Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_l085 _database_code_CSD 172561 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Jin, Guo-Xin' 'Hu, Ninghai' 'Zhang, Dao' _publ_contact_author_name 'Dr. Guo-Xin Jin' _publ_contact_author_address ; Professor of Chemistry Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022 ; _publ_contact_author_email 'gxjin@ciac.jl.cn' _publ_section_title ; Self-immobilized catalysts for ethylene polymerization: Neutral, single-component salicylaldiminato phenyl nickel(II) complexes bearing allyl substituents ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H42 N Ni O P' _chemical_formula_weight 738.51 _chemical_melting_point ? _chemical_compound_source ? 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' 'P' 'P' 0.1023 0.0942 '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 9.481(4) _cell_length_b 9.610(2) _cell_length_c 22.451(10) _cell_angle_alpha 101.01(3) _cell_angle_beta 100.84(3) _cell_angle_gamma 92.93(3) _cell_volume 1964.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 4.88 _cell_measurement_theta_max 9.81 _exptl_crystal_description ? _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method ? _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.5185 _exptl_absorpt_correction_T_max 0.5503 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4 diffractometer' _diffrn_measurement_method 'w\ scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8568 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.1261 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6927 _reflns_number_observed 3492 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6927 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1008 _refine_ls_R_factor_obs 0.0437 _refine_ls_wR_factor_all 0.0734 _refine_ls_wR_factor_obs 0.0665 _refine_ls_goodness_of_fit_all 0.847 _refine_ls_goodness_of_fit_obs 1.119 _refine_ls_restrained_S_all 0.847 _refine_ls_restrained_S_obs 1.119 _refine_ls_shift/esd_max -0.029 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni Ni 0.98491(5) 0.17811(5) 0.24488(2) 0.04076(14) Uani 1 d . . P P 0.87256(10) 0.06520(9) 0.30047(4) 0.0379(3) Uani 1 d . . O O 1.1289(2) 0.2557(2) 0.31655(9) 0.0436(6) Uani 1 d . . N N 1.0596(3) 0.2968(3) 0.19541(12) 0.0465(8) Uani 1 d . . C1 C 0.8632(5) 0.0587(4) 0.1756(2) 0.0578(12) Uani 1 d . . C2 C 0.7317(5) 0.0909(5) 0.1442(2) 0.085(2) Uani 1 d . . H2 H 0.6954(5) 0.1762(5) 0.1586(2) 0.085 Uiso 1 calc R . C3 C 0.6536(7) -0.0024(7) 0.0918(2) 0.131(3) Uani 1 d . . H3 H 0.5675(7) 0.0222(7) 0.0707(2) 0.131 Uiso 1 calc R . C4 C 0.7033(9) -0.1293(9) 0.0716(3) 0.165(5) Uani 1 d . . H4 H 0.6502(9) -0.1922(9) 0.0370(3) 0.165 Uiso 1 calc R . C5 C 0.8314(7) -0.1651(7) 0.1019(2) 0.132(3) Uani 1 d . . H5 H 0.8658(7) -0.2516(7) 0.0877(2) 0.132 Uiso 1 calc R . C6 C 0.9094(5) -0.0717(5) 0.1540(2) 0.0814(15) Uani 1 d . . H6 H 0.9952(5) -0.0977(5) 0.1749(2) 0.081 Uiso 1 calc R . C7 C 0.9851(4) 0.3032(4) 0.1335(2) 0.0502(10) Uani 1 d . . C8 C 0.8753(5) 0.3906(4) 0.1256(2) 0.0615(12) Uani 1 d . . C9 C 0.8068(5) 0.3947(4) 0.0658(2) 0.0709(13) Uani 1 d . . H9 H 0.7338(5) 0.4548(4) 0.0600(2) 0.071 Uiso 1 calc R . C10 C 0.8441(5) 0.3121(5) 0.0147(2) 0.0739(14) Uani 1 d . . C11 C 0.9542(5) 0.2300(4) 0.0244(2) 0.0721(14) Uani 1 d . . H11 H 0.9820(5) 0.1769(4) -0.0099(2) 0.072 Uiso 1 calc R . C12 C 1.0286(5) 0.2203(4) 0.0832(2) 0.0571(11) Uani 1 d . . C13 C 0.8321(5) 0.4815(4) 0.1810(2) 0.087(2) Uani 1 d . . H13A H 0.7437(13) 0.5215(19) 0.1677(2) 0.087 Uiso 1 calc R . H13B H 0.9066(11) 0.5569(14) 0.2000(6) 0.087 Uiso 1 calc R . H13C H 0.8186(23) 0.4239(6) 0.2103(5) 0.087 Uiso 1 calc R . C14 C 1.1520(4) 0.1289(4) 0.0912(2) 0.0775(14) Uani 1 d . . H14A H 1.1611(14) 0.0763(16) 0.0514(2) 0.078 Uiso 1 calc R . H14B H 1.1341(11) 0.0639(14) 0.1171(7) 0.078 Uiso 1 calc R . H14C H 1.2396(5) 0.1882(4) 0.1102(8) 0.078 Uiso 1 calc R . C15 C 0.7588(6) 0.3149(5) -0.0502(2) 0.113(2) Uani 1 d . . H15A H 0.8090(6) 0.2649(5) -0.0805(2) 0.113 Uiso 1 calc R . H15B H 0.6653(6) 0.2629(5) -0.0559(2) 0.113 Uiso 1 calc R . C16 C 0.7374(9) 0.4522(8) -0.0625(2) 0.142(3) Uani 1 d . . H16 H 0.8201(9) 0.5085(8) -0.0626(2) 0.142 Uiso 1 calc R . C17 C 0.6173(7) 0.5088(8) -0.0737(3) 0.144(3) Uani 1 d . . H17A H 0.5309(7) 0.4577(8) -0.0742(3) 0.144 Uiso 1 calc R . H17B H 0.6171(7) 0.6007(8) -0.0812(3) 0.144 Uiso 1 calc R . C18 C 1.1735(4) 0.3855(4) 0.21561(15) 0.0509(10) Uani 1 d . . H18 H 1.1948(4) 0.4413(4) 0.18829(15) 0.051 Uiso 1 calc R . C19 C 1.2696(4) 0.4093(3) 0.2735(2) 0.0461(10) Uani 1 d . . C20 C 1.3929(4) 0.5044(4) 0.2821(2) 0.0620(12) Uani 1 d . . H20 H 1.4083(4) 0.5473(4) 0.2498(2) 0.062 Uiso 1 calc R . C21 C 1.4896(4) 0.5350(4) 0.3366(2) 0.0703(13) Uani 1 d . . H21 H 1.5685(4) 0.6013(4) 0.3425(2) 0.070 Uiso 1 calc R . C22 C 1.4688(4) 0.4655(4) 0.3834(2) 0.0547(10) Uani 1 d . . H22 H 1.5371(4) 0.4845(4) 0.4202(2) 0.055 Uiso 1 calc R . C23 C 1.3506(4) 0.3688(3) 0.3780(2) 0.0422(9) Uani 1 d . . C24 C 1.2440(4) 0.3415(3) 0.32275(15) 0.0383(9) Uani 1 d . . C25 C 1.3482(4) 0.2930(3) 0.42985(15) 0.0403(9) Uani 1 d . . C26 C 1.4753(4) 0.2417(4) 0.4559(2) 0.0561(11) Uani 1 d . . H26 H 1.5566(4) 0.2497(4) 0.4387(2) 0.056 Uiso 1 calc R . C27 C 1.4826(4) 0.1791(4) 0.5067(2) 0.0652(12) Uani 1 d . . H27 H 1.5688(4) 0.1463(4) 0.5236(2) 0.065 Uiso 1 calc R . C28 C 1.3632(4) 0.1647(4) 0.5327(2) 0.0560(11) Uani 1 d . . H28 H 1.3681(4) 0.1235(4) 0.5672(2) 0.056 Uiso 1 calc R . C29 C 1.2372(4) 0.2124(4) 0.5064(2) 0.0540(10) Uani 1 d . . H29 H 1.1556(4) 0.2026(4) 0.5231(2) 0.054 Uiso 1 calc R . C30 C 1.2294(4) 0.2750(3) 0.4554(2) 0.0462(10) Uani 1 d . . H30 H 1.1423(4) 0.3053(3) 0.4381(2) 0.046 Uiso 1 calc R . C31 C 0.6834(4) 0.0009(4) 0.27142(14) 0.0414(9) Uani 1 d . . C32 C 0.5758(4) 0.0802(4) 0.2854(2) 0.0673(12) Uani 1 d . . H32 H 0.5994(4) 0.1671(4) 0.3131(2) 0.067 Uiso 1 calc R . C33 C 0.4334(5) 0.0373(5) 0.2603(2) 0.093(2) Uani 1 d . . H33 H 0.3629(5) 0.0962(5) 0.2704(2) 0.093 Uiso 1 calc R . C34 C 0.3946(5) -0.0904(5) 0.2209(2) 0.0846(15) Uani 1 d . . H34 H 0.2979(5) -0.1204(5) 0.2045(2) 0.085 Uiso 1 calc R . C35 C 0.4987(5) -0.1732(4) 0.2060(2) 0.0658(12) Uani 1 d . . H35 H 0.4735(5) -0.2608(4) 0.1790(2) 0.066 Uiso 1 calc R . C36 C 0.6427(4) -0.1288(4) 0.23058(14) 0.0532(11) Uani 1 d . . H36 H 0.7131(4) -0.1868(4) 0.21954(14) 0.053 Uiso 1 calc R . C37 C 0.8661(3) 0.1740(3) 0.37497(14) 0.0370(8) Uani 1 d . . C38 C 0.8548(3) 0.3191(3) 0.37962(15) 0.0429(9) Uani 1 d . . H38 H 0.8544(3) 0.3590(3) 0.34497(15) 0.043 Uiso 1 calc R . C39 C 0.8443(4) 0.4041(4) 0.4348(2) 0.0509(10) Uani 1 d . . H39 H 0.8354(4) 0.5009(4) 0.4374(2) 0.051 Uiso 1 calc R . C40 C 0.8469(4) 0.3451(4) 0.4866(2) 0.0515(10) Uani 1 d . . H40 H 0.8407(4) 0.4029(4) 0.5241(2) 0.052 Uiso 1 calc R . C41 C 0.8586(4) 0.2019(4) 0.48301(15) 0.0484(10) Uani 1 d . . H41 H 0.8594(4) 0.1625(4) 0.51782(15) 0.048 Uiso 1 calc R . C42 C 0.8689(4) 0.1183(3) 0.42804(14) 0.0440(9) Uani 1 d . . H42 H 0.8779(4) 0.0216(3) 0.42585(14) 0.044 Uiso 1 calc R . C43 C 0.9649(4) -0.0869(4) 0.32011(14) 0.0455(9) Uani 1 d . . C44 C 0.8958(5) -0.2064(4) 0.33125(15) 0.0665(12) Uani 1 d . . H44 H 0.7964(5) -0.2140(4) 0.32820(15) 0.067 Uiso 1 calc R . C45 C 0.9770(7) -0.3154(5) 0.3471(2) 0.095(2) Uani 1 d . . H45 H 0.9313(7) -0.3965(5) 0.3545(2) 0.095 Uiso 1 calc R . C46 C 1.1224(7) -0.3045(6) 0.3518(2) 0.105(2) Uani 1 d . . H46 H 1.1754(7) -0.3781(6) 0.3623(2) 0.105 Uiso 1 calc R . C47 C 1.1903(6) -0.1864(6) 0.3414(2) 0.100(2) Uani 1 d . . H47 H 1.2898(6) -0.1788(6) 0.3448(2) 0.100 Uiso 1 calc R . C48 C 1.1117(5) -0.0790(4) 0.3258(2) 0.0703(13) Uani 1 d . . H48 H 1.1591(5) 0.0017(4) 0.3188(2) 0.070 Uiso 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 Ni 0.0478(3) 0.0394(3) 0.0344(3) 0.0067(2) 0.0103(2) -0.0058(2) P 0.0443(6) 0.0333(5) 0.0358(5) 0.0044(4) 0.0119(5) -0.0031(5) O 0.040(2) 0.0485(15) 0.0406(14) 0.0112(11) 0.0068(12) -0.0107(13) N 0.066(2) 0.041(2) 0.032(2) 0.0063(14) 0.013(2) -0.008(2) C1 0.071(3) 0.063(3) 0.038(2) 0.005(2) 0.019(2) -0.025(3) C2 0.082(4) 0.104(4) 0.063(3) 0.036(3) -0.009(3) -0.040(3) C3 0.127(6) 0.188(7) 0.056(4) 0.038(4) -0.026(4) -0.078(6) C4 0.209(10) 0.192(9) 0.059(4) -0.019(5) 0.032(5) -0.139(9) C5 0.194(7) 0.106(5) 0.082(4) -0.045(4) 0.085(4) -0.089(6) C6 0.103(4) 0.071(3) 0.067(3) -0.012(3) 0.048(3) -0.035(3) C7 0.064(3) 0.050(2) 0.033(2) 0.007(2) 0.008(2) -0.015(2) C8 0.082(3) 0.067(3) 0.036(2) 0.018(2) 0.008(2) 0.003(3) C9 0.095(4) 0.064(3) 0.048(3) 0.011(2) 0.000(3) 0.012(3) C10 0.099(4) 0.081(3) 0.036(2) 0.012(2) 0.004(3) -0.010(3) C11 0.105(4) 0.069(3) 0.040(3) 0.000(2) 0.026(3) -0.015(3) C12 0.078(3) 0.050(2) 0.043(2) 0.006(2) 0.020(2) -0.018(2) C13 0.123(4) 0.085(3) 0.053(3) 0.011(2) 0.013(3) 0.041(3) C14 0.100(4) 0.070(3) 0.067(3) 0.005(2) 0.040(3) -0.007(3) C15 0.174(6) 0.114(4) 0.040(3) 0.017(3) 0.000(3) -0.020(4) C16 0.214(9) 0.148(7) 0.044(3) 0.022(4) -0.010(5) -0.066(7) C17 0.178(8) 0.147(6) 0.090(5) 0.014(4) -0.006(5) 0.002(6) C18 0.074(3) 0.042(2) 0.040(2) 0.014(2) 0.020(2) -0.011(2) C19 0.051(3) 0.043(2) 0.043(2) 0.008(2) 0.012(2) -0.008(2) C20 0.068(3) 0.058(3) 0.066(3) 0.025(2) 0.021(2) -0.015(2) C21 0.056(3) 0.068(3) 0.082(3) 0.022(2) 0.004(3) -0.030(2) C22 0.041(2) 0.058(3) 0.059(2) 0.014(2) -0.003(2) -0.007(2) C23 0.036(2) 0.041(2) 0.049(2) 0.006(2) 0.011(2) 0.002(2) C24 0.040(2) 0.030(2) 0.044(2) 0.002(2) 0.010(2) 0.001(2) C25 0.036(2) 0.034(2) 0.047(2) 0.003(2) 0.005(2) 0.004(2) C26 0.033(2) 0.070(3) 0.066(3) 0.018(2) 0.009(2) 0.004(2) C27 0.044(3) 0.079(3) 0.078(3) 0.037(2) 0.004(2) 0.016(2) C28 0.053(3) 0.060(3) 0.055(2) 0.020(2) 0.003(2) 0.003(2) C29 0.043(3) 0.068(3) 0.055(2) 0.018(2) 0.014(2) 0.004(2) C30 0.035(2) 0.054(2) 0.050(2) 0.010(2) 0.008(2) 0.009(2) C31 0.040(2) 0.043(2) 0.041(2) 0.003(2) 0.013(2) -0.003(2) C32 0.047(3) 0.064(3) 0.082(3) -0.009(2) 0.018(3) -0.010(2) C33 0.052(3) 0.088(4) 0.118(4) -0.035(3) 0.022(3) 0.002(3) C34 0.045(3) 0.098(4) 0.096(4) -0.006(3) 0.010(3) -0.017(3) C35 0.066(3) 0.066(3) 0.054(3) -0.002(2) 0.008(3) -0.028(3) C36 0.056(3) 0.055(3) 0.048(2) 0.003(2) 0.017(2) -0.001(2) C37 0.034(2) 0.036(2) 0.040(2) 0.004(2) 0.008(2) -0.002(2) C38 0.046(2) 0.038(2) 0.044(2) 0.003(2) 0.015(2) -0.004(2) C39 0.050(3) 0.039(2) 0.056(2) -0.007(2) 0.009(2) -0.003(2) C40 0.044(2) 0.062(3) 0.041(2) -0.012(2) 0.014(2) -0.001(2) C41 0.054(3) 0.054(3) 0.037(2) 0.004(2) 0.014(2) 0.001(2) C42 0.055(3) 0.038(2) 0.039(2) 0.006(2) 0.013(2) -0.004(2) C43 0.061(3) 0.041(2) 0.040(2) 0.013(2) 0.018(2) 0.009(2) C44 0.107(4) 0.042(2) 0.053(2) 0.013(2) 0.020(3) -0.001(3) C45 0.187(6) 0.045(3) 0.056(3) 0.015(2) 0.032(4) 0.012(4) C46 0.208(7) 0.075(4) 0.053(3) 0.029(3) 0.041(5) 0.083(5) C47 0.109(5) 0.119(4) 0.102(4) 0.053(4) 0.045(3) 0.073(4) C48 0.075(3) 0.073(3) 0.082(3) 0.037(3) 0.036(3) 0.032(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 Ni C1 1.891(4) . ? Ni O 1.903(2) . ? Ni N 1.932(3) . ? Ni P 2.1838(12) . ? P C37 1.809(3) . ? P C43 1.824(3) . ? P C31 1.821(3) . ? O C24 1.302(3) . ? N C18 1.293(4) . ? N C7 1.451(4) . ? C1 C2 1.392(5) . ? C1 C6 1.379(5) . ? C2 C3 1.391(6) . ? C2 H2 0.93 . ? C3 C4 1.358(9) . ? C3 H3 0.93 . ? C4 C5 1.370(9) . ? C4 H4 0.93 . ? C5 C6 1.388(6) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C8 1.378(5) . ? C7 C12 1.393(5) . ? C8 C9 1.385(4) . ? C8 C13 1.514(5) . ? C9 C10 1.381(5) . ? C9 H9 0.93 . ? C10 C11 1.351(5) . ? C10 C15 1.533(5) . ? C11 C12 1.398(5) . ? C11 H11 0.93 . ? C12 C14 1.502(5) . ? C13 H13A 0.96 . ? C13 H13B 0.96 . ? C13 H13C 0.96 . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C14 H14C 0.96 . ? C15 C16 1.417(7) . ? C15 H15A 0.97 . ? C15 H15B 0.97 . ? C16 C17 1.289(8) . ? C16 H16 0.93 . ? C17 H17A 0.93 . ? C17 H17B 0.93 . ? C18 C19 1.411(4) . ? C18 H18 0.93 . ? C19 C20 1.406(4) . ? C19 C24 1.438(4) . ? C20 C21 1.356(4) . ? C20 H20 0.93 . ? C21 C22 1.386(4) . ? C21 H21 0.93 . ? C22 C23 1.390(4) . ? C22 H22 0.93 . ? C23 C24 1.416(4) . ? C23 C25 1.490(4) . ? C25 C30 1.374(4) . ? C25 C26 1.394(4) . ? C26 C27 1.380(4) . ? C26 H26 0.93 . ? C27 C28 1.380(5) . ? C27 H27 0.93 . ? C28 C29 1.372(4) . ? C28 H28 0.93 . ? C29 C30 1.384(4) . ? C29 H29 0.93 . ? C30 H30 0.93 . ? C31 C32 1.352(4) . ? C31 C36 1.387(4) . ? C32 C33 1.370(5) . ? C32 H32 0.93 . ? C33 C34 1.357(5) . ? C33 H33 0.93 . ? C34 C35 1.350(5) . ? C34 H34 0.93 . ? C35 C36 1.384(5) . ? C35 H35 0.93 . ? C36 H36 0.93 . ? C37 C38 1.389(4) . ? C37 C42 1.393(4) . ? C38 C39 1.371(4) . ? C38 H38 0.93 . ? C39 C40 1.384(4) . ? C39 H39 0.93 . ? C40 C41 1.375(4) . ? C40 H40 0.93 . ? C41 C42 1.361(4) . ? C41 H41 0.93 . ? C42 H42 0.93 . ? C43 C44 1.380(4) . ? C43 C48 1.371(5) . ? C44 C45 1.392(5) . ? C44 H44 0.93 . ? C45 C46 1.359(7) . ? C45 H45 0.93 . ? C46 C47 1.357(6) . ? C46 H46 0.93 . ? C47 C48 1.364(5) . ? C47 H47 0.93 . ? C48 H48 0.93 . ? 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 C1 Ni O 165.7(2) . . ? C1 Ni N 93.56(13) . . ? O Ni N 93.08(11) . . ? C1 Ni P 85.61(11) . . ? O Ni P 89.75(7) . . ? N Ni P 171.01(10) . . ? C37 P C43 103.79(15) . . ? C37 P C31 101.4(2) . . ? C43 P C31 106.3(2) . . ? C37 P Ni 112.61(11) . . ? C43 P Ni 112.05(12) . . ? C31 P Ni 119.14(11) . . ? C24 O Ni 129.9(2) . . ? C18 N C7 113.5(3) . . ? C18 N Ni 123.7(2) . . ? C7 N Ni 122.6(2) . . ? C2 C1 C6 117.2(4) . . ? C2 C1 Ni 125.9(4) . . ? C6 C1 Ni 116.9(4) . . ? C1 C2 C3 121.2(5) . . ? C1 C2 H2 119.4(3) . . ? C3 C2 H2 119.4(4) . . ? C4 C3 C2 119.9(7) . . ? C4 C3 H3 120.0(5) . . ? C2 C3 H3 120.0(4) . . ? C5 C4 C3 120.3(7) . . ? C5 C4 H4 119.9(5) . . ? C3 C4 H4 119.9(5) . . ? C4 C5 C6 119.7(7) . . ? C4 C5 H5 120.2(5) . . ? C6 C5 H5 120.2(4) . . ? C5 C6 C1 121.7(5) . . ? C5 C6 H6 119.2(4) . . ? C1 C6 H6 119.2(3) . . ? C8 C7 C12 121.9(4) . . ? C8 C7 N 119.9(3) . . ? C12 C7 N 118.3(4) . . ? C7 C8 C9 118.5(4) . . ? C7 C8 C13 120.7(3) . . ? C9 C8 C13 120.8(4) . . ? C10 C9 C8 121.7(4) . . ? C10 C9 H9 119.1(3) . . ? C8 C9 H9 119.1(3) . . ? C11 C10 C9 117.9(4) . . ? C11 C10 C15 122.7(4) . . ? C9 C10 C15 119.4(5) . . ? C10 C11 C12 123.7(4) . . ? C10 C11 H11 118.2(3) . . ? C12 C11 H11 118.2(3) . . ? C7 C12 C11 116.3(4) . . ? C7 C12 C14 122.3(4) . . ? C11 C12 C14 121.3(4) . . ? C8 C13 H13A 109.5(2) . . ? C8 C13 H13B 109.5(2) . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5(2) . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5(2) . . ? C12 C14 H14B 109.5(2) . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5(2) . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C10 115.3(4) . . ? C16 C15 H15A 108.4(4) . . ? C10 C15 H15A 108.4(3) . . ? C16 C15 H15B 108.4(4) . . ? C10 C15 H15B 108.4(3) . . ? H15A C15 H15B 107.5 . . ? C17 C16 C15 128.0(9) . . ? C17 C16 H16 116.0(6) . . ? C15 C16 H16 116.0(4) . . ? C16 C17 H17A 120.0(6) . . ? C16 C17 H17B 120.0(6) . . ? H17A C17 H17B 120.0 . . ? N C18 C19 128.8(3) . . ? N C18 H18 115.6(2) . . ? C19 C18 H18 115.6(2) . . ? C20 C19 C18 117.5(3) . . ? C20 C19 C24 120.3(3) . . ? C18 C19 C24 122.2(3) . . ? C21 C20 C19 121.3(3) . . ? C21 C20 H20 119.4(2) . . ? C19 C20 H20 119.4(2) . . ? C20 C21 C22 118.8(3) . . ? C20 C21 H21 120.6(2) . . ? C22 C21 H21 120.6(2) . . ? C23 C22 C21 123.2(4) . . ? C23 C22 H22 118.4(2) . . ? C21 C22 H22 118.4(2) . . ? C22 C23 C24 119.0(3) . . ? C22 C23 C25 117.3(3) . . ? C24 C23 C25 123.6(3) . . ? O C24 C23 121.1(3) . . ? O C24 C19 121.5(3) . . ? C23 C24 C19 117.4(3) . . ? C30 C25 C26 117.6(3) . . ? C30 C25 C23 124.0(3) . . ? C26 C25 C23 118.4(3) . . ? C27 C26 C25 121.1(4) . . ? C27 C26 H26 119.4(2) . . ? C25 C26 H26 119.4(2) . . ? C28 C27 C26 120.6(4) . . ? C28 C27 H27 119.7(2) . . ? C26 C27 H27 119.7(2) . . ? C29 C28 C27 118.4(3) . . ? C29 C28 H28 120.8(2) . . ? C27 C28 H28 120.8(2) . . ? C28 C29 C30 121.2(4) . . ? C28 C29 H29 119.4(2) . . ? C30 C29 H29 119.4(2) . . ? C25 C30 C29 121.1(3) . . ? C25 C30 H30 119.5(2) . . ? C29 C30 H30 119.5(2) . . ? C32 C31 C36 116.6(3) . . ? C32 C31 P 122.0(3) . . ? C36 C31 P 121.3(3) . . ? C31 C32 C33 122.5(4) . . ? C31 C32 H32 118.7(2) . . ? C33 C32 H32 118.7(3) . . ? C34 C33 C32 120.5(4) . . ? C34 C33 H33 119.8(3) . . ? C32 C33 H33 119.8(3) . . ? C35 C34 C33 118.9(4) . . ? C35 C34 H34 120.6(3) . . ? C33 C34 H34 120.6(3) . . ? C34 C35 C36 120.7(4) . . ? C34 C35 H35 119.7(3) . . ? C36 C35 H35 119.7(3) . . ? C35 C36 C31 120.9(4) . . ? C35 C36 H36 119.5(3) . . ? C31 C36 H36 119.5(2) . . ? C38 C37 C42 118.1(3) . . ? C38 C37 P 119.0(2) . . ? C42 C37 P 122.9(2) . . ? C39 C38 C37 120.6(3) . . ? C39 C38 H38 119.7(2) . . ? C37 C38 H38 119.7(2) . . ? C38 C39 C40 119.7(3) . . ? C38 C39 H39 120.1(2) . . ? C40 C39 H39 120.1(2) . . ? C41 C40 C39 120.5(3) . . ? C41 C40 H40 119.7(2) . . ? C39 C40 H40 119.7(2) . . ? C40 C41 C42 119.4(3) . . ? C40 C41 H41 120.3(2) . . ? C42 C41 H41 120.3(2) . . ? C41 C42 C37 121.6(3) . . ? C41 C42 H42 119.2(2) . . ? C37 C42 H42 119.2(2) . . ? C44 C43 C48 118.6(4) . . ? C44 C43 P 123.7(3) . . ? C48 C43 P 117.6(3) . . ? C43 C44 C45 119.1(4) . . ? C43 C44 H44 120.5(3) . . ? C45 C44 H44 120.5(3) . . ? C46 C45 C44 120.7(5) . . ? C46 C45 H45 119.7(4) . . ? C44 C45 H45 119.7(3) . . ? C47 C46 C45 120.2(6) . . ? C47 C46 H46 119.9(4) . . ? C45 C46 H46 119.9(4) . . ? C46 C47 C48 119.6(5) . . ? C46 C47 H47 120.2(4) . . ? C48 C47 H47 120.2(3) . . ? C47 C48 C43 121.8(4) . . ? C47 C48 H48 119.1(3) . . ? C43 C48 H48 119.1(2) . . ? _refine_diff_density_max 0.227 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.046