# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _database_code_CSD 183730 _journal_coden_Cambridge 440 loop_ _publ_author_name _publ_author_address 'Zilong Li' ; the Center of Molecular Sciences Institute of Chemistry Chinese Academy of Sciences Beijing 100080 P. R. China ; 'Wen-Hua Sun' ; the Center of Molecular Sciences Institute of Chemistry Chinese Academy of Sciences Beijing 100080 P. R. China ; 'Huaiming Hu' ; the Center of Molecular Sciences Institute of Chemistry Chinese Academy of Sciences Beijing 100080 P. R. China ; 'Biao Wu' ; the Center of Molecular Sciences Institute of Chemistry Chinese Academy of Sciences Beijing 100080 P. R. China ; 'Haijian Yang' ; the Center of Molecular Sciences Institute of Chemistry Chinese Academy of Sciences Beijing 100080 P. R. China ; 'Ning Zhu' ; the Center of Molecular Sciences Institute of Chemistry Chinese Academy of Sciences Beijing 100080 P. R. China ; 'Youliang Hu' ; the Center of Molecular Sciences Institute of Chemistry Chinese Academy of Sciences Beijing 100080 P. R. China ; 'Xuebing Leng' ; State of Key Laboratory of Functional Polmer Department of Chemistry Nankai University Tianjing 300071 P. R. China ; 'Honggen Wang' ; State of Key Laboratory of Functional Polmer Department of Chemistry Nankai University Tianjing 300071 P. R. China ; _publ_contact_author_name 'Prof Wen-Hua Sun' _publ_contact_author_address ; Prof Wen-Hua Sun Chinese Academy of Sciences Institute of Chemistry Zhongguancun Beiyijie 2# Beijing 100080 CHINA ; _publ_contact_author_email 'WHSUN@INFOC3.ICAS.AC.CN' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Synthesis, characterization and their ethylene oligomerization of novel nickel(II) complexes bearing N, P ligands ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[2-Methyl-8-(diphenylphosphino)quinoline]nickel(II) dichloride' _chemical_melting_point 240 _chemical_formula_moiety ? _chemical_formula_sum 'C23 H20 Cl4 N Ni P' _chemical_formula_weight 541.88 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9073(7) _cell_length_b 11.0443(3) _cell_length_c 11.5761(5) _cell_angle_alpha 95.605(4) _cell_angle_beta 103.724(6) _cell_angle_gamma 114.101(6) _cell_volume 1206.46(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5387 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'Block' _exptl_crystal_colour 'Light green' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 1.324 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.6843 _exptl_absorpt_correction_T_max 0.8261 _exptl_absorpt_process_details 'PSI scans' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method 'Oscillation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8314 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -13 _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 2.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5387 _reflns_number_gt 4221 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO (Rigaku, 2001)' _computing_cell_refinement 'RAPID AUTO (Rigaku, 2001)' _computing_data_reduction 'RAPID AUTO (Rigaku, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXTL (Siemens, 1994)' _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^)+(0.0920P)^2^+1.0914P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.013(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5387 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1604 _refine_ls_wR_factor_gt 0.1497 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni -0.58680(5) -0.42991(4) -0.92174(4) 0.03112(17) Uani 1 1 d . . . P1 P -0.41537(10) -0.23702(9) -0.78482(8) 0.0307(2) Uani 1 1 d . . . Cl1 Cl -0.46148(10) -0.57014(9) -0.89145(8) 0.0384(2) Uani 1 1 d . . . Cl2 Cl -0.73287(11) -0.53881(12) -0.81599(10) 0.0524(3) Uani 1 1 d . . . N1 N -0.6875(3) -0.3077(3) -0.9671(3) 0.0340(6) Uani 1 1 d . . . C1 C -0.4043(4) -0.2379(4) -0.6271(3) 0.0365(8) Uani 1 1 d . . . C2 C -0.4295(7) -0.1533(6) -0.5525(4) 0.0643(14) Uani 1 1 d . . . H2A H -0.4536 -0.0885 -0.5829 0.077 Uiso 1 1 calc R . . C3 C -0.4199(8) -0.1619(7) -0.4327(5) 0.0790(18) Uani 1 1 d . . . H3A H -0.4366 -0.1025 -0.3832 0.095 Uiso 1 1 calc R . . C4 C -0.3866(6) -0.2560(6) -0.3871(4) 0.0606(12) Uani 1 1 d . . . H4A H -0.3832 -0.2636 -0.3073 0.073 Uiso 1 1 calc R . . C5 C -0.3579(7) -0.3401(5) -0.4589(4) 0.0674(14) Uani 1 1 d . . . H5A H -0.3321 -0.4033 -0.4270 0.081 Uiso 1 1 calc R . . C6 C -0.3670(7) -0.3316(5) -0.5786(4) 0.0648(14) Uani 1 1 d . . . H6A H -0.3478 -0.3897 -0.6270 0.078 Uiso 1 1 calc R . . C7 C -0.2334(4) -0.1582(4) -0.7848(3) 0.0373(8) Uani 1 1 d . . . C8 C -0.1999(4) -0.1970(4) -0.8859(4) 0.0423(8) Uani 1 1 d . . . H8A H -0.2701 -0.2655 -0.9507 0.051 Uiso 1 1 calc R . . C9 C -0.0638(5) -0.1351(5) -0.8916(5) 0.0575(11) Uani 1 1 d . . . H9A H -0.0427 -0.1616 -0.9602 0.069 Uiso 1 1 calc R . . C10 C 0.0401(5) -0.0349(6) -0.7963(6) 0.0701(14) Uani 1 1 d . . . H10A H 0.1318 0.0071 -0.8003 0.084 Uiso 1 1 calc R . . C11 C 0.0092(5) 0.0036(6) -0.6954(5) 0.0754(16) Uani 1 1 d . . . H11A H 0.0804 0.0718 -0.6310 0.091 Uiso 1 1 calc R . . C12 C -0.1265(5) -0.0575(5) -0.6879(4) 0.0574(12) Uani 1 1 d . . . H12A H -0.1462 -0.0315 -0.6183 0.069 Uiso 1 1 calc R . . C13 C -0.4830(4) -0.1167(3) -0.8265(3) 0.0321(7) Uani 1 1 d . . . C14 C -0.4102(4) 0.0211(4) -0.7808(3) 0.0400(8) Uani 1 1 d . . . H14A H -0.3212 0.0567 -0.7240 0.048 Uiso 1 1 calc R . . C15 C -0.4667(5) 0.1098(4) -0.8174(4) 0.0454(9) Uani 1 1 d . . . H15A H -0.4151 0.2029 -0.7852 0.054 Uiso 1 1 calc R . . C16 C -0.5957(5) 0.0601(4) -0.8992(4) 0.0447(9) Uani 1 1 d . . . H16A H -0.6335 0.1191 -0.9218 0.054 Uiso 1 1 calc R . . C17 C -0.6746(4) -0.0809(4) -0.9513(3) 0.0386(8) Uani 1 1 d . . . C18 C -0.8064(4) -0.1362(5) -1.0404(4) 0.0461(9) Uani 1 1 d . . . H18A H -0.8468 -0.0801 -1.0664 0.055 Uiso 1 1 calc R . . C19 C -0.8745(4) -0.2712(5) -1.0883(4) 0.0508(10) Uani 1 1 d . . . H19A H -0.9627 -0.3082 -1.1467 0.061 Uiso 1 1 calc R . . C20 C -0.8128(4) -0.3567(4) -1.0505(4) 0.0424(8) Uani 1 1 d . . . C21 C -0.6168(4) -0.1706(4) -0.9159(3) 0.0333(7) Uani 1 1 d . . . C22 C -0.8886(5) -0.5061(5) -1.1070(4) 0.0556(11) Uani 1 1 d . . . H22A H -0.8339 -0.5499 -1.0707 0.083 Uiso 1 1 calc R . . H22B H -0.9014 -0.5196 -1.1930 0.083 Uiso 1 1 calc R . . H22C H -0.9789 -0.5445 -1.0933 0.083 Uiso 1 1 calc R . . C23 C -0.1896(15) 0.3779(14) -0.4297(11) 0.170(5) Uani 1 1 d . . . Cl3 Cl -0.2039(5) 0.4149(5) -0.5771(4) 0.1358(14) Uani 0.70 1 d P A 1 Cl4 Cl -0.1781(9) 0.2310(8) -0.4203(8) 0.190(3) Uani 0.70 1 d P A 1 Cl3' Cl -0.164(3) 0.340(2) -0.564(3) 0.38(2) Uani 0.30 1 d P A 2 Cl4' Cl -0.145(4) 0.243(3) -0.391(5) 0.68(6) Uani 0.30 1 d P A 2 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 0.0361(3) 0.0288(2) 0.0280(2) 0.00456(16) 0.00830(18) 0.01517(19) P1 0.0351(4) 0.0304(4) 0.0259(4) 0.0046(3) 0.0081(3) 0.0149(4) Cl1 0.0552(5) 0.0382(5) 0.0312(4) 0.0103(3) 0.0138(4) 0.0287(4) Cl2 0.0459(5) 0.0647(7) 0.0492(6) 0.0250(5) 0.0207(5) 0.0212(5) N1 0.0353(15) 0.0370(15) 0.0334(15) 0.0084(12) 0.0115(12) 0.0191(13) C1 0.0409(18) 0.0336(18) 0.0266(16) 0.0051(13) 0.0048(14) 0.0119(15) C2 0.099(4) 0.083(4) 0.044(2) 0.027(2) 0.037(3) 0.061(3) C3 0.122(5) 0.110(5) 0.047(3) 0.029(3) 0.047(3) 0.078(4) C4 0.068(3) 0.072(3) 0.033(2) 0.017(2) 0.016(2) 0.022(3) C5 0.102(4) 0.063(3) 0.038(2) 0.020(2) 0.009(2) 0.041(3) C6 0.109(4) 0.060(3) 0.041(2) 0.015(2) 0.019(3) 0.054(3) C7 0.0359(18) 0.0374(19) 0.0365(18) 0.0076(15) 0.0087(15) 0.0158(15) C8 0.046(2) 0.0385(19) 0.047(2) 0.0089(16) 0.0176(18) 0.0211(17) C9 0.052(2) 0.062(3) 0.070(3) 0.017(2) 0.032(2) 0.029(2) C10 0.041(2) 0.078(4) 0.086(4) 0.017(3) 0.025(3) 0.018(2) C11 0.037(2) 0.081(4) 0.071(3) -0.004(3) 0.007(2) 0.001(2) C12 0.042(2) 0.066(3) 0.045(2) -0.001(2) 0.0079(19) 0.011(2) C13 0.0432(18) 0.0320(16) 0.0289(16) 0.0097(13) 0.0170(14) 0.0202(15) C14 0.052(2) 0.0341(18) 0.0337(18) 0.0054(14) 0.0148(16) 0.0186(16) C15 0.071(3) 0.0325(18) 0.040(2) 0.0101(15) 0.026(2) 0.0242(19) C16 0.069(3) 0.040(2) 0.049(2) 0.0210(17) 0.034(2) 0.035(2) C17 0.049(2) 0.044(2) 0.0395(19) 0.0173(16) 0.0239(17) 0.0293(17) C18 0.047(2) 0.059(3) 0.053(2) 0.025(2) 0.0228(19) 0.036(2) C19 0.038(2) 0.066(3) 0.056(3) 0.021(2) 0.0113(19) 0.030(2) C20 0.0367(18) 0.050(2) 0.041(2) 0.0113(17) 0.0108(16) 0.0202(17) C21 0.0398(18) 0.0370(18) 0.0337(17) 0.0124(14) 0.0200(15) 0.0215(15) C22 0.043(2) 0.050(2) 0.055(3) 0.000(2) -0.0020(19) 0.0142(19) C23 0.200(13) 0.169(11) 0.109(8) -0.032(8) -0.002(8) 0.092(10) Cl3 0.115(3) 0.150(4) 0.099(2) 0.015(2) 0.0070(19) 0.035(3) Cl4 0.219(7) 0.146(6) 0.184(5) 0.008(4) -0.007(5) 0.104(5) Cl3' 0.31(3) 0.19(2) 0.35(3) -0.04(2) -0.09(3) -0.028(19) Cl4' 0.56(5) 0.123(13) 0.83(8) -0.16(3) -0.56(6) 0.14(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.093(3) . ? Ni1 Cl2 2.2653(10) . ? Ni1 P1 2.2865(10) . ? Ni1 Cl1 2.3439(9) 2_443 ? Ni1 Cl1 2.4490(10) . ? P1 C1 1.802(4) . ? P1 C7 1.813(4) . ? P1 C13 1.817(4) . ? Cl1 Ni1 2.3439(9) 2_443 ? N1 C20 1.327(5) . ? N1 C21 1.376(5) . ? C1 C2 1.364(6) . ? C1 C6 1.378(6) . ? C2 C3 1.382(6) . ? C2 H2A 0.9300 . ? C3 C4 1.347(8) . ? C3 H3A 0.9300 . ? C4 C5 1.364(8) . ? C4 H4A 0.9300 . ? C5 C6 1.381(6) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.385(5) . ? C7 C12 1.390(6) . ? C8 C9 1.380(6) . ? C8 H8A 0.9300 . ? C9 C10 1.367(8) . ? C9 H9A 0.9300 . ? C10 C11 1.366(8) . ? C10 H10A 0.9300 . ? C11 C12 1.382(7) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.372(5) . ? C13 C21 1.417(5) . ? C14 C15 1.403(6) . ? C14 H14A 0.9300 . ? C15 C16 1.347(6) . ? C15 H15A 0.9300 . ? C16 C17 1.416(6) . ? C16 H16A 0.9300 . ? C17 C18 1.400(6) . ? C17 C21 1.419(5) . ? C18 C19 1.350(7) . ? C18 H18A 0.9300 . ? C19 C20 1.413(6) . ? C19 H19A 0.9300 . ? C20 C22 1.501(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 Cl4 1.689(15) . ? C23 Cl3' 1.69(4) . ? C23 Cl3 1.779(15) . ? C23 Cl4' 1.82(3) . ? Cl3' Cl4' 2.38(6) . ? 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 Cl2 93.37(9) . . ? N1 Ni1 P1 84.48(9) . . ? Cl2 Ni1 P1 104.64(4) . . ? N1 Ni1 Cl1 89.37(8) . 2_443 ? Cl2 Ni1 Cl1 146.99(4) . 2_443 ? P1 Ni1 Cl1 108.37(4) . 2_443 ? N1 Ni1 Cl1 173.11(8) . . ? Cl2 Ni1 Cl1 92.69(4) . . ? P1 Ni1 Cl1 97.15(4) . . ? Cl1 Ni1 Cl1 83.76(3) 2_443 . ? C1 P1 C7 104.51(18) . . ? C1 P1 C13 106.98(16) . . ? C7 P1 C13 105.03(17) . . ? C1 P1 Ni1 115.39(12) . . ? C7 P1 Ni1 123.60(12) . . ? C13 P1 Ni1 99.71(12) . . ? Ni1 Cl1 Ni1 96.24(3) 2_443 . ? C20 N1 C21 119.1(3) . . ? C20 N1 Ni1 121.9(3) . . ? C21 N1 Ni1 118.8(2) . . ? C2 C1 C6 117.8(4) . . ? C2 C1 P1 125.1(3) . . ? C6 C1 P1 117.1(3) . . ? C1 C2 C3 121.3(5) . . ? C1 C2 H2A 119.3 . . ? C3 C2 H2A 119.3 . . ? C4 C3 C2 120.3(5) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C4 C5 C6 120.2(5) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C1 C6 C5 120.7(5) . . ? C1 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C8 C7 C12 118.7(4) . . ? C8 C7 P1 119.0(3) . . ? C12 C7 P1 122.2(3) . . ? C9 C8 C7 120.8(4) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C10 C9 C8 119.9(4) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C11 C10 C9 120.0(4) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 120.9(5) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C11 C12 C7 119.6(4) . . ? C11 C12 H12A 120.2 . . ? C7 C12 H12A 120.2 . . ? C14 C13 C21 119.2(3) . . ? C14 C13 P1 124.1(3) . . ? C21 C13 P1 116.6(3) . . ? C13 C14 C15 121.7(4) . . ? C13 C14 H14A 119.1 . . ? C15 C14 H14A 119.1 . . ? C16 C15 C14 119.9(4) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C17 120.8(4) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C18 C17 C16 122.7(4) . . ? C18 C17 C21 117.9(4) . . ? C16 C17 C21 119.4(4) . . ? C19 C18 C17 119.7(4) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? C18 C19 C20 120.4(4) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? N1 C20 C19 121.5(4) . . ? N1 C20 C22 118.8(4) . . ? C19 C20 C22 119.7(4) . . ? N1 C21 C13 119.8(3) . . ? N1 C21 C17 121.3(3) . . ? C13 C21 C17 118.8(3) . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Cl4 C23 Cl3' 78.9(12) . . ? Cl4 C23 Cl3 113.8(7) . . ? Cl3' C23 Cl3 36.5(11) . . ? Cl4 C23 Cl4' 12.4(9) . . ? Cl3' C23 Cl4' 85(2) . . ? Cl3 C23 Cl4' 122(2) . . ? C23 Cl3' Cl4' 49.6(15) . . ? C23 Cl4' Cl3' 45.2(13) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.913 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.101 data_1 _database_code_CSD 183920 _journal_coden_Cambridge 440 loop_ _publ_author_name _publ_author_address 'Zilong Li' ; the Center of Molecular Sciences Institute of Chemistry Chinese Academy of Sciences Beijing 100080 P. R. China ; 'Wen-Hua Sun' ; the Center of Molecular Sciences Institute of Chemistry Chinese Academy of Sciences Beijing 100080 P. R. China ; 'Huaiming Hu' ; the Center of Molecular Sciences Institute of Chemistry Chinese Academy of Sciences Beijing 100080 P. R. China ; 'Biao Wu' ; the Center of Molecular Sciences Institute of Chemistry Chinese Academy of Sciences Beijing 100080 P. R. China ; 'Haijian Yang' ; the Center of Molecular Sciences Institute of Chemistry Chinese Academy of Sciences Beijing 100080 P. R. China ; 'Ning Zhu' ; the Center of Molecular Sciences Institute of Chemistry Chinese Academy of Sciences Beijing 100080 P. R. China ; 'Youliang Hu' ; the Center of Molecular Sciences Institute of Chemistry Chinese Academy of Sciences Beijing 100080 P. R. China ; 'Xuebing Leng' ; State of Key Laboratory of Functional Polmer Department of Chemistry Nankai University Tianjing 300071 P. R. China ; 'Honggen Wang' ; State of Key Laboratory of Functional Polmer Department of Chemistry Nankai University Tianjing 300071 P. R. China ; _publ_contact_author_name 'Prof Wen-Hua Sun' _publ_contact_author_address ; Prof Wen-Hua Sun Chinese Academy of Sciences Institute of Chemistry Zhongguancun Beiyijie 2# Beijing 100080 CHINA ; _publ_contact_author_email 'WHSUN@INFOC3.ICAS.AC.CN' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Synthesis, characterization and their ethylene oligomerization of novel nickel(II) complexes bearing N, P ligands ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'chloro(1-naphthyl)[8-(diphenylphosphino)quinoline]nickel(II)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H24.50 Cl N Ni O6 P' _chemical_formula_weight 608.13 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.606(5) _cell_length_b 9.184(2) _cell_length_c 34.005(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.381(5) _cell_angle_gamma 90.00 _cell_volume 5774(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2508 _exptl_absorpt_coefficient_mu 0.862 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8465 _exptl_absorpt_correction_T_max 0.9188 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 11609 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_sigmaI/netI 0.1173 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5052 _reflns_number_gt 2443 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5052 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1303 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1305 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.149 _refine_ls_shift/su_mean 0.004 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 0.22993(3) 1.01015(7) 0.142368(18) 0.0360(2) Uani 1 1 d . . . Cl1 Cl 0.33937(6) 1.02510(15) 0.17493(4) 0.0503(4) Uani 1 1 d . . . P1 P 0.13069(7) 1.01120(15) 0.10589(4) 0.0372(3) Uani 1 1 d . . . N1 N 0.1832(2) 1.1390(4) 0.18001(12) 0.0395(11) Uani 1 1 d . . . C31 C 0.2646(2) 0.8786(5) 0.10556(16) 0.0381(13) Uani 1 1 d . . . C1 C 0.0757(3) 1.1283(5) 0.13356(15) 0.0386(13) Uani 1 1 d . . . C2 C 0.0060(3) 1.1716(6) 0.12156(18) 0.0529(16) Uani 1 1 d . . . H2A H -0.0177 1.1372 0.0979 0.063 Uiso 1 1 calc R . . C3 C -0.0296(3) 1.2683(6) 0.1452(2) 0.0628(17) Uani 1 1 d . . . H3A H -0.0771 1.2961 0.1372 0.075 Uiso 1 1 calc R . . C4 C 0.0048(3) 1.3214(6) 0.17967(19) 0.0569(16) Uani 1 1 d . . . H4A H -0.0192 1.3861 0.1947 0.068 Uiso 1 1 calc R . . C5 C 0.0763(3) 1.2800(6) 0.19295(17) 0.0498(15) Uani 1 1 d . . . C6 C 0.1148(4) 1.3271(7) 0.22888(18) 0.0638(17) Uani 1 1 d . . . H6A H 0.0937 1.3916 0.2453 0.077 Uiso 1 1 calc R . . C7 C 0.1827(3) 1.2773(7) 0.23913(17) 0.0624(18) Uani 1 1 d . . . H7A H 0.2075 1.3046 0.2633 0.075 Uiso 1 1 calc R . . C8 C 0.2156(3) 1.1862(6) 0.21416(16) 0.0498(15) Uani 1 1 d . . . H8A H 0.2629 1.1566 0.2218 0.060 Uiso 1 1 calc R . . C9 C 0.1115(3) 1.1834(5) 0.16924(16) 0.0400(13) Uani 1 1 d . . . C10 C 0.0807(3) 0.8456(5) 0.09519(15) 0.0416(13) Uani 1 1 d . . . C11 C 0.0238(3) 0.8057(7) 0.11594(17) 0.0597(17) Uani 1 1 d . . . H11A H 0.0085 0.8687 0.1347 0.072 Uiso 1 1 calc R . . C12 C -0.0111(4) 0.6703(8) 0.1089(2) 0.078(2) Uani 1 1 d . . . H12A H -0.0490 0.6438 0.1231 0.093 Uiso 1 1 calc R . . C13 C 0.0112(4) 0.5776(7) 0.0808(2) 0.084(2) Uani 1 1 d . . . H13A H -0.0119 0.4887 0.0757 0.101 Uiso 1 1 calc R . . C14 C 0.0683(4) 0.6174(7) 0.0600(2) 0.075(2) Uani 1 1 d . . . H14A H 0.0833 0.5548 0.0411 0.090 Uiso 1 1 calc R . . C15 C 0.1030(3) 0.7490(6) 0.06730(17) 0.0567(16) Uani 1 1 d . . . H15A H 0.1417 0.7735 0.0535 0.068 Uiso 1 1 calc R . . C16 C 0.1311(3) 1.1096(5) 0.05959(15) 0.0360(13) Uani 1 1 d . . . C17 C 0.0855(3) 1.0792(6) 0.02571(17) 0.0517(15) Uani 1 1 d . . . H17A H 0.0543 0.9998 0.0251 0.062 Uiso 1 1 calc R . . C18 C 0.0862(3) 1.1673(7) -0.00751(17) 0.0640(17) Uani 1 1 d . . . H18A H 0.0553 1.1461 -0.0302 0.077 Uiso 1 1 calc R . . C19 C 0.1317(3) 1.2849(6) -0.00746(18) 0.0595(17) Uani 1 1 d . . . H19A H 0.1320 1.3433 -0.0298 0.071 Uiso 1 1 calc R . . C20 C 0.1760(3) 1.3139(6) 0.0257(2) 0.0610(17) Uani 1 1 d . . . H20A H 0.2070 1.3933 0.0261 0.073 Uiso 1 1 calc R . . C21 C 0.1765(3) 1.2291(6) 0.05912(17) 0.0494(15) Uani 1 1 d . . . H21A H 0.2076 1.2522 0.0816 0.059 Uiso 1 1 calc R . . C22 C 0.2886(3) 0.9210(6) 0.07084(17) 0.0511(15) Uani 1 1 d . . . H22A H 0.2849 1.0187 0.0636 0.061 Uiso 1 1 calc R . . C23 C 0.3190(3) 0.8220(8) 0.04539(18) 0.0699(19) Uani 1 1 d . . . H23A H 0.3328 0.8546 0.0215 0.084 Uiso 1 1 calc R . . C24 C 0.3282(3) 0.6779(7) 0.05580(19) 0.0659(18) Uani 1 1 d . . . H24A H 0.3492 0.6133 0.0394 0.079 Uiso 1 1 calc R . . C25 C 0.3055(3) 0.6297(6) 0.09170(18) 0.0475(15) Uani 1 1 d . . . C26 C 0.3158(3) 0.4831(7) 0.1038(2) 0.0667(17) Uani 1 1 d . . . H26A H 0.3381 0.4183 0.0880 0.080 Uiso 1 1 calc R . . C27 C 0.2933(4) 0.4367(7) 0.1382(3) 0.083(2) Uani 1 1 d . . . H27A H 0.3009 0.3403 0.1459 0.100 Uiso 1 1 calc R . . C28 C 0.2591(4) 0.5313(7) 0.1623(2) 0.077(2) Uani 1 1 d . . . H28A H 0.2439 0.4981 0.1859 0.092 Uiso 1 1 calc R . . C29 C 0.2481(3) 0.6722(6) 0.15103(17) 0.0546(16) Uani 1 1 d . . . H29A H 0.2244 0.7341 0.1670 0.065 Uiso 1 1 calc R . . C30 C 0.2716(3) 0.7276(6) 0.11569(15) 0.0396(13) Uani 1 1 d . . . O1 O 0.4031(7) 0.298(2) 0.2715(5) 0.240(9) Uani 0.50 1 d P . . O2 O 0.505(2) 0.306(6) 0.2673(6) 0.39(4) Uani 0.25 1 d P . . 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 0.0301(4) 0.0402(4) 0.0374(4) 0.0017(3) 0.0029(3) 0.0086(3) Cl1 0.0331(7) 0.0575(10) 0.0582(9) -0.0046(7) -0.0050(6) 0.0107(7) P1 0.0331(7) 0.0427(9) 0.0354(8) -0.0023(7) 0.0017(6) 0.0072(7) N1 0.040(3) 0.044(3) 0.035(3) 0.001(2) 0.005(2) 0.010(2) C31 0.024(3) 0.045(4) 0.045(4) 0.003(3) 0.001(3) 0.004(2) C1 0.028(3) 0.042(3) 0.046(4) 0.002(3) 0.005(3) 0.008(2) C2 0.032(3) 0.060(4) 0.067(4) -0.007(3) 0.011(3) 0.010(3) C3 0.032(4) 0.075(5) 0.083(5) 0.006(4) 0.013(4) 0.019(3) C4 0.048(4) 0.059(4) 0.066(5) -0.011(3) 0.016(3) 0.017(3) C5 0.045(4) 0.055(4) 0.052(4) -0.007(3) 0.018(3) 0.009(3) C6 0.070(5) 0.074(5) 0.050(4) -0.020(3) 0.018(4) 0.009(4) C7 0.064(5) 0.086(5) 0.036(4) -0.014(3) 0.000(3) 0.009(4) C8 0.048(4) 0.066(4) 0.034(4) -0.012(3) -0.003(3) 0.010(3) C9 0.029(3) 0.047(4) 0.044(4) -0.001(3) 0.007(3) 0.007(3) C10 0.040(3) 0.041(3) 0.042(4) 0.003(3) 0.000(3) 0.010(3) C11 0.066(4) 0.064(5) 0.049(4) 0.010(3) 0.006(3) 0.001(4) C12 0.075(5) 0.076(5) 0.081(6) 0.030(4) 0.003(4) -0.025(4) C13 0.105(6) 0.045(4) 0.096(6) 0.002(4) -0.019(5) -0.010(4) C14 0.081(5) 0.055(5) 0.089(6) -0.005(4) 0.010(4) 0.010(4) C15 0.054(4) 0.042(4) 0.074(5) -0.003(3) 0.008(3) 0.004(3) C16 0.033(3) 0.035(3) 0.040(3) -0.003(2) 0.006(3) 0.000(2) C17 0.047(4) 0.059(4) 0.048(4) 0.013(3) 0.000(3) -0.014(3) C18 0.067(4) 0.083(5) 0.039(4) 0.011(3) -0.007(3) -0.012(4) C19 0.066(4) 0.061(4) 0.053(4) 0.017(3) 0.010(4) 0.000(3) C20 0.057(4) 0.047(4) 0.078(5) 0.011(4) 0.004(4) -0.009(3) C21 0.051(4) 0.044(4) 0.049(4) 0.003(3) -0.011(3) -0.001(3) C22 0.056(4) 0.041(4) 0.060(4) 0.009(3) 0.022(3) 0.016(3) C23 0.071(5) 0.095(6) 0.049(4) 0.009(4) 0.031(4) 0.020(4) C24 0.063(4) 0.066(5) 0.070(5) -0.017(4) 0.009(4) 0.018(3) C25 0.044(3) 0.035(4) 0.061(4) -0.006(3) -0.006(3) 0.009(3) C26 0.067(4) 0.039(4) 0.090(5) -0.019(4) -0.007(4) 0.007(3) C27 0.116(6) 0.032(4) 0.097(6) 0.007(4) -0.010(5) -0.010(4) C28 0.112(6) 0.049(5) 0.070(5) 0.014(4) 0.017(4) -0.001(4) C29 0.066(4) 0.037(4) 0.061(4) 0.003(3) 0.010(3) 0.002(3) C30 0.031(3) 0.041(4) 0.046(4) 0.001(3) -0.001(3) 0.001(2) O1 0.109(11) 0.39(2) 0.213(16) -0.209(16) -0.018(10) -0.030(12) O2 0.33(4) 0.81(9) 0.038(17) 0.05(3) -0.01(2) 0.41(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C31 1.903(5) . ? Ni1 N1 2.010(4) . ? Ni1 P1 2.1071(15) . ? Ni1 Cl1 2.2113(15) . ? P1 C10 1.798(5) . ? P1 C16 1.816(5) . ? P1 C1 1.817(5) . ? N1 C8 1.320(6) . ? N1 C9 1.404(6) . ? C31 C22 1.365(6) . ? C31 C30 1.431(6) . ? C1 C2 1.374(6) . ? C1 C9 1.411(7) . ? C2 C3 1.412(7) . ? C3 C4 1.362(7) . ? C4 C5 1.408(7) . ? C5 C9 1.409(6) . ? C5 C6 1.414(7) . ? C6 C7 1.352(7) . ? C7 C8 1.383(7) . ? C10 C11 1.385(7) . ? C10 C15 1.395(7) . ? C11 C12 1.411(8) . ? C12 C13 1.378(9) . ? C13 C14 1.386(8) . ? C14 C15 1.380(7) . ? C16 C17 1.381(7) . ? C16 C21 1.385(6) . ? C17 C18 1.391(7) . ? C18 C19 1.372(7) . ? C19 C20 1.348(7) . ? C20 C21 1.376(7) . ? C22 C23 1.416(7) . ? C23 C24 1.376(7) . ? C24 C25 1.407(7) . ? C25 C30 1.409(6) . ? C25 C26 1.415(7) . ? C26 C27 1.354(8) . ? C27 C28 1.396(8) . ? C28 C29 1.358(7) . ? C29 C30 1.419(6) . ? O2 O2 1.17(4) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C31 Ni1 N1 174.01(19) . . ? C31 Ni1 P1 87.38(14) . . ? N1 Ni1 P1 87.69(13) . . ? C31 Ni1 Cl1 90.49(14) . . ? N1 Ni1 Cl1 94.81(13) . . ? P1 Ni1 Cl1 172.97(6) . . ? C10 P1 C16 107.3(2) . . ? C10 P1 C1 107.3(2) . . ? C16 P1 C1 102.2(2) . . ? C10 P1 Ni1 120.97(17) . . ? C16 P1 Ni1 115.13(17) . . ? C1 P1 Ni1 101.80(17) . . ? C8 N1 C9 117.4(4) . . ? C8 N1 Ni1 124.5(4) . . ? C9 N1 Ni1 118.0(3) . . ? C22 C31 C30 117.0(5) . . ? C22 C31 Ni1 123.7(4) . . ? C30 C31 Ni1 119.0(4) . . ? C2 C1 C9 119.4(5) . . ? C2 C1 P1 125.8(4) . . ? C9 C1 P1 114.7(4) . . ? C1 C2 C3 120.0(6) . . ? C4 C3 C2 120.6(5) . . ? C3 C4 C5 121.1(5) . . ? C4 C5 C9 118.0(5) . . ? C4 C5 C6 124.4(5) . . ? C9 C5 C6 117.6(5) . . ? C7 C6 C5 119.3(6) . . ? C6 C7 C8 120.7(6) . . ? N1 C8 C7 123.3(5) . . ? N1 C9 C5 121.5(5) . . ? N1 C9 C1 117.7(4) . . ? C5 C9 C1 120.8(5) . . ? C11 C10 C15 118.7(5) . . ? C11 C10 P1 121.9(4) . . ? C15 C10 P1 119.3(4) . . ? C10 C11 C12 120.7(6) . . ? C13 C12 C11 119.6(6) . . ? C12 C13 C14 119.8(7) . . ? C15 C14 C13 120.7(6) . . ? C14 C15 C10 120.6(6) . . ? C17 C16 C21 118.0(5) . . ? C17 C16 P1 124.1(4) . . ? C21 C16 P1 117.7(4) . . ? C16 C17 C18 119.9(5) . . ? C19 C18 C17 121.3(6) . . ? C20 C19 C18 118.4(6) . . ? C19 C20 C21 121.8(6) . . ? C20 C21 C16 120.6(5) . . ? C31 C22 C23 122.5(5) . . ? C24 C23 C22 120.5(5) . . ? C23 C24 C25 119.0(5) . . ? C24 C25 C30 119.9(5) . . ? C24 C25 C26 120.5(6) . . ? C30 C25 C26 119.6(6) . . ? C27 C26 C25 120.4(6) . . ? C26 C27 C28 121.1(6) . . ? C29 C28 C27 119.4(6) . . ? C28 C29 C30 122.0(5) . . ? C25 C30 C29 117.5(5) . . ? C25 C30 C31 120.9(5) . . ? C29 C30 C31 121.5(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C31 Ni1 P1 C10 59.0(3) . . . . ? N1 Ni1 P1 C10 -117.6(2) . . . . ? Cl1 Ni1 P1 C10 131.4(5) . . . . ? C31 Ni1 P1 C16 -72.7(2) . . . . ? N1 Ni1 P1 C16 110.7(2) . . . . ? Cl1 Ni1 P1 C16 -0.2(6) . . . . ? C31 Ni1 P1 C1 177.7(2) . . . . ? N1 Ni1 P1 C1 1.1(2) . . . . ? Cl1 Ni1 P1 C1 -109.9(5) . . . . ? C31 Ni1 N1 C8 143.6(18) . . . . ? P1 Ni1 N1 C8 178.2(4) . . . . ? Cl1 Ni1 N1 C8 -8.4(4) . . . . ? C31 Ni1 N1 C9 -37(2) . . . . ? P1 Ni1 N1 C9 -2.5(3) . . . . ? Cl1 Ni1 N1 C9 171.0(3) . . . . ? N1 Ni1 C31 C22 115.2(18) . . . . ? P1 Ni1 C31 C22 80.7(4) . . . . ? Cl1 Ni1 C31 C22 -92.6(4) . . . . ? N1 Ni1 C31 C30 -70(2) . . . . ? P1 Ni1 C31 C30 -104.6(4) . . . . ? Cl1 Ni1 C31 C30 82.1(4) . . . . ? C10 P1 C1 C2 -55.5(5) . . . . ? C16 P1 C1 C2 57.2(5) . . . . ? Ni1 P1 C1 C2 176.5(4) . . . . ? C10 P1 C1 C9 128.2(4) . . . . ? C16 P1 C1 C9 -119.1(4) . . . . ? Ni1 P1 C1 C9 0.2(4) . . . . ? C9 C1 C2 C3 -1.1(8) . . . . ? P1 C1 C2 C3 -177.2(4) . . . . ? C1 C2 C3 C4 1.0(9) . . . . ? C2 C3 C4 C5 -0.9(9) . . . . ? C3 C4 C5 C9 0.8(8) . . . . ? C3 C4 C5 C6 -178.1(6) . . . . ? C4 C5 C6 C7 178.3(6) . . . . ? C9 C5 C6 C7 -0.6(8) . . . . ? C5 C6 C7 C8 2.7(9) . . . . ? C9 N1 C8 C7 -0.8(8) . . . . ? Ni1 N1 C8 C7 178.6(4) . . . . ? C6 C7 C8 N1 -2.1(9) . . . . ? C8 N1 C9 C5 2.9(7) . . . . ? Ni1 N1 C9 C5 -176.5(4) . . . . ? C8 N1 C9 C1 -177.4(5) . . . . ? Ni1 N1 C9 C1 3.2(6) . . . . ? C4 C5 C9 N1 178.8(5) . . . . ? C6 C5 C9 N1 -2.2(8) . . . . ? C4 C5 C9 C1 -0.9(8) . . . . ? C6 C5 C9 C1 178.1(5) . . . . ? C2 C1 C9 N1 -178.6(4) . . . . ? P1 C1 C9 N1 -2.1(6) . . . . ? C2 C1 C9 C5 1.1(8) . . . . ? P1 C1 C9 C5 177.6(4) . . . . ? C16 P1 C10 C11 -127.5(4) . . . . ? C1 P1 C10 C11 -18.3(5) . . . . ? Ni1 P1 C10 C11 97.6(4) . . . . ? C16 P1 C10 C15 57.4(5) . . . . ? C1 P1 C10 C15 166.6(4) . . . . ? Ni1 P1 C10 C15 -77.5(5) . . . . ? C15 C10 C11 C12 -0.3(8) . . . . ? P1 C10 C11 C12 -175.5(4) . . . . ? C10 C11 C12 C13 -0.6(9) . . . . ? C11 C12 C13 C14 0.7(10) . . . . ? C12 C13 C14 C15 0.1(11) . . . . ? C13 C14 C15 C10 -1.0(10) . . . . ? C11 C10 C15 C14 1.1(8) . . . . ? P1 C10 C15 C14 176.4(5) . . . . ? C10 P1 C16 C17 15.3(5) . . . . ? C1 P1 C16 C17 -97.4(5) . . . . ? Ni1 P1 C16 C17 153.2(4) . . . . ? C10 P1 C16 C21 -169.5(4) . . . . ? C1 P1 C16 C21 77.8(4) . . . . ? Ni1 P1 C16 C21 -31.6(4) . . . . ? C21 C16 C17 C18 0.1(8) . . . . ? P1 C16 C17 C18 175.3(4) . . . . ? C16 C17 C18 C19 0.1(9) . . . . ? C17 C18 C19 C20 -0.1(9) . . . . ? C18 C19 C20 C21 0.0(9) . . . . ? C19 C20 C21 C16 0.2(9) . . . . ? C17 C16 C21 C20 -0.3(8) . . . . ? P1 C16 C21 C20 -175.8(4) . . . . ? C30 C31 C22 C23 0.4(8) . . . . ? Ni1 C31 C22 C23 175.3(4) . . . . ? C31 C22 C23 C24 -2.8(9) . . . . ? C22 C23 C24 C25 1.5(9) . . . . ? C23 C24 C25 C30 2.1(9) . . . . ? C23 C24 C25 C26 -178.4(5) . . . . ? C24 C25 C26 C27 -179.5(6) . . . . ? C30 C25 C26 C27 0.0(9) . . . . ? C25 C26 C27 C28 0.6(10) . . . . ? C26 C27 C28 C29 0.0(10) . . . . ? C27 C28 C29 C30 -1.2(9) . . . . ? C24 C25 C30 C29 178.4(5) . . . . ? C26 C25 C30 C29 -1.2(7) . . . . ? C24 C25 C30 C31 -4.5(8) . . . . ? C26 C25 C30 C31 176.0(5) . . . . ? C28 C29 C30 C25 1.8(8) . . . . ? C28 C29 C30 C31 -175.3(5) . . . . ? C22 C31 C30 C25 3.2(7) . . . . ? Ni1 C31 C30 C25 -171.9(4) . . . . ? C22 C31 C30 C29 -179.8(5) . . . . ? Ni1 C31 C30 C29 5.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.467 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.076