# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- CIF.CIF' #SUBMISSION DETAILS: _publ_contact_author ; Wen-Hua_Sun Institute_of_Chemistry Chinese_Academy_of_Sciences Beijing_100080 China ; loop_ _publ_author_name _publ_author_address 'Xiaohua Hou' ; Zhengguo_Cai College of Material Science and Engineering Donghua University Shanghai 201620 China ; 'Zhengguo Cai' ; Xia_Chen School_of_Chemistry_and_Chemical_Engineering Shanxi_University Taiyuan_030006 China ; 'Jiangang Yu' ; Wen-Hua_Sun Institute_of_Chemistry Chinese_Academy_of_Sciences Beijing_100190 China ; 'Lin Wang' Dalton_Transactions 'Xia Chen' '' 'Carl Redshaw' '' 'Wen Hua Sun' '' _publ_contact_author_name 'Wen-Hua Sun' _publ_contact_author_email whsun@iccas.ac.cn data_Ni2 _database_code_depnum_ccdc_archive 'CCDC 843822' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H64 Cl4 N4 Ni2 O2' _chemical_formula_weight 1156.39 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' 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' 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 P2(1)/n 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 14.895(3) _cell_length_b 15.229(3) _cell_length_c 15.550(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.64(3) _cell_angle_gamma 90.00 _cell_volume 3427.6(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7623 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7835 _exptl_absorpt_correction_T_max 0.8562 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 25336 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6266 _reflns_number_gt 5370 _reflns_threshold_expression >2sigma(I) __computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.0934P)^2^+4.5384P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6266 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0723 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1924 _refine_ls_wR_factor_gt 0.1859 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.61633(3) 0.00604(3) 0.04545(3) 0.03038(19) Uani 1 1 d . . . Cl2 Cl 0.47491(7) 0.06107(6) 0.08417(6) 0.0336(2) Uani 1 1 d . . . Cl1 Cl 0.60834(7) -0.12349(7) 0.13425(7) 0.0378(3) Uani 1 1 d . . . N2 N 0.7463(2) -0.0155(2) 0.0136(2) 0.0301(7) Uani 1 1 d . . . N1 N 0.7056(2) 0.0620(2) 0.1526(2) 0.0343(7) Uani 1 1 d . . . C5 C 0.7968(3) 0.0576(3) 0.1510(3) 0.0347(9) Uani 1 1 d . . . C9 C 0.8164(3) 0.0167(3) 0.0709(3) 0.0334(9) Uani 1 1 d . . . C15 C 0.7601(3) -0.1446(2) -0.0768(2) 0.0287(8) Uani 1 1 d . . . C19 C 0.8519(3) -0.2074(3) 0.0666(3) 0.0317(8) Uani 1 1 d . . . C13 C 0.7749(3) -0.1272(3) -0.2284(3) 0.0319(8) Uani 1 1 d . . . C12 C 0.7760(3) -0.0363(3) -0.2163(3) 0.0325(9) Uani 1 1 d . . . H12A H 0.7813 0.0006 -0.2641 0.039 Uiso 1 1 calc R . . C1 C 0.6847(3) 0.0955(3) 0.2242(3) 0.0445(11) Uani 1 1 d . . . H1A H 0.6214 0.0987 0.2259 0.053 Uiso 1 1 calc R . . C11 C 0.7697(3) 0.0023(2) -0.1365(3) 0.0317(9) Uani 1 1 d . . . C14 C 0.7671(3) -0.1793(3) -0.1587(3) 0.0320(8) Uani 1 1 d . . . H14A H 0.7663 -0.2413 -0.1661 0.038 Uiso 1 1 calc R . . C16 C 0.7713(3) 0.1008(3) -0.1282(3) 0.0416(10) Uani 1 1 d . . . H16A H 0.7665 0.1173 -0.0686 0.062 Uiso 1 1 calc R . . H16B H 0.7192 0.1258 -0.1719 0.062 Uiso 1 1 calc R . . H16C H 0.8294 0.1234 -0.1388 0.062 Uiso 1 1 calc R . . C30 C 0.6172(3) -0.3010(3) -0.0372(3) 0.0444(10) Uani 1 1 d . . . H30A H 0.5806 -0.2507 -0.0337 0.053 Uiso 1 1 calc R . . C18 C 0.7567(3) -0.2023(3) 0.0019(3) 0.0328(8) Uani 1 1 d . . . H18A H 0.7151 -0.1717 0.0343 0.039 Uiso 1 1 calc R . . C4 C 0.8665(3) 0.0880(3) 0.2193(3) 0.0416(10) Uani 1 1 d . . . C8 C 0.9147(3) 0.0148(3) 0.0653(3) 0.0385(9) Uani 1 1 d . . . H8A H 0.9173 0.0185 0.0024 0.046 Uiso 1 1 calc R . . H8B H 0.9424 -0.0420 0.0888 0.046 Uiso 1 1 calc R . . C17 C 0.7806(3) -0.1658(3) -0.3154(3) 0.0421(10) Uani 1 1 d . . . H17A H 0.7787 -0.2300 -0.3119 0.063 Uiso 1 1 calc R . . H17B H 0.8385 -0.1476 -0.3296 0.063 Uiso 1 1 calc R . . H17C H 0.7283 -0.1452 -0.3617 0.063 Uiso 1 1 calc R . . C6 C 0.9654(3) 0.0860(4) 0.2128(3) 0.0532(12) Uani 1 1 d . . . H6A H 0.9953 0.0317 0.2409 0.064 Uiso 1 1 calc R . . H6B H 0.9988 0.1369 0.2448 0.064 Uiso 1 1 calc R . . C25 C 0.7146(3) -0.2923(3) -0.0227(2) 0.0331(9) Uani 1 1 d . . . C24 C 0.9316(3) -0.2269(3) 0.0379(3) 0.0431(10) Uani 1 1 d . . . H24A H 0.9281 -0.2353 -0.0233 0.052 Uiso 1 1 calc R . . C21 C 0.9433(4) -0.2004(4) 0.2172(3) 0.0595(14) Uani 1 1 d . . . H21A H 0.9473 -0.1904 0.2783 0.071 Uiso 1 1 calc R . . C7 C 0.9714(3) 0.0888(3) 0.1160(3) 0.0508(12) Uani 1 1 d . . . H7A H 0.9479 0.1459 0.0895 0.061 Uiso 1 1 calc R . . H7B H 1.0367 0.0829 0.1125 0.061 Uiso 1 1 calc R . . C29 C 0.5754(4) -0.3815(3) -0.0563(4) 0.0543(13) Uani 1 1 d . . . H29A H 0.5101 -0.3862 -0.0670 0.065 Uiso 1 1 calc R . . C23 C 1.0153(3) -0.2341(3) 0.0984(4) 0.0512(12) Uani 1 1 d . . . H23A H 1.0690 -0.2474 0.0780 0.061 Uiso 1 1 calc R . . C27 C 0.7229(4) -0.4494(3) -0.0494(3) 0.0515(12) Uani 1 1 d . . . H27A H 0.7588 -0.4995 -0.0556 0.062 Uiso 1 1 calc R . . C28 C 0.6282(4) -0.4560(3) -0.0600(3) 0.0538(13) Uani 1 1 d . . . H28A H 0.5992 -0.5118 -0.0699 0.065 Uiso 1 1 calc R . . C3 C 0.8407(3) 0.1232(3) 0.2939(3) 0.0480(11) Uani 1 1 d . . . H3A H 0.8865 0.1451 0.3424 0.058 Uiso 1 1 calc R . . C2 C 0.7496(4) 0.1258(3) 0.2962(3) 0.0490(12) Uani 1 1 d . . . H2A H 0.7314 0.1481 0.3466 0.059 Uiso 1 1 calc R . . C20 C 0.8591(3) -0.1934(3) 0.1566(3) 0.0444(10) Uani 1 1 d . . . H20A H 0.8055 -0.1788 0.1766 0.053 Uiso 1 1 calc R . . C22 C 1.0232(4) -0.2226(4) 0.1879(4) 0.0576(13) Uani 1 1 d . . . H22A H 1.0811 -0.2294 0.2289 0.069 Uiso 1 1 calc R . . C10 C 0.7597(3) -0.0533(3) -0.0671(2) 0.0291(8) Uani 1 1 d . . . C26 C 0.7641(3) -0.3675(3) -0.0293(3) 0.0393(10) Uani 1 1 d . . . H26A H 0.8294 -0.3633 -0.0196 0.047 Uiso 1 1 calc R . . O1 O 0.6003(2) 0.12107(19) -0.0355(2) 0.0386(7) Uani 1 1 d . . . H93 H 0.5388 0.1144 -0.0572 0.10(3) Uiso 1 1 d R . . C31 C 0.6155(4) 0.2061(3) 0.0028(4) 0.0536(12) Uani 1 1 d . . . H31A H 0.6043 0.2504 -0.0442 0.080 Uiso 1 1 calc R . . H31B H 0.6795 0.2106 0.0374 0.080 Uiso 1 1 calc R . . H31C H 0.5733 0.2157 0.0416 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0296(3) 0.0326(3) 0.0300(3) -0.00320(19) 0.0093(2) -0.00074(19) Cl2 0.0331(5) 0.0365(5) 0.0328(5) -0.0043(4) 0.0109(4) -0.0009(4) Cl1 0.0393(6) 0.0411(6) 0.0345(5) 0.0021(4) 0.0119(4) 0.0032(4) N2 0.0309(17) 0.0299(16) 0.0302(17) -0.0031(13) 0.0083(14) 0.0008(13) N1 0.0350(18) 0.0383(18) 0.0324(18) -0.0055(14) 0.0134(14) -0.0004(14) C5 0.038(2) 0.037(2) 0.031(2) -0.0046(17) 0.0110(17) -0.0033(17) C9 0.037(2) 0.0313(19) 0.032(2) -0.0022(16) 0.0092(17) -0.0010(16) C15 0.031(2) 0.0290(19) 0.0261(18) -0.0002(15) 0.0066(15) 0.0015(15) C19 0.034(2) 0.0319(19) 0.0288(19) 0.0021(15) 0.0068(16) -0.0006(16) C13 0.031(2) 0.036(2) 0.028(2) -0.0008(16) 0.0058(16) -0.0010(16) C12 0.037(2) 0.0286(19) 0.033(2) 0.0050(16) 0.0092(17) -0.0008(16) C1 0.047(3) 0.051(3) 0.036(2) -0.010(2) 0.012(2) 0.003(2) C11 0.032(2) 0.032(2) 0.032(2) 0.0003(15) 0.0092(17) 0.0012(15) C14 0.034(2) 0.031(2) 0.031(2) -0.0039(16) 0.0070(16) -0.0006(16) C16 0.054(3) 0.034(2) 0.043(2) -0.0004(18) 0.023(2) -0.0020(19) C30 0.042(2) 0.043(2) 0.048(3) 0.001(2) 0.011(2) -0.0005(19) C18 0.039(2) 0.031(2) 0.031(2) 0.0015(16) 0.0136(17) 0.0028(16) C4 0.041(2) 0.046(2) 0.037(2) -0.0048(19) 0.0055(19) -0.0014(19) C8 0.035(2) 0.040(2) 0.040(2) -0.0049(18) 0.0090(18) -0.0001(17) C17 0.056(3) 0.037(2) 0.035(2) -0.0054(18) 0.016(2) -0.0039(19) C6 0.044(3) 0.068(3) 0.044(3) -0.011(2) 0.003(2) -0.006(2) C25 0.045(2) 0.029(2) 0.0254(19) -0.0003(15) 0.0094(17) -0.0026(17) C24 0.046(3) 0.040(2) 0.045(2) 0.0043(19) 0.014(2) 0.0023(19) C21 0.061(3) 0.074(4) 0.039(3) 0.005(2) 0.005(2) -0.004(3) C7 0.038(3) 0.056(3) 0.058(3) -0.009(2) 0.010(2) -0.003(2) C29 0.050(3) 0.052(3) 0.057(3) 0.002(2) 0.006(2) -0.016(2) C23 0.038(3) 0.054(3) 0.062(3) 0.008(2) 0.012(2) 0.002(2) C27 0.070(3) 0.040(3) 0.043(3) -0.002(2) 0.010(2) -0.001(2) C28 0.072(4) 0.039(2) 0.048(3) -0.003(2) 0.009(2) -0.013(2) C3 0.046(3) 0.060(3) 0.037(2) -0.009(2) 0.007(2) -0.004(2) C2 0.058(3) 0.055(3) 0.036(2) -0.009(2) 0.016(2) 0.000(2) C20 0.045(3) 0.052(3) 0.035(2) 0.000(2) 0.0078(19) 0.002(2) C22 0.047(3) 0.070(3) 0.049(3) 0.007(3) -0.001(2) -0.001(2) C10 0.0274(19) 0.0316(19) 0.030(2) -0.0026(15) 0.0101(15) -0.0002(15) C26 0.047(2) 0.038(2) 0.034(2) 0.0012(17) 0.0117(19) 0.0024(18) O1 0.0379(17) 0.0379(16) 0.0419(17) 0.0000(12) 0.0131(13) -0.0009(12) C31 0.057(3) 0.042(3) 0.065(3) -0.005(2) 0.020(2) -0.003(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 N1 2.056(3) . ? Ni1 N2 2.134(3) . ? Ni1 O1 2.137(3) . ? Ni1 Cl2 2.3794(12) 3_655 ? Ni1 Cl1 2.4268(12) . ? Ni1 Cl2 2.4696(12) . ? Cl2 Ni1 2.3794(12) 3_655 ? N2 C9 1.300(5) . ? N2 C10 1.436(5) . ? N1 C1 1.327(5) . ? N1 C5 1.366(5) . ? C5 C4 1.380(6) . ? C5 C9 1.481(6) . ? C9 C8 1.487(6) . ? C15 C10 1.399(5) . ? C15 C14 1.406(5) . ? C15 C18 1.516(5) . ? C19 C20 1.394(6) . ? C19 C24 1.395(6) . ? C19 C18 1.535(6) . ? C13 C14 1.369(6) . ? C13 C12 1.396(6) . ? C13 C17 1.496(6) . ? C12 C11 1.396(6) . ? C12 H12A 0.9500 . ? C1 C2 1.374(7) . ? C1 H1A 0.9500 . ? C11 C10 1.407(5) . ? C11 C16 1.506(6) . ? C14 H14A 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C30 C29 1.375(7) . ? C30 C25 1.420(6) . ? C30 H30A 0.9500 . ? C18 C25 1.518(5) . ? C18 H18A 1.0000 . ? C4 C3 1.411(6) . ? C4 C6 1.500(7) . ? C8 C7 1.514(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C6 C7 1.529(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C25 C26 1.380(6) . ? C24 C23 1.378(7) . ? C24 H24A 0.9500 . ? C21 C20 1.383(7) . ? C21 C22 1.412(8) . ? C21 H21A 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C29 C28 1.390(8) . ? C29 H29A 0.9500 . ? C23 C22 1.380(7) . ? C23 H23A 0.9500 . ? C27 C28 1.383(8) . ? C27 C26 1.393(7) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C3 C2 1.366(7) . ? C3 H3A 0.9500 . ? C2 H2A 0.9500 . ? C20 H20A 0.9500 . ? C22 H22A 0.9500 . ? C26 H26A 0.9500 . ? O1 C31 1.420(6) . ? O1 H93 0.9044 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 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 N1 Ni1 N2 78.66(13) . . ? N1 Ni1 O1 95.66(13) . . ? N2 Ni1 O1 88.33(12) . . ? N1 Ni1 Cl2 174.69(10) . 3_655 ? N2 Ni1 Cl2 96.05(9) . 3_655 ? O1 Ni1 Cl2 83.74(9) . 3_655 ? N1 Ni1 Cl1 89.14(10) . . ? N2 Ni1 Cl1 100.14(9) . . ? O1 Ni1 Cl1 170.97(9) . . ? Cl2 Ni1 Cl1 92.17(4) 3_655 . ? N1 Ni1 Cl2 95.02(10) . . ? N2 Ni1 Cl2 168.93(9) . . ? O1 Ni1 Cl2 83.23(9) . . ? Cl2 Ni1 Cl2 90.15(4) 3_655 . ? Cl1 Ni1 Cl2 88.74(4) . . ? Ni1 Cl2 Ni1 89.85(4) 3_655 . ? C9 N2 C10 119.7(3) . . ? C9 N2 Ni1 114.2(3) . . ? C10 N2 Ni1 125.8(2) . . ? C1 N1 C5 117.8(4) . . ? C1 N1 Ni1 127.2(3) . . ? C5 N1 Ni1 114.8(3) . . ? N1 C5 C4 122.7(4) . . ? N1 C5 C9 115.6(3) . . ? C4 C5 C9 121.8(4) . . ? N2 C9 C5 116.7(4) . . ? N2 C9 C8 126.5(4) . . ? C5 C9 C8 116.8(4) . . ? C10 C15 C14 118.3(4) . . ? C10 C15 C18 119.2(3) . . ? C14 C15 C18 122.5(3) . . ? C20 C19 C24 118.9(4) . . ? C20 C19 C18 119.5(4) . . ? C24 C19 C18 121.7(4) . . ? C14 C13 C12 117.9(4) . . ? C14 C13 C17 121.4(4) . . ? C12 C13 C17 120.7(4) . . ? C11 C12 C13 122.4(4) . . ? C11 C12 H12A 118.8 . . ? C13 C12 H12A 118.8 . . ? N1 C1 C2 123.5(4) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C12 C11 C10 118.0(3) . . ? C12 C11 C16 119.5(4) . . ? C10 C11 C16 122.5(4) . . ? C13 C14 C15 122.5(4) . . ? C13 C14 H14A 118.8 . . ? C15 C14 H14A 118.8 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C29 C30 C25 120.7(4) . . ? C29 C30 H30A 119.6 . . ? C25 C30 H30A 119.6 . . ? C15 C18 C25 114.2(3) . . ? C15 C18 C19 110.9(3) . . ? C25 C18 C19 112.5(3) . . ? C15 C18 H18A 106.2 . . ? C25 C18 H18A 106.2 . . ? C19 C18 H18A 106.2 . . ? C5 C4 C3 117.3(4) . . ? C5 C4 C6 120.9(4) . . ? C3 C4 C6 121.8(4) . . ? C9 C8 C7 113.0(4) . . ? C9 C8 H8A 109.0 . . ? C7 C8 H8A 109.0 . . ? C9 C8 H8B 109.0 . . ? C7 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C6 C7 110.7(4) . . ? C4 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C26 C25 C30 117.1(4) . . ? C26 C25 C18 124.9(4) . . ? C30 C25 C18 118.1(4) . . ? C23 C24 C19 120.0(4) . . ? C23 C24 H24A 120.0 . . ? C19 C24 H24A 120.0 . . ? C20 C21 C22 119.7(5) . . ? C20 C21 H21A 120.1 . . ? C22 C21 H21A 120.1 . . ? C8 C7 C6 109.6(4) . . ? C8 C7 H7A 109.7 . . ? C6 C7 H7A 109.7 . . ? C8 C7 H7B 109.7 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C30 C29 C28 120.3(5) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C24 C23 C22 121.8(5) . . ? C24 C23 H23A 119.1 . . ? C22 C23 H23A 119.1 . . ? C28 C27 C26 118.4(5) . . ? C28 C27 H27A 120.8 . . ? C26 C27 H27A 120.8 . . ? C27 C28 C29 120.4(5) . . ? C27 C28 H28A 119.8 . . ? C29 C28 H28A 119.8 . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C3 C2 C1 118.8(4) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C21 C20 C19 121.0(5) . . ? C21 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? C23 C22 C21 118.6(5) . . ? C23 C22 H22A 120.7 . . ? C21 C22 H22A 120.7 . . ? C15 C10 C11 120.8(3) . . ? C15 C10 N2 119.8(3) . . ? C11 C10 N2 119.3(3) . . ? C25 C26 C27 123.0(4) . . ? C25 C26 H26A 118.5 . . ? C27 C26 H26A 118.5 . . ? C31 O1 Ni1 121.0(3) . . ? C31 O1 H93 107.9 . . ? Ni1 O1 H93 95.2 . . ? O1 C31 H31A 109.5 . . ? O1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 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 N1 Ni1 Cl2 Ni1 178.80(10) . . . 3_655 ? N2 Ni1 Cl2 Ni1 124.2(5) . . . 3_655 ? O1 Ni1 Cl2 Ni1 83.68(9) . . . 3_655 ? Cl2 Ni1 Cl2 Ni1 0.0 3_655 . . 3_655 ? Cl1 Ni1 Cl2 Ni1 -92.17(4) . . . 3_655 ? N1 Ni1 N2 C9 -1.9(3) . . . . ? O1 Ni1 N2 C9 94.2(3) . . . . ? Cl2 Ni1 N2 C9 177.7(3) 3_655 . . . ? Cl1 Ni1 N2 C9 -89.0(3) . . . . ? Cl2 Ni1 N2 C9 54.0(6) . . . . ? N1 Ni1 N2 C10 -175.5(3) . . . . ? O1 Ni1 N2 C10 -79.4(3) . . . . ? Cl2 Ni1 N2 C10 4.1(3) 3_655 . . . ? Cl1 Ni1 N2 C10 97.4(3) . . . . ? Cl2 Ni1 N2 C10 -119.6(5) . . . . ? N2 Ni1 N1 C1 -175.3(4) . . . . ? O1 Ni1 N1 C1 97.5(4) . . . . ? Cl2 Ni1 N1 C1 -179(47) 3_655 . . . ? Cl1 Ni1 N1 C1 -74.8(4) . . . . ? Cl2 Ni1 N1 C1 13.9(4) . . . . ? N2 Ni1 N1 C5 -0.4(3) . . . . ? O1 Ni1 N1 C5 -87.6(3) . . . . ? Cl2 Ni1 N1 C5 -4.4(13) 3_655 . . . ? Cl1 Ni1 N1 C5 100.1(3) . . . . ? Cl2 Ni1 N1 C5 -171.3(3) . . . . ? C1 N1 C5 C4 -1.5(6) . . . . ? Ni1 N1 C5 C4 -176.9(3) . . . . ? C1 N1 C5 C9 177.9(4) . . . . ? Ni1 N1 C5 C9 2.5(5) . . . . ? C10 N2 C9 C5 177.8(3) . . . . ? Ni1 N2 C9 C5 3.8(5) . . . . ? C10 N2 C9 C8 -3.8(6) . . . . ? Ni1 N2 C9 C8 -177.8(3) . . . . ? N1 C5 C9 N2 -4.3(5) . . . . ? C4 C5 C9 N2 175.1(4) . . . . ? N1 C5 C9 C8 177.2(4) . . . . ? C4 C5 C9 C8 -3.5(6) . . . . ? C14 C13 C12 C11 0.1(6) . . . . ? C17 C13 C12 C11 179.2(4) . . . . ? C5 N1 C1 C2 0.1(7) . . . . ? Ni1 N1 C1 C2 174.8(4) . . . . ? C13 C12 C11 C10 -1.4(6) . . . . ? C13 C12 C11 C16 -180.0(4) . . . . ? C12 C13 C14 C15 0.1(6) . . . . ? C17 C13 C14 C15 -179.0(4) . . . . ? C10 C15 C14 C13 1.0(6) . . . . ? C18 C15 C14 C13 -176.6(4) . . . . ? C10 C15 C18 C25 153.5(4) . . . . ? C14 C15 C18 C25 -28.9(5) . . . . ? C10 C15 C18 C19 -78.1(4) . . . . ? C14 C15 C18 C19 99.5(4) . . . . ? C20 C19 C18 C15 131.2(4) . . . . ? C24 C19 C18 C15 -49.7(5) . . . . ? C20 C19 C18 C25 -99.5(4) . . . . ? C24 C19 C18 C25 79.6(5) . . . . ? N1 C5 C4 C3 1.3(7) . . . . ? C9 C5 C4 C3 -178.0(4) . . . . ? N1 C5 C4 C6 -176.9(4) . . . . ? C9 C5 C4 C6 3.8(7) . . . . ? N2 C9 C8 C7 154.2(4) . . . . ? C5 C9 C8 C7 -27.4(6) . . . . ? C5 C4 C6 C7 26.1(7) . . . . ? C3 C4 C6 C7 -152.1(5) . . . . ? C29 C30 C25 C26 0.4(7) . . . . ? C29 C30 C25 C18 -177.4(4) . . . . ? C15 C18 C25 C26 95.1(5) . . . . ? C19 C18 C25 C26 -32.4(5) . . . . ? C15 C18 C25 C30 -87.2(4) . . . . ? C19 C18 C25 C30 145.2(4) . . . . ? C20 C19 C24 C23 1.5(7) . . . . ? C18 C19 C24 C23 -177.6(4) . . . . ? C9 C8 C7 C6 56.7(5) . . . . ? C4 C6 C7 C8 -55.2(6) . . . . ? C25 C30 C29 C28 1.2(8) . . . . ? C19 C24 C23 C22 0.1(8) . . . . ? C26 C27 C28 C29 4.1(8) . . . . ? C30 C29 C28 C27 -3.5(8) . . . . ? C5 C4 C3 C2 0.2(7) . . . . ? C6 C4 C3 C2 178.4(5) . . . . ? C4 C3 C2 C1 -1.5(8) . . . . ? N1 C1 C2 C3 1.4(8) . . . . ? C22 C21 C20 C19 -0.4(8) . . . . ? C24 C19 C20 C21 -1.3(7) . . . . ? C18 C19 C20 C21 177.7(4) . . . . ? C24 C23 C22 C21 -1.8(8) . . . . ? C20 C21 C22 C23 1.9(8) . . . . ? C14 C15 C10 C11 -2.4(6) . . . . ? C18 C15 C10 C11 175.3(3) . . . . ? C14 C15 C10 N2 175.7(3) . . . . ? C18 C15 C10 N2 -6.6(5) . . . . ? C12 C11 C10 C15 2.6(6) . . . . ? C16 C11 C10 C15 -178.9(4) . . . . ? C12 C11 C10 N2 -175.5(3) . . . . ? C16 C11 C10 N2 3.0(6) . . . . ? C9 N2 C10 C15 103.8(4) . . . . ? Ni1 N2 C10 C15 -82.9(4) . . . . ? C9 N2 C10 C11 -78.1(5) . . . . ? Ni1 N2 C10 C11 95.2(4) . . . . ? C30 C25 C26 C27 0.2(6) . . . . ? C18 C25 C26 C27 177.9(4) . . . . ? C28 C27 C26 C25 -2.5(7) . . . . ? N1 Ni1 O1 C31 -24.3(3) . . . . ? N2 Ni1 O1 C31 -102.7(3) . . . . ? Cl2 Ni1 O1 C31 161.0(3) 3_655 . . . ? Cl1 Ni1 O1 C31 97.5(6) . . . . ? Cl2 Ni1 O1 C31 70.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.571 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.173 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.000 475.8 174.1 2 0.035 0.131 0.411 8.6 3.0 3 0.500 0.000 0.500 475.9 174.3 4 0.465 0.631 0.090 8.6 2.3 5 0.535 0.369 0.910 8.9 3.2 6 0.965 0.869 0.590 8.9 2.3 _platon_squeeze_details ; ? ; #==END data_Ni3 _database_code_depnum_ccdc_archive 'CCDC 843823' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H82 Cl4 N4 Ni2 O2' _chemical_formula_weight 1486.80 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' 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' 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 P2(1)/c 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 16.059 _cell_length_b 17.764 _cell_length_c 15.868 _cell_angle_alpha 90.00 _cell_angle_beta 108.03 _cell_angle_gamma 90.00 _cell_volume 4304.0 _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10806 _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 25.34 _exptl_crystal_description Prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2100 _exptl_crystal_size_mid 0.1800 _exptl_crystal_size_min 0.0600 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1556 _exptl_absorpt_coefficient_mu 0.607 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_absorpt_correction_T_min 0.5993 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 17249 _diffrn_reflns_av_R_equivalents 0.0826 _diffrn_reflns_av_sigmaI/netI 0.1137 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.34 _reflns_number_total 7802 _reflns_number_gt 5175 _reflns_threshold_expression >2sigma(I) __computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.1317P)^2^+13.8917P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7802 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.1398 _refine_ls_R_factor_gt 0.1030 _refine_ls_wR_factor_ref 0.2920 _refine_ls_wR_factor_gt 0.2662 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.41295(6) 0.54953(5) 0.93123(6) 0.0319(3) Uani 1 1 d . . . Cl2 Cl 0.42528(11) 0.43587(9) 1.01425(12) 0.0356(4) Uani 1 1 d . . . O1 O 0.4441(3) 0.4796(3) 0.8344(3) 0.0380(12) Uani 1 1 d . . . Cl1 Cl 0.40242(12) 0.62885(10) 1.04977(12) 0.0408(5) Uani 1 1 d . . . N2 N 0.2752(3) 0.5364(3) 0.8633(4) 0.0301(12) Uani 1 1 d . . . C11 C 0.1824(4) 0.4832(4) 0.9439(4) 0.0301(15) Uani 1 1 d . . . N1 N 0.3891(4) 0.6402(3) 0.8464(4) 0.0382(14) Uani 1 1 d . . . C9 C 0.2453(4) 0.5867(4) 0.8036(4) 0.0316(15) Uani 1 1 d . . . C12 C 0.1361(5) 0.4214(4) 0.9621(5) 0.0382(17) Uani 1 1 d . . . H12A H 0.1096 0.4256 1.0078 0.046 Uiso 1 1 calc R . . C19 C 0.1839(5) 0.5486(4) 1.0894(5) 0.0374(16) Uani 1 1 d . . . C14 C 0.1665(5) 0.3492(4) 0.8498(5) 0.0425(18) Uani 1 1 d . . . H14A H 0.1604 0.3038 0.8169 0.051 Uiso 1 1 calc R . . C15 C 0.2144(4) 0.4083(4) 0.8300(4) 0.0347(16) Uani 1 1 d . . . C17 C 0.1879(4) 0.5576(4) 0.9944(5) 0.0326(15) Uani 1 1 d . . . H17A H 0.2465 0.5799 0.9995 0.039 Uiso 1 1 calc R . . C18 C 0.2567(5) 0.3985(4) 0.7551(5) 0.0389(17) Uani 1 1 d . . . H18A H 0.3079 0.4336 0.7696 0.047 Uiso 1 1 calc R . . C10 C 0.2216(4) 0.4763(3) 0.8765(4) 0.0274(14) Uani 1 1 d . . . C16 C 0.0755(5) 0.2896(4) 0.9349(6) 0.0454(19) Uani 1 1 d . . . H16A H 0.0759 0.2476 0.8950 0.068 Uiso 1 1 calc R . . H16B H 0.0150 0.3058 0.9258 0.068 Uiso 1 1 calc R . . H16C H 0.1017 0.2734 0.9965 0.068 Uiso 1 1 calc R . . C36 C 0.1081(7) 0.4060(6) 0.6339(6) 0.065(3) Uani 1 1 d . . . H36A H 0.0803 0.3862 0.6739 0.077 Uiso 1 1 calc R . . C5 C 0.3053(5) 0.6475(4) 0.7947(5) 0.0397(17) Uani 1 1 d . . . C37 C 0.2940(5) 0.3189(4) 0.7519(5) 0.0407(17) Uani 1 1 d . . . C25 C 0.1191(5) 0.6142(4) 0.9412(5) 0.0395(17) Uani 1 1 d . . . C24 C 0.2533(6) 0.5120(5) 1.1498(6) 0.054(2) Uani 1 1 d . . . H24A H 0.2998 0.4920 1.1314 0.065 Uiso 1 1 calc R . . C8 C 0.1512(5) 0.5925(5) 0.7432(5) 0.0453(19) Uani 1 1 d . . . H8A H 0.1285 0.5411 0.7259 0.054 Uiso 1 1 calc R . . H8B H 0.1151 0.6155 0.7768 0.054 Uiso 1 1 calc R . . C13 C 0.1280(4) 0.3548(4) 0.9155(5) 0.0377(17) Uani 1 1 d . . . C20 C 0.1163(6) 0.5754(5) 1.1154(6) 0.052(2) Uani 1 1 d . . . H20A H 0.0681 0.5998 1.0740 0.062 Uiso 1 1 calc R . . C4 C 0.2760(6) 0.7074(5) 0.7343(6) 0.052(2) Uani 1 1 d . . . C31 C 0.1973(6) 0.4217(4) 0.6637(5) 0.0464(19) Uani 1 1 d . . . C6 C 0.1827(6) 0.7135(5) 0.6781(7) 0.065(3) Uani 1 1 d . . . H6A H 0.1796 0.7376 0.6209 0.078 Uiso 1 1 calc R . . H6B H 0.1503 0.7457 0.7082 0.078 Uiso 1 1 calc R . . C26 C 0.1420(7) 0.6882(5) 0.9389(6) 0.061(2) Uani 1 1 d . . . H26A H 0.1999 0.7043 0.9697 0.073 Uiso 1 1 calc R . . C42 C 0.3699(5) 0.3004(5) 0.8136(6) 0.051(2) Uani 1 1 d . . . H42A H 0.3973 0.3356 0.8588 0.061 Uiso 1 1 calc R . . C39 C 0.2939(9) 0.2004(6) 0.6839(8) 0.081(3) Uani 1 1 d . . . H39A H 0.2652 0.1647 0.6399 0.097 Uiso 1 1 calc R . . C38 C 0.2557(7) 0.2696(5) 0.6837(6) 0.063(3) Uani 1 1 d . . . H38A H 0.2042 0.2831 0.6377 0.076 Uiso 1 1 calc R . . C7 C 0.1409(6) 0.6376(5) 0.6612(6) 0.060(2) Uani 1 1 d . . . H7A H 0.1667 0.6092 0.6217 0.072 Uiso 1 1 calc R . . H7B H 0.0776 0.6440 0.6297 0.072 Uiso 1 1 calc R . . C1 C 0.4472(5) 0.6928(5) 0.8457(6) 0.055(2) Uani 1 1 d . . . H1A H 0.5052 0.6890 0.8852 0.066 Uiso 1 1 calc R . . C2 C 0.4241(6) 0.7547(5) 0.7870(7) 0.064(3) Uani 1 1 d . . . H2A H 0.4659 0.7920 0.7853 0.076 Uiso 1 1 calc R . . C23 C 0.2543(7) 0.5048(6) 1.2380(6) 0.069(3) Uani 1 1 d . . . H23A H 0.3031 0.4814 1.2796 0.083 Uiso 1 1 calc R . . C30 C 0.0332(6) 0.5930(6) 0.8951(6) 0.064(3) Uani 1 1 d . . . H30A H 0.0152 0.5422 0.8968 0.077 Uiso 1 1 calc R . . C35 C 0.0594(8) 0.4191(6) 0.5469(7) 0.083(3) Uani 1 1 d . . . H35A H -0.0017 0.4091 0.5274 0.099 Uiso 1 1 calc R . . C3 C 0.3409(7) 0.7589(6) 0.7336(7) 0.076(3) Uani 1 1 d . . . H3A H 0.3255 0.7996 0.6929 0.092 Uiso 1 1 calc R . . C40 C 0.3676(8) 0.1818(6) 0.7419(9) 0.080(3) Uani 1 1 d . . . H40A H 0.3938 0.1348 0.7367 0.096 Uiso 1 1 calc R . . C22 C 0.1865(8) 0.5308(6) 1.2659(7) 0.072(3) Uani 1 1 d . . . H22A H 0.1871 0.5241 1.3254 0.087 Uiso 1 1 calc R . . C27 C 0.0788(9) 0.7409(6) 0.8903(8) 0.088(4) Uani 1 1 d . . . H27A H 0.0932 0.7928 0.8905 0.105 Uiso 1 1 calc R . . C21 C 0.1185(7) 0.5665(6) 1.2061(7) 0.070(3) Uani 1 1 d . . . H21A H 0.0718 0.5858 1.2246 0.084 Uiso 1 1 calc R . . C32 C 0.2323(7) 0.4535(6) 0.6033(6) 0.063(2) Uani 1 1 d . . . H32A H 0.2928 0.4662 0.6216 0.076 Uiso 1 1 calc R . . C41 C 0.4093(7) 0.2302(6) 0.8123(9) 0.081(3) Uani 1 1 d . . . H41 H 0.4616 0.2160 0.8570 0.097 Uiso 1 1 calc R . . C34 C 0.0995(9) 0.4463(7) 0.4889(7) 0.086(4) Uani 1 1 d . . . H34A H 0.0677 0.4502 0.4276 0.103 Uiso 1 1 calc R . . C29 C -0.0251(7) 0.6457(6) 0.8474(6) 0.068(3) Uani 1 1 d . . . H29A H -0.0834 0.6308 0.8164 0.082 Uiso 1 1 calc R . . C28 C -0.0018(8) 0.7165(7) 0.8438(7) 0.079(3) Uani 1 1 d . . . H28A H -0.0427 0.7510 0.8077 0.095 Uiso 1 1 calc R . . C44 C 0.5045(7) 0.4508(5) 0.7150(6) 0.066(3) Uani 1 1 d . . . H44A H 0.5246 0.4736 0.6684 0.099 Uiso 1 1 calc R . . H44B H 0.4553 0.4169 0.6879 0.099 Uiso 1 1 calc R . . H44D H 0.5526 0.4222 0.7555 0.099 Uiso 1 1 calc R . . C43 C 0.4748(6) 0.5128(5) 0.7665(5) 0.051(2) Uani 1 1 d . . . H43A H 0.5243 0.5472 0.7940 0.061 Uiso 1 1 calc R . . H43C H 0.4271 0.5426 0.7255 0.061 Uiso 1 1 calc R . . C33 C 0.1832(9) 0.4673(6) 0.5182(7) 0.079(3) Uani 1 1 d . . . H33B H 0.2088 0.4921 0.4792 0.094 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0276(5) 0.0259(5) 0.0392(5) 0.0025(4) 0.0062(4) -0.0008(3) Cl2 0.0293(9) 0.0286(9) 0.0463(10) 0.0036(7) 0.0077(7) -0.0029(6) O1 0.033(3) 0.033(3) 0.046(3) 0.000(2) 0.010(2) -0.006(2) Cl1 0.0352(10) 0.0358(10) 0.0492(10) -0.0041(8) 0.0099(8) 0.0000(7) N2 0.026(3) 0.027(3) 0.038(3) 0.007(2) 0.011(2) 0.003(2) C11 0.032(4) 0.026(3) 0.029(3) 0.004(3) 0.005(3) -0.001(3) N1 0.045(4) 0.023(3) 0.046(3) 0.004(3) 0.013(3) -0.005(3) C9 0.033(4) 0.029(4) 0.031(3) 0.010(3) 0.007(3) 0.001(3) C12 0.041(4) 0.031(4) 0.042(4) -0.003(3) 0.013(3) -0.001(3) C19 0.034(4) 0.034(4) 0.044(4) 0.001(3) 0.013(3) 0.001(3) C14 0.041(4) 0.030(4) 0.056(5) 0.004(4) 0.013(4) -0.009(3) C15 0.029(4) 0.036(4) 0.034(4) -0.002(3) 0.003(3) 0.008(3) C17 0.027(3) 0.032(4) 0.042(4) -0.001(3) 0.016(3) 0.000(3) C18 0.035(4) 0.038(4) 0.041(4) -0.006(3) 0.009(3) -0.009(3) C10 0.017(3) 0.022(3) 0.038(4) 0.002(3) 0.000(3) 0.000(2) C16 0.047(5) 0.031(4) 0.068(5) -0.004(4) 0.032(4) -0.001(3) C36 0.067(6) 0.064(6) 0.048(5) 0.001(5) -0.004(4) -0.009(5) C5 0.039(4) 0.035(4) 0.044(4) 0.006(3) 0.012(3) 0.001(3) C37 0.038(4) 0.036(4) 0.048(4) -0.007(4) 0.014(3) -0.011(3) C25 0.054(5) 0.035(4) 0.030(4) 0.002(3) 0.013(3) 0.008(3) C24 0.049(5) 0.053(5) 0.063(5) 0.010(4) 0.024(4) 0.007(4) C8 0.043(5) 0.041(4) 0.044(4) 0.005(4) 0.003(3) 0.000(3) C13 0.027(4) 0.040(4) 0.045(4) 0.000(3) 0.010(3) -0.008(3) C20 0.053(5) 0.050(5) 0.054(5) 0.001(4) 0.019(4) 0.007(4) C4 0.057(5) 0.046(5) 0.054(5) 0.014(4) 0.017(4) -0.003(4) C31 0.050(5) 0.038(4) 0.047(4) -0.002(4) 0.010(4) -0.001(3) C6 0.059(6) 0.060(6) 0.069(6) 0.020(5) 0.008(5) 0.014(5) C26 0.078(7) 0.046(5) 0.052(5) 0.003(4) 0.009(5) 0.009(5) C42 0.042(5) 0.042(5) 0.068(5) -0.005(4) 0.015(4) -0.002(4) C39 0.102(9) 0.058(6) 0.084(8) -0.029(6) 0.031(7) -0.006(6) C38 0.077(7) 0.053(6) 0.055(5) -0.013(5) 0.013(5) -0.010(5) C7 0.053(5) 0.061(6) 0.053(5) 0.013(5) -0.003(4) -0.001(4) C1 0.036(4) 0.050(5) 0.068(6) 0.008(4) -0.001(4) -0.006(4) C2 0.062(6) 0.041(5) 0.081(6) 0.022(5) 0.012(5) -0.001(4) C23 0.070(7) 0.079(7) 0.053(5) 0.012(5) 0.011(5) 0.011(5) C30 0.064(6) 0.066(6) 0.058(5) 0.003(5) 0.012(5) 0.015(5) C35 0.091(9) 0.070(7) 0.064(7) -0.004(6) -0.009(6) -0.007(6) C3 0.078(7) 0.057(6) 0.085(7) 0.030(6) 0.011(6) -0.004(5) C40 0.082(8) 0.060(7) 0.107(9) 0.008(7) 0.043(7) 0.023(6) C22 0.096(8) 0.076(7) 0.053(6) 0.006(5) 0.033(6) -0.007(6) C27 0.126(11) 0.041(6) 0.090(8) 0.009(6) 0.024(8) 0.027(6) C21 0.080(7) 0.074(7) 0.071(6) -0.002(5) 0.047(6) 0.008(5) C32 0.069(6) 0.071(6) 0.045(5) 0.002(5) 0.011(4) -0.003(5) C41 0.053(6) 0.065(7) 0.117(9) 0.002(7) 0.015(6) 0.009(5) C34 0.115(11) 0.087(8) 0.045(5) 0.009(6) 0.009(6) -0.012(7) C29 0.059(6) 0.080(7) 0.062(6) 0.014(5) 0.014(5) 0.030(5) C28 0.081(8) 0.076(8) 0.072(7) 0.006(6) 0.013(6) 0.038(6) C44 0.084(7) 0.060(6) 0.050(5) 0.000(5) 0.015(5) 0.002(5) C43 0.068(6) 0.040(4) 0.045(4) -0.006(4) 0.018(4) -0.010(4) C33 0.103(10) 0.069(7) 0.066(7) -0.003(6) 0.030(7) -0.003(6) _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 N1 2.057(6) . ? Ni1 O1 2.153(5) . ? Ni1 N2 2.153(5) . ? Ni1 Cl2 2.3854(18) . ? Ni1 Cl1 2.398(2) . ? Ni1 Cl2 2.4844(18) 3_667 ? Cl2 Ni1 2.4844(18) 3_667 ? O1 C43 1.441(9) . ? N2 C9 1.282(8) . ? N2 C10 1.428(8) . ? C11 C10 1.405(9) . ? C11 C12 1.405(10) . ? C11 C17 1.533(9) . ? N1 C1 1.324(10) . ? N1 C5 1.348(9) . ? C9 C5 1.483(10) . ? C9 C8 1.521(10) . ? C12 C13 1.380(10) . ? C12 H12A 0.9500 . ? C19 C20 1.361(11) . ? C19 C24 1.386(11) . ? C19 C17 1.537(10) . ? C14 C13 1.370(11) . ? C14 C15 1.394(10) . ? C14 H14A 0.9500 . ? C15 C10 1.401(10) . ? C15 C18 1.551(10) . ? C17 C25 1.538(10) . ? C17 H17A 1.0000 . ? C18 C31 1.525(10) . ? C18 C37 1.543(10) . ? C18 H18A 1.0000 . ? C16 C13 1.519(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C36 C35 1.379(13) . ? C36 C31 1.391(12) . ? C36 H36A 0.9500 . ? C5 C4 1.412(11) . ? C37 C42 1.347(11) . ? C37 C38 1.381(11) . ? C25 C26 1.369(12) . ? C25 C30 1.398(12) . ? C24 C23 1.401(12) . ? C24 H24A 0.9500 . ? C8 C7 1.493(11) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C20 C21 1.438(12) . ? C20 H20A 0.9500 . ? C4 C3 1.388(13) . ? C4 C6 1.493(12) . ? C31 C32 1.374(12) . ? C6 C7 1.493(13) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C26 C27 1.420(13) . ? C26 H26A 0.9500 . ? C42 C41 1.401(13) . ? C42 H42A 0.9500 . ? C39 C40 1.297(15) . ? C39 C38 1.372(14) . ? C39 H39A 0.9500 . ? C38 H38A 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C1 C2 1.414(12) . ? C1 H1A 0.9500 . ? C2 C3 1.345(13) . ? C2 H2A 0.9500 . ? C23 C22 1.377(14) . ? C23 H23A 0.9500 . ? C30 C29 1.373(12) . ? C30 H30A 0.9500 . ? C35 C34 1.364(16) . ? C35 H35A 0.9500 . ? C3 H3A 0.9500 . ? C40 C41 1.404(16) . ? C40 H40A 0.9500 . ? C22 C21 1.361(15) . ? C22 H22A 0.9500 . ? C27 C28 1.349(16) . ? C27 H27A 0.9500 . ? C21 H21A 0.9500 . ? C32 C33 1.359(14) . ? C32 H32A 0.9500 . ? C41 H41 0.9500 . ? C34 C33 1.333(16) . ? C34 H34A 0.9500 . ? C29 C28 1.319(15) . ? C29 H29A 0.9500 . ? C28 H28A 0.9500 . ? C44 C43 1.535(12) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44D 0.9800 . ? C43 H43A 0.9900 . ? C43 H43C 0.9900 . ? C33 H33B 0.9500 . ? 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 N1 Ni1 O1 91.3(2) . . ? N1 Ni1 N2 78.6(2) . . ? O1 Ni1 N2 90.6(2) . . ? N1 Ni1 Cl2 172.18(17) . . ? O1 Ni1 Cl2 84.71(14) . . ? N2 Ni1 Cl2 94.69(15) . . ? N1 Ni1 Cl1 90.52(18) . . ? O1 Ni1 Cl1 171.07(14) . . ? N2 Ni1 Cl1 98.36(16) . . ? Cl2 Ni1 Cl1 94.48(7) . . ? N1 Ni1 Cl2 96.27(18) . 3_667 ? O1 Ni1 Cl2 81.93(14) . 3_667 ? N2 Ni1 Cl2 170.87(16) . 3_667 ? Cl2 Ni1 Cl2 89.82(6) . 3_667 ? Cl1 Ni1 Cl2 89.17(7) . 3_667 ? Ni1 Cl2 Ni1 90.18(6) . 3_667 ? C43 O1 Ni1 120.3(4) . . ? C9 N2 C10 121.7(6) . . ? C9 N2 Ni1 112.7(4) . . ? C10 N2 Ni1 125.4(4) . . ? C10 C11 C12 118.5(6) . . ? C10 C11 C17 120.4(6) . . ? C12 C11 C17 121.1(6) . . ? C1 N1 C5 120.0(6) . . ? C1 N1 Ni1 124.7(5) . . ? C5 N1 Ni1 115.0(5) . . ? N2 C9 C5 118.2(6) . . ? N2 C9 C8 125.8(6) . . ? C5 C9 C8 116.0(6) . . ? C13 C12 C11 121.9(7) . . ? C13 C12 H12A 119.0 . . ? C11 C12 H12A 119.0 . . ? C20 C19 C24 120.0(7) . . ? C20 C19 C17 122.7(7) . . ? C24 C19 C17 117.2(7) . . ? C13 C14 C15 121.8(7) . . ? C13 C14 H14A 119.1 . . ? C15 C14 H14A 119.1 . . ? C14 C15 C10 119.5(7) . . ? C14 C15 C18 119.4(6) . . ? C10 C15 C18 121.1(6) . . ? C11 C17 C19 114.1(5) . . ? C11 C17 C25 111.2(6) . . ? C19 C17 C25 111.4(6) . . ? C11 C17 H17A 106.6 . . ? C19 C17 H17A 106.6 . . ? C25 C17 H17A 106.6 . . ? C31 C18 C37 110.5(6) . . ? C31 C18 C15 113.9(6) . . ? C37 C18 C15 113.3(6) . . ? C31 C18 H18A 106.2 . . ? C37 C18 H18A 106.2 . . ? C15 C18 H18A 106.2 . . ? C15 C10 C11 119.6(6) . . ? C15 C10 N2 121.5(6) . . ? C11 C10 N2 118.7(6) . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C35 C36 C31 120.8(10) . . ? C35 C36 H36A 119.6 . . ? C31 C36 H36A 119.6 . . ? N1 C5 C4 123.1(7) . . ? N1 C5 C9 115.3(6) . . ? C4 C5 C9 121.6(7) . . ? C42 C37 C38 119.9(8) . . ? C42 C37 C18 118.2(7) . . ? C38 C37 C18 121.6(7) . . ? C26 C25 C30 118.3(8) . . ? C26 C25 C17 119.3(7) . . ? C30 C25 C17 122.4(7) . . ? C19 C24 C23 119.4(8) . . ? C19 C24 H24A 120.3 . . ? C23 C24 H24A 120.3 . . ? C7 C8 C9 114.0(7) . . ? C7 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? C7 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C14 C13 C12 118.7(7) . . ? C14 C13 C16 120.6(7) . . ? C12 C13 C16 120.7(7) . . ? C19 C20 C21 119.4(8) . . ? C19 C20 H20A 120.3 . . ? C21 C20 H20A 120.3 . . ? C3 C4 C5 114.1(8) . . ? C3 C4 C6 124.4(8) . . ? C5 C4 C6 121.5(8) . . ? C32 C31 C36 116.5(8) . . ? C32 C31 C18 120.3(8) . . ? C36 C31 C18 123.0(8) . . ? C4 C6 C7 110.7(7) . . ? C4 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C25 C26 C27 119.7(10) . . ? C25 C26 H26A 120.2 . . ? C27 C26 H26A 120.2 . . ? C37 C42 C41 121.2(9) . . ? C37 C42 H42A 119.4 . . ? C41 C42 H42A 119.4 . . ? C40 C39 C38 122.6(10) . . ? C40 C39 H39A 118.7 . . ? C38 C39 H39A 118.7 . . ? C39 C38 C37 118.4(10) . . ? C39 C38 H38A 120.8 . . ? C37 C38 H38A 120.8 . . ? C6 C7 C8 114.0(8) . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N1 C1 C2 120.8(8) . . ? N1 C1 H1A 119.6 . . ? C2 C1 H1A 119.6 . . ? C3 C2 C1 117.7(9) . . ? C3 C2 H2A 121.2 . . ? C1 C2 H2A 121.2 . . ? C22 C23 C24 121.7(9) . . ? C22 C23 H23A 119.2 . . ? C24 C23 H23A 119.2 . . ? C29 C30 C25 120.0(10) . . ? C29 C30 H30A 120.0 . . ? C25 C30 H30A 120.0 . . ? C34 C35 C36 119.7(12) . . ? C34 C35 H35A 120.2 . . ? C36 C35 H35A 120.2 . . ? C2 C3 C4 124.1(9) . . ? C2 C3 H3A 117.9 . . ? C4 C3 H3A 117.9 . . ? C39 C40 C41 121.0(10) . . ? C39 C40 H40A 119.5 . . ? C41 C40 H40A 119.5 . . ? C21 C22 C23 118.4(9) . . ? C21 C22 H22A 120.8 . . ? C23 C22 H22A 120.8 . . ? C28 C27 C26 119.2(10) . . ? C28 C27 H27A 120.4 . . ? C26 C27 H27A 120.4 . . ? C22 C21 C20 121.0(9) . . ? C22 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? C33 C32 C31 122.0(10) . . ? C33 C32 H32A 119.0 . . ? C31 C32 H32A 119.0 . . ? C42 C41 C40 116.7(10) . . ? C42 C41 H41 121.6 . . ? C40 C41 H41 121.6 . . ? C33 C34 C35 120.0(10) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C28 C29 C30 121.3(11) . . ? C28 C29 H29A 119.4 . . ? C30 C29 H29A 119.4 . . ? C29 C28 C27 121.4(10) . . ? C29 C28 H28A 119.3 . . ? C27 C28 H28A 119.3 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44D 109.5 . . ? H44A C44 H44D 109.5 . . ? H44B C44 H44D 109.5 . . ? O1 C43 C44 109.8(7) . . ? O1 C43 H43A 109.7 . . ? C44 C43 H43A 109.7 . . ? O1 C43 H43C 109.7 . . ? C44 C43 H43C 109.7 . . ? H43A C43 H43C 108.2 . . ? C34 C33 C32 120.6(11) . . ? C34 C33 H33B 119.7 . . ? C32 C33 H33B 119.7 . . ? 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 N1 Ni1 Cl2 Ni1 141.3(14) . . . 3_667 ? O1 Ni1 Cl2 Ni1 81.91(13) . . . 3_667 ? N2 Ni1 Cl2 Ni1 172.06(16) . . . 3_667 ? Cl1 Ni1 Cl2 Ni1 -89.16(7) . . . 3_667 ? Cl2 Ni1 Cl2 Ni1 0.0 3_667 . . 3_667 ? N1 Ni1 O1 C43 24.8(5) . . . . ? N2 Ni1 O1 C43 103.4(5) . . . . ? Cl2 Ni1 O1 C43 -161.9(5) . . . . ? Cl1 Ni1 O1 C43 -76.7(11) . . . . ? Cl2 Ni1 O1 C43 -71.3(5) 3_667 . . . ? N1 Ni1 N2 C9 2.0(5) . . . . ? O1 Ni1 N2 C9 -89.2(5) . . . . ? Cl2 Ni1 N2 C9 -173.9(5) . . . . ? Cl1 Ni1 N2 C9 90.8(5) . . . . ? Cl2 Ni1 N2 C9 -54.5(12) 3_667 . . . ? N1 Ni1 N2 C10 177.8(6) . . . . ? O1 Ni1 N2 C10 86.6(5) . . . . ? Cl2 Ni1 N2 C10 1.9(5) . . . . ? Cl1 Ni1 N2 C10 -93.4(5) . . . . ? Cl2 Ni1 N2 C10 121.3(9) 3_667 . . . ? O1 Ni1 N1 C1 -94.8(7) . . . . ? N2 Ni1 N1 C1 174.9(7) . . . . ? Cl2 Ni1 N1 C1 -153.7(11) . . . . ? Cl1 Ni1 N1 C1 76.5(7) . . . . ? Cl2 Ni1 N1 C1 -12.7(7) 3_667 . . . ? O1 Ni1 N1 C5 91.3(5) . . . . ? N2 Ni1 N1 C5 0.9(5) . . . . ? Cl2 Ni1 N1 C5 32.3(17) . . . . ? Cl1 Ni1 N1 C5 -97.5(5) . . . . ? Cl2 Ni1 N1 C5 173.3(5) 3_667 . . . ? C10 N2 C9 C5 179.6(6) . . . . ? Ni1 N2 C9 C5 -4.4(8) . . . . ? C10 N2 C9 C8 3.2(11) . . . . ? Ni1 N2 C9 C8 179.1(6) . . . . ? C10 C11 C12 C13 -0.3(10) . . . . ? C17 C11 C12 C13 177.9(6) . . . . ? C13 C14 C15 C10 -1.8(11) . . . . ? C13 C14 C15 C18 179.8(7) . . . . ? C10 C11 C17 C19 -152.1(6) . . . . ? C12 C11 C17 C19 29.7(9) . . . . ? C10 C11 C17 C25 80.9(8) . . . . ? C12 C11 C17 C25 -97.3(8) . . . . ? C20 C19 C17 C11 -114.3(8) . . . . ? C24 C19 C17 C11 66.4(9) . . . . ? C20 C19 C17 C25 12.6(10) . . . . ? C24 C19 C17 C25 -166.8(7) . . . . ? C14 C15 C18 C31 89.4(8) . . . . ? C10 C15 C18 C31 -88.9(8) . . . . ? C14 C15 C18 C37 -38.0(9) . . . . ? C10 C15 C18 C37 143.6(6) . . . . ? C14 C15 C10 C11 1.6(9) . . . . ? C18 C15 C10 C11 179.9(6) . . . . ? C14 C15 C10 N2 175.3(6) . . . . ? C18 C15 C10 N2 -6.4(9) . . . . ? C12 C11 C10 C15 -0.6(9) . . . . ? C17 C11 C10 C15 -178.8(6) . . . . ? C12 C11 C10 N2 -174.5(6) . . . . ? C17 C11 C10 N2 7.3(9) . . . . ? C9 N2 C10 C15 88.8(8) . . . . ? Ni1 N2 C10 C15 -86.6(7) . . . . ? C9 N2 C10 C11 -97.4(8) . . . . ? Ni1 N2 C10 C11 87.2(7) . . . . ? C1 N1 C5 C4 3.8(12) . . . . ? Ni1 N1 C5 C4 178.1(6) . . . . ? C1 N1 C5 C9 -177.7(7) . . . . ? Ni1 N1 C5 C9 -3.4(8) . . . . ? N2 C9 C5 N1 5.4(10) . . . . ? C8 C9 C5 N1 -177.8(7) . . . . ? N2 C9 C5 C4 -176.1(7) . . . . ? C8 C9 C5 C4 0.7(11) . . . . ? C31 C18 C37 C42 155.4(7) . . . . ? C15 C18 C37 C42 -75.4(9) . . . . ? C31 C18 C37 C38 -19.0(10) . . . . ? C15 C18 C37 C38 110.2(8) . . . . ? C11 C17 C25 C26 -138.6(7) . . . . ? C19 C17 C25 C26 92.9(8) . . . . ? C11 C17 C25 C30 41.7(10) . . . . ? C19 C17 C25 C30 -86.7(9) . . . . ? C20 C19 C24 C23 -1.8(13) . . . . ? C17 C19 C24 C23 177.6(8) . . . . ? N2 C9 C8 C7 -159.8(8) . . . . ? C5 C9 C8 C7 23.7(10) . . . . ? C15 C14 C13 C12 1.0(11) . . . . ? C15 C14 C13 C16 179.4(7) . . . . ? C11 C12 C13 C14 0.1(11) . . . . ? C11 C12 C13 C16 -178.3(7) . . . . ? C24 C19 C20 C21 1.0(13) . . . . ? C17 C19 C20 C21 -178.3(8) . . . . ? N1 C5 C4 C3 -0.8(13) . . . . ? C9 C5 C4 C3 -179.2(8) . . . . ? N1 C5 C4 C6 180.0(8) . . . . ? C9 C5 C4 C6 1.6(13) . . . . ? C35 C36 C31 C32 2.8(14) . . . . ? C35 C36 C31 C18 -171.3(9) . . . . ? C37 C18 C31 C32 -85.0(9) . . . . ? C15 C18 C31 C32 146.1(8) . . . . ? C37 C18 C31 C36 88.9(10) . . . . ? C15 C18 C31 C36 -40.0(11) . . . . ? C3 C4 C6 C7 153.4(10) . . . . ? C5 C4 C6 C7 -27.5(13) . . . . ? C30 C25 C26 C27 -0.1(13) . . . . ? C17 C25 C26 C27 -179.8(8) . . . . ? C38 C37 C42 C41 -2.9(14) . . . . ? C18 C37 C42 C41 -177.3(9) . . . . ? C40 C39 C38 C37 -5.1(17) . . . . ? C42 C37 C38 C39 4.0(14) . . . . ? C18 C37 C38 C39 178.3(9) . . . . ? C4 C6 C7 C8 52.2(12) . . . . ? C9 C8 C7 C6 -51.4(11) . . . . ? C5 N1 C1 C2 -4.1(13) . . . . ? Ni1 N1 C1 C2 -177.8(7) . . . . ? N1 C1 C2 C3 1.4(15) . . . . ? C19 C24 C23 C22 2.4(15) . . . . ? C26 C25 C30 C29 1.5(13) . . . . ? C17 C25 C30 C29 -178.8(8) . . . . ? C31 C36 C35 C34 1.2(17) . . . . ? C1 C2 C3 C4 1.7(17) . . . . ? C5 C4 C3 C2 -2.0(16) . . . . ? C6 C4 C3 C2 177.2(10) . . . . ? C38 C39 C40 C41 4.9(19) . . . . ? C24 C23 C22 C21 -2.2(17) . . . . ? C25 C26 C27 C28 -2.9(16) . . . . ? C23 C22 C21 C20 1.4(17) . . . . ? C19 C20 C21 C22 -0.9(15) . . . . ? C36 C31 C32 C33 -1.6(14) . . . . ? C18 C31 C32 C33 172.7(9) . . . . ? C37 C42 C41 C40 2.5(15) . . . . ? C39 C40 C41 C42 -3.5(18) . . . . ? C36 C35 C34 C33 -6.8(18) . . . . ? C25 C30 C29 C28 0.2(15) . . . . ? C30 C29 C28 C27 -3.4(18) . . . . ? C26 C27 C28 C29 4.7(18) . . . . ? Ni1 O1 C43 C44 172.0(5) . . . . ? C35 C34 C33 C32 8.1(19) . . . . ? C31 C32 C33 C34 -3.9(17) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.700 _refine_diff_density_min -0.999 _refine_diff_density_rms 0.169 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 1.000 0.000 479.4 175.0 2 0.500 0.500 0.500 479.5 174.9 _platon_squeeze_details ; ? ; #==END