9 0.0402(17) 0.062(2) 0.0338(16) -0.0003(15) 0.0119(14) 0.0026(15) N10 0.064(2) 0.045(2) 0.053(2) 0.0052(17) 0.0193(19) 0.0191(19) N11 0.056(2) 0.054(2) 0.062(2) -0.0068(19) 0.0267(19) 0.0023(18) N12 0.051(2) 0.048(2) 0.051(2) -0.0027(16) 0.0157(16) 0.0059(16) N13 0.056(2) 0.043(2) 0.046(2) -0.0028(15) 0.0100(17) 0.0111(16) N14 0.050(2) 0.089(3) 0.067(3) -0.013(2) 0.011(2) 0.016(2) N15 0.054(2) 0.067(3) 0.064(3) -0.006(2) 0.0025(19) 0.019(2) C2 0.0432(19) 0.036(2) 0.0366(19) 0.0010(16) 0.0121(16) 0.0052(15) C3 0.0348(18) 0.0346(19) 0.0340(17) -0.0003(14) 0.0141(15) -0.0018(14) C4 0.071(3) 0.059(3) 0.037(2) -0.005(2) 0.005(2) 0.005(2) C5 0.056(3) 0.089(4) 0.032(2) -0.005(2) 0.0082(18) 0.012(2) C6 0.0389(18) 0.038(2) 0.043(2) 0.0009(17) 0.0102(16) -0.0019(15) C9 0.083(4) 0.065(4) 0.074(4) 0.010(3) 0.041(3) -0.001(3) C8 0.097(5) 0.047(3) 0.082(5) 0.015(3) 0.043(3) 0.012(3) C7 0.066(3) 0.060(3) 0.060(3) 0.005(2) 0.009(2) 0.032(3) C16 0.076(4) 0.104(6) 0.072(4) -0.014(4) 0.001(3) 0.006(4) C14 0.044(2) 0.070(3) 0.072(3) -0.008(3) 0.020(2) 0.006(2) C13 0.064(3) 0.063(3) 0.062(3) 0.006(2) 0.023(2) -0.007(2) C12 0.083(3) 0.045(3) 0.055(3) 0.010(2) 0.014(3) 0.003(2) C11 0.061(3) 0.063(3) 0.063(3) -0.004(3) 0.005(2) 0.028(3) C1 0.066(4) 0.139(7) 0.090(5) -0.030(5) 0.014(4) -0.009(4) C10 0.044(2) 0.089(4) 0.080(4) -0.016(3) 0.025(3) 0.013(3) C17 0.044(2) 0.041(2) 0.055(2) 0.0048(19) 0.0159(18) 0.0043(17) C18 0.047(2) 0.051(3) 0.054(2) -0.004(2) 0.0179(19) -0.0039(19) C19 0.0383(19) 0.059(3) 0.036(2) 0.0063(18) 0.0067(16) 0.0071(18) C20 0.041(2) 0.061(3) 0.038(2) -0.0094(19) 0.0077(17) -0.0026(19) C21 0.040(2) 0.074(3) 0.038(2) 0.003(2) 0.0106(18) 0.004(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 Ni1 N7 2.067(3) 2_655 ? Ni1 N7 2.067(3) . ? Ni1 N8 2.070(3) . ? Ni1 N8 2.070(3) 2_655 ? Ni1 N3 2.153(3) 2_655 ? Ni1 N3 2.153(3) . ? Ni2 N10 2.048(4) . ? Ni2 N13 2.055(4) . ? Ni2 N11 2.063(4) . ? Ni2 N12 2.068(4) . ? Ni2 N6 2.103(3) 4 ? Ni2 N2 2.106(4) . ? Cr N1 1.868(6) . ? Cr C5 1.926(5) . ? Cr C4 1.968(5) . ? Cr C2 2.064(4) . ? Cr C6 2.075(4) . ? Cr C3 2.083(4) . ? O1 N1 1.166(8) . ? N2 C2 1.145(5) . ? N3 C3 1.145(5) . ? N4 C4 1.144(7) . ? N5 C5 1.154(7) . ? N6 C6 1.141(5) . ? N6 Ni2 2.103(3) 4_545 ? N7 C17 1.472(5) . ? N7 C19 1.489(5) . ? N8 C18 1.466(6) . ? N8 C20 1.493(5) . ? N9 C20 1.435(6) . ? N9 C19 1.442(6) . ? N9 C21 1.452(5) . ? N10 C7 1.484(6) . ? N10 C8 1.508(10) . ? N11 C9 1.483(7) . ? N11 C10 1.496(7) . ? N12 C13 1.475(6) . ? N12 C14 1.502(6) . ? N13 C12 1.478(7) . ? N13 C11 1.487(6) . ? N14 C11 1.421(8) . ? N14 C10 1.429(8) . ? N14 C1 1.443(9) . ? N15 C14 1.439(7) . ? N15 C7 1.444(8) . ? N15 C16 1.454(8) . ? C9 C8 1.483(10) . ? C13 C12 1.500(8) . ? C17 C17 1.521(9) 2_655 ? C18 C18 1.529(9) 2_655 ? 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 N7 Ni1 N7 85.72(19) 2_655 . ? N7 Ni1 N8 179.58(13) 2_655 . ? N7 Ni1 N8 94.20(13) . . ? N7 Ni1 N8 94.20(13) 2_655 2_655 ? N7 Ni1 N8 179.58(13) . 2_655 ? N8 Ni1 N8 85.89(19) . 2_655 ? N7 Ni1 N3 90.73(13) 2_655 2_655 ? N7 Ni1 N3 87.84(13) . 2_655 ? N8 Ni1 N3 88.86(13) . 2_655 ? N8 Ni1 N3 92.58(13) 2_655 2_655 ? N7 Ni1 N3 87.84(13) 2_655 . ? N7 Ni1 N3 90.73(13) . . ? N8 Ni1 N3 92.58(13) . . ? N8 Ni1 N3 88.86(13) 2_655 . ? N3 Ni1 N3 178.04(19) 2_655 . ? N10 Ni2 N13 179.42(16) . . ? N10 Ni2 N11 85.74(18) . . ? N13 Ni2 N11 94.32(17) . . ? N10 Ni2 N12 94.10(17) . . ? N13 Ni2 N12 85.84(16) . . ? N11 Ni2 N12 179.47(16) . . ? N10 Ni2 N6 91.37(16) . 4 ? N13 Ni2 N6 89.21(15) . 4 ? N11 Ni2 N6 89.77(16) . 4 ? N12 Ni2 N6 90.74(15) . 4 ? N10 Ni2 N2 88.42(15) . . ? N13 Ni2 N2 91.01(15) . . ? N11 Ni2 N2 90.64(16) . . ? N12 Ni2 N2 88.85(16) . . ? N6 Ni2 N2 179.52(16) 4 . ? N1 Cr C5 95.1(3) . . ? N1 Cr C4 91.4(2) . . ? C5 Cr C4 96.9(2) . . ? N1 Cr C2 90.6(2) . . ? C5 Cr C2 172.50(18) . . ? C4 Cr C2 87.76(18) . . ? N1 Cr C6 176.9(2) . . ? C5 Cr C6 87.4(2) . . ? C4 Cr C6 89.91(19) . . ? C2 Cr C6 86.66(16) . . ? N1 Cr C3 90.28(18) . . ? C5 Cr C3 87.64(17) . . ? C4 Cr C3 175.02(17) . . ? C2 Cr C3 87.55(15) . . ? C6 Cr C3 88.16(14) . . ? O1 N1 Cr 178.2(7) . . ? C2 N2 Ni2 172.8(4) . . ? C3 N3 Ni1 164.3(3) . . ? C6 N6 Ni2 166.3(4) . 4_545 ? C17 N7 C19 114.9(3) . . ? C17 N7 Ni1 105.4(2) . . ? C19 N7 Ni1 114.2(3) . . ? C18 N8 C20 114.2(3) . . ? C18 N8 Ni1 105.3(2) . . ? C20 N8 Ni1 113.3(3) . . ? C20 N9 C19 117.8(3) . . ? C20 N9 C21 114.5(4) . . ? C19 N9 C21 114.1(4) . . ? C7 N10 C8 114.6(5) . . ? C7 N10 Ni2 114.2(3) . . ? C8 N10 Ni2 105.7(4) . . ? C9 N11 C10 114.4(4) . . ? C9 N11 Ni2 105.2(3) . . ? C10 N11 Ni2 112.7(4) . . ? C13 N12 C14 115.4(4) . . ? C13 N12 Ni2 105.3(3) . . ? C14 N12 Ni2 113.9(3) . . ? C12 N13 C11 114.1(4) . . ? C12 N13 Ni2 105.0(3) . . ? C11 N13 Ni2 113.6(3) . . ? C11 N14 C10 117.4(5) . . ? C11 N14 C1 113.8(5) . . ? C10 N14 C1 114.5(6) . . ? C14 N15 C7 117.2(4) . . ? C14 N15 C16 114.0(5) . . ? C7 N15 C16 114.0(5) . . ? N2 C2 Cr 177.0(4) . . ? N3 C3 Cr 172.5(3) . . ? N4 C4 Cr 176.6(5) . . ? N5 C5 Cr 176.0(5) . . ? N6 C6 Cr 176.7(4) . . ? N11 C9 C8 109.4(5) . . ? C9 C8 N10 107.9(5) . . ? N15 C7 N10 114.4(4) . . ? N15 C14 N12 113.8(4) . . ? N12 C13 C12 108.6(4) . . ? N13 C12 C13 109.3(4) . . ? N14 C11 N13 115.3(4) . . ? N14 C10 N11 114.7(4) . . ? N7 C17 C17 108.7(3) . 2_655 ? N8 C18 C18 109.0(3) . 2_655 ? N9 C19 N7 114.1(3) . . ? N9 C20 N8 113.8(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.078 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.109