# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Douglas W Stephan' 'Michael J. Sgro' _publ_contact_author_name 'Douglas W Stephan' _publ_contact_author_email DSTEPHAN@CHEM.UTORONTO.CA _publ_section_title ; Synthesis and Exchange Reactions of Ni-Dimine-COD, Acteylene and Olefin Complexes ; # Attachment 'Ni-diimines-cif_files.cif' data_C28H36N2Ni_Compound1 _database_code_depnum_ccdc_archive 'CCDC 762663' #TrackingRef 'Ni-diimines-cif_files.cif' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C28 H36 N2 Ni' _chemical_formula_weight 459.30 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2740(3) _cell_length_b 10.5006(3) _cell_length_c 15.2269(5) _cell_angle_alpha 72.275(2) _cell_angle_beta 87.470(2) _cell_angle_gamma 81.677(2) _cell_volume 1246.87(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9952 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description irregular _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method ? _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7417 _exptl_absorpt_correction_T_max 0.8573 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18907 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4380 _reflns_number_gt 3950 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0511P)^2^+0.9126P] 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 4380 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0944 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 0.84576(3) 0.94805(2) 0.293533(16) 0.02050(10) Uani 1 1 d . . . N1 N 0.9269(2) 0.94573(17) 0.17251(11) 0.0236(4) Uani 1 1 d . . . N2 N 0.7502(2) 1.12918(17) 0.22548(12) 0.0248(4) Uani 1 1 d . . . C12 C 0.4201(3) 1.3450(2) 0.30591(14) 0.0255(4) Uani 1 1 d . . . H12A H 0.3047 1.3530 0.3130 0.031 Uiso 1 1 calc R . . C16 C 0.4035(3) 1.1517(2) 0.24324(18) 0.0339(5) Uani 1 1 d . . . H16A H 0.2872 1.1730 0.2560 0.051 Uiso 1 1 calc R . . H16B H 0.4426 1.0582 0.2786 0.051 Uiso 1 1 calc R . . H16C H 0.4187 1.1631 0.1772 0.051 Uiso 1 1 calc R . . C10 C 0.6683(2) 1.23493(19) 0.25896(14) 0.0229(4) Uani 1 1 d . . . C25 C 1.0157(3) 0.9231(2) 0.39469(15) 0.0298(5) Uani 1 1 d . . . H25A H 1.0992 0.9865 0.3772 0.036 Uiso 1 1 calc R . . C21 C 0.6861(3) 0.8161(2) 0.35952(15) 0.0320(5) Uani 1 1 d . . . H21A H 0.5989 0.8073 0.3192 0.038 Uiso 1 1 calc R . . C6 C 1.1797(2) 0.8086(2) 0.14940(14) 0.0245(4) Uani 1 1 d . . . C11 C 0.4984(2) 1.2452(2) 0.27071(14) 0.0227(4) Uani 1 1 d . . . C24 C 0.8666(3) 0.9782(2) 0.42039(14) 0.0288(5) Uani 1 1 d . . . H24A H 0.8605 1.0751 0.4177 0.035 Uiso 1 1 calc R . . C1 C 1.0086(2) 0.8354(2) 0.14423(13) 0.0226(4) Uani 1 1 d . . . C14 C 0.6715(3) 1.4215(2) 0.31849(17) 0.0317(5) Uani 1 1 d . . . H14A H 0.7306 1.4819 0.3350 0.038 Uiso 1 1 calc R . . C4 C 1.1753(3) 0.6133(2) 0.09626(14) 0.0280(5) Uani 1 1 d . . . C13 C 0.5041(3) 1.4334(2) 0.33107(15) 0.0269(5) Uani 1 1 d . . . C2 C 0.9213(3) 0.7518(2) 0.11452(14) 0.0286(5) Uani 1 1 d . . . C28 C 0.8378(3) 0.7443(2) 0.35116(15) 0.0323(5) Uani 1 1 d . . . H28A H 0.8407 0.6935 0.3051 0.039 Uiso 1 1 calc R . . C5 C 1.2594(3) 0.6981(2) 0.12524(14) 0.0285(5) Uani 1 1 d . . . H5A H 1.3752 0.6802 0.1287 0.034 Uiso 1 1 calc R . . C15 C 0.7563(3) 1.3241(2) 0.28252(16) 0.0295(5) Uani 1 1 d . . . C19 C 0.8762(3) 1.0587(2) 0.10695(15) 0.0376(6) Uani 1 1 d . . . H19A H 0.8990 1.0694 0.0436 0.045 Uiso 1 1 calc R . . C3 C 1.0071(3) 0.6422(2) 0.09141(15) 0.0318(5) Uani 1 1 d . . . H3A H 0.9476 0.5851 0.0715 0.038 Uiso 1 1 calc R . . C27 C 0.9608(3) 0.6819(2) 0.42880(17) 0.0407(6) Uani 1 1 d . . . H27A H 1.0194 0.5965 0.4216 0.049 Uiso 1 1 calc R . . H27B H 0.9020 0.6599 0.4884 0.049 Uiso 1 1 calc R . . C17 C 0.4137(3) 1.5392(2) 0.37042(18) 0.0396(6) Uani 1 1 d . . . H17A H 0.2968 1.5313 0.3740 0.059 Uiso 1 1 calc R . . H17B H 0.4302 1.6291 0.3305 0.059 Uiso 1 1 calc R . . H17C H 0.4553 1.5259 0.4323 0.059 Uiso 1 1 calc R . . C20 C 0.7868(3) 1.1615(2) 0.13682(16) 0.0380(6) Uani 1 1 d . . . H20A H 0.7544 1.2492 0.0958 0.046 Uiso 1 1 calc R . . C26 C 1.0856(3) 0.7760(2) 0.43049(17) 0.0394(6) Uani 1 1 d . . . H26A H 1.1239 0.7562 0.4946 0.047 Uiso 1 1 calc R . . H26B H 1.1812 0.7579 0.3925 0.047 Uiso 1 1 calc R . . C9 C 1.2747(3) 0.9017(3) 0.17767(18) 0.0379(6) Uani 1 1 d . . . H9A H 1.3917 0.8686 0.1777 0.057 Uiso 1 1 calc R . . H9B H 1.2411 0.9043 0.2397 0.057 Uiso 1 1 calc R . . H9C H 1.2530 0.9926 0.1341 0.057 Uiso 1 1 calc R . . C23 C 0.7529(3) 0.9001(3) 0.49091(15) 0.0381(6) Uani 1 1 d . . . H23A H 0.6978 0.9589 0.5263 0.046 Uiso 1 1 calc R . . H23B H 0.8180 0.8218 0.5347 0.046 Uiso 1 1 calc R . . C22 C 0.6243(3) 0.8502(3) 0.44563(16) 0.0402(6) Uani 1 1 d . . . H22A H 0.5887 0.7689 0.4904 0.048 Uiso 1 1 calc R . . H22B H 0.5280 0.9208 0.4297 0.048 Uiso 1 1 calc R . . C8 C 1.2657(3) 0.4947(2) 0.06976(17) 0.0406(6) Uani 1 1 d . . . H8A H 1.1870 0.4464 0.0511 0.061 Uiso 1 1 calc R . . H8B H 1.3289 0.4335 0.1227 0.061 Uiso 1 1 calc R . . H8C H 1.3397 0.5272 0.0183 0.061 Uiso 1 1 calc R . . C18 C 0.9394(3) 1.3150(3) 0.2706(2) 0.0466(7) Uani 1 1 d . . . H18A H 0.9788 1.3853 0.2906 0.070 Uiso 1 1 calc R . . H18B H 0.9671 1.3276 0.2056 0.070 Uiso 1 1 calc R . . H18C H 0.9911 1.2260 0.3080 0.070 Uiso 1 1 calc R . . C7 C 0.7370(3) 0.7779(3) 0.1076(2) 0.0485(7) Uani 1 1 d . . . H7A H 0.6981 0.7091 0.0856 0.073 Uiso 1 1 calc R . . H7B H 0.7033 0.8674 0.0642 0.073 Uiso 1 1 calc R . . H7C H 0.6901 0.7739 0.1684 0.073 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 0.02520(16) 0.01682(15) 0.01725(15) -0.00411(10) 0.00322(10) 0.00111(10) N1 0.0241(9) 0.0241(9) 0.0207(9) -0.0064(7) 0.0049(7) 0.0004(7) N2 0.0261(9) 0.0199(9) 0.0240(9) -0.0037(7) 0.0045(7) 0.0027(7) C12 0.0212(10) 0.0242(11) 0.0288(11) -0.0067(9) 0.0012(8) 0.0009(8) C16 0.0283(12) 0.0295(12) 0.0476(14) -0.0173(11) -0.0082(10) -0.0010(9) C10 0.0258(11) 0.0155(9) 0.0223(10) -0.0006(8) 0.0022(8) 0.0016(8) C25 0.0335(12) 0.0322(12) 0.0242(11) -0.0114(9) -0.0051(9) 0.0017(9) C21 0.0365(13) 0.0278(11) 0.0295(12) -0.0034(9) 0.0072(10) -0.0115(10) C6 0.0249(11) 0.0275(11) 0.0227(10) -0.0105(9) 0.0020(8) -0.0025(9) C11 0.0226(10) 0.0198(10) 0.0239(10) -0.0049(8) -0.0013(8) -0.0002(8) C24 0.0390(13) 0.0268(11) 0.0206(10) -0.0109(9) -0.0019(9) 0.0038(9) C1 0.0252(11) 0.0248(10) 0.0161(9) -0.0058(8) 0.0034(8) 0.0003(8) C14 0.0322(12) 0.0180(10) 0.0450(14) -0.0083(10) -0.0052(10) -0.0047(9) C4 0.0398(13) 0.0235(11) 0.0190(10) -0.0065(9) 0.0003(9) 0.0013(9) C13 0.0323(12) 0.0183(10) 0.0274(11) -0.0052(9) -0.0014(9) 0.0016(9) C2 0.0253(11) 0.0385(12) 0.0233(11) -0.0114(9) 0.0010(8) -0.0040(9) C28 0.0487(14) 0.0176(10) 0.0292(12) -0.0053(9) 0.0106(10) -0.0071(10) C5 0.0256(11) 0.0337(12) 0.0243(11) -0.0096(9) -0.0006(8) 0.0044(9) C15 0.0238(11) 0.0185(10) 0.0407(13) -0.0013(9) 0.0025(9) -0.0022(8) C19 0.0484(15) 0.0363(13) 0.0177(11) -0.0018(10) 0.0086(10) 0.0105(11) C3 0.0395(13) 0.0342(12) 0.0269(11) -0.0153(10) 0.0006(9) -0.0090(10) C27 0.0547(16) 0.0235(12) 0.0316(13) 0.0012(10) 0.0093(11) 0.0108(11) C17 0.0487(15) 0.0282(12) 0.0434(14) -0.0172(11) 0.0007(11) 0.0041(11) C20 0.0480(15) 0.0274(12) 0.0250(12) 0.0032(9) 0.0079(10) 0.0116(10) C26 0.0402(14) 0.0375(13) 0.0329(13) -0.0086(11) -0.0042(10) 0.0159(11) C9 0.0278(12) 0.0465(14) 0.0490(15) -0.0275(12) 0.0056(10) -0.0088(10) C23 0.0478(15) 0.0399(13) 0.0215(11) -0.0093(10) 0.0072(10) 0.0078(11) C22 0.0371(13) 0.0438(14) 0.0318(13) -0.0035(11) 0.0140(10) -0.0016(11) C8 0.0587(16) 0.0301(12) 0.0323(13) -0.0140(10) -0.0001(11) 0.0067(11) C18 0.0262(13) 0.0315(13) 0.077(2) -0.0083(13) 0.0075(12) -0.0057(10) C7 0.0280(13) 0.0723(19) 0.0547(17) -0.0340(15) -0.0032(11) -0.0046(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.9374(17) . ? Ni1 N1 1.9392(16) . ? Ni1 C21 2.059(2) . ? Ni1 C28 2.061(2) . ? Ni1 C25 2.064(2) . ? Ni1 C24 2.068(2) . ? N1 C19 1.324(3) . ? N1 C1 1.427(3) . ? N2 C20 1.321(3) . ? N2 C10 1.431(3) . ? C12 C13 1.385(3) . ? C12 C11 1.385(3) . ? C16 C11 1.503(3) . ? C10 C15 1.400(3) . ? C10 C11 1.402(3) . ? C25 C24 1.378(3) . ? C25 C26 1.508(3) . ? C21 C28 1.389(3) . ? C21 C22 1.511(3) . ? C6 C5 1.391(3) . ? C6 C1 1.404(3) . ? C6 C9 1.505(3) . ? C24 C23 1.519(3) . ? C1 C2 1.397(3) . ? C14 C13 1.383(3) . ? C14 C15 1.392(3) . ? C4 C3 1.381(3) . ? C4 C5 1.385(3) . ? C4 C8 1.511(3) . ? C13 C17 1.509(3) . ? C2 C3 1.394(3) . ? C2 C7 1.512(3) . ? C28 C27 1.518(3) . ? C15 C18 1.510(3) . ? C19 C20 1.399(3) . ? C27 C26 1.535(4) . ? C23 C22 1.526(4) . ? 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 82.44(7) . . ? N2 Ni1 C21 116.71(9) . . ? N1 Ni1 C21 118.86(8) . . ? N2 Ni1 C28 152.61(9) . . ? N1 Ni1 C28 98.51(8) . . ? C21 Ni1 C28 39.41(9) . . ? N2 Ni1 C25 118.91(8) . . ? N1 Ni1 C25 117.57(8) . . ? C21 Ni1 C25 102.74(9) . . ? C28 Ni1 C25 85.12(9) . . ? N2 Ni1 C24 98.34(8) . . ? N1 Ni1 C24 152.89(9) . . ? C21 Ni1 C24 85.20(9) . . ? C28 Ni1 C24 93.00(9) . . ? C25 Ni1 C24 38.96(9) . . ? C19 N1 C1 117.35(17) . . ? C19 N1 Ni1 112.73(14) . . ? C1 N1 Ni1 129.12(13) . . ? C20 N2 C10 116.97(17) . . ? C20 N2 Ni1 112.87(14) . . ? C10 N2 Ni1 129.51(13) . . ? C13 C12 C11 122.3(2) . . ? C15 C10 C11 120.31(19) . . ? C15 C10 N2 120.85(18) . . ? C11 C10 N2 118.81(18) . . ? C24 C25 C26 124.5(2) . . ? C24 C25 Ni1 70.70(13) . . ? C26 C25 Ni1 109.25(15) . . ? C28 C21 C22 124.8(2) . . ? C28 C21 Ni1 70.36(12) . . ? C22 C21 Ni1 108.52(16) . . ? C5 C6 C1 119.07(19) . . ? C5 C6 C9 120.9(2) . . ? C1 C6 C9 120.00(19) . . ? C12 C11 C10 118.75(19) . . ? C12 C11 C16 120.92(19) . . ? C10 C11 C16 120.31(18) . . ? C25 C24 C23 124.7(2) . . ? C25 C24 Ni1 70.33(12) . . ? C23 C24 Ni1 111.24(15) . . ? C2 C1 C6 119.87(19) . . ? C2 C1 N1 121.18(18) . . ? C6 C1 N1 118.92(18) . . ? C13 C14 C15 122.3(2) . . ? C3 C4 C5 117.7(2) . . ? C3 C4 C8 121.6(2) . . ? C5 C4 C8 120.8(2) . . ? C14 C13 C12 117.90(19) . . ? C14 C13 C17 121.7(2) . . ? C12 C13 C17 120.4(2) . . ? C3 C2 C1 118.7(2) . . ? C3 C2 C7 119.9(2) . . ? C1 C2 C7 121.4(2) . . ? C21 C28 C27 124.8(2) . . ? C21 C28 Ni1 70.23(12) . . ? C27 C28 Ni1 111.65(16) . . ? C4 C5 C6 122.1(2) . . ? C14 C15 C10 118.50(19) . . ? C14 C15 C18 120.2(2) . . ? C10 C15 C18 121.3(2) . . ? N1 C19 C20 115.77(19) . . ? C4 C3 C2 122.6(2) . . ? C28 C27 C26 112.36(18) . . ? N2 C20 C19 115.89(19) . . ? C25 C26 C27 112.5(2) . . ? C24 C23 C22 111.96(18) . . ? C21 C22 C23 112.82(19) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.454 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.053 #=== END data_C36H52N2Ni_Compound3 _database_code_depnum_ccdc_archive 'CCDC 762664' #TrackingRef 'Ni-diimines-cif_files.cif' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C36 H52 N2 Ni' _chemical_formula_weight 571.51 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' _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 17.3270(9) _cell_length_b 10.2591(5) _cell_length_c 19.7575(10) _cell_angle_alpha 90.00 _cell_angle_beta 114.763(2) _cell_angle_gamma 90.00 _cell_volume 3189.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4959 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 23.97 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.634 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6260 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 19397 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5614 _reflns_number_gt 4374 _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^)+(0.0601P)^2^+4.1199P] 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 5614 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.26509(2) 0.44791(4) 0.52856(2) 0.02106(14) Uani 1 1 d . . . N1 N 0.27775(15) 0.2600(2) 0.52276(13) 0.0212(6) Uani 1 1 d . . . N2 N 0.27451(15) 0.4395(2) 0.43435(13) 0.0195(5) Uani 1 1 d . . . C1 C 0.2944(2) 0.2211(3) 0.46594(16) 0.0240(7) Uani 1 1 d . . . C2 C 0.29152(19) 0.3215(3) 0.41551(16) 0.0220(7) Uani 1 1 d . . . C3 C 0.3129(2) 0.0816(3) 0.45263(19) 0.0337(8) Uani 1 1 d . . . H3A H 0.3046 0.0244 0.4887 0.051 Uiso 1 1 calc R . . H3B H 0.3718 0.0747 0.4586 0.051 Uiso 1 1 calc R . . H3C H 0.2743 0.0553 0.4020 0.051 Uiso 1 1 calc R . . C4 C 0.3051(2) 0.2924(3) 0.34619(17) 0.0295(7) Uani 1 1 d . . . H4A H 0.2951 0.3716 0.3160 0.044 Uiso 1 1 calc R . . H4B H 0.2654 0.2242 0.3172 0.044 Uiso 1 1 calc R . . H4C H 0.3636 0.2626 0.3606 0.044 Uiso 1 1 calc R . . C7 C 0.3375(2) 0.4787(4) 0.63996(18) 0.0367(9) Uani 1 1 d . . . H7 H 0.3892 0.4221 0.6616 0.044 Uiso 1 1 calc R . . C8 C 0.3468(2) 0.5848(3) 0.60154(19) 0.0326(8) Uani 1 1 d . . . H8 H 0.4035 0.5913 0.5999 0.039 Uiso 1 1 calc R . . C9 C 0.3036(2) 0.7135(4) 0.5977(2) 0.0416(9) Uani 1 1 d . . . H9A H 0.2937 0.7246 0.6432 0.050 Uiso 1 1 calc R . . H9B H 0.3416 0.7846 0.5965 0.050 Uiso 1 1 calc R . . C10 C 0.2209(3) 0.7243(4) 0.5310(2) 0.0481(10) Uani 1 1 d . . . H10A H 0.2310 0.7614 0.4891 0.058 Uiso 1 1 calc R . . H10B H 0.1835 0.7853 0.5422 0.058 Uiso 1 1 calc R . . C11 C 0.1761(2) 0.5951(4) 0.5072(2) 0.0400(9) Uani 1 1 d . . . H11 H 0.1309 0.5948 0.4550 0.048 Uiso 1 1 calc R . . C12 C 0.1636(2) 0.5052(4) 0.5523(2) 0.0456(10) Uani 1 1 d . . . H12 H 0.1111 0.4514 0.5274 0.055 Uiso 1 1 calc R . . C13 C 0.1916(3) 0.5246(5) 0.6355(2) 0.0596(13) Uani 1 1 d . . . H13A H 0.1510 0.4801 0.6511 0.072 Uiso 1 1 calc R . . H13B H 0.1908 0.6187 0.6461 0.072 Uiso 1 1 calc R . . C14 C 0.2810(3) 0.4706(5) 0.6805(2) 0.0579(12) Uani 1 1 d . . . H14A H 0.3077 0.5197 0.7279 0.069 Uiso 1 1 calc R . . H14B H 0.2764 0.3783 0.6931 0.069 Uiso 1 1 calc R . . C15 C 0.26527(19) 0.1660(3) 0.57116(16) 0.0224(7) Uani 1 1 d . . . C16 C 0.1811(2) 0.1299(3) 0.55535(18) 0.0283(7) Uani 1 1 d . . . C17 C 0.1664(2) 0.0459(3) 0.60417(19) 0.0331(8) Uani 1 1 d . . . H17 H 0.1096 0.0231 0.5948 0.040 Uiso 1 1 calc R . . C18 C 0.2327(2) -0.0045(3) 0.66587(18) 0.0318(8) Uani 1 1 d . . . H18 H 0.2218 -0.0622 0.6985 0.038 Uiso 1 1 calc R . . C19 C 0.3145(2) 0.0292(3) 0.67975(17) 0.0270(7) Uani 1 1 d . . . H19 H 0.3599 -0.0068 0.7220 0.032 Uiso 1 1 calc R . . C20 C 0.3335(2) 0.1147(3) 0.63396(16) 0.0223(7) Uani 1 1 d . . . C21 C 0.1068(2) 0.1784(4) 0.48507(19) 0.0372(9) Uani 1 1 d . . . H21 H 0.1251 0.2615 0.4698 0.045 Uiso 1 1 calc R . . C22 C 0.0266(2) 0.2082(4) 0.4971(3) 0.0517(11) Uani 1 1 d . . . H22A H 0.0017 0.1265 0.5041 0.078 Uiso 1 1 calc R . . H22B H -0.0146 0.2541 0.4534 0.078 Uiso 1 1 calc R . . H22C H 0.0417 0.2632 0.5414 0.078 Uiso 1 1 calc R . . C23 C 0.0859(3) 0.0822(4) 0.4212(2) 0.0532(11) Uani 1 1 d . . . H23A H 0.1363 0.0687 0.4114 0.080 Uiso 1 1 calc R . . H23B H 0.0395 0.1169 0.3764 0.080 Uiso 1 1 calc R . . H23C H 0.0684 -0.0011 0.4346 0.080 Uiso 1 1 calc R . . C24 C 0.4253(2) 0.1476(3) 0.65259(17) 0.0276(7) Uani 1 1 d . . . H24 H 0.4263 0.2181 0.6180 0.033 Uiso 1 1 calc R . . C25 C 0.4723(2) 0.1973(4) 0.73323(18) 0.0408(9) Uani 1 1 d . . . H25A H 0.4389 0.2666 0.7424 0.061 Uiso 1 1 calc R . . H25B H 0.5280 0.2317 0.7405 0.061 Uiso 1 1 calc R . . H25C H 0.4800 0.1253 0.7681 0.061 Uiso 1 1 calc R . . C26 C 0.4735(2) 0.0288(4) 0.6419(2) 0.0390(9) Uani 1 1 d . . . H26A H 0.4709 -0.0429 0.6737 0.058 Uiso 1 1 calc R . . H26B H 0.5330 0.0525 0.6557 0.058 Uiso 1 1 calc R . . H26C H 0.4472 0.0013 0.5896 0.058 Uiso 1 1 calc R . . C27 C 0.25006(19) 0.5450(3) 0.38187(16) 0.0210(6) Uani 1 1 d . . . C28 C 0.1646(2) 0.5555(3) 0.33014(17) 0.0267(7) Uani 1 1 d . . . C29 C 0.1394(2) 0.6677(3) 0.28738(18) 0.0315(8) Uani 1 1 d . . . H29 H 0.0815 0.6776 0.2536 0.038 Uiso 1 1 calc R . . C30 C 0.1963(2) 0.7656(3) 0.29243(18) 0.0298(8) Uani 1 1 d . . . H30 H 0.1775 0.8420 0.2629 0.036 Uiso 1 1 calc R . . C31 C 0.2811(2) 0.7513(3) 0.34106(17) 0.0267(7) Uani 1 1 d . . . H31 H 0.3206 0.8173 0.3433 0.032 Uiso 1 1 calc R . . C32 C 0.30958(19) 0.6421(3) 0.38681(16) 0.0208(6) Uani 1 1 d . . . C33 C 0.1003(2) 0.4467(4) 0.32016(19) 0.0367(8) Uani 1 1 d . . . H33 H 0.1256 0.3864 0.3637 0.044 Uiso 1 1 calc R . . C34 C 0.0152(2) 0.4962(5) 0.3171(2) 0.0480(10) Uani 1 1 d . . . H34A H -0.0154 0.5436 0.2704 0.072 Uiso 1 1 calc R . . H34B H 0.0259 0.5547 0.3593 0.072 Uiso 1 1 calc R . . H34C H -0.0190 0.4220 0.3197 0.072 Uiso 1 1 calc R . . C35 C 0.0834(3) 0.3681(4) 0.2494(2) 0.0501(11) Uani 1 1 d . . . H35A H 0.0447 0.2958 0.2454 0.075 Uiso 1 1 calc R . . H35B H 0.1371 0.3334 0.2517 0.075 Uiso 1 1 calc R . . H35C H 0.0574 0.4248 0.2057 0.075 Uiso 1 1 calc R . . C36 C 0.40284(19) 0.6270(3) 0.43814(17) 0.0256(7) Uani 1 1 d . . . H36 H 0.4080 0.5552 0.4740 0.031 Uiso 1 1 calc R . . C37 C 0.4415(2) 0.7501(4) 0.4837(2) 0.0393(9) Uani 1 1 d . . . H37A H 0.4413 0.8206 0.4501 0.059 Uiso 1 1 calc R . . H37B H 0.5001 0.7322 0.5193 0.059 Uiso 1 1 calc R . . H37C H 0.4078 0.7763 0.5108 0.059 Uiso 1 1 calc R . . C38 C 0.4534(2) 0.5873(4) 0.3940(2) 0.0353(8) Uani 1 1 d . . . H38A H 0.4343 0.5014 0.3716 0.053 Uiso 1 1 calc R . . H38B H 0.5140 0.5836 0.4276 0.053 Uiso 1 1 calc R . . H38C H 0.4443 0.6515 0.3547 0.053 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 0.0262(2) 0.0189(2) 0.0197(2) -0.00269(16) 0.01131(16) -0.00227(17) N1 0.0244(13) 0.0182(13) 0.0192(13) 0.0009(10) 0.0073(11) -0.0040(10) N2 0.0195(12) 0.0181(13) 0.0192(12) 0.0020(10) 0.0063(10) -0.0014(10) C1 0.0309(17) 0.0247(17) 0.0166(15) -0.0037(13) 0.0102(13) -0.0078(13) C2 0.0274(16) 0.0200(16) 0.0192(15) -0.0017(12) 0.0105(13) -0.0015(13) C3 0.053(2) 0.0212(18) 0.0290(18) 0.0015(14) 0.0194(17) 0.0049(15) C4 0.0397(19) 0.0275(18) 0.0255(17) 0.0030(14) 0.0177(15) 0.0046(15) C7 0.045(2) 0.039(2) 0.0183(16) -0.0074(15) 0.0054(15) 0.0083(17) C8 0.0263(17) 0.032(2) 0.0363(19) -0.0174(16) 0.0099(15) -0.0061(14) C9 0.047(2) 0.027(2) 0.058(3) -0.0096(18) 0.029(2) -0.0047(16) C10 0.064(3) 0.031(2) 0.050(2) -0.0029(18) 0.025(2) 0.0137(19) C11 0.0332(19) 0.045(2) 0.038(2) -0.0108(18) 0.0116(17) 0.0126(17) C12 0.031(2) 0.059(3) 0.056(2) -0.029(2) 0.0277(19) -0.0090(18) C13 0.080(3) 0.063(3) 0.065(3) -0.018(2) 0.058(3) -0.015(2) C14 0.099(4) 0.053(3) 0.030(2) 0.0057(19) 0.034(2) 0.015(2) C15 0.0323(17) 0.0160(16) 0.0195(15) -0.0005(12) 0.0115(14) -0.0057(13) C16 0.0334(18) 0.0248(18) 0.0264(17) -0.0022(14) 0.0123(14) -0.0080(14) C17 0.0367(19) 0.0310(19) 0.0337(19) -0.0027(15) 0.0169(16) -0.0126(15) C18 0.054(2) 0.0236(17) 0.0267(17) 0.0000(14) 0.0256(17) -0.0086(16) C19 0.0404(19) 0.0220(18) 0.0182(15) 0.0007(13) 0.0119(14) -0.0004(14) C20 0.0324(17) 0.0150(15) 0.0180(15) -0.0018(12) 0.0089(13) -0.0038(13) C21 0.0309(18) 0.037(2) 0.037(2) 0.0062(16) 0.0078(16) -0.0110(16) C22 0.032(2) 0.051(3) 0.071(3) 0.017(2) 0.019(2) -0.0044(18) C23 0.049(2) 0.059(3) 0.035(2) 0.0001(19) 0.0016(19) -0.019(2) C24 0.0303(17) 0.0222(17) 0.0239(16) 0.0074(13) 0.0050(14) -0.0033(14) C25 0.041(2) 0.036(2) 0.0287(19) 0.0061(16) -0.0015(16) -0.0066(17) C26 0.035(2) 0.034(2) 0.046(2) 0.0100(17) 0.0158(17) 0.0035(16) C27 0.0260(16) 0.0190(15) 0.0196(15) 0.0027(12) 0.0111(13) 0.0022(13) C28 0.0265(16) 0.0283(18) 0.0249(16) 0.0049(14) 0.0103(14) -0.0009(14) C29 0.0245(17) 0.039(2) 0.0285(18) 0.0076(15) 0.0085(14) 0.0062(15) C30 0.0399(19) 0.0237(18) 0.0296(18) 0.0115(14) 0.0185(16) 0.0097(15) C31 0.0338(18) 0.0214(17) 0.0293(17) 0.0042(14) 0.0176(15) -0.0006(14) C32 0.0248(15) 0.0199(16) 0.0210(15) 0.0007(12) 0.0130(13) -0.0009(12) C33 0.0279(18) 0.041(2) 0.0323(19) 0.0095(16) 0.0041(15) -0.0076(16) C34 0.0283(19) 0.074(3) 0.040(2) -0.010(2) 0.0129(17) -0.014(2) C35 0.041(2) 0.041(2) 0.065(3) -0.010(2) 0.019(2) -0.0124(18) C36 0.0259(16) 0.0247(18) 0.0257(16) 0.0043(13) 0.0102(14) -0.0041(13) C37 0.038(2) 0.041(2) 0.036(2) -0.0047(17) 0.0121(17) -0.0145(17) C38 0.0277(18) 0.040(2) 0.040(2) 0.0050(16) 0.0165(16) 0.0037(15) _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 1.937(2) . ? Ni1 N1 1.949(3) . ? Ni1 C7 2.050(3) . ? Ni1 C11 2.072(3) . ? Ni1 C12 2.084(3) . ? Ni1 C8 2.084(3) . ? N1 C1 1.331(4) . ? N1 C15 1.437(4) . ? N2 C2 1.335(4) . ? N2 C27 1.435(4) . ? C1 C2 1.419(4) . ? C1 C3 1.514(4) . ? C2 C4 1.513(4) . ? C7 C8 1.374(5) . ? C7 C14 1.506(6) . ? C8 C9 1.504(5) . ? C9 C10 1.490(5) . ? C10 C11 1.508(6) . ? C11 C12 1.360(6) . ? C12 C13 1.521(6) . ? C13 C14 1.530(6) . ? C15 C16 1.408(4) . ? C15 C20 1.409(4) . ? C16 C17 1.394(5) . ? C16 C21 1.528(5) . ? C17 C18 1.379(5) . ? C18 C19 1.370(5) . ? C19 C20 1.394(4) . ? C20 C24 1.513(4) . ? C21 C23 1.522(5) . ? C21 C22 1.534(5) . ? C24 C26 1.541(5) . ? C24 C25 1.541(4) . ? C27 C32 1.408(4) . ? C27 C28 1.408(4) . ? C28 C29 1.386(5) . ? C28 C33 1.530(5) . ? C29 C30 1.381(5) . ? C30 C31 1.385(5) . ? C31 C32 1.394(4) . ? C32 C36 1.513(4) . ? C33 C35 1.533(5) . ? C33 C34 1.536(5) . ? C36 C38 1.527(4) . ? C36 C37 1.532(5) . ? 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 80.94(10) . . ? N2 Ni1 C7 141.08(13) . . ? N1 Ni1 C7 100.49(13) . . ? N2 Ni1 C11 101.07(13) . . ? N1 Ni1 C11 143.29(13) . . ? C7 Ni1 C11 100.08(15) . . ? N2 Ni1 C12 130.30(14) . . ? N1 Ni1 C12 114.73(15) . . ? C7 Ni1 C12 84.85(15) . . ? C11 Ni1 C12 38.21(16) . . ? N2 Ni1 C8 112.87(12) . . ? N1 Ni1 C8 130.28(12) . . ? C7 Ni1 C8 38.81(14) . . ? C11 Ni1 C8 83.19(14) . . ? C12 Ni1 C8 92.68(14) . . ? C1 N1 C15 120.4(3) . . ? C1 N1 Ni1 114.5(2) . . ? C15 N1 Ni1 124.94(19) . . ? C2 N2 C27 121.0(2) . . ? C2 N2 Ni1 115.19(19) . . ? C27 N2 Ni1 122.85(19) . . ? N1 C1 C2 114.7(3) . . ? N1 C1 C3 124.5(3) . . ? C2 C1 C3 120.8(3) . . ? N2 C2 C1 114.1(3) . . ? N2 C2 C4 124.5(3) . . ? C1 C2 C4 121.3(3) . . ? C8 C7 C14 126.1(3) . . ? C8 C7 Ni1 71.92(19) . . ? C14 C7 Ni1 108.7(3) . . ? C7 C8 C9 123.6(3) . . ? C7 C8 Ni1 69.26(19) . . ? C9 C8 Ni1 112.1(2) . . ? C10 C9 C8 112.6(3) . . ? C9 C10 C11 112.9(3) . . ? C12 C11 C10 126.5(4) . . ? C12 C11 Ni1 71.4(2) . . ? C10 C11 Ni1 109.6(2) . . ? C11 C12 C13 123.6(4) . . ? C11 C12 Ni1 70.4(2) . . ? C13 C12 Ni1 111.3(3) . . ? C12 C13 C14 111.6(3) . . ? C7 C14 C13 113.4(3) . . ? C16 C15 C20 120.4(3) . . ? C16 C15 N1 117.4(3) . . ? C20 C15 N1 122.2(3) . . ? C17 C16 C15 118.8(3) . . ? C17 C16 C21 120.1(3) . . ? C15 C16 C21 121.1(3) . . ? C18 C17 C16 121.1(3) . . ? C19 C18 C17 119.5(3) . . ? C18 C19 C20 122.3(3) . . ? C19 C20 C15 117.9(3) . . ? C19 C20 C24 119.5(3) . . ? C15 C20 C24 122.7(3) . . ? C23 C21 C16 111.1(3) . . ? C23 C21 C22 110.0(3) . . ? C16 C21 C22 113.4(3) . . ? C20 C24 C26 111.4(3) . . ? C20 C24 C25 111.9(3) . . ? C26 C24 C25 108.7(3) . . ? C32 C27 C28 120.9(3) . . ? C32 C27 N2 119.9(3) . . ? C28 C27 N2 119.0(3) . . ? C29 C28 C27 118.2(3) . . ? C29 C28 C33 120.1(3) . . ? C27 C28 C33 121.7(3) . . ? C30 C29 C28 121.8(3) . . ? C29 C30 C31 119.4(3) . . ? C30 C31 C32 121.3(3) . . ? C31 C32 C27 118.3(3) . . ? C31 C32 C36 120.4(3) . . ? C27 C32 C36 121.3(3) . . ? C28 C33 C35 110.6(3) . . ? C28 C33 C34 113.5(3) . . ? C35 C33 C34 109.0(3) . . ? C32 C36 C38 110.6(3) . . ? C32 C36 C37 113.0(3) . . ? C38 C36 C37 109.9(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.313 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.068 #=== END data_C72H80N4Ni_Compound4 _database_code_depnum_ccdc_archive 'CCDC 762665' #TrackingRef 'Ni-diimines-cif_files.cif' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C72 H80 N4 Ni' _chemical_formula_weight 1060.11 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ccca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x, y+1/2, z-1/2' _cell_length_a 16.524(3) _cell_length_b 23.805(4) _cell_length_c 14.728(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5793.2(16) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4028 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 26.74 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 0.382 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6271 _exptl_absorpt_correction_T_max 0.7456 _diffrn_ambient_temperature 296(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_reflns_number 11917 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2558 _reflns_number_gt 2131 _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^)+(0.0456P)^2^+3.6991P] 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 2558 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 0.0000 0.2500 0.2500 0.02003(14) Uani 1 4 d S . . N1 N 0.03180(8) 0.18847(5) 0.33082(9) 0.0223(3) Uani 1 1 d . . . C1 C 0.05908(10) 0.18719(6) 0.42325(11) 0.0230(4) Uani 1 1 d . . . C8 C 0.01624(9) 0.13874(7) 0.29494(11) 0.0233(4) Uani 1 1 d . . . C6 C 0.14175(11) 0.18998(7) 0.44041(11) 0.0275(4) Uani 1 1 d . . . C3 C 0.03282(12) 0.17887(7) 0.58206(12) 0.0312(4) Uani 1 1 d . . . H3 H -0.0039 0.1760 0.6297 0.037 Uiso 1 1 calc R . . C4 C 0.11424(12) 0.18136(8) 0.60166(12) 0.0336(4) Uani 1 1 d . . . C2 C 0.00352(11) 0.18056(7) 0.49363(12) 0.0260(4) Uani 1 1 d . . . C9 C 0.02664(11) 0.08058(7) 0.32448(12) 0.0280(4) Uani 1 1 d . . . C5 C 0.16821(12) 0.18659(8) 0.53003(12) 0.0344(4) Uani 1 1 d . . . H5 H 0.2234 0.1879 0.5421 0.041 Uiso 1 1 calc R . . C7 C 0.20082(11) 0.19447(9) 0.36343(13) 0.0394(5) Uani 1 1 d . . . H7A H 0.2545 0.1990 0.3872 0.059 Uiso 1 1 calc R . . H7B H 0.1873 0.2264 0.3265 0.059 Uiso 1 1 calc R . . H7C H 0.1984 0.1610 0.3273 0.059 Uiso 1 1 calc R . . C10 C 0.05474(12) 0.05389(8) 0.40096(13) 0.0358(5) Uani 1 1 d . . . H10 H 0.0729 0.0743 0.4508 0.043 Uiso 1 1 calc R . . C14 C 0.0000 0.04772(10) 0.2500 0.0309(6) Uani 1 2 d S . . C11 C 0.05527(14) -0.00547(9) 0.40156(14) 0.0474(6) Uani 1 1 d . . . H11 H 0.0742 -0.0239 0.4530 0.057 Uiso 1 1 calc R . . C12 C 0.02918(15) -0.03680(8) 0.32992(15) 0.0498(6) Uani 1 1 d . . . H12 H 0.0305 -0.0758 0.3335 0.060 Uiso 1 1 calc R . . C13 C 0.0000 -0.01066(11) 0.2500 0.0406(7) Uani 1 2 d S . . C15 C 0.20862(17) 0.44648(12) 0.3517(2) 0.0792(9) Uani 1 1 d . . . H15A H 0.1522 0.4577 0.3522 0.095 Uiso 1 1 calc R . . H15B H 0.2107 0.4058 0.3516 0.095 Uiso 1 1 calc R . . C16 C 0.2481(2) 0.46833(12) 0.2672(2) 0.0798(9) Uani 1 1 d . . . H16A H 0.2179 0.4557 0.2145 0.096 Uiso 1 1 calc R . . H16B H 0.3025 0.4533 0.2627 0.096 Uiso 1 1 calc R . . C17 C 0.2491(2) 0.46802(13) 0.4350(2) 0.0894(10) Uani 1 1 d . . . H17A H 0.3040 0.4537 0.4379 0.107 Uiso 1 1 calc R . . H17B H 0.2202 0.4548 0.4883 0.107 Uiso 1 1 calc R . . C18 C -0.08510(11) 0.17313(8) 0.47570(14) 0.0368(5) Uani 1 1 d . . . H18A H -0.0964 0.1341 0.4650 0.055 Uiso 1 1 calc R . . H18B H -0.1002 0.1946 0.4233 0.055 Uiso 1 1 calc R . . H18C H -0.1154 0.1858 0.5274 0.055 Uiso 1 1 calc R . . C19 C 0.14403(16) 0.17703(10) 0.69848(13) 0.0536(6) Uani 1 1 d . . . H19A H 0.1435 0.1384 0.7172 0.080 Uiso 1 1 calc R . . H19B H 0.1093 0.1985 0.7375 0.080 Uiso 1 1 calc R . . H19C H 0.1982 0.1914 0.7022 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 0.0203(2) 0.0182(2) 0.0216(2) 0.000 0.000 0.000 N1 0.0206(7) 0.0232(7) 0.0231(7) 0.0015(6) -0.0004(6) -0.0001(6) C1 0.0265(9) 0.0190(8) 0.0236(8) 0.0016(6) -0.0025(7) 0.0005(7) C8 0.0215(9) 0.0217(8) 0.0267(9) 0.0018(7) 0.0015(7) 0.0009(6) C6 0.0263(9) 0.0301(9) 0.0260(9) 0.0032(7) -0.0021(8) -0.0009(7) C3 0.0425(11) 0.0235(9) 0.0276(9) 0.0038(7) 0.0088(8) 0.0005(8) C4 0.0457(12) 0.0297(10) 0.0252(9) 0.0038(7) -0.0042(9) -0.0021(8) C2 0.0285(9) 0.0188(8) 0.0305(9) 0.0021(7) 0.0029(8) 0.0012(7) C9 0.0275(9) 0.0236(9) 0.0330(9) 0.0017(7) 0.0075(8) 0.0026(7) C5 0.0301(10) 0.0380(11) 0.0351(11) 0.0049(8) -0.0084(8) -0.0033(8) C7 0.0257(10) 0.0578(13) 0.0347(11) 0.0058(9) 0.0005(9) -0.0031(9) C10 0.0422(11) 0.0295(10) 0.0358(10) 0.0062(8) 0.0074(9) 0.0069(9) C14 0.0342(14) 0.0217(12) 0.0370(13) 0.000 0.0140(12) 0.000 C11 0.0647(15) 0.0334(11) 0.0442(11) 0.0146(9) 0.0154(11) 0.0160(11) C12 0.0739(16) 0.0221(10) 0.0533(13) 0.0073(9) 0.0260(12) 0.0076(10) C13 0.0553(18) 0.0209(13) 0.0457(16) 0.000 0.0222(15) 0.000 C15 0.0511(16) 0.0738(18) 0.113(3) 0.0169(17) 0.0000(16) -0.0090(14) C16 0.084(2) 0.0668(17) 0.088(2) -0.0001(15) -0.0049(18) -0.0194(16) C17 0.0665(19) 0.117(2) 0.085(2) 0.0237(18) 0.0056(18) 0.016(2) C18 0.0287(10) 0.0360(10) 0.0456(12) 0.0038(9) 0.0081(9) 0.0007(8) C19 0.0740(17) 0.0571(14) 0.0296(11) 0.0076(10) -0.0112(11) -0.0069(12) _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 1.9592(13) 8_455 ? Ni1 N1 1.9592(13) 3 ? Ni1 N1 1.9592(13) 6_455 ? Ni1 N1 1.9592(13) . ? N1 C8 1.322(2) . ? N1 C1 1.434(2) . ? C1 C6 1.391(2) . ? C1 C2 1.394(2) . ? C8 C8 1.428(3) 3 ? C8 C9 1.461(2) . ? C6 C5 1.393(2) . ? C6 C7 1.500(3) . ? C3 C4 1.377(3) . ? C3 C2 1.390(3) . ? C4 C5 1.387(3) . ? C4 C19 1.512(3) . ? C2 C18 1.498(3) . ? C9 C10 1.374(3) . ? C9 C14 1.417(2) . ? C10 C11 1.413(3) . ? C14 C13 1.390(4) . ? C14 C9 1.417(2) 3 ? C11 C12 1.362(3) . ? C12 C13 1.416(2) . ? C13 C12 1.416(2) 3 ? C15 C17 1.489(4) . ? C15 C16 1.499(4) . ? C16 C16 1.509(6) 2_565 ? C17 C17 1.523(6) 2_565 ? 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 N1 105.17(8) 8_455 3 ? N1 Ni1 N1 83.23(8) 8_455 6_455 ? N1 Ni1 N1 148.89(8) 3 6_455 ? N1 Ni1 N1 148.89(8) 8_455 . ? N1 Ni1 N1 83.23(8) 3 . ? N1 Ni1 N1 105.17(8) 6_455 . ? C8 N1 C1 114.94(13) . . ? C8 N1 Ni1 111.99(11) . . ? C1 N1 Ni1 132.59(10) . . ? C6 C1 C2 121.15(15) . . ? C6 C1 N1 118.70(15) . . ? C2 C1 N1 120.07(15) . . ? N1 C8 C8 116.34(9) . 3 ? N1 C8 C9 134.96(15) . . ? C8 C8 C9 108.67(10) 3 . ? C1 C6 C5 118.54(16) . . ? C1 C6 C7 120.35(15) . . ? C5 C6 C7 121.07(16) . . ? C4 C3 C2 122.38(17) . . ? C3 C4 C5 118.20(16) . . ? C3 C4 C19 120.85(18) . . ? C5 C4 C19 120.94(19) . . ? C3 C2 C1 118.07(17) . . ? C3 C2 C18 120.14(16) . . ? C1 C2 C18 121.74(16) . . ? C10 C9 C14 118.96(17) . . ? C10 C9 C8 136.22(17) . . ? C14 C9 C8 104.82(16) . . ? C4 C5 C6 121.61(18) . . ? C9 C10 C11 118.01(19) . . ? C13 C14 C9 123.49(11) . . ? C13 C14 C9 123.49(11) . 3 ? C9 C14 C9 113.0(2) . 3 ? C12 C11 C10 122.7(2) . . ? C11 C12 C13 120.72(19) . . ? C14 C13 C12 116.07(13) . . ? C14 C13 C12 116.07(13) . 3 ? C12 C13 C12 127.9(3) . 3 ? C17 C15 C16 111.7(2) . . ? C15 C16 C16 111.4(2) . 2_565 ? C15 C17 C17 110.7(2) . 2_565 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.271 _refine_diff_density_min -0.175 _refine_diff_density_rms 0.040 #=== END data_C44H52N2Ni_Compound5 _database_code_depnum_ccdc_archive 'CCDC 762666' #TrackingRef 'Ni-diimines-cif_files.cif' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C44 H52 N2 Ni' _chemical_formula_weight 667.59 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5009(6) _cell_length_b 17.8623(9) _cell_length_c 18.3510(9) _cell_angle_alpha 99.293(2) _cell_angle_beta 92.622(2) _cell_angle_gamma 99.846(2) _cell_volume 3655.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9963 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 24.01 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.563 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6688 _exptl_absorpt_correction_T_max 0.7450 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 40556 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 24.16 _reflns_number_total 11362 _reflns_number_gt 8634 _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^)+(0.0379P)^2^+3.4354P] 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 11362 _refine_ls_number_parameters 863 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.80018(3) 0.79042(2) 0.434971(19) 0.01889(10) Uani 1 1 d . . . Ni2 Ni 0.95606(3) 0.69939(2) 0.903929(19) 0.02030(10) Uani 1 1 d . . . N1 N 0.81823(19) 0.70525(13) 0.35725(12) 0.0192(5) Uani 1 1 d . . . N2 N 0.64416(19) 0.78069(13) 0.38156(12) 0.0189(5) Uani 1 1 d . . . N3 N 0.81777(18) 0.73783(13) 0.86812(12) 0.0188(5) Uani 1 1 d . . . N4 N 1.04358(18) 0.79629(12) 0.88291(12) 0.0176(5) Uani 1 1 d . . . C1 C 0.7247(2) 0.68616(16) 0.30769(15) 0.0198(6) Uani 1 1 d . . . C2 C 0.6326(2) 0.73011(15) 0.31914(15) 0.0188(6) Uani 1 1 d . . . C3 C 0.5432(2) 0.70341(16) 0.25583(15) 0.0221(6) Uani 1 1 d . . . C4 C 0.5853(2) 0.64362(16) 0.21019(16) 0.0250(7) Uani 1 1 d . . . C5 C 0.6946(2) 0.62950(16) 0.23887(16) 0.0239(7) Uani 1 1 d . . . C6 C 0.7464(3) 0.57360(17) 0.19975(16) 0.0308(7) Uani 1 1 d . . . H6 H 0.8190 0.5624 0.2181 0.037 Uiso 1 1 calc R . . C7 C 0.6892(3) 0.53293(19) 0.13126(18) 0.0431(9) Uani 1 1 d . . . H7 H 0.7252 0.4947 0.1034 0.052 Uiso 1 1 calc R . . C8 C 0.5841(3) 0.5467(2) 0.10394(18) 0.0442(9) Uani 1 1 d . . . H8 H 0.5484 0.5178 0.0580 0.053 Uiso 1 1 calc R . . C9 C 0.5275(3) 0.60350(18) 0.14302(16) 0.0318(7) Uani 1 1 d . . . C10 C 0.9268(3) 0.77060(17) 0.51060(15) 0.0252(7) Uani 1 1 d . . . H10 H 0.9485 0.7183 0.4991 0.030 Uiso 1 1 calc R . . C11 C 0.8218(3) 0.77118(16) 0.54359(15) 0.0258(7) Uani 1 1 d . . . H11 H 0.7811 0.7195 0.5520 0.031 Uiso 1 1 calc R . . C12 C 0.7918(3) 0.83851(17) 0.59542(16) 0.0329(7) Uani 1 1 d . . . H12A H 0.8325 0.8419 0.6448 0.039 Uiso 1 1 calc R . . H12B H 0.7055 0.8295 0.6008 0.039 Uiso 1 1 calc R . . C13 C 0.8278(3) 0.91527(17) 0.56789(16) 0.0314(7) Uani 1 1 d . . . H13A H 0.7770 0.9518 0.5884 0.038 Uiso 1 1 calc R . . H13B H 0.9107 0.9378 0.5861 0.038 Uiso 1 1 calc R . . C14 C 0.8165(3) 0.90484(15) 0.48404(16) 0.0249(7) Uani 1 1 d . . . H14 H 0.7564 0.9320 0.4639 0.030 Uiso 1 1 calc R . . C15 C 0.9084(2) 0.89626(15) 0.43922(16) 0.0242(7) Uani 1 1 d . . . H15 H 0.9040 0.9189 0.3930 0.029 Uiso 1 1 calc R . . C16 C 1.0319(3) 0.89141(17) 0.46731(17) 0.0293(7) Uani 1 1 d . . . H16A H 1.0733 0.9436 0.4908 0.035 Uiso 1 1 calc R . . H16B H 1.0761 0.8735 0.4248 0.035 Uiso 1 1 calc R . . C17 C 1.0324(3) 0.83646(17) 0.52357(17) 0.0302(7) Uani 1 1 d . . . H17A H 1.1060 0.8148 0.5209 0.036 Uiso 1 1 calc R . . H17B H 1.0326 0.8661 0.5741 0.036 Uiso 1 1 calc R . . C18 C 0.9012(2) 0.65318(16) 0.35234(15) 0.0219(6) Uani 1 1 d . . . C19 C 0.8761(2) 0.58593(16) 0.38347(16) 0.0256(7) Uani 1 1 d . . . C20 C 0.9569(3) 0.53552(18) 0.37539(18) 0.0348(8) Uani 1 1 d . . . H20 H 0.9418 0.4893 0.3954 0.042 Uiso 1 1 calc R . . C21 C 1.0579(3) 0.5515(2) 0.3390(2) 0.0420(9) Uani 1 1 d . . . H21 H 1.1104 0.5157 0.3327 0.050 Uiso 1 1 calc R . . C22 C 1.0828(3) 0.61937(19) 0.31160(18) 0.0338(8) Uani 1 1 d . . . H22 H 1.1536 0.6304 0.2876 0.041 Uiso 1 1 calc R . . C23 C 1.0059(2) 0.67227(17) 0.31837(16) 0.0255(7) Uani 1 1 d . . . C24 C 1.0331(2) 0.74733(18) 0.28838(16) 0.0284(7) Uani 1 1 d . . . H24 H 0.9938 0.7857 0.3194 0.034 Uiso 1 1 calc R . . C25 C 0.7673(3) 0.56751(17) 0.42536(17) 0.0318(7) Uani 1 1 d . . . H25 H 0.7303 0.6147 0.4338 0.038 Uiso 1 1 calc R . . C26 C 0.6756(3) 0.5023(2) 0.3808(2) 0.0461(9) Uani 1 1 d . . . H26A H 0.6550 0.5158 0.3328 0.069 Uiso 1 1 calc R . . H26B H 0.6044 0.4945 0.4081 0.069 Uiso 1 1 calc R . . H26C H 0.7084 0.4547 0.3731 0.069 Uiso 1 1 calc R . . C27 C 0.7979(3) 0.5477(2) 0.50158(19) 0.0492(10) Uani 1 1 d . . . H27A H 0.8290 0.4995 0.4950 0.074 Uiso 1 1 calc R . . H27B H 0.7265 0.5416 0.5288 0.074 Uiso 1 1 calc R . . H27C H 0.8577 0.5895 0.5295 0.074 Uiso 1 1 calc R . . C28 C 1.1654(3) 0.7807(2) 0.2945(2) 0.0529(10) Uani 1 1 d . . . H28A H 1.1986 0.7823 0.3450 0.079 Uiso 1 1 calc R . . H28B H 1.1771 0.8331 0.2830 0.079 Uiso 1 1 calc R . . H28C H 1.2053 0.7482 0.2594 0.079 Uiso 1 1 calc R . . C29 C 0.9816(3) 0.7388(2) 0.20861(18) 0.0503(10) Uani 1 1 d . . . H29A H 1.0112 0.6972 0.1775 0.076 Uiso 1 1 calc R . . H29B H 1.0056 0.7872 0.1902 0.076 Uiso 1 1 calc R . . H29C H 0.8951 0.7264 0.2069 0.076 Uiso 1 1 calc R . . C30 C 0.5531(2) 0.82548(16) 0.39845(15) 0.0211(6) Uani 1 1 d . . . C31 C 0.4715(2) 0.80243(17) 0.44937(16) 0.0258(7) Uani 1 1 d . . . C32 C 0.3876(3) 0.84745(19) 0.46881(17) 0.0331(8) Uani 1 1 d . . . H32 H 0.3316 0.8321 0.5025 0.040 Uiso 1 1 calc R . . C33 C 0.3828(3) 0.91408(19) 0.44061(18) 0.0344(8) Uani 1 1 d . . . H33 H 0.3240 0.9439 0.4546 0.041 Uiso 1 1 calc R . . C34 C 0.4638(3) 0.93689(18) 0.39212(17) 0.0310(7) Uani 1 1 d . . . H34 H 0.4605 0.9830 0.3732 0.037 Uiso 1 1 calc R . . C35 C 0.5509(2) 0.89396(16) 0.36986(15) 0.0234(7) Uani 1 1 d . . . C36 C 0.6396(3) 0.92395(17) 0.31759(16) 0.0280(7) Uani 1 1 d . . . H36 H 0.7031 0.8919 0.3150 0.034 Uiso 1 1 calc R . . C37 C 0.6982(3) 1.00790(18) 0.34531(18) 0.0382(8) Uani 1 1 d . . . H37A H 0.6390 1.0412 0.3438 0.057 Uiso 1 1 calc R . . H37B H 0.7613 1.0230 0.3136 0.057 Uiso 1 1 calc R . . H37C H 0.7318 1.0133 0.3963 0.057 Uiso 1 1 calc R . . C38 C 0.5823(3) 0.91632(19) 0.23892(17) 0.0377(8) Uani 1 1 d . . . H38A H 0.5521 0.8618 0.2190 0.057 Uiso 1 1 calc R . . H38B H 0.6414 0.9373 0.2072 0.057 Uiso 1 1 calc R . . H38C H 0.5168 0.9450 0.2403 0.057 Uiso 1 1 calc R . . C39 C 0.4750(3) 0.72850(19) 0.48014(18) 0.0353(8) Uani 1 1 d . . . H39 H 0.5590 0.7206 0.4818 0.042 Uiso 1 1 calc R . . C40 C 0.4354(3) 0.7323(2) 0.5590(2) 0.0535(10) Uani 1 1 d . . . H40A H 0.4803 0.7786 0.5907 0.080 Uiso 1 1 calc R . . H40B H 0.4499 0.6864 0.5783 0.080 Uiso 1 1 calc R . . H40C H 0.3508 0.7344 0.5584 0.080 Uiso 1 1 calc R . . C41 C 0.4015(4) 0.6586(2) 0.4297(2) 0.0583(11) Uani 1 1 d . . . H41A H 0.3183 0.6643 0.4272 0.088 Uiso 1 1 calc R . . H41B H 0.4092 0.6118 0.4494 0.088 Uiso 1 1 calc R . . H41C H 0.4299 0.6549 0.3799 0.088 Uiso 1 1 calc R . . C42 C 0.8492(2) 0.80541(15) 0.84698(14) 0.0176(6) Uani 1 1 d . . . C43 C 0.9730(2) 0.83601(15) 0.85205(14) 0.0181(6) Uani 1 1 d . . . C44 C 0.9979(3) 0.59820(17) 0.84629(18) 0.0344(8) Uani 1 1 d . . . H44 H 1.0059 0.5980 0.7922 0.041 Uiso 1 1 calc R . . C45 C 1.0949(3) 0.63979(17) 0.89204(16) 0.0270(7) Uani 1 1 d . . . H45 H 1.1605 0.6642 0.8649 0.032 Uiso 1 1 calc R . . C46 C 1.1353(3) 0.6195(2) 0.96451(18) 0.0391(8) Uani 1 1 d . . . H46A H 1.2223 0.6359 0.9728 0.047 Uiso 1 1 calc R . . H46B H 1.1173 0.5628 0.9610 0.047 Uiso 1 1 calc R . . C47 C 1.0784(3) 0.65626(19) 1.03051(17) 0.0367(8) Uani 1 1 d . . . H47A H 1.1334 0.7031 1.0555 0.044 Uiso 1 1 calc R . . H47B H 1.0667 0.6199 1.0660 0.044 Uiso 1 1 calc R . . C48 C 0.9605(3) 0.67834(17) 1.01172(16) 0.0270(7) Uani 1 1 d . . . H48 H 0.9370 0.7192 1.0491 0.032 Uiso 1 1 calc R . . C49 C 0.8674(3) 0.62842(18) 0.96974(17) 0.0318(8) Uani 1 1 d . . . H49 H 0.7872 0.6391 0.9816 0.038 Uiso 1 1 calc R . . C50 C 0.8707(4) 0.54410(19) 0.9393(2) 0.0510(10) Uani 1 1 d . . . H50A H 0.9214 0.5245 0.9742 0.061 Uiso 1 1 calc R . . H50B H 0.7897 0.5138 0.9374 0.061 Uiso 1 1 calc R . . C51 C 0.9158(3) 0.53014(19) 0.8637(2) 0.0499(10) Uani 1 1 d . . . H51A H 0.9575 0.4857 0.8600 0.060 Uiso 1 1 calc R . . H51B H 0.8475 0.5162 0.8262 0.060 Uiso 1 1 calc R . . C52 C 0.6935(2) 0.71275(16) 0.87486(15) 0.0209(6) Uani 1 1 d . . . C53 C 0.6412(2) 0.74479(16) 0.93740(16) 0.0254(7) Uani 1 1 d . . . C54 C 0.5192(3) 0.72183(18) 0.93975(18) 0.0329(8) Uani 1 1 d . . . H54 H 0.4808 0.7436 0.9806 0.039 Uiso 1 1 calc R . . C55 C 0.4537(3) 0.66846(19) 0.88418(19) 0.0384(8) Uani 1 1 d . . . H55 H 0.3705 0.6548 0.8863 0.046 Uiso 1 1 calc R . . C56 C 0.5079(3) 0.63468(18) 0.82543(18) 0.0348(8) Uani 1 1 d . . . H56 H 0.4617 0.5967 0.7882 0.042 Uiso 1 1 calc R . . C57 C 0.6292(2) 0.65501(16) 0.81936(16) 0.0245(7) Uani 1 1 d . . . C58 C 0.7105(3) 0.80289(17) 1.00113(16) 0.0292(7) Uani 1 1 d . . . H58 H 0.7959 0.8100 0.9908 0.035 Uiso 1 1 calc R . . C59 C 0.6887(3) 0.61814(17) 0.75464(16) 0.0309(7) Uani 1 1 d . . . H59 H 0.7745 0.6240 0.7707 0.037 Uiso 1 1 calc R . . C60 C 0.6408(3) 0.53186(18) 0.7312(2) 0.0433(9) Uani 1 1 d . . . H60A H 0.6440 0.5061 0.7744 0.065 Uiso 1 1 calc R . . H60B H 0.6890 0.5099 0.6936 0.065 Uiso 1 1 calc R . . H60C H 0.5586 0.5243 0.7106 0.065 Uiso 1 1 calc R . . C61 C 0.6803(4) 0.6597(2) 0.6892(2) 0.0676(13) Uani 1 1 d . . . H61A H 0.5972 0.6535 0.6709 0.101 Uiso 1 1 calc R . . H61B H 0.7254 0.6378 0.6496 0.101 Uiso 1 1 calc R . . H61C H 0.7130 0.7147 0.7047 0.101 Uiso 1 1 calc R . . C62 C 1.1683(2) 0.82383(15) 0.88178(15) 0.0188(6) Uani 1 1 d . . . C63 C 1.2301(2) 0.86661(16) 0.94775(15) 0.0212(6) Uani 1 1 d . . . C64 C 1.3467(2) 0.90163(17) 0.94350(17) 0.0285(7) Uani 1 1 d . . . H64 H 1.3896 0.9328 0.9864 0.034 Uiso 1 1 calc R . . C65 C 1.2250(2) 0.80880(16) 0.81618(15) 0.0215(6) Uani 1 1 d . . . C66 C 1.1692(2) 0.87349(17) 1.01966(15) 0.0253(7) Uani 1 1 d . . . H66 H 1.1099 0.8250 1.0170 0.030 Uiso 1 1 calc R . . C67 C 1.1622(3) 0.75381(17) 0.74824(15) 0.0264(7) Uani 1 1 d . . . H67 H 1.0842 0.7287 0.7628 0.032 Uiso 1 1 calc R . . C68 C 1.2309(3) 0.68961(18) 0.72097(17) 0.0367(8) Uani 1 1 d . . . H68A H 1.3065 0.7122 0.7041 0.055 Uiso 1 1 calc R . . H68B H 1.1844 0.6534 0.6799 0.055 Uiso 1 1 calc R . . H68C H 1.2458 0.6621 0.7616 0.055 Uiso 1 1 calc R . . C69 C 1.1373(3) 0.79566(19) 0.68437(17) 0.0380(8) Uani 1 1 d . . . H69A H 1.0913 0.8357 0.7013 0.057 Uiso 1 1 calc R . . H69B H 1.0922 0.7586 0.6433 0.057 Uiso 1 1 calc R . . H69C H 1.2123 0.8194 0.6676 0.057 Uiso 1 1 calc R . . C70 C 0.8752(2) 0.91839(15) 0.79975(14) 0.0172(6) Uani 1 1 d . . . C71 C 0.9908(2) 0.90890(15) 0.82294(14) 0.0183(6) Uani 1 1 d . . . C72 C 1.0851(2) 0.96446(16) 0.81473(15) 0.0230(6) Uani 1 1 d . . . H72 H 1.1631 0.9606 0.8310 0.028 Uiso 1 1 calc R . . C73 C 1.0643(2) 1.02761(16) 0.78154(16) 0.0253(7) Uani 1 1 d . . . H73 H 1.1297 1.0663 0.7763 0.030 Uiso 1 1 calc R . . C74 C 0.9531(2) 1.03527(16) 0.75649(15) 0.0241(7) Uani 1 1 d . . . H74 H 0.9433 1.0775 0.7328 0.029 Uiso 1 1 calc R . . C75 C 0.8525(2) 0.97971(15) 0.76608(14) 0.0194(6) Uani 1 1 d . . . C76 C 0.7323(2) 0.97954(17) 0.74477(15) 0.0242(7) Uani 1 1 d . . . H76 H 0.7119 1.0198 0.7215 0.029 Uiso 1 1 calc R . . C77 C 0.6460(2) 0.92155(16) 0.75770(15) 0.0242(7) Uani 1 1 d . . . H77 H 0.5662 0.9226 0.7428 0.029 Uiso 1 1 calc R . . C100 C 0.7855(2) 0.85822(15) 0.81382(14) 0.0181(6) Uani 1 1 d . . . C101 C 0.6701(2) 0.85978(16) 0.79247(15) 0.0226(6) Uani 1 1 d . . . H101 H 0.6078 0.8204 0.8008 0.027 Uiso 1 1 calc R . . C102 C 0.6993(3) 0.7733(2) 1.07480(17) 0.0398(8) Uani 1 1 d . . . H10A H 0.6169 0.7683 1.0877 0.060 Uiso 1 1 calc R . . H10B H 0.7503 0.8098 1.1138 0.060 Uiso 1 1 calc R . . H10C H 0.7237 0.7229 1.0701 0.060 Uiso 1 1 calc R . . C103 C 0.6731(3) 0.88138(18) 1.00748(19) 0.0413(9) Uani 1 1 d . . . H10D H 0.6794 0.8993 0.9598 0.062 Uiso 1 1 calc R . . H10E H 0.7249 0.9184 1.0457 0.062 Uiso 1 1 calc R . . H10F H 0.5911 0.8769 1.0210 0.062 Uiso 1 1 calc R . . C104 C 1.3416(2) 0.84457(17) 0.81598(17) 0.0287(7) Uani 1 1 d . . . H104 H 1.3816 0.8363 0.7720 0.034 Uiso 1 1 calc R . . C105 C 1.4012(3) 0.89198(18) 0.87798(17) 0.0329(8) Uani 1 1 d . . . H105 H 1.4799 0.9180 0.8756 0.039 Uiso 1 1 calc R . . C106 C 1.2545(3) 0.8791(2) 1.08737(17) 0.0415(9) Uani 1 1 d . . . H10G H 1.3027 0.8387 1.0782 0.062 Uiso 1 1 calc R . . H10H H 1.2094 0.8722 1.1306 0.062 Uiso 1 1 calc R . . H10I H 1.3062 0.9298 1.0967 0.062 Uiso 1 1 calc R . . C107 C 1.1009(3) 0.94021(18) 1.02935(18) 0.0358(8) Uani 1 1 d . . . H10J H 1.1566 0.9892 1.0351 0.054 Uiso 1 1 calc R . . H10K H 1.0562 0.9389 1.0735 0.054 Uiso 1 1 calc R . . H10L H 1.0460 0.9353 0.9857 0.054 Uiso 1 1 calc R . . C108 C 0.4373(3) 0.72207(18) 0.23433(17) 0.0309(7) Uani 1 1 d . . . H108 H 0.4052 0.7610 0.2642 0.037 Uiso 1 1 calc R . . C109 C 0.3769(3) 0.6819(2) 0.16648(19) 0.0408(9) Uani 1 1 d . . . H109 H 0.3040 0.6950 0.1513 0.049 Uiso 1 1 calc R . . C110 C 0.4192(3) 0.6253(2) 0.12195(19) 0.0413(9) Uani 1 1 d . . . H110 H 0.3760 0.6003 0.0767 0.050 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 0.01699(19) 0.0238(2) 0.01548(19) 0.00103(15) -0.00145(15) 0.00557(15) Ni2 0.01742(19) 0.0248(2) 0.0206(2) 0.00831(15) -0.00013(15) 0.00550(15) N1 0.0157(12) 0.0259(13) 0.0165(12) 0.0010(10) 0.0019(10) 0.0069(10) N2 0.0157(12) 0.0263(13) 0.0158(12) 0.0039(10) 0.0009(10) 0.0069(10) N3 0.0141(12) 0.0253(13) 0.0164(12) 0.0045(10) -0.0016(10) 0.0021(10) N4 0.0138(12) 0.0237(13) 0.0156(12) 0.0036(10) 0.0001(10) 0.0045(10) C1 0.0151(14) 0.0262(16) 0.0177(15) 0.0032(12) 0.0000(12) 0.0034(12) C2 0.0129(14) 0.0252(15) 0.0178(15) 0.0036(12) -0.0004(11) 0.0027(11) C3 0.0146(14) 0.0334(17) 0.0178(15) 0.0068(13) -0.0011(12) 0.0017(12) C4 0.0219(16) 0.0289(17) 0.0218(16) 0.0062(13) -0.0028(13) -0.0027(13) C5 0.0220(15) 0.0255(16) 0.0223(16) 0.0025(13) -0.0015(13) 0.0016(12) C6 0.0306(17) 0.0314(18) 0.0278(18) -0.0026(14) -0.0031(14) 0.0071(14) C7 0.050(2) 0.041(2) 0.033(2) -0.0111(16) 0.0019(17) 0.0106(17) C8 0.055(2) 0.045(2) 0.0236(18) -0.0098(16) -0.0113(17) 0.0020(18) C9 0.0319(18) 0.0371(19) 0.0215(17) 0.0042(14) -0.0061(14) -0.0044(14) C10 0.0303(17) 0.0268(16) 0.0195(16) 0.0054(12) -0.0068(13) 0.0084(13) C11 0.0373(18) 0.0251(16) 0.0143(15) 0.0048(12) -0.0037(13) 0.0044(13) C12 0.044(2) 0.0343(18) 0.0201(16) 0.0036(13) 0.0041(14) 0.0066(15) C13 0.0418(19) 0.0316(18) 0.0205(16) 0.0001(13) 0.0012(14) 0.0103(15) C14 0.0321(17) 0.0167(15) 0.0253(17) 0.0003(12) -0.0052(14) 0.0081(12) C15 0.0285(17) 0.0211(16) 0.0219(16) 0.0050(12) -0.0021(13) 0.0009(13) C16 0.0229(16) 0.0329(18) 0.0276(17) 0.0027(14) -0.0041(13) -0.0029(13) C17 0.0256(17) 0.0344(18) 0.0288(18) 0.0030(14) -0.0071(14) 0.0047(14) C18 0.0167(15) 0.0286(17) 0.0184(15) -0.0045(12) -0.0049(12) 0.0085(12) C19 0.0244(16) 0.0249(16) 0.0261(17) -0.0013(13) -0.0051(13) 0.0076(13) C20 0.0341(19) 0.0288(18) 0.042(2) 0.0024(15) -0.0056(16) 0.0133(14) C21 0.0324(19) 0.043(2) 0.052(2) -0.0020(17) -0.0054(17) 0.0230(16) C22 0.0211(16) 0.044(2) 0.0352(19) -0.0031(15) 0.0006(14) 0.0118(14) C23 0.0186(15) 0.0355(18) 0.0210(16) -0.0030(13) -0.0048(13) 0.0100(13) C24 0.0177(15) 0.0388(19) 0.0269(17) -0.0001(14) 0.0028(13) 0.0056(13) C25 0.0339(18) 0.0252(17) 0.0373(19) 0.0041(14) 0.0040(15) 0.0087(14) C26 0.038(2) 0.048(2) 0.050(2) 0.0092(18) 0.0030(17) 0.0008(17) C27 0.061(3) 0.049(2) 0.039(2) 0.0139(17) 0.0036(19) 0.0055(19) C28 0.0236(18) 0.048(2) 0.086(3) 0.009(2) 0.0060(19) 0.0049(16) C29 0.060(2) 0.058(2) 0.0266(19) 0.0089(17) 0.0003(18) -0.0062(19) C30 0.0138(14) 0.0301(17) 0.0191(15) -0.0003(12) -0.0005(12) 0.0083(12) C31 0.0156(15) 0.0384(18) 0.0232(16) 0.0029(13) 0.0021(12) 0.0064(13) C32 0.0215(16) 0.051(2) 0.0291(18) 0.0071(15) 0.0089(14) 0.0105(15) C33 0.0222(17) 0.047(2) 0.0374(19) 0.0009(16) 0.0046(15) 0.0208(15) C34 0.0272(17) 0.0360(18) 0.0328(18) 0.0043(14) 0.0001(14) 0.0159(14) C35 0.0186(15) 0.0300(17) 0.0218(16) 0.0017(13) 0.0003(12) 0.0083(13) C36 0.0270(17) 0.0340(18) 0.0291(17) 0.0119(14) 0.0075(14) 0.0149(14) C37 0.0358(19) 0.042(2) 0.039(2) 0.0158(16) 0.0056(16) 0.0044(16) C38 0.043(2) 0.048(2) 0.0265(18) 0.0142(15) 0.0079(15) 0.0137(16) C39 0.0259(17) 0.050(2) 0.0365(19) 0.0187(16) 0.0119(15) 0.0129(15) C40 0.050(2) 0.079(3) 0.041(2) 0.031(2) 0.0172(19) 0.015(2) C41 0.073(3) 0.046(2) 0.055(3) 0.0187(19) 0.013(2) -0.002(2) C42 0.0161(14) 0.0223(15) 0.0150(14) 0.0037(12) 0.0013(11) 0.0042(11) C43 0.0161(14) 0.0244(15) 0.0147(14) 0.0026(12) 0.0014(11) 0.0066(12) C44 0.041(2) 0.0295(18) 0.0342(19) 0.0001(14) 0.0001(16) 0.0167(15) C45 0.0252(16) 0.0325(17) 0.0285(17) 0.0085(14) 0.0078(14) 0.0147(14) C46 0.0283(18) 0.061(2) 0.038(2) 0.0235(17) 0.0039(15) 0.0200(16) C47 0.0395(19) 0.047(2) 0.0287(18) 0.0117(15) -0.0025(15) 0.0184(16) C48 0.0274(17) 0.0391(18) 0.0196(16) 0.0120(13) 0.0066(13) 0.0124(14) C49 0.0291(17) 0.0411(19) 0.0297(18) 0.0233(15) 0.0035(14) 0.0020(15) C50 0.065(3) 0.035(2) 0.052(2) 0.0249(18) -0.007(2) -0.0083(18) C51 0.048(2) 0.029(2) 0.070(3) 0.0047(18) -0.008(2) 0.0093(17) C52 0.0140(14) 0.0273(16) 0.0241(16) 0.0117(13) -0.0002(12) 0.0050(12) C53 0.0207(16) 0.0296(17) 0.0276(17) 0.0097(13) 0.0036(13) 0.0044(13) C54 0.0254(17) 0.0396(19) 0.0351(19) 0.0081(15) 0.0106(15) 0.0063(14) C55 0.0139(16) 0.049(2) 0.050(2) 0.0081(17) 0.0026(15) -0.0013(15) C56 0.0198(16) 0.042(2) 0.036(2) 0.0014(15) -0.0050(14) -0.0041(14) C57 0.0186(15) 0.0302(17) 0.0252(16) 0.0093(13) -0.0025(13) 0.0030(13) C58 0.0240(16) 0.0370(18) 0.0248(17) 0.0030(14) 0.0039(13) 0.0025(14) C59 0.0256(17) 0.0379(19) 0.0259(17) 0.0011(14) 0.0001(14) 0.0007(14) C60 0.0337(19) 0.042(2) 0.048(2) -0.0047(17) -0.0007(17) 0.0030(16) C61 0.125(4) 0.059(3) 0.026(2) 0.0120(18) 0.020(2) 0.028(3) C62 0.0141(14) 0.0236(15) 0.0212(15) 0.0084(12) -0.0007(12) 0.0066(12) C63 0.0183(15) 0.0262(16) 0.0212(16) 0.0040(12) 0.0003(12) 0.0097(12) C64 0.0178(16) 0.0355(18) 0.0287(17) -0.0024(14) -0.0026(13) 0.0044(13) C65 0.0187(15) 0.0283(16) 0.0195(15) 0.0060(12) 0.0014(12) 0.0080(12) C66 0.0236(16) 0.0301(17) 0.0214(16) 0.0027(13) 0.0016(13) 0.0043(13) C67 0.0236(16) 0.0354(18) 0.0200(16) 0.0045(13) 0.0000(13) 0.0052(13) C68 0.042(2) 0.040(2) 0.0272(18) 0.0019(15) 0.0032(15) 0.0103(16) C69 0.047(2) 0.044(2) 0.0233(18) 0.0046(15) -0.0045(15) 0.0112(16) C70 0.0164(14) 0.0215(15) 0.0145(14) 0.0017(11) 0.0025(11) 0.0061(11) C71 0.0152(14) 0.0244(15) 0.0167(15) 0.0039(12) 0.0027(11) 0.0068(12) C72 0.0163(15) 0.0290(17) 0.0244(16) 0.0055(13) 0.0015(12) 0.0054(12) C73 0.0193(15) 0.0282(17) 0.0289(17) 0.0085(13) 0.0069(13) 0.0013(13) C74 0.0273(17) 0.0246(16) 0.0228(16) 0.0074(13) 0.0030(13) 0.0078(13) C75 0.0218(15) 0.0250(16) 0.0125(14) 0.0015(12) 0.0021(12) 0.0084(12) C76 0.0278(17) 0.0303(17) 0.0178(15) 0.0062(13) -0.0013(13) 0.0137(13) C77 0.0173(15) 0.0346(17) 0.0233(16) 0.0063(13) -0.0020(12) 0.0114(13) C100 0.0164(14) 0.0235(15) 0.0157(14) 0.0030(12) 0.0030(12) 0.0068(12) C101 0.0160(15) 0.0302(17) 0.0223(16) 0.0063(13) 0.0022(12) 0.0044(12) C102 0.045(2) 0.049(2) 0.0260(18) 0.0059(15) 0.0038(16) 0.0100(17) C103 0.046(2) 0.038(2) 0.036(2) 0.0002(15) 0.0028(17) 0.0026(16) C104 0.0199(16) 0.0397(19) 0.0274(17) 0.0045(14) 0.0064(13) 0.0078(14) C105 0.0143(15) 0.044(2) 0.039(2) 0.0036(15) 0.0036(14) 0.0021(14) C106 0.045(2) 0.058(2) 0.0219(18) 0.0037(16) -0.0017(15) 0.0139(17) C107 0.0332(18) 0.043(2) 0.0315(19) -0.0005(15) 0.0072(15) 0.0142(15) C108 0.0213(16) 0.0408(19) 0.0310(18) 0.0079(14) -0.0015(14) 0.0060(14) C109 0.0214(17) 0.062(2) 0.038(2) 0.0130(18) -0.0111(15) 0.0031(16) C110 0.0340(19) 0.054(2) 0.0287(19) 0.0059(17) -0.0171(16) -0.0066(17) _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 1.956(2) . ? Ni1 N2 1.972(2) . ? Ni1 C15 2.066(3) . ? Ni1 C14 2.069(3) . ? Ni1 C10 2.079(3) . ? Ni1 C11 2.088(3) . ? Ni2 N4 1.953(2) . ? Ni2 N3 1.964(2) . ? Ni2 C45 2.066(3) . ? Ni2 C49 2.067(3) . ? Ni2 C48 2.072(3) . ? Ni2 C44 2.084(3) . ? N1 C1 1.336(3) . ? N1 C18 1.438(3) . ? N2 C2 1.325(3) . ? N2 C30 1.439(3) . ? N3 C42 1.324(3) . ? N3 C52 1.440(3) . ? N4 C43 1.330(3) . ? N4 C62 1.436(3) . ? C1 C2 1.426(4) . ? C1 C5 1.472(4) . ? C2 C3 1.476(4) . ? C3 C108 1.375(4) . ? C3 C4 1.415(4) . ? C4 C9 1.397(4) . ? C4 C5 1.419(4) . ? C5 C6 1.371(4) . ? C6 C7 1.417(4) . ? C7 C8 1.363(5) . ? C8 C9 1.414(5) . ? C9 C110 1.422(4) . ? C10 C11 1.376(4) . ? C10 C17 1.520(4) . ? C11 C12 1.508(4) . ? C12 C13 1.535(4) . ? C13 C14 1.517(4) . ? C14 C15 1.383(4) . ? C15 C16 1.509(4) . ? C16 C17 1.536(4) . ? C18 C23 1.398(4) . ? C18 C19 1.404(4) . ? C19 C20 1.397(4) . ? C19 C25 1.515(4) . ? C20 C21 1.378(5) . ? C21 C22 1.376(5) . ? C22 C23 1.395(4) . ? C23 C24 1.520(4) . ? C24 C29 1.528(4) . ? C24 C28 1.528(4) . ? C25 C26 1.527(4) . ? C25 C27 1.537(4) . ? C30 C35 1.410(4) . ? C30 C31 1.413(4) . ? C31 C32 1.382(4) . ? C31 C39 1.524(4) . ? C32 C33 1.380(4) . ? C33 C34 1.374(4) . ? C34 C35 1.399(4) . ? C35 C36 1.522(4) . ? C36 C37 1.529(4) . ? C36 C38 1.535(4) . ? C39 C41 1.524(5) . ? C39 C40 1.531(4) . ? C42 C43 1.428(4) . ? C42 C100 1.476(4) . ? C43 C71 1.472(4) . ? C44 C45 1.390(4) . ? C44 C51 1.494(5) . ? C45 C46 1.507(4) . ? C46 C47 1.513(4) . ? C47 C48 1.515(4) . ? C48 C49 1.383(4) . ? C49 C50 1.527(5) . ? C50 C51 1.501(5) . ? C52 C53 1.405(4) . ? C52 C57 1.407(4) . ? C53 C54 1.398(4) . ? C53 C58 1.523(4) . ? C54 C55 1.373(4) . ? C55 C56 1.377(5) . ? C56 C57 1.394(4) . ? C57 C59 1.513(4) . ? C58 C103 1.524(4) . ? C58 C102 1.532(4) . ? C59 C61 1.519(5) . ? C59 C60 1.529(4) . ? C62 C65 1.405(4) . ? C62 C63 1.411(4) . ? C63 C64 1.391(4) . ? C63 C66 1.519(4) . ? C64 C105 1.381(4) . ? C65 C104 1.384(4) . ? C65 C67 1.523(4) . ? C66 C106 1.527(4) . ? C66 C107 1.528(4) . ? C67 C69 1.530(4) . ? C67 C68 1.533(4) . ? C70 C75 1.397(4) . ? C70 C100 1.421(4) . ? C70 C71 1.423(4) . ? C71 C72 1.371(4) . ? C72 C73 1.415(4) . ? C73 C74 1.375(4) . ? C74 C75 1.427(4) . ? C75 C76 1.418(4) . ? C76 C77 1.365(4) . ? C77 C101 1.420(4) . ? C100 C101 1.373(4) . ? C104 C105 1.378(4) . ? C108 C109 1.417(4) . ? C109 C110 1.365(5) . ? 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 83.44(9) . . ? N1 Ni1 C15 118.64(11) . . ? N2 Ni1 C15 114.02(10) . . ? N1 Ni1 C14 155.48(11) . . ? N2 Ni1 C14 97.19(10) . . ? C15 Ni1 C14 39.07(11) . . ? N1 Ni1 C10 95.74(10) . . ? N2 Ni1 C10 158.53(10) . . ? C15 Ni1 C10 85.29(11) . . ? C14 Ni1 C10 92.35(11) . . ? N1 Ni1 C11 115.90(10) . . ? N2 Ni1 C11 123.33(11) . . ? C15 Ni1 C11 102.19(11) . . ? C14 Ni1 C11 84.32(11) . . ? C10 Ni1 C11 38.57(11) . . ? N4 Ni2 N3 83.68(9) . . ? N4 Ni2 C45 95.81(11) . . ? N3 Ni2 C45 154.46(11) . . ? N4 Ni2 C49 154.98(11) . . ? N3 Ni2 C49 96.76(11) . . ? C45 Ni2 C49 94.26(12) . . ? N4 Ni2 C48 119.28(11) . . ? N3 Ni2 C48 117.21(10) . . ? C45 Ni2 C48 85.38(11) . . ? C49 Ni2 C48 39.03(11) . . ? N4 Ni2 C44 116.69(11) . . ? N3 Ni2 C44 119.18(11) . . ? C45 Ni2 C44 39.12(12) . . ? C49 Ni2 C44 85.03(13) . . ? C48 Ni2 C44 101.61(13) . . ? C1 N1 C18 116.2(2) . . ? C1 N1 Ni1 111.59(17) . . ? C18 N1 Ni1 131.11(17) . . ? C2 N2 C30 119.6(2) . . ? C2 N2 Ni1 111.59(17) . . ? C30 N2 Ni1 128.47(17) . . ? C42 N3 C52 116.9(2) . . ? C42 N3 Ni2 111.39(17) . . ? C52 N3 Ni2 130.46(17) . . ? C43 N4 C62 115.6(2) . . ? C43 N4 Ni2 111.74(17) . . ? C62 N4 Ni2 131.44(17) . . ? N1 C1 C2 116.7(2) . . ? N1 C1 C5 133.9(3) . . ? C2 C1 C5 109.3(2) . . ? N2 C2 C1 116.2(2) . . ? N2 C2 C3 136.1(2) . . ? C1 C2 C3 107.7(2) . . ? C108 C3 C4 118.4(3) . . ? C108 C3 C2 136.0(3) . . ? C4 C3 C2 105.5(2) . . ? C9 C4 C3 124.0(3) . . ? C9 C4 C5 123.1(3) . . ? C3 C4 C5 112.9(2) . . ? C6 C5 C4 119.1(3) . . ? C6 C5 C1 136.3(3) . . ? C4 C5 C1 104.6(2) . . ? C5 C6 C7 118.4(3) . . ? C8 C7 C6 122.3(3) . . ? C7 C8 C9 121.0(3) . . ? C4 C9 C8 116.2(3) . . ? C4 C9 C110 115.9(3) . . ? C8 C9 C110 127.9(3) . . ? C11 C10 C17 125.2(3) . . ? C11 C10 Ni1 71.07(16) . . ? C17 C10 Ni1 110.76(19) . . ? C10 C11 C12 125.2(3) . . ? C10 C11 Ni1 70.36(16) . . ? C12 C11 Ni1 108.74(19) . . ? C11 C12 C13 112.4(2) . . ? C14 C13 C12 111.8(2) . . ? C15 C14 C13 124.7(3) . . ? C15 C14 Ni1 70.34(16) . . ? C13 C14 Ni1 112.20(19) . . ? C14 C15 C16 124.2(3) . . ? C14 C15 Ni1 70.59(16) . . ? C16 C15 Ni1 108.95(19) . . ? C15 C16 C17 112.7(2) . . ? C10 C17 C16 113.1(2) . . ? C23 C18 C19 122.0(3) . . ? C23 C18 N1 118.8(2) . . ? C19 C18 N1 119.2(2) . . ? C20 C19 C18 117.5(3) . . ? C20 C19 C25 120.0(3) . . ? C18 C19 C25 122.5(3) . . ? C21 C20 C19 121.3(3) . . ? C22 C21 C20 120.0(3) . . ? C21 C22 C23 121.3(3) . . ? C22 C23 C18 117.7(3) . . ? C22 C23 C24 121.5(3) . . ? C18 C23 C24 120.8(2) . . ? C23 C24 C29 112.0(2) . . ? C23 C24 C28 112.8(3) . . ? C29 C24 C28 110.2(3) . . ? C19 C25 C26 111.8(3) . . ? C19 C25 C27 112.2(3) . . ? C26 C25 C27 109.9(3) . . ? C35 C30 C31 120.7(2) . . ? C35 C30 N2 121.1(2) . . ? C31 C30 N2 118.1(2) . . ? C32 C31 C30 118.4(3) . . ? C32 C31 C39 121.4(3) . . ? C30 C31 C39 120.2(3) . . ? C33 C32 C31 121.8(3) . . ? C34 C33 C32 119.5(3) . . ? C33 C34 C35 121.7(3) . . ? C34 C35 C30 117.9(3) . . ? C34 C35 C36 118.8(3) . . ? C30 C35 C36 123.4(2) . . ? C35 C36 C37 112.0(2) . . ? C35 C36 C38 111.8(2) . . ? C37 C36 C38 109.3(2) . . ? C31 C39 C41 111.4(3) . . ? C31 C39 C40 113.1(3) . . ? C41 C39 C40 109.8(3) . . ? N3 C42 C43 116.7(2) . . ? N3 C42 C100 134.8(2) . . ? C43 C42 C100 108.3(2) . . ? N4 C43 C42 116.2(2) . . ? N4 C43 C71 134.9(2) . . ? C42 C43 C71 108.8(2) . . ? C45 C44 C51 125.0(3) . . ? C45 C44 Ni2 69.73(17) . . ? C51 C44 Ni2 109.7(2) . . ? C44 C45 C46 124.3(3) . . ? C44 C45 Ni2 71.15(17) . . ? C46 C45 Ni2 111.6(2) . . ? C45 C46 C47 113.8(3) . . ? C46 C47 C48 114.5(3) . . ? C49 C48 C47 123.8(3) . . ? C49 C48 Ni2 70.26(16) . . ? C47 C48 Ni2 108.8(2) . . ? C48 C49 C50 123.6(3) . . ? C48 C49 Ni2 70.71(16) . . ? C50 C49 Ni2 110.2(2) . . ? C51 C50 C49 114.8(3) . . ? C44 C51 C50 113.3(3) . . ? C53 C52 C57 122.2(2) . . ? C53 C52 N3 119.2(2) . . ? C57 C52 N3 118.6(2) . . ? C54 C53 C52 117.3(3) . . ? C54 C53 C58 119.4(3) . . ? C52 C53 C58 123.3(2) . . ? C55 C54 C53 121.3(3) . . ? C54 C55 C56 120.4(3) . . ? C55 C56 C57 121.4(3) . . ? C56 C57 C52 117.2(3) . . ? C56 C57 C59 121.4(3) . . ? C52 C57 C59 121.3(2) . . ? C53 C58 C103 112.0(2) . . ? C53 C58 C102 111.5(2) . . ? C103 C58 C102 110.2(3) . . ? C57 C59 C61 111.0(3) . . ? C57 C59 C60 113.1(3) . . ? C61 C59 C60 110.4(3) . . ? C65 C62 C63 121.9(2) . . ? C65 C62 N4 120.2(2) . . ? C63 C62 N4 118.0(2) . . ? C64 C63 C62 117.3(3) . . ? C64 C63 C66 122.4(3) . . ? C62 C63 C66 120.2(2) . . ? C105 C64 C63 121.2(3) . . ? C104 C65 C62 117.4(3) . . ? C104 C65 C67 120.9(3) . . ? C62 C65 C67 121.6(2) . . ? C63 C66 C106 112.6(2) . . ? C63 C66 C107 112.4(2) . . ? C106 C66 C107 110.7(2) . . ? C65 C67 C69 112.4(2) . . ? C65 C67 C68 112.4(2) . . ? C69 C67 C68 109.3(2) . . ? C75 C70 C100 123.7(2) . . ? C75 C70 C71 123.6(2) . . ? C100 C70 C71 112.7(2) . . ? C72 C71 C70 118.5(2) . . ? C72 C71 C43 136.5(2) . . ? C70 C71 C43 105.0(2) . . ? C71 C72 C73 118.9(3) . . ? C74 C73 C72 122.6(3) . . ? C73 C74 C75 120.0(3) . . ? C70 C75 C76 116.4(2) . . ? C70 C75 C74 116.3(2) . . ? C76 C75 C74 127.3(3) . . ? C77 C76 C75 120.0(3) . . ? C76 C77 C101 123.0(3) . . ? C101 C100 C70 118.4(2) . . ? C101 C100 C42 136.4(3) . . ? C70 C100 C42 105.2(2) . . ? C100 C101 C77 118.5(3) . . ? C105 C104 C65 121.6(3) . . ? C104 C105 C64 120.0(3) . . ? C3 C108 C109 118.4(3) . . ? C110 C109 C108 122.8(3) . . ? C109 C110 C9 120.3(3) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 24.16 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.698 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.055 #=== END data_C40H48N2Ni_Compound6 _database_code_depnum_ccdc_archive 'CCDC 762667' #TrackingRef 'Ni-diimines-cif_files.cif' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C40 H48 N2 Ni' _chemical_formula_weight 615.51 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2811(5) _cell_length_b 12.4920(5) _cell_length_c 13.1402(5) _cell_angle_alpha 74.338(2) _cell_angle_beta 75.174(2) _cell_angle_gamma 64.761(2) _cell_volume 1732.68(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9923 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 33.38 _exptl_crystal_description irregular _exptl_crystal_colour blue _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.180 _exptl_crystal_density_method ? _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 0.589 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6892 _exptl_absorpt_correction_T_max 0.7466 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 30569 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6075 _reflns_number_gt 5676 _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^)+(0.0451P)^2^+4.2667P] 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 6075 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 -0.03335(3) 0.20546(4) 0.21846(3) 0.02199(13) Uani 1 1 d . . . N1 N -0.1843(2) 0.1882(2) 0.23009(19) 0.0212(5) Uani 1 1 d . . . N2 N 0.0091(2) 0.1334(2) 0.09461(19) 0.0217(5) Uani 1 1 d . . . C1 C -0.1890(3) 0.1441(3) 0.1521(2) 0.0240(6) Uani 1 1 d . . . H1A H -0.2589 0.1322 0.1474 0.029 Uiso 1 1 calc R . . C2 C -0.0805(3) 0.1153(3) 0.0752(2) 0.0241(6) Uani 1 1 d . . . H2A H -0.0735 0.0850 0.0138 0.029 Uiso 1 1 calc R . . C3 C -0.0226(3) 0.2803(3) 0.3174(2) 0.0243(6) Uani 1 1 d . . . H3A H 0.0126 0.2018 0.3663 0.029 Uiso 1 1 calc R . . C4 C 0.0752(3) 0.2568(3) 0.2474(2) 0.0235(6) Uani 1 1 d . . . H4A H 0.0392 0.3372 0.2014 0.028 Uiso 1 1 calc R . . C5 C -0.2879(3) 0.2174(3) 0.3138(2) 0.0232(6) Uani 1 1 d . . . C6 C -0.3101(3) 0.1246(3) 0.3917(2) 0.0262(6) Uani 1 1 d . . . C7 C -0.4056(3) 0.1577(3) 0.4772(3) 0.0343(8) Uani 1 1 d . . . H7A H -0.4223 0.0968 0.5321 0.041 Uiso 1 1 calc R . . C8 C -0.4753(3) 0.2770(4) 0.4828(3) 0.0380(8) Uani 1 1 d . . . H8A H -0.5396 0.2975 0.5412 0.046 Uiso 1 1 calc R . . C9 C -0.4524(3) 0.3666(3) 0.4043(3) 0.0353(8) Uani 1 1 d . . . H9A H -0.5017 0.4483 0.4093 0.042 Uiso 1 1 calc R . . C10 C -0.3584(3) 0.3402(3) 0.3177(3) 0.0274(7) Uani 1 1 d . . . C11 C 0.1205(3) 0.1098(3) 0.0190(2) 0.0224(6) Uani 1 1 d . . . C12 C 0.1233(3) 0.1867(3) -0.0801(2) 0.0261(6) Uani 1 1 d . . . C13 C 0.2355(3) 0.1657(3) -0.1480(3) 0.0349(8) Uani 1 1 d . . . H13A H 0.2396 0.2168 -0.2159 0.042 Uiso 1 1 calc R . . C14 C 0.3403(3) 0.0723(3) -0.1185(3) 0.0368(8) Uani 1 1 d . . . H14A H 0.4160 0.0600 -0.1654 0.044 Uiso 1 1 calc R . . C15 C 0.3351(3) -0.0031(3) -0.0210(3) 0.0351(8) Uani 1 1 d . . . H15A H 0.4076 -0.0677 -0.0015 0.042 Uiso 1 1 calc R . . C16 C 0.2263(3) 0.0131(3) 0.0496(3) 0.0296(7) Uani 1 1 d . . . C17 C -0.2309(3) -0.0075(3) 0.3902(3) 0.0337(7) Uani 1 1 d . . . H17A H -0.1891 -0.0142 0.3148 0.040 Uiso 1 1 calc R . . C18 C -0.3321(3) 0.4373(3) 0.2307(3) 0.0347(8) Uani 1 1 d . . . H18A H -0.2418 0.4068 0.2064 0.042 Uiso 1 1 calc R . . C19 C 0.2247(3) -0.0780(4) 0.1539(3) 0.0433(9) Uani 1 1 d . . . H19A H 0.1381 -0.0614 0.1892 0.052 Uiso 1 1 calc R . . C20 C 0.0118(3) 0.2947(3) -0.1143(3) 0.0373(8) Uani 1 1 d . . . H20A H -0.0611 0.2891 -0.0613 0.045 Uiso 1 1 calc R . . C21 C -0.1320(4) -0.0511(4) 0.4589(4) 0.0628(13) Uani 1 1 d . . . H21A H -0.0861 0.0014 0.4355 0.094 Uiso 1 1 calc R . . H21B H -0.0766 -0.1338 0.4515 0.094 Uiso 1 1 calc R . . H21C H -0.1697 -0.0490 0.5341 0.094 Uiso 1 1 calc R . . C22 C -0.3043(4) -0.0874(4) 0.4235(3) 0.0459(9) Uani 1 1 d . . . H22A H -0.3665 -0.0578 0.3775 0.069 Uiso 1 1 calc R . . H22B H -0.3440 -0.0854 0.4982 0.069 Uiso 1 1 calc R . . H22C H -0.2496 -0.1703 0.4162 0.069 Uiso 1 1 calc R . . C23 C -0.3689(4) 0.5559(3) 0.2681(4) 0.0497(10) Uani 1 1 d . . . H23A H -0.3295 0.5405 0.3296 0.074 Uiso 1 1 calc R . . H23B H -0.4577 0.5908 0.2891 0.074 Uiso 1 1 calc R . . H23C H -0.3431 0.6122 0.2096 0.074 Uiso 1 1 calc R . . C24 C -0.3910(5) 0.4592(4) 0.1343(4) 0.0545(11) Uani 1 1 d . . . H24A H -0.3662 0.3828 0.1110 0.082 Uiso 1 1 calc R . . H24B H -0.3648 0.5153 0.0758 0.082 Uiso 1 1 calc R . . H24C H -0.4800 0.4938 0.1541 0.082 Uiso 1 1 calc R . . C25 C 0.2939(5) -0.0683(4) 0.2302(3) 0.0625(13) Uani 1 1 d . . . H25A H 0.2572 0.0136 0.2453 0.094 Uiso 1 1 calc R . . H25B H 0.3794 -0.0866 0.1970 0.094 Uiso 1 1 calc R . . H25C H 0.2895 -0.1257 0.2972 0.094 Uiso 1 1 calc R . . C26 C 0.2849(4) -0.2096(4) 0.1330(4) 0.0524(10) Uani 1 1 d . . . H26A H 0.2412 -0.2187 0.0851 0.079 Uiso 1 1 calc R . . H26B H 0.2811 -0.2656 0.2011 0.079 Uiso 1 1 calc R . . H26C H 0.3703 -0.2273 0.0997 0.079 Uiso 1 1 calc R . . C27 C 0.0229(5) 0.4115(4) -0.1115(4) 0.0730(16) Uani 1 1 d . . . H27A H 0.0356 0.4085 -0.0399 0.109 Uiso 1 1 calc R . . H27B H -0.0521 0.4801 -0.1281 0.109 Uiso 1 1 calc R . . H27C H 0.0923 0.4205 -0.1645 0.109 Uiso 1 1 calc R . . C28 C -0.0091(4) 0.2975(4) -0.2239(4) 0.0573(11) Uani 1 1 d . . . H28A H -0.0168 0.2227 -0.2241 0.086 Uiso 1 1 calc R . . H28B H 0.0601 0.3055 -0.2778 0.086 Uiso 1 1 calc R . . H28C H -0.0841 0.3662 -0.2407 0.086 Uiso 1 1 calc R . . C29 C 0.1959(3) 0.2611(3) 0.2140(2) 0.0230(6) Uani 1 1 d . . . C30 C 0.2550(3) 0.2585(3) 0.1084(3) 0.0262(6) Uani 1 1 d . . . H30A H 0.2153 0.2555 0.0565 0.031 Uiso 1 1 calc R . . C31 C 0.3709(3) 0.2601(3) 0.0782(3) 0.0336(8) Uani 1 1 d . . . H31A H 0.4095 0.2598 0.0057 0.040 Uiso 1 1 calc R . . C32 C 0.4304(3) 0.2621(3) 0.1532(3) 0.0436(9) Uani 1 1 d . . . H32A H 0.5104 0.2622 0.1324 0.052 Uiso 1 1 calc R . . C33 C 0.3740(3) 0.2640(4) 0.2584(3) 0.0443(9) Uani 1 1 d . . . H33A H 0.4151 0.2654 0.3099 0.053 Uiso 1 1 calc R . . C34 C 0.2569(3) 0.2638(3) 0.2892(3) 0.0336(7) Uani 1 1 d . . . H34A H 0.2182 0.2655 0.3616 0.040 Uiso 1 1 calc R . . C35 C -0.0927(3) 0.3421(3) 0.4069(2) 0.0239(6) Uani 1 1 d . . . C36 C -0.0777(3) 0.4435(3) 0.4158(3) 0.0329(7) Uani 1 1 d . . . H36A H -0.0195 0.4698 0.3649 0.039 Uiso 1 1 calc R . . C37 C -0.1463(3) 0.5064(3) 0.4977(3) 0.0382(8) Uani 1 1 d . . . H37A H -0.1357 0.5760 0.5020 0.046 Uiso 1 1 calc R . . C38 C -0.2302(3) 0.4684(3) 0.5734(3) 0.0370(8) Uani 1 1 d . . . H38A H -0.2767 0.5112 0.6300 0.044 Uiso 1 1 calc R . . C39 C -0.2458(3) 0.3675(3) 0.5661(3) 0.0330(7) Uani 1 1 d . . . H39A H -0.3035 0.3414 0.6178 0.040 Uiso 1 1 calc R . . C40 C -0.1779(3) 0.3039(3) 0.4837(2) 0.0262(6) Uani 1 1 d . . . H40A H -0.1893 0.2347 0.4795 0.031 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 0.0183(2) 0.0299(2) 0.0220(2) -0.00842(15) -0.00078(14) -0.01230(16) N1 0.0167(12) 0.0246(13) 0.0225(12) -0.0046(10) -0.0023(10) -0.0086(10) N2 0.0190(12) 0.0238(13) 0.0219(12) -0.0050(10) -0.0023(10) -0.0080(10) C1 0.0196(14) 0.0258(15) 0.0291(16) -0.0070(12) -0.0059(12) -0.0088(12) C2 0.0201(15) 0.0275(16) 0.0250(15) -0.0075(12) -0.0046(12) -0.0074(12) C3 0.0244(15) 0.0239(15) 0.0251(15) -0.0028(12) -0.0076(12) -0.0089(12) C4 0.0239(15) 0.0218(15) 0.0265(15) -0.0036(12) -0.0064(12) -0.0098(12) C5 0.0145(14) 0.0327(16) 0.0252(15) -0.0080(12) -0.0031(11) -0.0100(12) C6 0.0189(14) 0.0354(17) 0.0256(15) -0.0049(13) -0.0041(12) -0.0118(13) C7 0.0258(17) 0.049(2) 0.0293(17) -0.0087(15) 0.0023(13) -0.0179(16) C8 0.0221(16) 0.058(2) 0.0344(18) -0.0200(17) 0.0054(14) -0.0149(16) C9 0.0196(16) 0.041(2) 0.048(2) -0.0237(17) -0.0040(14) -0.0057(14) C10 0.0175(14) 0.0319(17) 0.0363(17) -0.0122(14) -0.0065(12) -0.0080(13) C11 0.0222(15) 0.0243(15) 0.0237(15) -0.0091(12) -0.0003(12) -0.0108(12) C12 0.0277(16) 0.0269(16) 0.0233(15) -0.0057(12) -0.0027(12) -0.0101(13) C13 0.0362(19) 0.042(2) 0.0252(16) -0.0078(14) 0.0051(14) -0.0185(16) C14 0.0252(17) 0.045(2) 0.041(2) -0.0200(16) 0.0111(14) -0.0160(15) C15 0.0203(16) 0.0309(18) 0.049(2) -0.0119(15) -0.0026(14) -0.0040(14) C16 0.0221(15) 0.0291(17) 0.0355(18) -0.0036(14) -0.0037(13) -0.0098(13) C17 0.0323(18) 0.0315(18) 0.0326(17) -0.0008(14) -0.0016(14) -0.0129(15) C18 0.0284(17) 0.0257(17) 0.049(2) -0.0097(15) -0.0053(15) -0.0088(14) C19 0.0277(18) 0.046(2) 0.042(2) 0.0077(17) -0.0089(15) -0.0088(16) C20 0.0338(19) 0.0321(18) 0.0321(18) 0.0056(14) -0.0043(14) -0.0071(15) C21 0.049(3) 0.042(2) 0.093(4) -0.001(2) -0.037(3) -0.006(2) C22 0.054(2) 0.043(2) 0.045(2) -0.0044(17) -0.0015(18) -0.0282(19) C23 0.044(2) 0.031(2) 0.078(3) -0.0166(19) -0.017(2) -0.0101(17) C24 0.078(3) 0.037(2) 0.056(3) 0.0058(19) -0.029(2) -0.028(2) C25 0.114(4) 0.036(2) 0.047(2) -0.0030(18) -0.034(3) -0.028(2) C26 0.064(3) 0.038(2) 0.055(3) -0.0030(18) -0.021(2) -0.017(2) C27 0.093(4) 0.032(2) 0.083(4) -0.016(2) -0.048(3) 0.008(2) C28 0.061(3) 0.057(3) 0.058(3) 0.004(2) -0.032(2) -0.023(2) C29 0.0179(14) 0.0197(14) 0.0326(16) -0.0069(12) -0.0049(12) -0.0067(12) C30 0.0231(15) 0.0235(15) 0.0324(16) -0.0069(13) -0.0034(13) -0.0090(12) C31 0.0250(16) 0.0281(17) 0.046(2) -0.0101(15) 0.0034(14) -0.0114(14) C32 0.0217(17) 0.046(2) 0.069(3) -0.0187(19) -0.0010(17) -0.0168(16) C33 0.0278(18) 0.054(2) 0.064(3) -0.023(2) -0.0147(17) -0.0164(17) C34 0.0277(17) 0.0384(19) 0.0394(19) -0.0142(15) -0.0079(14) -0.0115(15) C35 0.0184(14) 0.0291(16) 0.0240(15) -0.0077(12) -0.0058(12) -0.0060(12) C36 0.0293(17) 0.0371(19) 0.0368(18) -0.0120(15) -0.0066(14) -0.0132(15) C37 0.0367(19) 0.0365(19) 0.046(2) -0.0185(16) -0.0104(16) -0.0096(16) C38 0.0289(17) 0.045(2) 0.0343(18) -0.0202(16) -0.0071(14) -0.0024(15) C39 0.0246(16) 0.046(2) 0.0245(16) -0.0093(14) -0.0021(13) -0.0096(15) C40 0.0223(15) 0.0282(16) 0.0271(16) -0.0053(13) -0.0060(12) -0.0077(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C3 1.852(3) . ? Ni1 C4 1.858(3) . ? Ni1 N1 1.919(2) . ? Ni1 N2 1.920(2) . ? N1 C1 1.311(4) . ? N1 C5 1.437(4) . ? N2 C2 1.309(4) . ? N2 C11 1.437(4) . ? C1 C2 1.423(4) . ? C1 H1A 0.9500 . ? C2 H2A 0.9500 . ? C3 C4 1.286(4) . ? C3 C35 1.458(4) . ? C3 H3A 1.0000 . ? C4 C29 1.455(4) . ? C4 H4A 1.0000 . ? C5 C6 1.397(4) . ? C5 C10 1.412(4) . ? C6 C7 1.404(4) . ? C6 C17 1.519(5) . ? C7 C8 1.378(5) . ? C7 H7A 0.9500 . ? C8 C9 1.376(5) . ? C8 H8A 0.9500 . ? C9 C10 1.394(5) . ? C9 H9A 0.9500 . ? C10 C18 1.510(5) . ? C11 C12 1.396(4) . ? C11 C16 1.406(4) . ? C12 C13 1.397(4) . ? C12 C20 1.519(4) . ? C13 C14 1.378(5) . ? C13 H13A 0.9500 . ? C14 C15 1.375(5) . ? C14 H14A 0.9500 . ? C15 C16 1.386(5) . ? C15 H15A 0.9500 . ? C16 C19 1.529(5) . ? C17 C21 1.522(5) . ? C17 C22 1.528(5) . ? C17 H17A 1.0000 . ? C18 C24 1.522(5) . ? C18 C23 1.533(5) . ? C18 H18A 1.0000 . ? C19 C25 1.527(6) . ? C19 C26 1.558(6) . ? C19 H19A 1.0000 . ? C20 C28 1.515(5) . ? C20 C27 1.532(6) . ? C20 H20A 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.394(4) . ? C29 C34 1.398(4) . ? C30 C31 1.383(4) . ? C30 H30A 0.9500 . ? C31 C32 1.380(5) . ? C31 H31A 0.9500 . ? C32 C33 1.380(6) . ? C32 H32A 0.9500 . ? C33 C34 1.392(5) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.394(5) . ? C35 C40 1.403(4) . ? C36 C37 1.383(5) . ? C36 H36A 0.9500 . ? C37 C38 1.384(5) . ? C37 H37A 0.9500 . ? C38 C39 1.384(5) . ? C38 H38A 0.9500 . ? C39 C40 1.391(4) . ? C39 H39A 0.9500 . ? C40 H40A 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 C3 Ni1 C4 40.56(13) . . ? C3 Ni1 N1 117.61(12) . . ? C4 Ni1 N1 157.90(12) . . ? C3 Ni1 N2 159.86(12) . . ? C4 Ni1 N2 119.34(12) . . ? N1 Ni1 N2 82.33(10) . . ? C1 N1 C5 118.9(2) . . ? C1 N1 Ni1 114.2(2) . . ? C5 N1 Ni1 126.91(19) . . ? C2 N2 C11 118.8(2) . . ? C2 N2 Ni1 113.5(2) . . ? C11 N2 Ni1 127.35(19) . . ? N1 C1 C2 114.3(3) . . ? N1 C1 H1A 122.8 . . ? C2 C1 H1A 122.8 . . ? N2 C2 C1 115.5(3) . . ? N2 C2 H2A 122.2 . . ? C1 C2 H2A 122.2 . . ? C4 C3 C35 146.3(3) . . ? C4 C3 Ni1 69.95(19) . . ? C35 C3 Ni1 143.0(2) . . ? C4 C3 H3A 92.4 . . ? C35 C3 H3A 92.4 . . ? Ni1 C3 H3A 92.4 . . ? C3 C4 C29 145.8(3) . . ? C3 C4 Ni1 69.49(18) . . ? C29 C4 Ni1 144.7(2) . . ? C3 C4 H4A 90.8 . . ? C29 C4 H4A 90.8 . . ? Ni1 C4 H4A 90.8 . . ? C6 C5 C10 122.6(3) . . ? C6 C5 N1 119.3(3) . . ? C10 C5 N1 117.9(3) . . ? C5 C6 C7 117.3(3) . . ? C5 C6 C17 122.6(3) . . ? C7 C6 C17 119.9(3) . . ? C8 C7 C6 121.1(3) . . ? C8 C7 H7A 119.5 . . ? C6 C7 H7A 119.5 . . ? C9 C8 C7 120.5(3) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C8 C9 C10 121.5(3) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C9 C10 C5 117.1(3) . . ? C9 C10 C18 122.2(3) . . ? C5 C10 C18 120.7(3) . . ? C12 C11 C16 121.5(3) . . ? C12 C11 N2 119.7(3) . . ? C16 C11 N2 118.6(3) . . ? C11 C12 C13 117.8(3) . . ? C11 C12 C20 123.0(3) . . ? C13 C12 C20 119.1(3) . . ? C14 C13 C12 121.3(3) . . ? C14 C13 H13A 119.3 . . ? C12 C13 H13A 119.3 . . ? C15 C14 C13 119.8(3) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C14 C15 C16 121.5(3) . . ? C14 C15 H15A 119.2 . . ? C16 C15 H15A 119.2 . . ? C15 C16 C11 118.0(3) . . ? C15 C16 C19 119.1(3) . . ? C11 C16 C19 122.8(3) . . ? C6 C17 C21 110.3(3) . . ? C6 C17 C22 112.9(3) . . ? C21 C17 C22 111.3(3) . . ? C6 C17 H17A 107.3 . . ? C21 C17 H17A 107.3 . . ? C22 C17 H17A 107.3 . . ? C10 C18 C24 110.8(3) . . ? C10 C18 C23 113.9(3) . . ? C24 C18 C23 110.4(3) . . ? C10 C18 H18A 107.1 . . ? C24 C18 H18A 107.1 . . ? C23 C18 H18A 107.1 . . ? C25 C19 C16 110.9(3) . . ? C25 C19 C26 107.8(3) . . ? C16 C19 C26 111.5(3) . . ? C25 C19 H19A 108.9 . . ? C16 C19 H19A 108.9 . . ? C26 C19 H19A 108.9 . . ? C28 C20 C12 112.5(3) . . ? C28 C20 C27 110.6(3) . . ? C12 C20 C27 110.1(3) . . ? C28 C20 H20A 107.8 . . ? C12 C20 H20A 107.8 . . ? C27 C20 H20A 107.8 . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C18 C24 H24A 109.5 . . ? C18 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C18 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C25 H25A 109.5 . . ? C19 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C19 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C19 C26 H26A 109.5 . . ? C19 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C19 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C20 C27 H27A 109.5 . . ? C20 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C20 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C20 C28 H28A 109.5 . . ? C20 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C20 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 118.6(3) . . ? C30 C29 C4 121.3(3) . . ? C34 C29 C4 120.1(3) . . ? C31 C30 C29 120.7(3) . . ? C31 C30 H30A 119.6 . . ? C29 C30 H30A 119.6 . . ? C32 C31 C30 120.2(3) . . ? C32 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? C31 C32 C33 120.1(3) . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C32 C33 C34 120.1(3) . . ? C32 C33 H33A 119.9 . . ? C34 C33 H33A 119.9 . . ? C33 C34 C29 120.3(3) . . ? C33 C34 H34A 119.8 . . ? C29 C34 H34A 119.8 . . ? C36 C35 C40 118.6(3) . . ? C36 C35 C3 119.8(3) . . ? C40 C35 C3 121.6(3) . . ? C37 C36 C35 120.9(3) . . ? C37 C36 H36A 119.5 . . ? C35 C36 H36A 119.5 . . ? C36 C37 C38 120.3(3) . . ? C36 C37 H37A 119.9 . . ? C38 C37 H37A 119.9 . . ? C39 C38 C37 119.5(3) . . ? C39 C38 H38A 120.2 . . ? C37 C38 H38A 120.2 . . ? C38 C39 C40 120.7(3) . . ? C38 C39 H39A 119.6 . . ? C40 C39 H39A 119.6 . . ? C39 C40 C35 119.9(3) . . ? C39 C40 H40A 120.0 . . ? C35 C40 H40A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.217 _refine_diff_density_min -0.898 _refine_diff_density_rms 0.075 #=== END data_C42H50N2Ni_Compound7 _database_code_depnum_ccdc_archive 'CCDC 762668' #TrackingRef 'Ni-diimines-cif_files.cif' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C42 H50 N2 Ni' _chemical_formula_weight 641.55 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' _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 10.7742(11) _cell_length_b 13.0819(14) _cell_length_c 25.749(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.216(5) _cell_angle_gamma 90.00 _cell_volume 3614.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9929 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.44 _exptl_crystal_description irregular _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.567 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6613 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 28394 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6360 _reflns_number_gt 5571 _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^)+(0.0306P)^2^+1.6771P] 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 6360 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.546398(16) 0.134734(14) 0.146949(7) 0.01788(6) Uani 1 1 d . . . N1 N 0.45625(11) 0.07643(9) 0.20060(5) 0.0193(2) Uani 1 1 d . . . N2 N 0.38973(11) 0.20187(9) 0.13022(5) 0.0183(2) Uani 1 1 d . . . C2 C 0.67701(13) 0.16131(11) 0.10678(6) 0.0199(3) Uani 1 1 d . . . C98 C 0.39235(14) 0.35870(11) 0.07789(6) 0.0230(3) Uani 1 1 d . . . C1 C 0.71082(13) 0.09610(12) 0.14312(6) 0.0205(3) Uani 1 1 d . . . C3 C 0.34372(13) 0.11287(11) 0.20373(6) 0.0206(3) Uani 1 1 d . . . C4 C 0.30508(13) 0.18574(11) 0.16298(6) 0.0207(3) Uani 1 1 d . . . C9 C 0.35549(13) 0.25688(11) 0.08274(6) 0.0196(3) Uani 1 1 d . . . C10 C 0.50302(13) -0.00594(12) 0.23396(6) 0.0215(3) Uani 1 1 d . . . C7 C 0.81321(13) 0.02902(11) 0.16252(6) 0.0219(3) Uani 1 1 d . . . C12 C 0.64130(15) 0.25141(11) 0.02130(6) 0.0242(3) Uani 1 1 d . . . H12A H 0.5580 0.2317 0.0189 0.029 Uiso 1 1 calc R . . C13 C 0.29021(13) 0.20401(12) 0.04120(6) 0.0232(3) Uani 1 1 d . . . C14 C 0.29499(17) 0.35791(14) -0.01054(7) 0.0361(4) Uani 1 1 d . . . H14A H 0.2737 0.3923 -0.0417 0.043 Uiso 1 1 calc R . . C5 C 0.25734(14) 0.08031(13) 0.24305(6) 0.0289(3) Uani 1 1 d . . . H5A H 0.2991 0.0323 0.2668 0.043 Uiso 1 1 calc R . . H5B H 0.1848 0.0488 0.2255 0.043 Uiso 1 1 calc R . . H5C H 0.2328 0.1390 0.2620 0.043 Uiso 1 1 calc R . . C17 C 0.68559(17) 0.30941(13) -0.01813(6) 0.0316(4) Uani 1 1 d . . . H17A H 0.6320 0.3276 -0.0470 0.038 Uiso 1 1 calc R . . C8 C 0.72108(13) 0.22241(11) 0.06467(6) 0.0206(3) Uani 1 1 d . . . C19 C 0.51009(14) -0.10291(12) 0.21078(6) 0.0250(3) Uani 1 1 d . . . C20 C 0.54509(16) 0.11787(13) 0.31064(6) 0.0298(4) Uani 1 1 d . . . H20A H 0.4900 0.1608 0.2874 0.036 Uiso 1 1 calc R . . C21 C 0.90743(15) 0.00575(13) 0.13043(7) 0.0296(4) Uani 1 1 d . . . H21A H 0.9050 0.0341 0.0972 0.036 Uiso 1 1 calc R . . C22 C 0.60043(15) -0.07023(14) 0.31483(6) 0.0310(4) Uani 1 1 d . . . H22A H 0.6305 -0.0603 0.3495 0.037 Uiso 1 1 calc R . . C23 C 0.56390(16) -0.18209(13) 0.24147(7) 0.0317(4) Uani 1 1 d . . . H23A H 0.5691 -0.2470 0.2271 0.038 Uiso 1 1 calc R . . C24 C 0.54690(14) 0.01206(12) 0.28625(6) 0.0249(3) Uani 1 1 d . . . C25 C 0.46030(16) -0.12190(12) 0.15444(7) 0.0304(4) Uani 1 1 d . . . H25A H 0.4450 -0.0551 0.1379 0.037 Uiso 1 1 calc R . . C26 C 0.26126(15) 0.25690(14) -0.00528(6) 0.0317(4) Uani 1 1 d . . . H26A H 0.2184 0.2235 -0.0333 0.038 Uiso 1 1 calc R . . C27 C 0.81970(15) -0.01556(13) 0.21189(6) 0.0297(4) Uani 1 1 d . . . H27A H 0.7579 -0.0015 0.2338 0.036 Uiso 1 1 calc R . . C28 C 0.91686(15) -0.08053(14) 0.22878(7) 0.0354(4) Uani 1 1 d . . . H28A H 0.9197 -0.1097 0.2618 0.042 Uiso 1 1 calc R . . C29 C 0.25852(15) 0.09125(13) 0.04526(7) 0.0290(3) Uani 1 1 d . . . H29A H 0.2628 0.0740 0.0824 0.035 Uiso 1 1 calc R . . C30 C 0.36056(16) 0.40794(13) 0.03058(7) 0.0320(4) Uani 1 1 d . . . H30A H 0.3839 0.4757 0.0266 0.038 Uiso 1 1 calc R . . C6 C 0.17661(14) 0.23091(14) 0.15832(7) 0.0315(4) Uani 1 1 d . . . H6A H 0.1679 0.2770 0.1292 0.047 Uiso 1 1 calc R . . H6B H 0.1636 0.2675 0.1897 0.047 Uiso 1 1 calc R . . H6C H 0.1161 0.1772 0.1531 0.047 Uiso 1 1 calc R . . C32 C 0.60961(16) -0.16587(14) 0.29279(7) 0.0338(4) Uani 1 1 d . . . H32A H 0.6465 -0.2193 0.3124 0.041 Uiso 1 1 calc R . . C33 C 1.00403(16) -0.05900(14) 0.14752(8) 0.0387(4) Uani 1 1 d . . . H33A H 1.0660 -0.0737 0.1258 0.046 Uiso 1 1 calc R . . C34 C 0.84551(15) 0.25388(13) 0.06732(7) 0.0296(4) Uani 1 1 d . . . H34A H 0.9001 0.2350 0.0958 0.035 Uiso 1 1 calc R . . C35 C 1.00919(16) -0.10204(14) 0.19673(8) 0.0377(4) Uani 1 1 d . . . H35A H 1.0746 -0.1453 0.2081 0.045 Uiso 1 1 calc R . . C36 C 0.46267(16) 0.41379(12) 0.12337(6) 0.0301(4) Uani 1 1 d . . . H36A H 0.4956 0.3621 0.1485 0.036 Uiso 1 1 calc R . . C37 C 0.55139(18) -0.17856(18) 0.12344(8) 0.0453(5) Uani 1 1 d . . . H37A H 0.6287 -0.1418 0.1251 0.068 Uiso 1 1 calc R . . H37B H 0.5175 -0.1842 0.0878 0.068 Uiso 1 1 calc R . . H37C H 0.5657 -0.2457 0.1378 0.068 Uiso 1 1 calc R . . C38 C 0.80829(19) 0.34038(14) -0.01492(7) 0.0402(4) Uani 1 1 d . . . H38A H 0.8373 0.3796 -0.0414 0.048 Uiso 1 1 calc R . . C39 C 0.12805(18) 0.06579(17) 0.02168(8) 0.0466(5) Uani 1 1 d . . . H39A H 0.0686 0.1068 0.0379 0.070 Uiso 1 1 calc R . . H39B H 0.1112 -0.0052 0.0273 0.070 Uiso 1 1 calc R . . H39C H 0.1217 0.0796 -0.0151 0.070 Uiso 1 1 calc R . . C40 C 0.57205(18) 0.47565(15) 0.10708(8) 0.0426(5) Uani 1 1 d . . . H40A H 0.6275 0.4315 0.0904 0.064 Uiso 1 1 calc R . . H40B H 0.6158 0.5062 0.1373 0.064 Uiso 1 1 calc R . . H40C H 0.5419 0.5283 0.0832 0.064 Uiso 1 1 calc R . . C41 C 0.3553(2) 0.02722(15) 0.02110(9) 0.0507(5) Uani 1 1 d . . . H41A H 0.4367 0.0444 0.0369 0.076 Uiso 1 1 calc R . . H41B H 0.3512 0.0406 -0.0157 0.076 Uiso 1 1 calc R . . H41C H 0.3392 -0.0439 0.0268 0.076 Uiso 1 1 calc R . . C42 C 0.88820(17) 0.31285(15) 0.02796(8) 0.0405(4) Uani 1 1 d . . . H42A H 0.9709 0.3340 0.0303 0.049 Uiso 1 1 calc R . . C43 C 0.33662(18) -0.1778(2) 0.15207(9) 0.0625(7) Uani 1 1 d . . . H43A H 0.3062 -0.1889 0.1163 0.094 Uiso 1 1 calc R . . H43B H 0.2775 -0.1374 0.1689 0.094 Uiso 1 1 calc R . . H43C H 0.3478 -0.2424 0.1695 0.094 Uiso 1 1 calc R . . C44 C 0.3750(2) 0.48217(17) 0.15048(8) 0.0503(5) Uani 1 1 d . . . H44A H 0.3066 0.4423 0.1608 0.075 Uiso 1 1 calc R . . H44B H 0.3438 0.5352 0.1270 0.075 Uiso 1 1 calc R . . H44C H 0.4190 0.5123 0.1808 0.075 Uiso 1 1 calc R . . C45 C 0.4931(3) 0.11729(19) 0.36411(8) 0.0594(6) Uani 1 1 d . . . H45A H 0.4938 0.1856 0.3778 0.089 Uiso 1 1 calc R . . H45B H 0.5437 0.0740 0.3875 0.089 Uiso 1 1 calc R . . H45C H 0.4091 0.0920 0.3605 0.089 Uiso 1 1 calc R . . C47 C 0.67382(18) 0.16602(16) 0.31434(11) 0.0582(6) Uani 1 1 d . . . H47A H 0.7049 0.1656 0.2806 0.087 Uiso 1 1 calc R . . H47B H 0.7291 0.1277 0.3384 0.087 Uiso 1 1 calc R . . H47C H 0.6688 0.2352 0.3264 0.087 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 0.01456(10) 0.02201(10) 0.01750(10) 0.00322(7) 0.00378(7) 0.00137(7) N1 0.0181(6) 0.0220(6) 0.0181(6) 0.0015(5) 0.0030(5) -0.0004(5) N2 0.0178(6) 0.0191(6) 0.0180(6) 0.0009(5) 0.0019(5) 0.0005(5) C2 0.0166(7) 0.0243(7) 0.0194(7) -0.0014(6) 0.0045(5) -0.0005(6) C98 0.0229(7) 0.0231(7) 0.0232(7) 0.0017(6) 0.0018(6) 0.0038(6) C1 0.0166(7) 0.0255(7) 0.0200(7) -0.0006(6) 0.0040(5) -0.0004(6) C3 0.0178(7) 0.0240(7) 0.0205(7) -0.0002(6) 0.0040(6) -0.0007(6) C4 0.0184(7) 0.0224(7) 0.0216(7) -0.0009(6) 0.0037(6) 0.0014(6) C9 0.0162(7) 0.0226(7) 0.0203(7) 0.0017(6) 0.0038(5) 0.0044(5) C10 0.0163(7) 0.0270(8) 0.0221(7) 0.0066(6) 0.0063(5) 0.0006(6) C7 0.0159(7) 0.0245(7) 0.0252(8) 0.0020(6) 0.0015(6) -0.0008(6) C12 0.0283(8) 0.0228(7) 0.0221(8) -0.0015(6) 0.0048(6) 0.0024(6) C13 0.0184(7) 0.0286(8) 0.0227(7) 0.0007(6) 0.0021(6) 0.0005(6) C14 0.0368(10) 0.0436(10) 0.0266(9) 0.0139(8) -0.0037(7) 0.0018(8) C5 0.0216(8) 0.0385(9) 0.0279(8) 0.0063(7) 0.0094(6) 0.0006(7) C17 0.0458(10) 0.0281(8) 0.0215(8) 0.0041(6) 0.0057(7) 0.0055(7) C8 0.0233(7) 0.0198(7) 0.0196(7) -0.0007(6) 0.0066(6) 0.0016(6) C19 0.0233(8) 0.0269(8) 0.0255(8) 0.0058(6) 0.0054(6) 0.0012(6) C20 0.0287(8) 0.0361(9) 0.0240(8) 0.0009(7) -0.0006(6) -0.0001(7) C21 0.0263(8) 0.0320(9) 0.0316(9) 0.0060(7) 0.0083(7) 0.0040(7) C22 0.0258(8) 0.0448(10) 0.0226(8) 0.0113(7) 0.0030(6) 0.0008(7) C23 0.0318(9) 0.0280(8) 0.0364(9) 0.0085(7) 0.0091(7) 0.0053(7) C24 0.0194(7) 0.0337(8) 0.0220(7) 0.0054(6) 0.0050(6) -0.0007(6) C25 0.0369(9) 0.0254(8) 0.0287(8) -0.0006(7) 0.0010(7) 0.0053(7) C26 0.0283(8) 0.0422(10) 0.0234(8) 0.0016(7) -0.0038(7) -0.0024(7) C27 0.0213(8) 0.0400(9) 0.0279(8) 0.0068(7) 0.0032(6) 0.0025(7) C28 0.0262(8) 0.0413(10) 0.0374(10) 0.0147(8) -0.0036(7) 0.0006(7) C29 0.0294(8) 0.0308(8) 0.0264(8) -0.0026(7) -0.0002(6) -0.0059(7) C30 0.0373(9) 0.0260(8) 0.0326(9) 0.0095(7) 0.0020(7) 0.0022(7) C6 0.0215(8) 0.0400(10) 0.0341(9) 0.0071(7) 0.0091(7) 0.0097(7) C32 0.0298(9) 0.0375(9) 0.0347(9) 0.0189(8) 0.0055(7) 0.0067(7) C33 0.0259(8) 0.0376(10) 0.0545(12) 0.0066(9) 0.0151(8) 0.0087(7) C34 0.0244(8) 0.0356(9) 0.0295(9) 0.0053(7) 0.0067(7) -0.0006(7) C35 0.0212(8) 0.0340(9) 0.0571(12) 0.0122(9) -0.0005(8) 0.0057(7) C36 0.0399(9) 0.0213(8) 0.0283(8) -0.0001(6) -0.0017(7) -0.0004(7) C37 0.0347(10) 0.0670(14) 0.0351(10) -0.0122(10) 0.0073(8) -0.0021(9) C38 0.0512(11) 0.0385(10) 0.0335(10) 0.0126(8) 0.0187(8) -0.0019(9) C39 0.0365(10) 0.0520(12) 0.0511(12) -0.0038(10) 0.0028(9) -0.0172(9) C40 0.0394(10) 0.0397(10) 0.0483(12) -0.0145(9) 0.0030(9) -0.0071(8) C41 0.0473(12) 0.0330(10) 0.0736(15) -0.0101(10) 0.0151(11) -0.0010(9) C42 0.0329(9) 0.0467(11) 0.0442(11) 0.0104(9) 0.0151(8) -0.0071(8) C43 0.0280(10) 0.110(2) 0.0497(13) -0.0285(13) 0.0062(9) -0.0071(12) C44 0.0561(13) 0.0535(13) 0.0437(12) -0.0225(10) 0.0182(10) -0.0065(10) C45 0.0899(18) 0.0597(14) 0.0302(11) -0.0112(10) 0.0144(11) -0.0067(12) C47 0.0324(11) 0.0353(11) 0.105(2) -0.0009(12) -0.0053(11) -0.0007(9) _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 C2 1.8534(14) . ? Ni1 C1 1.8535(14) . ? Ni1 N2 1.9168(12) . ? Ni1 N1 1.9178(12) . ? N1 C3 1.3120(18) . ? N1 C10 1.4402(18) . ? N2 C4 1.3144(18) . ? N2 C9 1.4375(18) . ? C2 C1 1.294(2) . ? C2 C8 1.461(2) . ? C98 C30 1.393(2) . ? C98 C9 1.399(2) . ? C98 C36 1.518(2) . ? C1 C7 1.462(2) . ? C3 C4 1.450(2) . ? C3 C5 1.498(2) . ? C4 C6 1.500(2) . ? C9 C13 1.407(2) . ? C10 C24 1.406(2) . ? C10 C19 1.407(2) . ? C7 C27 1.395(2) . ? C7 C21 1.399(2) . ? C12 C17 1.387(2) . ? C12 C8 1.398(2) . ? C13 C26 1.393(2) . ? C13 C29 1.520(2) . ? C14 C26 1.380(2) . ? C14 C30 1.383(3) . ? C17 C38 1.378(3) . ? C8 C34 1.398(2) . ? C19 C23 1.396(2) . ? C19 C25 1.521(2) . ? C20 C47 1.518(3) . ? C20 C24 1.521(2) . ? C20 C45 1.533(3) . ? C21 C33 1.382(2) . ? C22 C32 1.381(3) . ? C22 C24 1.398(2) . ? C23 C32 1.384(3) . ? C25 C37 1.514(2) . ? C25 C43 1.516(3) . ? C27 C28 1.387(2) . ? C28 C35 1.378(3) . ? C29 C41 1.514(3) . ? C29 C39 1.517(2) . ? C33 C35 1.383(3) . ? C34 C42 1.385(2) . ? C36 C44 1.517(2) . ? C36 C40 1.520(2) . ? C38 C42 1.385(3) . ? 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 C2 Ni1 C1 40.86(6) . . ? C2 Ni1 N2 119.11(6) . . ? C1 Ni1 N2 159.96(6) . . ? C2 Ni1 N1 159.47(6) . . ? C1 Ni1 N1 118.62(6) . . ? N2 Ni1 N1 81.42(5) . . ? C3 N1 C10 120.70(12) . . ? C3 N1 Ni1 115.53(10) . . ? C10 N1 Ni1 123.68(9) . . ? C4 N2 C9 119.13(12) . . ? C4 N2 Ni1 115.50(10) . . ? C9 N2 Ni1 124.97(9) . . ? C1 C2 C8 143.94(14) . . ? C1 C2 Ni1 69.57(9) . . ? C8 C2 Ni1 146.24(11) . . ? C30 C98 C9 117.98(14) . . ? C30 C98 C36 121.41(14) . . ? C9 C98 C36 120.60(13) . . ? C2 C1 C7 142.86(14) . . ? C2 C1 Ni1 69.57(9) . . ? C7 C1 Ni1 147.24(11) . . ? N1 C3 C4 113.62(12) . . ? N1 C3 C5 124.92(14) . . ? C4 C3 C5 121.38(13) . . ? N2 C4 C3 113.54(12) . . ? N2 C4 C6 125.07(14) . . ? C3 C4 C6 121.26(13) . . ? C98 C9 C13 121.76(13) . . ? C98 C9 N2 119.98(13) . . ? C13 C9 N2 118.19(13) . . ? C24 C10 C19 122.07(14) . . ? C24 C10 N1 120.99(14) . . ? C19 C10 N1 116.81(13) . . ? C27 C7 C21 117.92(14) . . ? C27 C7 C1 122.43(13) . . ? C21 C7 C1 119.63(14) . . ? C17 C12 C8 120.38(15) . . ? C26 C13 C9 117.80(14) . . ? C26 C13 C29 120.47(14) . . ? C9 C13 C29 121.63(13) . . ? C26 C14 C30 119.90(15) . . ? C38 C17 C12 120.60(16) . . ? C34 C8 C12 118.44(14) . . ? C34 C8 C2 119.99(14) . . ? C12 C8 C2 121.57(13) . . ? C23 C19 C10 117.67(15) . . ? C23 C19 C25 120.73(15) . . ? C10 C19 C25 121.60(14) . . ? C47 C20 C24 110.95(15) . . ? C47 C20 C45 110.63(18) . . ? C24 C20 C45 112.69(15) . . ? C33 C21 C7 120.73(16) . . ? C32 C22 C24 121.51(16) . . ? C32 C23 C19 121.33(17) . . ? C22 C24 C10 117.50(15) . . ? C22 C24 C20 120.23(15) . . ? C10 C24 C20 122.15(14) . . ? C37 C25 C43 110.63(16) . . ? C37 C25 C19 113.17(14) . . ? C43 C25 C19 110.47(15) . . ? C14 C26 C13 121.30(16) . . ? C28 C27 C7 121.05(15) . . ? C35 C28 C27 120.17(16) . . ? C41 C29 C39 111.19(16) . . ? C41 C29 C13 109.95(14) . . ? C39 C29 C13 113.04(15) . . ? C14 C30 C98 121.25(16) . . ? C22 C32 C23 119.91(15) . . ? C21 C33 C35 120.49(16) . . ? C42 C34 C8 120.60(16) . . ? C28 C35 C33 119.63(16) . . ? C44 C36 C98 110.30(15) . . ? C44 C36 C40 110.12(15) . . ? C98 C36 C40 112.65(14) . . ? C17 C38 C42 119.68(16) . . ? C38 C42 C34 120.30(17) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.295 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.046 #=== END data_C16H26N2NiO4_Compound9 _database_code_depnum_ccdc_archive 'CCDC 762669' #TrackingRef 'Ni-diimines-cif_files.cif' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C16 H26 N2 Ni O4' _chemical_formula_weight 369.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.5058(6) _cell_length_b 12.0233(5) _cell_length_c 19.8419(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3699.1(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9155 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description irregular _exptl_crystal_colour blue _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method ? _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 1.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6614 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 63962 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0090 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3255 _reflns_number_gt 3001 _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^)+(0.0277P)^2^+1.6379P] 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 3255 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0224 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0543 _refine_ls_wR_factor_gt 0.0514 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.212469(10) 0.368384(13) 0.220094(8) 0.01881(7) Uani 1 1 d . . . O1 O 0.02323(7) 0.45971(8) 0.09843(5) 0.0331(2) Uani 1 1 d . . . O2 O 0.08497(6) 0.30824(8) 0.05376(5) 0.0297(2) Uani 1 1 d . . . O3 O 0.01202(7) 0.29132(11) 0.32203(5) 0.0438(3) Uani 1 1 d . . . O4 O -0.01439(6) 0.18819(8) 0.23074(5) 0.0300(2) Uani 1 1 d . . . N1 N 0.31204(7) 0.44314(9) 0.18178(5) 0.0209(2) Uani 1 1 d . . . N2 N 0.28195(7) 0.36885(9) 0.30107(6) 0.0216(2) Uani 1 1 d . . . C1 C 0.37000(9) 0.46436(12) 0.22632(7) 0.0258(3) Uani 1 1 d . . . H1 H 0.4207 0.5053 0.2158 0.031 Uiso 1 1 calc R . . C2 C 0.35344(9) 0.42220(12) 0.29337(7) 0.0261(3) Uani 1 1 d . . . H2 H 0.3928 0.4331 0.3295 0.031 Uiso 1 1 calc R . . C3 C 0.32458(9) 0.48087(11) 0.11079(6) 0.0237(3) Uani 1 1 d . . . C4 C 0.25895(9) 0.32179(12) 0.36825(7) 0.0257(3) Uani 1 1 d . . . C5 C 0.25620(10) 0.56979(12) 0.09767(7) 0.0315(3) Uani 1 1 d . . . H5A H 0.1989 0.5390 0.1069 0.047 Uiso 1 1 calc R . . H5B H 0.2593 0.5937 0.0505 0.047 Uiso 1 1 calc R . . H5C H 0.2665 0.6337 0.1272 0.047 Uiso 1 1 calc R . . C6 C 0.31066(11) 0.37887(12) 0.06628(7) 0.0322(3) Uani 1 1 d . . . H6A H 0.3539 0.3222 0.0772 0.048 Uiso 1 1 calc R . . H6B H 0.3163 0.4002 0.0188 0.048 Uiso 1 1 calc R . . H6C H 0.2528 0.3488 0.0742 0.048 Uiso 1 1 calc R . . C7 C 0.41464(10) 0.52828(13) 0.09722(7) 0.0322(3) Uani 1 1 d . . . H7A H 0.4235 0.5949 0.1249 0.048 Uiso 1 1 calc R . . H7B H 0.4198 0.5479 0.0494 0.048 Uiso 1 1 calc R . . H7C H 0.4583 0.4724 0.1087 0.048 Uiso 1 1 calc R . . C8 C 0.18588(10) 0.39327(12) 0.39605(7) 0.0300(3) Uani 1 1 d . . . H8A H 0.2065 0.4696 0.4025 0.045 Uiso 1 1 calc R . . H8B H 0.1666 0.3629 0.4393 0.045 Uiso 1 1 calc R . . H8C H 0.1376 0.3933 0.3641 0.045 Uiso 1 1 calc R . . C9 C 0.22937(10) 0.20217(12) 0.35694(8) 0.0324(3) Uani 1 1 d . . . H9A H 0.1806 0.2015 0.3255 0.049 Uiso 1 1 calc R . . H9B H 0.2115 0.1696 0.4000 0.049 Uiso 1 1 calc R . . H9C H 0.2770 0.1586 0.3380 0.049 Uiso 1 1 calc R . . C10 C 0.33478(10) 0.32208(15) 0.41765(8) 0.0400(4) Uani 1 1 d . . . H10A H 0.3834 0.2814 0.3979 0.060 Uiso 1 1 calc R . . H10B H 0.3173 0.2861 0.4598 0.060 Uiso 1 1 calc R . . H10C H 0.3522 0.3989 0.4269 0.060 Uiso 1 1 calc R . . C11 C 0.11520(8) 0.35090(10) 0.16590(7) 0.0225(3) Uani 1 1 d . . . C12 C 0.10116(9) 0.31147(11) 0.22555(6) 0.0224(3) Uani 1 1 d . . . C13 C 0.06932(8) 0.37944(11) 0.10413(7) 0.0224(3) Uani 1 1 d . . . C14 C 0.03005(8) 0.26546(11) 0.26524(7) 0.0242(3) Uani 1 1 d . . . C15 C 0.04264(10) 0.33358(15) -0.00938(7) 0.0361(4) Uani 1 1 d . . . H15A H -0.0197 0.3386 -0.0021 0.054 Uiso 1 1 calc R . . H15B H 0.0549 0.2746 -0.0421 0.054 Uiso 1 1 calc R . . H15C H 0.0641 0.4047 -0.0267 0.054 Uiso 1 1 calc R . . C16 C -0.08356(11) 0.13521(13) 0.26824(9) 0.0396(4) Uani 1 1 d . . . H16A H -0.0607 0.1049 0.3104 0.059 Uiso 1 1 calc R . . H16B H -0.1083 0.0749 0.2412 0.059 Uiso 1 1 calc R . . H16C H -0.1284 0.1902 0.2783 0.059 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 0.02016(11) 0.01943(10) 0.01686(10) 0.00282(6) 0.00015(6) -0.00067(6) O1 0.0346(5) 0.0353(6) 0.0295(5) -0.0028(4) -0.0068(4) 0.0114(5) O2 0.0354(5) 0.0329(5) 0.0207(5) -0.0023(4) -0.0041(4) 0.0086(4) O3 0.0351(6) 0.0677(8) 0.0286(6) -0.0099(5) 0.0098(5) -0.0122(6) O4 0.0284(5) 0.0288(5) 0.0328(5) 0.0016(4) 0.0027(4) -0.0073(4) N1 0.0254(5) 0.0190(5) 0.0185(6) 0.0011(4) 0.0024(4) 0.0007(4) N2 0.0245(6) 0.0215(6) 0.0189(6) 0.0039(4) 0.0005(4) 0.0021(4) C1 0.0251(7) 0.0282(7) 0.0241(7) 0.0029(5) 0.0019(5) -0.0053(6) C2 0.0255(7) 0.0309(7) 0.0218(7) 0.0025(6) -0.0034(5) -0.0029(6) C3 0.0302(7) 0.0241(7) 0.0169(6) 0.0037(5) 0.0030(5) -0.0030(6) C4 0.0277(7) 0.0308(7) 0.0187(6) 0.0075(5) 0.0003(6) -0.0011(6) C5 0.0393(8) 0.0303(7) 0.0249(7) 0.0090(6) 0.0011(6) 0.0008(6) C6 0.0415(8) 0.0318(8) 0.0234(8) -0.0045(6) 0.0072(6) -0.0055(6) C7 0.0361(8) 0.0363(8) 0.0243(7) 0.0051(6) 0.0066(6) -0.0085(6) C8 0.0358(8) 0.0319(7) 0.0223(7) 0.0001(6) 0.0046(6) -0.0042(6) C9 0.0385(8) 0.0269(7) 0.0317(8) 0.0106(6) 0.0057(6) 0.0028(6) C10 0.0359(8) 0.0580(10) 0.0259(8) 0.0184(7) -0.0048(6) -0.0050(8) C11 0.0230(6) 0.0208(6) 0.0236(7) -0.0004(5) 0.0000(5) 0.0010(5) C12 0.0234(6) 0.0202(6) 0.0235(7) -0.0008(5) 0.0002(5) 0.0008(5) C13 0.0192(6) 0.0253(7) 0.0228(7) 0.0019(5) 0.0016(5) -0.0033(5) C14 0.0211(6) 0.0260(7) 0.0255(7) 0.0034(5) -0.0009(5) 0.0018(5) C15 0.0358(8) 0.0531(9) 0.0194(7) -0.0025(7) -0.0029(6) 0.0109(7) C16 0.0312(8) 0.0383(9) 0.0494(10) 0.0162(7) 0.0005(7) -0.0117(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 Ni1 C12 1.8597(13) . ? Ni1 C11 1.8642(13) . ? Ni1 N2 1.9345(12) . ? Ni1 N1 1.9415(11) . ? O1 C13 1.2062(16) . ? O2 C13 1.3382(16) . ? O2 C15 1.4467(16) . ? O3 C14 1.2020(17) . ? O4 C14 1.3440(16) . ? O4 C16 1.4526(18) . ? N1 C1 1.2861(18) . ? N1 C3 1.4926(16) . ? N2 C2 1.2898(17) . ? N2 C4 1.4914(17) . ? C1 C2 1.4467(18) . ? C3 C6 1.5266(19) . ? C3 C5 1.528(2) . ? C3 C7 1.5322(19) . ? C4 C8 1.525(2) . ? C4 C9 1.526(2) . ? C4 C10 1.531(2) . ? C11 C12 1.2934(19) . ? C11 C13 1.4582(19) . ? C12 C14 1.4635(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Ni1 C11 40.65(6) . . ? C12 Ni1 N2 118.01(5) . . ? C11 Ni1 N2 158.43(5) . . ? C12 Ni1 N1 158.61(5) . . ? C11 Ni1 N1 118.02(5) . . ? N2 Ni1 N1 83.16(5) . . ? C13 O2 C15 115.45(11) . . ? C14 O4 C16 114.89(11) . . ? C1 N1 C3 119.81(11) . . ? C1 N1 Ni1 112.24(9) . . ? C3 N1 Ni1 127.87(8) . . ? C2 N2 C4 120.00(12) . . ? C2 N2 Ni1 112.45(9) . . ? C4 N2 Ni1 127.45(9) . . ? N1 C1 C2 116.00(12) . . ? N2 C2 C1 115.83(12) . . ? N1 C3 C6 106.46(10) . . ? N1 C3 C5 106.44(11) . . ? C6 C3 C5 111.43(12) . . ? N1 C3 C7 113.43(11) . . ? C6 C3 C7 109.03(12) . . ? C5 C3 C7 110.01(11) . . ? N2 C4 C8 106.68(11) . . ? N2 C4 C9 107.33(11) . . ? C8 C4 C9 111.16(11) . . ? N2 C4 C10 112.82(11) . . ? C8 C4 C10 109.74(12) . . ? C9 C4 C10 109.10(12) . . ? C12 C11 C13 140.66(13) . . ? C12 C11 Ni1 69.49(8) . . ? C13 C11 Ni1 148.54(10) . . ? C11 C12 C14 139.26(13) . . ? C11 C12 Ni1 69.86(8) . . ? C14 C12 Ni1 150.41(10) . . ? O1 C13 O2 123.32(12) . . ? O1 C13 C11 123.79(12) . . ? O2 C13 C11 112.88(11) . . ? O3 C14 O4 122.48(12) . . ? O3 C14 C12 125.59(13) . . ? O4 C14 C12 111.93(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.234 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.037 #=== END data_c37h62n2nisi2_Compound11 _database_code_depnum_ccdc_archive 'CCDC 762670' #TrackingRef 'Ni-diimines-cif_files.cif' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C37 H62 N2 Ni Si2' _chemical_formula_weight 649.78 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' Si Si 0.0817 0.0704 '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 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 22.3895(5) _cell_length_b 9.7738(2) _cell_length_c 18.2857(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.8870(10) _cell_angle_gamma 90.00 _cell_volume 3762.84(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9951 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.44 _exptl_crystal_description blocks _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8393 _exptl_absorpt_correction_T_max 0.9420 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 27639 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6619 _reflns_number_gt 5807 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (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^)+(0.0456P)^2^+3.0236P] 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 6619 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.251889(10) 0.11063(2) 0.251838(13) 0.01776(8) Uani 1 1 d . . . Si1 Si 0.38509(3) -0.01257(6) 0.20463(3) 0.02386(13) Uani 1 1 d . . . Si2 Si 0.20070(3) -0.19123(6) 0.13560(3) 0.02876(14) Uani 1 1 d . . . N1 N 0.17457(7) 0.19662(17) 0.25153(9) 0.0209(3) Uani 1 1 d . . . N2 N 0.28758(7) 0.23922(15) 0.33555(8) 0.0173(3) Uani 1 1 d . . . C1 C 0.11176(9) 0.1635(2) 0.20021(11) 0.0246(4) Uani 1 1 d . . . C2 C 0.07153(11) 0.0889(3) 0.22971(13) 0.0409(6) Uani 1 1 d . . . C3 C 0.09328(14) 0.0425(5) 0.31482(14) 0.0732(12) Uani 1 1 d . . . H3 H 0.1224 0.1152 0.3459 0.088 Uiso 1 1 calc R . . C4 C 0.0381(2) 0.0322(8) 0.34609(19) 0.165(3) Uani 1 1 d . . . C5 C 0.1325(2) -0.0901(5) 0.3267(2) 0.1128(19) Uani 1 1 d . . . H5A H 0.1505 -0.1108 0.3824 0.169 Uiso 1 1 calc R . . H5B H 0.1670 -0.0783 0.3056 0.169 Uiso 1 1 calc R . . H5C H 0.1051 -0.1657 0.2998 0.169 Uiso 1 1 calc R . . C6 C 0.01143(11) 0.0540(3) 0.17847(14) 0.0489(7) Uani 1 1 d . . . H6 H -0.0167 0.0040 0.1973 0.059 Uiso 1 1 calc R . . C7 C -0.00801(10) 0.0905(3) 0.10111(14) 0.0421(6) Uani 1 1 d . . . H7 H -0.0490 0.0648 0.0671 0.051 Uiso 1 1 calc R . . C8 C 0.03181(10) 0.1638(2) 0.07337(13) 0.0327(5) Uani 1 1 d . . . H8 H 0.0180 0.1888 0.0200 0.039 Uiso 1 1 calc R . . C9 C 0.09251(9) 0.2026(2) 0.12221(12) 0.0253(4) Uani 1 1 d . . . C10 C 0.13406(10) 0.2887(2) 0.09020(12) 0.0307(5) Uani 1 1 d . . . H10 H 0.1760 0.3003 0.1325 0.037 Uiso 1 1 calc R . . C11 C 0.14610(13) 0.2202(3) 0.02166(15) 0.0461(6) Uani 1 1 d . . . H11A H 0.1680 0.1329 0.0385 0.069 Uiso 1 1 calc R . . H11B H 0.1726 0.2799 0.0023 0.069 Uiso 1 1 calc R . . H11C H 0.1055 0.2038 -0.0199 0.069 Uiso 1 1 calc R . . C12 C 0.10509(14) 0.4311(3) 0.06797(15) 0.0486(6) Uani 1 1 d . . . H12A H 0.0631 0.4226 0.0278 0.073 Uiso 1 1 calc R . . H12B H 0.1327 0.4861 0.0479 0.073 Uiso 1 1 calc R . . H12C H 0.1009 0.4758 0.1139 0.073 Uiso 1 1 calc R . . C13 C 0.18248(9) 0.3048(2) 0.29772(11) 0.0234(4) Uani 1 1 d . . . C14 C 0.13007(10) 0.3997(3) 0.29818(14) 0.0394(6) Uani 1 1 d . . . H14A H 0.0920 0.3800 0.2533 0.059 Uiso 1 1 calc R . . H14B H 0.1433 0.4945 0.2953 0.059 Uiso 1 1 calc R . . H14C H 0.1206 0.3867 0.3462 0.059 Uiso 1 1 calc R . . C15 C 0.24641(9) 0.32234(19) 0.34964(11) 0.0200(4) Uani 1 1 d . . . C16 C 0.26227(10) 0.4234(2) 0.41521(12) 0.0291(5) Uani 1 1 d . . . H16A H 0.3071 0.4140 0.4474 0.044 Uiso 1 1 calc R . . H16B H 0.2356 0.4059 0.4471 0.044 Uiso 1 1 calc R . . H16C H 0.2544 0.5164 0.3940 0.044 Uiso 1 1 calc R . . C17 C 0.35105(8) 0.23082(19) 0.39104(10) 0.0176(4) Uani 1 1 d . . . C18 C 0.39686(9) 0.32740(19) 0.38966(11) 0.0202(4) Uani 1 1 d . . . C19 C 0.45838(9) 0.3108(2) 0.44242(11) 0.0254(4) Uani 1 1 d . . . H19 H 0.4904 0.3746 0.4426 0.030 Uiso 1 1 calc R . . C20 C 0.47349(9) 0.2029(2) 0.49449(12) 0.0281(5) Uani 1 1 d . . . H20 H 0.5157 0.1925 0.5295 0.034 Uiso 1 1 calc R . . C21 C 0.42746(10) 0.1104(2) 0.49574(12) 0.0265(4) Uani 1 1 d . . . H21 H 0.4383 0.0371 0.5320 0.032 Uiso 1 1 calc R . . C22 C 0.36522(9) 0.12268(19) 0.44462(11) 0.0214(4) Uani 1 1 d . . . C23 C 0.31452(10) 0.0226(2) 0.44927(12) 0.0271(4) Uani 1 1 d . . . H23 H 0.2739 0.0473 0.4073 0.033 Uiso 1 1 calc R . . C24 C 0.33055(13) -0.1244(2) 0.43510(16) 0.0434(6) Uani 1 1 d . . . H24A H 0.3364 -0.1306 0.3845 0.065 Uiso 1 1 calc R . . H24B H 0.2958 -0.1849 0.4355 0.065 Uiso 1 1 calc R . . H24C H 0.3698 -0.1523 0.4762 0.065 Uiso 1 1 calc R . . C25 C 0.30374(13) 0.0359(3) 0.52744(15) 0.0463(6) Uani 1 1 d . . . H25A H 0.3421 0.0069 0.5695 0.069 Uiso 1 1 calc R . . H25B H 0.2679 -0.0221 0.5271 0.069 Uiso 1 1 calc R . . H25C H 0.2943 0.1315 0.5356 0.069 Uiso 1 1 calc R . . C26 C 0.38074(9) 0.4449(2) 0.33176(11) 0.0244(4) Uani 1 1 d . . . H26 H 0.3335 0.4560 0.3130 0.029 Uiso 1 1 calc R . . C27 C 0.39898(19) 0.4112(3) 0.26194(17) 0.0683(10) Uani 1 1 d . . . H27A H 0.4451 0.3979 0.2782 0.102 Uiso 1 1 calc R . . H27B H 0.3864 0.4866 0.2244 0.102 Uiso 1 1 calc R . . H27C H 0.3774 0.3271 0.2377 0.102 Uiso 1 1 calc R . . C28 C 0.40915(14) 0.5800(2) 0.36838(16) 0.0513(7) Uani 1 1 d . . . H28A H 0.4554 0.5765 0.3825 0.077 Uiso 1 1 calc R . . H28B H 0.3981 0.5962 0.4151 0.077 Uiso 1 1 calc R . . H28C H 0.3922 0.6544 0.3311 0.077 Uiso 1 1 calc R . . C29 C 0.30444(9) 0.0047(2) 0.21135(11) 0.0237(4) Uani 1 1 d . . . C30 C 0.39449(12) -0.1876(2) 0.16796(16) 0.0441(6) Uani 1 1 d . . . H30A H 0.3885 -0.2567 0.2037 0.066 Uiso 1 1 calc R . . H30B H 0.4371 -0.1966 0.1648 0.066 Uiso 1 1 calc R . . H30C H 0.3627 -0.2009 0.1162 0.066 Uiso 1 1 calc R . . C31 C 0.44668(10) 0.0120(3) 0.30199(13) 0.0368(5) Uani 1 1 d . . . H31A H 0.4410 0.1016 0.3227 0.055 Uiso 1 1 calc R . . H31B H 0.4889 0.0071 0.2973 0.055 Uiso 1 1 calc R . . H31C H 0.4426 -0.0600 0.3373 0.055 Uiso 1 1 calc R . . C32 C 0.39403(13) 0.1131(3) 0.13227(14) 0.0431(6) Uani 1 1 d . . . H32A H 0.3660 0.0874 0.0801 0.065 Uiso 1 1 calc R . . H32B H 0.4382 0.1133 0.1337 0.065 Uiso 1 1 calc R . . H32C H 0.3827 0.2047 0.1450 0.065 Uiso 1 1 calc R . . C33 C 0.24741(9) -0.0431(2) 0.18833(11) 0.0237(4) Uani 1 1 d . . . C34 C 0.20719(14) -0.1974(3) 0.03653(14) 0.0478(6) Uani 1 1 d . . . H34A H 0.1866 -0.1166 0.0069 0.072 Uiso 1 1 calc R . . H34B H 0.1863 -0.2803 0.0096 0.072 Uiso 1 1 calc R . . H34C H 0.2521 -0.1986 0.0411 0.072 Uiso 1 1 calc R . . C35 C 0.11475(11) -0.1825(3) 0.12236(17) 0.0469(6) Uani 1 1 d . . . H35A H 0.1091 -0.1927 0.1729 0.070 Uiso 1 1 calc R . . H35B H 0.0922 -0.2563 0.0876 0.070 Uiso 1 1 calc R . . H35C H 0.0976 -0.0940 0.0996 0.070 Uiso 1 1 calc R . . C36 C 0.23762(12) -0.3455(2) 0.19440(16) 0.0482(7) Uani 1 1 d . . . H36A H 0.2822 -0.3522 0.1980 0.072 Uiso 1 1 calc R . . H36B H 0.2148 -0.4278 0.1692 0.072 Uiso 1 1 calc R . . H36C H 0.2352 -0.3371 0.2467 0.072 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 0.01456(13) 0.01996(14) 0.01800(14) -0.00439(9) 0.00456(10) -0.00163(9) Si1 0.0226(3) 0.0254(3) 0.0249(3) -0.0028(2) 0.0098(2) 0.0029(2) Si2 0.0284(3) 0.0204(3) 0.0293(3) -0.0053(2) -0.0008(2) -0.0017(2) N1 0.0135(7) 0.0309(9) 0.0179(8) -0.0033(7) 0.0049(6) -0.0030(6) N2 0.0135(7) 0.0198(8) 0.0176(7) -0.0020(6) 0.0041(6) -0.0017(6) C1 0.0125(9) 0.0376(11) 0.0228(10) -0.0092(9) 0.0047(8) -0.0016(8) C2 0.0252(11) 0.0748(18) 0.0247(11) -0.0124(11) 0.0113(9) -0.0190(11) C3 0.0537(18) 0.144(3) 0.0211(13) -0.0077(17) 0.0118(12) -0.061(2) C4 0.085(3) 0.387(9) 0.0344(17) -0.043(3) 0.0372(18) -0.131(4) C5 0.133(4) 0.136(4) 0.0407(19) 0.043(2) -0.007(2) -0.051(3) C6 0.0261(12) 0.089(2) 0.0347(13) -0.0165(13) 0.0137(10) -0.0252(13) C7 0.0173(10) 0.0626(16) 0.0390(13) -0.0162(12) -0.0001(9) -0.0074(10) C8 0.0236(11) 0.0384(12) 0.0277(11) -0.0036(10) -0.0024(9) 0.0024(9) C9 0.0208(10) 0.0257(10) 0.0258(10) -0.0047(8) 0.0033(8) 0.0026(8) C10 0.0307(11) 0.0317(11) 0.0235(10) 0.0026(9) 0.0013(9) -0.0031(9) C11 0.0563(16) 0.0418(14) 0.0485(15) 0.0011(12) 0.0287(13) -0.0053(12) C12 0.0676(18) 0.0317(12) 0.0395(14) 0.0026(11) 0.0088(13) -0.0007(12) C13 0.0162(9) 0.0333(11) 0.0206(10) -0.0049(8) 0.0061(8) 0.0011(8) C14 0.0210(11) 0.0572(15) 0.0367(13) -0.0169(11) 0.0053(9) 0.0096(10) C15 0.0173(9) 0.0237(10) 0.0192(9) -0.0030(8) 0.0065(7) -0.0012(8) C16 0.0218(10) 0.0354(11) 0.0287(11) -0.0132(9) 0.0067(8) 0.0014(9) C17 0.0141(8) 0.0206(9) 0.0166(9) -0.0045(7) 0.0034(7) 0.0010(7) C18 0.0180(9) 0.0208(9) 0.0213(9) -0.0042(8) 0.0062(7) -0.0005(7) C19 0.0172(9) 0.0275(10) 0.0283(11) -0.0057(8) 0.0034(8) -0.0041(8) C20 0.0178(10) 0.0313(11) 0.0269(11) -0.0051(9) -0.0030(8) 0.0026(8) C21 0.0276(11) 0.0254(10) 0.0221(10) 0.0003(8) 0.0027(8) 0.0040(8) C22 0.0213(10) 0.0220(10) 0.0195(9) -0.0028(8) 0.0050(8) 0.0004(8) C23 0.0265(10) 0.0251(10) 0.0281(11) 0.0037(8) 0.0072(8) -0.0032(8) C24 0.0574(16) 0.0270(12) 0.0542(15) -0.0064(11) 0.0299(13) -0.0102(11) C25 0.0566(16) 0.0430(14) 0.0520(15) -0.0076(12) 0.0350(13) -0.0119(12) C26 0.0210(10) 0.0224(10) 0.0280(10) 0.0004(8) 0.0058(8) -0.0032(8) C27 0.134(3) 0.0412(15) 0.0488(17) 0.0158(13) 0.056(2) 0.0268(17) C28 0.0697(18) 0.0233(12) 0.0482(15) 0.0002(11) 0.0036(13) -0.0056(12) C29 0.0242(10) 0.0235(10) 0.0231(10) -0.0041(8) 0.0077(8) 0.0024(8) C30 0.0439(14) 0.0351(13) 0.0596(16) -0.0134(12) 0.0257(13) 0.0022(11) C31 0.0256(11) 0.0524(14) 0.0302(11) -0.0025(10) 0.0069(9) 0.0098(10) C32 0.0502(15) 0.0485(15) 0.0361(13) 0.0065(11) 0.0218(12) 0.0049(12) C33 0.0255(10) 0.0219(10) 0.0219(10) -0.0060(8) 0.0059(8) 0.0012(8) C34 0.0620(17) 0.0382(14) 0.0352(13) -0.0138(11) 0.0062(12) 0.0023(12) C35 0.0292(12) 0.0361(13) 0.0618(17) -0.0093(12) -0.0020(11) -0.0069(10) C36 0.0447(15) 0.0293(12) 0.0555(16) 0.0060(11) -0.0025(12) -0.0041(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 Ni1 C33 1.8807(19) . ? Ni1 C29 1.8963(19) . ? Ni1 N1 1.9227(15) . ? Ni1 N2 1.9311(15) . ? Si1 C29 1.859(2) . ? Si1 C31 1.860(2) . ? Si1 C32 1.865(2) . ? Si1 C30 1.875(2) . ? Si2 C33 1.853(2) . ? Si2 C35 1.858(2) . ? Si2 C34 1.867(3) . ? Si2 C36 1.873(2) . ? N1 C13 1.327(2) . ? N1 C1 1.437(2) . ? N2 C15 1.318(2) . ? N2 C17 1.440(2) . ? C1 C9 1.396(3) . ? C1 C2 1.402(3) . ? C2 C6 1.395(3) . ? C2 C3 1.533(4) . ? C3 C4 1.532(4) . ? C3 C5 1.540(6) . ? C3 H3 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.378(4) . ? C6 H6 0.9500 . ? C7 C8 1.368(3) . ? C7 H7 0.9500 . ? C8 C9 1.401(3) . ? C8 H8 0.9500 . ? C9 C10 1.512(3) . ? C10 C11 1.523(3) . ? C10 C12 1.531(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.434(3) . ? C13 C14 1.498(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.500(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.400(3) . ? C17 C22 1.402(3) . ? C18 C19 1.397(3) . ? C18 C26 1.520(3) . ? C19 C20 1.383(3) . ? C19 H19 0.9500 . ? C20 C21 1.377(3) . ? C20 H20 0.9500 . ? C21 C22 1.394(3) . ? C21 H21 0.9500 . ? C22 C23 1.523(3) . ? C23 C24 1.525(3) . ? C23 C25 1.534(3) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.503(3) . ? C26 C28 1.518(3) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C33 1.288(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 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 C33 Ni1 C29 39.89(8) . . ? C33 Ni1 N1 119.25(8) . . ? C29 Ni1 N1 156.21(7) . . ? C33 Ni1 N2 158.46(8) . . ? C29 Ni1 N2 121.35(7) . . ? N1 Ni1 N2 81.22(6) . . ? C29 Si1 C31 110.22(9) . . ? C29 Si1 C32 109.15(10) . . ? C31 Si1 C32 111.75(12) . . ? C29 Si1 C30 109.65(10) . . ? C31 Si1 C30 108.85(12) . . ? C32 Si1 C30 107.16(12) . . ? C33 Si2 C35 114.10(10) . . ? C33 Si2 C34 108.28(11) . . ? C35 Si2 C34 107.11(13) . . ? C33 Si2 C36 105.63(10) . . ? C35 Si2 C36 110.30(12) . . ? C34 Si2 C36 111.48(13) . . ? C13 N1 C1 118.98(16) . . ? C13 N1 Ni1 114.91(12) . . ? C1 N1 Ni1 125.69(12) . . ? C15 N2 C17 119.04(15) . . ? C15 N2 Ni1 115.32(12) . . ? C17 N2 Ni1 124.36(11) . . ? C9 C1 C2 121.35(18) . . ? C9 C1 N1 119.93(17) . . ? C2 C1 N1 118.70(18) . . ? C6 C2 C1 117.9(2) . . ? C6 C2 C3 120.7(2) . . ? C1 C2 C3 121.39(19) . . ? C4 C3 C2 112.4(3) . . ? C4 C3 C5 112.7(4) . . ? C2 C3 C5 111.2(3) . . ? C4 C3 H3 106.7 . . ? C2 C3 H3 106.7 . . ? C5 C3 H3 106.7 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C2 121.5(2) . . ? C7 C6 H6 119.3 . . ? C2 C6 H6 119.3 . . ? C8 C7 C6 119.9(2) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 121.2(2) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C1 C9 C8 118.21(19) . . ? C1 C9 C10 122.09(17) . . ? C8 C9 C10 119.67(19) . . ? C9 C10 C11 112.23(18) . . ? C9 C10 C12 110.36(19) . . ? C11 C10 C12 111.01(19) . . ? C9 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? 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 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C15 113.84(16) . . ? N1 C13 C14 124.18(17) . . ? C15 C13 C14 121.97(17) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C13 113.81(16) . . ? N2 C15 C16 124.82(16) . . ? C13 C15 C16 121.32(16) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 121.85(16) . . ? C18 C17 N2 120.13(16) . . ? C22 C17 N2 118.01(16) . . ? C19 C18 C17 117.73(17) . . ? C19 C18 C26 120.92(17) . . ? C17 C18 C26 121.34(16) . . ? C20 C19 C18 121.14(18) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C21 C20 C19 120.17(18) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 121.02(18) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C21 C22 C17 118.06(17) . . ? C21 C22 C23 120.08(17) . . ? C17 C22 C23 121.84(17) . . ? C22 C23 C24 111.90(18) . . ? C22 C23 C25 110.74(17) . . ? C24 C23 C25 111.05(19) . . ? C22 C23 H23 107.6 . . ? C24 C23 H23 107.6 . . ? C25 C23 H23 107.6 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C28 111.8(2) . . ? C27 C26 C18 110.91(18) . . ? C28 C26 C18 112.65(17) . . ? C27 C26 H26 107.0 . . ? C28 C26 H26 107.0 . . ? C18 C26 H26 107.0 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C33 C29 Si1 145.31(16) . . ? C33 C29 Ni1 69.40(12) . . ? Si1 C29 Ni1 145.20(11) . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 Si2 140.78(16) . . ? C29 C33 Ni1 70.71(12) . . ? Si2 C33 Ni1 147.95(12) . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si2 C36 H36A 109.5 . . ? Si2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si2 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.644 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.051 _vrf_C38H50N2NiO2_Compound15 ; PROBLEM:Large Non-Solvent C Ueq(max)/Ueq(min) ... 9.38 Ratio Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.83 Ratio RESPONSE: These atoms are part of a disordered CH3 group. ; #=== END data_C38H50N2NiO2_Compound15 _database_code_depnum_ccdc_archive 'CCDC 762671' #TrackingRef 'Ni-diimines-cif_files.cif' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C38 H50 N2 Ni O2' _chemical_formula_weight 625.51 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 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 14.6319(4) _cell_length_b 9.4273(3) _cell_length_c 25.7606(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.676(2) _cell_angle_gamma 90.00 _cell_volume 3541.57(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9885 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 25.66 _exptl_crystal_description needles _exptl_crystal_colour green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.581 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6892 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 96854 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6241 _reflns_number_gt 5280 _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^)+(0.0318P)^2^+4.9497P] 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 6241 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.24981(2) 0.25978(3) 0.363692(11) 0.02296(10) Uani 1 1 d . . . O1 O 0.36300(16) 0.4844(3) 0.29026(8) 0.0590(6) Uani 1 1 d . . . O2 O 0.22775(16) 0.4714(2) 0.24207(7) 0.0541(6) Uani 1 1 d . . . N1 N 0.29257(12) 0.1210(2) 0.41465(7) 0.0220(4) Uani 1 1 d . . . N2 N 0.22238(13) 0.0898(2) 0.32346(7) 0.0237(4) Uani 1 1 d . . . C1 C 0.28646(16) -0.0101(2) 0.40017(9) 0.0245(5) Uani 1 1 d . . . C2 C 0.24346(16) -0.0293(3) 0.34666(9) 0.0244(5) Uani 1 1 d . . . C3 C 0.26439(17) 0.4576(2) 0.38414(9) 0.0270(5) Uani 1 1 d . . . H3 H 0.3296 0.4901 0.3865 0.032 Uiso 1 1 calc R . . C4 C 0.22445(18) 0.4451(3) 0.33128(9) 0.0294(6) Uani 1 1 d . . . H4 H 0.1584 0.4720 0.3251 0.035 Uiso 1 1 calc R . . C5 C 0.21399(17) 0.5067(3) 0.42768(10) 0.0285(6) Uani 1 1 d . . . C6 C 0.1228(2) 0.5468(3) 0.42204(11) 0.0444(7) Uani 1 1 d . . . H6 H 0.0900 0.5398 0.3888 0.053 Uiso 1 1 calc R . . C7 C 0.0782(2) 0.5966(4) 0.46342(13) 0.0606(10) Uani 1 1 d . . . H7 H 0.0158 0.6248 0.4583 0.073 Uiso 1 1 calc R . . C8 C 0.1240(2) 0.6057(4) 0.51265(13) 0.0587(9) Uani 1 1 d . . . H8 H 0.0935 0.6401 0.5413 0.070 Uiso 1 1 calc R . . C9 C 0.2141(2) 0.5643(3) 0.51940(11) 0.0409(7) Uani 1 1 d . . . H9 H 0.2459 0.5684 0.5530 0.049 Uiso 1 1 calc R . . C10 C 0.25870(18) 0.5167(3) 0.47758(9) 0.0284(5) Uani 1 1 d . . . H10 H 0.3214 0.4900 0.4828 0.034 Uiso 1 1 calc R . . C11 C 0.2806(2) 0.4680(3) 0.28813(10) 0.0394(7) Uani 1 1 d . . . C12 C 0.2755(3) 0.4895(4) 0.19556(12) 0.0780(13) Uani 1 1 d . . . H12A H 0.3368 0.5283 0.2050 0.117 Uiso 1 1 calc R . . H12B H 0.2410 0.5550 0.1718 0.117 Uiso 1 1 calc R . . H12C H 0.2811 0.3975 0.1784 0.117 Uiso 1 1 calc R . . C13 C 0.3189(2) -0.1362(3) 0.43177(10) 0.0382(7) Uani 1 1 d . . . H13A H 0.3538 -0.1043 0.4637 0.057 Uiso 1 1 calc R . . H13B H 0.3582 -0.1950 0.4115 0.057 Uiso 1 1 calc R . . H13C H 0.2659 -0.1919 0.4408 0.057 Uiso 1 1 calc R . . C14 C 0.22788(19) -0.1744(3) 0.32479(10) 0.0344(6) Uani 1 1 d . . . H14A H 0.1932 -0.1679 0.2907 0.052 Uiso 1 1 calc R . . H14B H 0.1931 -0.2307 0.3484 0.052 Uiso 1 1 calc R . . H14C H 0.2871 -0.2202 0.3209 0.052 Uiso 1 1 calc R . . C15 C 0.33214(16) 0.1603(2) 0.46577(8) 0.0228(5) Uani 1 1 d . . . C16 C 0.41904(16) 0.2219(2) 0.46922(9) 0.0261(5) Uani 1 1 d . . . C17 C 0.45458(18) 0.2700(3) 0.51780(10) 0.0325(6) Uani 1 1 d . . . H17 H 0.5137 0.3123 0.5213 0.039 Uiso 1 1 calc R . . C18 C 0.40533(19) 0.2571(3) 0.56106(10) 0.0361(6) Uani 1 1 d . . . H18 H 0.4306 0.2906 0.5939 0.043 Uiso 1 1 calc R . . C19 C 0.31946(19) 0.1958(3) 0.55651(9) 0.0333(6) Uani 1 1 d . . . H19 H 0.2861 0.1877 0.5865 0.040 Uiso 1 1 calc R . . C20 C 0.28034(17) 0.1452(3) 0.50874(9) 0.0277(5) Uani 1 1 d . . . C21 C 0.47199(17) 0.2377(3) 0.42117(10) 0.0333(6) Uani 1 1 d . . . H21 H 0.4256 0.2482 0.3907 0.040 Uiso 1 1 calc R . . C22 C 0.5271(2) 0.1040(4) 0.41183(13) 0.0614(10) Uani 1 1 d . . . H22A H 0.5743 0.0909 0.4407 0.092 Uiso 1 1 calc R . . H22B H 0.5563 0.1134 0.3791 0.092 Uiso 1 1 calc R . . H22C H 0.4860 0.0217 0.4098 0.092 Uiso 1 1 calc R . . C23 C 0.5318(3) 0.3699(4) 0.42276(14) 0.0716(12) Uani 1 1 d . . . H23A H 0.4954 0.4523 0.4318 0.107 Uiso 1 1 calc R . . H23B H 0.5548 0.3849 0.3885 0.107 Uiso 1 1 calc R . . H23C H 0.5836 0.3577 0.4490 0.107 Uiso 1 1 calc R . . C24 C 0.18462(18) 0.0822(3) 0.50361(11) 0.0359(6) Uani 1 1 d . . . H24 H 0.1833 0.0106 0.4749 0.043 Uiso 1 1 calc R . . C25 C 0.1151(2) 0.1947(5) 0.4868(3) 0.129(3) Uani 1 1 d . . . H25A H 0.0559 0.1498 0.4765 0.194 Uiso 1 1 calc R . . H25B H 0.1360 0.2472 0.4571 0.194 Uiso 1 1 calc R . . H25C H 0.1082 0.2602 0.5157 0.194 Uiso 1 1 calc R . . C26 C 0.1603(4) 0.0051(7) 0.55148(15) 0.125(2) Uani 1 1 d . . . H26A H 0.2067 -0.0676 0.5607 0.187 Uiso 1 1 calc R . . H26B H 0.1002 -0.0400 0.5447 0.187 Uiso 1 1 calc R . . H26C H 0.1582 0.0726 0.5803 0.187 Uiso 1 1 calc R . . C27 C 0.18168(18) 0.0944(2) 0.27083(9) 0.0272(5) Uani 1 1 d . . . C28 C 0.08907(18) 0.1353(3) 0.26345(10) 0.0313(6) Uani 1 1 d . . . C29 C 0.0516(2) 0.1520(3) 0.21222(11) 0.0432(7) Uani 1 1 d . . . H29 H -0.0109 0.1789 0.2058 0.052 Uiso 1 1 calc R . . C30 C 0.1039(3) 0.1301(3) 0.17102(11) 0.0519(9) Uani 1 1 d . . . H30 H 0.0772 0.1430 0.1365 0.062 Uiso 1 1 calc R . . C31 C 0.1939(3) 0.0901(3) 0.17899(11) 0.0497(8) Uani 1 1 d . . . H31 H 0.2285 0.0756 0.1498 0.060 Uiso 1 1 calc R . . C32 C 0.2361(2) 0.0700(3) 0.22944(10) 0.0379(7) Uani 1 1 d . . . C33 C 0.03392(18) 0.1588(3) 0.30987(11) 0.0349(6) Uani 1 1 d . . . H33 H 0.0752 0.2062 0.3374 0.042 Uiso 1 1 calc R . . C34 C 0.0032(2) 0.0179(3) 0.33246(12) 0.0451(7) Uani 1 1 d . . . H34A H -0.0388 -0.0305 0.3067 0.068 Uiso 1 1 calc R . . H34B H -0.0281 0.0362 0.3640 0.068 Uiso 1 1 calc R . . H34C H 0.0570 -0.0422 0.3412 0.068 Uiso 1 1 calc R . . C35 C -0.0499(2) 0.2542(3) 0.29893(14) 0.0557(9) Uani 1 1 d . . . H35A H -0.0313 0.3430 0.2831 0.083 Uiso 1 1 calc R . . H35B H -0.0769 0.2751 0.3317 0.083 Uiso 1 1 calc R . . H35C H -0.0953 0.2058 0.2751 0.083 Uiso 1 1 calc R . . C36 C 0.3357(2) 0.0266(3) 0.23720(12) 0.0492(8) Uani 1 1 d . . . H36 H 0.3505 0.0104 0.2753 0.059 Uiso 1 1 calc R . . C37 C 0.3996(3) 0.1412(5) 0.22043(18) 0.0859(14) Uani 1 1 d . . . H37A H 0.3824 0.1670 0.1841 0.129 Uiso 1 1 calc R . . H37B H 0.4628 0.1058 0.2237 0.129 Uiso 1 1 calc R . . H37C H 0.3950 0.2248 0.2427 0.129 Uiso 1 1 calc R . . C38 C 0.3526(3) -0.1138(5) 0.20912(18) 0.1006(17) Uani 1 1 d . . . H38A H 0.3433 -0.0994 0.1714 0.151 Uiso 1 1 calc R . . H38B H 0.3096 -0.1858 0.2198 0.151 Uiso 1 1 calc R . . H38C H 0.4156 -0.1455 0.2183 0.151 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 0.02879(17) 0.01986(16) 0.01954(16) -0.00126(12) -0.00230(11) 0.00060(13) O1 0.0552(14) 0.0817(18) 0.0414(12) 0.0000(12) 0.0114(11) -0.0208(13) O2 0.0776(16) 0.0599(14) 0.0238(10) 0.0054(10) -0.0017(10) 0.0096(12) N1 0.0218(10) 0.0261(11) 0.0177(9) -0.0030(8) -0.0014(8) 0.0009(8) N2 0.0267(11) 0.0245(10) 0.0194(10) -0.0015(8) -0.0007(8) 0.0015(8) C1 0.0274(12) 0.0230(12) 0.0225(12) -0.0008(10) -0.0012(10) 0.0028(10) C2 0.0244(12) 0.0255(13) 0.0227(12) -0.0016(10) -0.0012(10) 0.0020(10) C3 0.0325(14) 0.0188(12) 0.0292(13) -0.0018(10) -0.0013(11) -0.0020(10) C4 0.0377(15) 0.0224(12) 0.0269(13) 0.0019(10) -0.0045(11) 0.0019(11) C5 0.0335(14) 0.0214(12) 0.0298(13) -0.0011(10) -0.0014(11) 0.0005(10) C6 0.0380(16) 0.059(2) 0.0358(16) -0.0091(14) -0.0012(13) 0.0100(14) C7 0.0424(18) 0.087(3) 0.053(2) -0.0087(19) 0.0035(15) 0.0216(18) C8 0.060(2) 0.074(2) 0.0437(18) -0.0125(17) 0.0139(16) 0.0163(19) C9 0.0486(18) 0.0421(16) 0.0315(15) -0.0067(13) 0.0007(13) -0.0004(14) C10 0.0339(14) 0.0233(12) 0.0277(13) -0.0027(10) 0.0003(11) -0.0014(11) C11 0.061(2) 0.0291(14) 0.0277(14) 0.0031(11) 0.0009(13) -0.0008(14) C12 0.141(4) 0.071(3) 0.0242(16) 0.0105(16) 0.017(2) 0.016(3) C13 0.0522(17) 0.0281(14) 0.0317(14) -0.0004(11) -0.0120(13) 0.0095(13) C14 0.0472(16) 0.0251(13) 0.0292(14) -0.0031(11) -0.0073(12) 0.0023(12) C15 0.0281(13) 0.0205(12) 0.0188(11) -0.0022(9) -0.0035(10) 0.0049(10) C16 0.0266(12) 0.0234(12) 0.0275(13) -0.0039(10) -0.0020(10) 0.0053(10) C17 0.0307(13) 0.0320(14) 0.0328(14) -0.0055(11) -0.0091(11) 0.0026(11) C18 0.0478(16) 0.0333(14) 0.0247(13) -0.0070(11) -0.0116(12) 0.0055(13) C19 0.0489(17) 0.0317(14) 0.0193(12) 0.0006(10) 0.0032(11) 0.0048(12) C20 0.0341(14) 0.0239(12) 0.0247(13) 0.0000(10) 0.0001(11) 0.0029(10) C21 0.0274(13) 0.0402(15) 0.0323(14) -0.0074(12) 0.0025(11) -0.0002(12) C22 0.059(2) 0.078(3) 0.0476(19) -0.0071(18) 0.0111(16) 0.0308(19) C23 0.068(2) 0.088(3) 0.063(2) -0.031(2) 0.0335(19) -0.045(2) C24 0.0384(15) 0.0349(15) 0.0354(15) -0.0059(12) 0.0094(12) -0.0072(12) C25 0.0254(19) 0.055(3) 0.305(8) -0.010(4) 0.002(3) -0.0013(18) C26 0.128(4) 0.198(6) 0.047(2) 0.022(3) 0.005(3) -0.116(4) C27 0.0422(15) 0.0190(12) 0.0193(12) -0.0020(9) -0.0044(11) -0.0024(11) C28 0.0421(15) 0.0190(12) 0.0307(14) 0.0011(10) -0.0102(12) -0.0031(11) C29 0.0552(18) 0.0311(15) 0.0394(16) 0.0056(12) -0.0206(14) -0.0078(13) C30 0.083(2) 0.0444(18) 0.0244(15) 0.0041(13) -0.0185(16) -0.0172(17) C31 0.084(3) 0.0445(18) 0.0208(14) -0.0032(13) 0.0047(15) -0.0143(17) C32 0.0577(18) 0.0304(14) 0.0255(14) -0.0039(11) 0.0041(13) -0.0041(13) C33 0.0331(14) 0.0265(13) 0.0433(16) 0.0001(12) -0.0067(12) 0.0019(11) C34 0.0415(17) 0.0385(16) 0.0562(19) 0.0062(14) 0.0093(14) 0.0042(13) C35 0.0470(18) 0.0412(18) 0.077(2) 0.0056(17) -0.0063(16) 0.0132(15) C36 0.059(2) 0.0543(19) 0.0365(16) -0.0041(14) 0.0177(15) 0.0103(16) C37 0.060(2) 0.106(4) 0.095(3) 0.023(3) 0.022(2) -0.003(2) C38 0.114(4) 0.099(4) 0.093(3) -0.036(3) 0.033(3) 0.037(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 N1 1.9213(19) . ? Ni1 N2 1.9324(19) . ? Ni1 C3 1.945(2) . ? Ni1 C4 1.958(2) . ? O1 C11 1.212(4) . ? O2 C11 1.363(3) . ? O2 C12 1.446(4) . ? N1 C1 1.292(3) . ? N1 C15 1.443(3) . ? N2 C2 1.297(3) . ? N2 C27 1.436(3) . ? C1 C2 1.479(3) . ? C1 C13 1.496(3) . ? C2 C14 1.490(3) . ? C3 C4 1.442(3) . ? C3 C5 1.467(3) . ? C4 C11 1.452(4) . ? C5 C6 1.384(4) . ? C5 C10 1.397(3) . ? C6 C7 1.376(4) . ? C7 C8 1.388(5) . ? C8 C9 1.371(4) . ? C9 C10 1.379(4) . ? C15 C16 1.394(3) . ? C15 C20 1.399(3) . ? C16 C17 1.391(3) . ? C16 C21 1.520(3) . ? C17 C18 1.381(4) . ? C18 C19 1.379(4) . ? C19 C20 1.398(3) . ? C20 C24 1.517(4) . ? C21 C23 1.521(4) . ? C21 C22 1.526(4) . ? C24 C26 1.499(4) . ? C24 C25 1.509(5) . ? C27 C32 1.401(4) . ? C27 C28 1.407(4) . ? C28 C29 1.396(4) . ? C28 C33 1.512(4) . ? C29 C30 1.374(5) . ? C30 C31 1.370(5) . ? C31 C32 1.405(4) . ? C32 C36 1.511(4) . ? C33 C35 1.529(4) . ? C33 C34 1.532(4) . ? C36 C37 1.515(5) . ? C36 C38 1.538(5) . ? 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 81.02(8) . . ? N1 Ni1 C3 116.43(9) . . ? N2 Ni1 C3 162.50(9) . . ? N1 Ni1 C4 159.76(9) . . ? N2 Ni1 C4 119.15(9) . . ? C3 Ni1 C4 43.37(10) . . ? C11 O2 C12 116.5(3) . . ? C1 N1 C15 121.48(19) . . ? C1 N1 Ni1 116.29(15) . . ? C15 N1 Ni1 122.20(15) . . ? C2 N2 C27 121.7(2) . . ? C2 N2 Ni1 116.07(15) . . ? C27 N2 Ni1 122.21(15) . . ? N1 C1 C2 113.6(2) . . ? N1 C1 C13 126.3(2) . . ? C2 C1 C13 120.1(2) . . ? N2 C2 C1 113.0(2) . . ? N2 C2 C14 126.7(2) . . ? C1 C2 C14 120.4(2) . . ? C4 C3 C5 123.9(2) . . ? C4 C3 Ni1 68.83(14) . . ? C5 C3 Ni1 117.34(17) . . ? C3 C4 C11 120.0(2) . . ? C3 C4 Ni1 67.80(13) . . ? C11 C4 Ni1 111.09(18) . . ? C6 C5 C10 117.0(2) . . ? C6 C5 C3 123.2(2) . . ? C10 C5 C3 119.9(2) . . ? C7 C6 C5 121.7(3) . . ? C6 C7 C8 120.3(3) . . ? C9 C8 C7 119.1(3) . . ? C8 C9 C10 120.3(3) . . ? C9 C10 C5 121.6(3) . . ? O1 C11 O2 121.9(3) . . ? O1 C11 C4 127.4(3) . . ? O2 C11 C4 110.7(3) . . ? C16 C15 C20 122.8(2) . . ? C16 C15 N1 117.5(2) . . ? C20 C15 N1 119.5(2) . . ? C17 C16 C15 117.7(2) . . ? C17 C16 C21 121.5(2) . . ? C15 C16 C21 120.8(2) . . ? C18 C17 C16 121.1(2) . . ? C19 C18 C17 120.0(2) . . ? C18 C19 C20 121.5(2) . . ? C19 C20 C15 116.9(2) . . ? C19 C20 C24 121.3(2) . . ? C15 C20 C24 121.8(2) . . ? C16 C21 C23 112.9(2) . . ? C16 C21 C22 111.0(2) . . ? C23 C21 C22 111.8(3) . . ? C26 C24 C25 112.2(4) . . ? C26 C24 C20 113.4(3) . . ? C25 C24 C20 110.2(2) . . ? C32 C27 C28 122.9(2) . . ? C32 C27 N2 119.7(2) . . ? C28 C27 N2 117.2(2) . . ? C29 C28 C27 117.3(3) . . ? C29 C28 C33 122.5(3) . . ? C27 C28 C33 120.2(2) . . ? C30 C29 C28 120.8(3) . . ? C31 C30 C29 121.0(3) . . ? C30 C31 C32 121.3(3) . . ? C27 C32 C31 116.6(3) . . ? C27 C32 C36 123.1(2) . . ? C31 C32 C36 120.3(3) . . ? C28 C33 C35 114.4(2) . . ? C28 C33 C34 111.4(2) . . ? C35 C33 C34 108.9(2) . . ? C32 C36 C37 112.4(3) . . ? C32 C36 C38 111.1(3) . . ? C37 C36 C38 110.7(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.646 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.052 _vrf_C38H50N2NiO2_Compound15 ; PROBLEM:Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.66 Ratio Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.06 Ratio Check Low Ueq as Compared to Neighbors for C24 RESPONSE: This atoms is part of a disordered CH3 group. ;