# 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 _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Reau, Regis' 'Bernardo-Gusmao, Katia' 'De Sousa, R. F.' 'Leca, Francois' 'Sauthier, Mathieu' 'Toupet, L.' 'Trevisan Queiroz, L. F.' _publ_contact_author_name 'Dr Regis Reau' _publ_contact_author_address ; Organometalliques et Catalyse, Chimie et \electrochimie Moleculaires Institut de Chimie, UMR 6509 CNRS-Universite de Rennes Campus de Beaulieu 35042 Rennes Cedex FRANCE ; _publ_contact_author_email 'REGIS.REAU@UNIV-RENNES1.FR' _publ_section_title ;; NiCl2(a-diiminophosphorane) complexes: a new family of readily accessible and tunable catalysts for oligomerisation of ethylene. ; data_flx _database_code_CSD 166395 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H36 Cl4 N2 Ni P2' _chemical_formula_weight 843.19 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.9254(2) _cell_length_b 15.1776(2) _cell_length_c 18.1566(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.4895(6) _cell_angle_gamma 90.00 _cell_volume 4109.16(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 0.843 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9244 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.59 _reflns_number_total 9244 _reflns_number_gt 7943 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0450P)^2^+4.3293P] 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 SHELXL _refine_ls_extinction_coef 0.0012(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9244 _refine_ls_number_parameters 494 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0992 _refine_ls_wR_factor_gt 0.0920 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Cl3 Cl 0.58169(9) 0.54864(6) 0.63771(5) 0.0801(3) Uani 1 1 d . . . Cl4 Cl 0.54063(5) 0.39282(5) 0.54875(4) 0.05008(18) Uani 1 1 d . . . C43 C 0.5687(2) 0.4330(2) 0.63712(19) 0.0580(8) Uani 1 1 d . . . H43A H 0.6242 0.4058 0.6552 0.070 Uiso 1 1 calc R . . H43B H 0.5221 0.4168 0.6702 0.070 Uiso 1 1 calc R . . C44 C 0.5333(6) 0.0863(6) 0.4815(5) 0.057(2) Uiso 0.50 1 d P . . C45 C 0.6053(4) 0.0038(3) 0.5485(3) 0.0310(11) Uiso 0.50 1 d P . . C46 C 0.5299(3) -0.0562(3) 0.5699(3) 0.0333(10) Uiso 0.50 1 d P . . C47 C 0.5547(5) -0.0061(5) 0.5365(4) 0.0335(17) Uiso 0.50 1 d P . . C49 C 0.5719(5) 0.0120(5) 0.5337(4) 0.0299(15) Uiso 0.50 1 d P . . C51 C 0.5216(4) 0.0694(4) 0.4954(3) 0.0308(13) Uiso 0.50 1 d P . . Ni1 Ni 0.500984(15) 0.312410(15) 0.834477(12) 0.01516(8) Uani 1 1 d . . . Cl1 Cl 0.44751(3) 0.25089(3) 0.93845(2) 0.02085(11) Uani 1 1 d . . . Cl2 Cl 0.59974(4) 0.42076(4) 0.82622(4) 0.03525(14) Uani 1 1 d . . . P1 P 0.31444(3) 0.38925(3) 0.76677(3) 0.01566(10) Uani 1 1 d . . . P2 P 0.62539(3) 0.15201(3) 0.78478(3) 0.01560(11) Uani 1 1 d . . . N1 N 0.39351(10) 0.31654(10) 0.76354(9) 0.0161(3) Uani 1 1 d . . . N2 N 0.53203(10) 0.20526(10) 0.77717(8) 0.0160(3) Uani 1 1 d . . . C1 C 0.38397(12) 0.23564(12) 0.72536(10) 0.0149(3) Uani 1 1 d . . . C2 C 0.45812(12) 0.17683(12) 0.73197(10) 0.0154(3) Uani 1 1 d . . . C3 C 0.45414(13) 0.09719(13) 0.69342(10) 0.0192(4) Uani 1 1 d . . . H3 H 0.5025 0.0586 0.6974 0.023 Uiso 1 1 calc R . . C4 C 0.37895(13) 0.07452(13) 0.64910(11) 0.0208(4) Uani 1 1 d . . . H4 H 0.3775 0.0214 0.6235 0.025 Uiso 1 1 calc R . . C5 C 0.30657(13) 0.13128(13) 0.64339(10) 0.0197(4) Uani 1 1 d . . . H5 H 0.2562 0.1163 0.6141 0.024 Uiso 1 1 calc R . . C6 C 0.30907(13) 0.21063(13) 0.68125(10) 0.0188(4) Uani 1 1 d . . . H6 H 0.2598 0.2481 0.6772 0.023 Uiso 1 1 calc R . . C7 C 0.35423(13) 0.47235(13) 0.83052(11) 0.0200(4) Uani 1 1 d . . . C8 C 0.39763(14) 0.54706(14) 0.80430(13) 0.0263(4) Uani 1 1 d . . . H8 H 0.4028 0.5554 0.7539 0.032 Uiso 1 1 calc R . . C9 C 0.43297(15) 0.60871(16) 0.85431(15) 0.0347(5) Uani 1 1 d . . . H9 H 0.4609 0.6590 0.8371 0.042 Uiso 1 1 calc R . . C10 C 0.42696(16) 0.59586(16) 0.92941(15) 0.0378(6) Uani 1 1 d . . . H10 H 0.4520 0.6368 0.9624 0.045 Uiso 1 1 calc R . . C11 C 0.38380(18) 0.52233(16) 0.95542(13) 0.0360(6) Uani 1 1 d . . . H11 H 0.3793 0.5141 1.0059 0.043 Uiso 1 1 calc R . . C12 C 0.34702(16) 0.46057(14) 0.90610(12) 0.0280(5) Uani 1 1 d . . . H12 H 0.3176 0.4113 0.9237 0.034 Uiso 1 1 calc R . . C13 C 0.21114(13) 0.34079(13) 0.79701(10) 0.0191(4) Uani 1 1 d . . . C14 C 0.21871(14) 0.27314(14) 0.84920(11) 0.0237(4) Uani 1 1 d . . . H14 H 0.2749 0.2569 0.8689 0.028 Uiso 1 1 calc R . . C15 C 0.14221(15) 0.23009(15) 0.87174(13) 0.0296(5) Uani 1 1 d . . . H15 H 0.1474 0.1849 0.9062 0.036 Uiso 1 1 calc R . . C16 C 0.05854(15) 0.25449(16) 0.84294(14) 0.0335(5) Uani 1 1 d . . . H16 H 0.0075 0.2260 0.8585 0.040 Uiso 1 1 calc R . . C17 C 0.05044(15) 0.32083(16) 0.79119(15) 0.0336(5) Uani 1 1 d . . . H17 H -0.0060 0.3367 0.7720 0.040 Uiso 1 1 calc R . . C18 C 0.12633(14) 0.36422(15) 0.76748(12) 0.0257(4) Uani 1 1 d . . . H18 H 0.1206 0.4085 0.7322 0.031 Uiso 1 1 calc R . . C19 C 0.28739(13) 0.44440(13) 0.68038(10) 0.0187(4) Uani 1 1 d . . . C20 C 0.22887(14) 0.51661(14) 0.67730(12) 0.0245(4) Uani 1 1 d . . . H20 H 0.2058 0.5387 0.7203 0.029 Uiso 1 1 calc R . . C21 C 0.20531(15) 0.55511(15) 0.60985(14) 0.0310(5) Uani 1 1 d . . . H21 H 0.1652 0.6020 0.6077 0.037 Uiso 1 1 calc R . . C22 C 0.24130(17) 0.52406(17) 0.54574(13) 0.0348(5) Uani 1 1 d . . . H22 H 0.2251 0.5499 0.5007 0.042 Uiso 1 1 calc R . . C23 C 0.30143(17) 0.45458(16) 0.54878(12) 0.0322(5) Uani 1 1 d . . . H23 H 0.3266 0.4347 0.5059 0.039 Uiso 1 1 calc R . . C24 C 0.32431(14) 0.41443(14) 0.61599(11) 0.0242(4) Uani 1 1 d . . . H24 H 0.3644 0.3675 0.6178 0.029 Uiso 1 1 calc R . . C25 C 0.60974(13) 0.04063(13) 0.81873(10) 0.0198(4) Uani 1 1 d . . . C26 C 0.66607(14) -0.03052(14) 0.80443(12) 0.0249(4) Uani 1 1 d . . . H26 H 0.7120 -0.0241 0.7718 0.030 Uiso 1 1 calc R . . C27 C 0.65307(16) -0.11070(14) 0.83918(13) 0.0303(5) Uani 1 1 d . . . H27 H 0.6910 -0.1577 0.8301 0.036 Uiso 1 1 calc R . . C28 C 0.58444(17) -0.12161(15) 0.88721(12) 0.0310(5) Uani 1 1 d . . . H28 H 0.5768 -0.1754 0.9106 0.037 Uiso 1 1 calc R . . C29 C 0.52698(16) -0.05175(15) 0.90042(13) 0.0306(5) Uani 1 1 d . . . H29 H 0.4800 -0.0591 0.9319 0.037 Uiso 1 1 calc R . . C30 C 0.53992(14) 0.02906(14) 0.86658(12) 0.0253(4) Uani 1 1 d . . . H30 H 0.5018 0.0758 0.8759 0.030 Uiso 1 1 calc R . . C31 C 0.69645(12) 0.20665(13) 0.85311(11) 0.0188(4) Uani 1 1 d . . . C32 C 0.76734(15) 0.25950(16) 0.83251(13) 0.0305(5) Uani 1 1 d . . . H32 H 0.7797 0.2657 0.7830 0.037 Uiso 1 1 calc R . . C33 C 0.81954(17) 0.30298(18) 0.88626(15) 0.0398(6) Uani 1 1 d . . . H33 H 0.8673 0.3378 0.8726 0.048 Uiso 1 1 calc R . . C34 C 0.80106(16) 0.29484(18) 0.95972(14) 0.0369(5) Uani 1 1 d . . . H34 H 0.8367 0.3238 0.9954 0.044 Uiso 1 1 calc R . . C35 C 0.72974(16) 0.24377(16) 0.98035(12) 0.0325(5) Uani 1 1 d . . . H35 H 0.7166 0.2395 1.0298 0.039 Uiso 1 1 calc R . . C36 C 0.67772(15) 0.19883(14) 0.92742(12) 0.0257(4) Uani 1 1 d . . . H36 H 0.6304 0.1636 0.9415 0.031 Uiso 1 1 calc R . . C37 C 0.68440(13) 0.15331(13) 0.69993(10) 0.0191(4) Uani 1 1 d . . . C38 C 0.64699(14) 0.20227(14) 0.64132(11) 0.0244(4) Uani 1 1 d . . . H38 H 0.5907 0.2277 0.6451 0.029 Uiso 1 1 calc R . . C39 C 0.69355(16) 0.21321(16) 0.57741(12) 0.0314(5) Uani 1 1 d . . . H39 H 0.6682 0.2457 0.5384 0.038 Uiso 1 1 calc R . . C40 C 0.77778(16) 0.17582(15) 0.57154(12) 0.0311(5) Uani 1 1 d . . . H40 H 0.8091 0.1836 0.5288 0.037 Uiso 1 1 calc R . . C41 C 0.81497(15) 0.12700(15) 0.62927(14) 0.0313(5) Uani 1 1 d . . . H41 H 0.8712 0.1015 0.6250 0.038 Uiso 1 1 calc R . . C42 C 0.76941(14) 0.11553(14) 0.69383(13) 0.0270(4) Uani 1 1 d . . . H42 H 0.7952 0.0830 0.7326 0.032 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 Cl3 0.1379(10) 0.0562(5) 0.0454(4) -0.0014(4) -0.0038(5) 0.0223(5) Cl4 0.0484(4) 0.0552(4) 0.0473(4) 0.0033(3) 0.0104(3) 0.0107(3) C43 0.061(2) 0.061(2) 0.0508(18) 0.0090(15) -0.0108(15) -0.0049(15) Ni1 0.01522(13) 0.01486(13) 0.01532(12) -0.00191(8) -0.00017(8) -0.00041(8) Cl1 0.0220(2) 0.0239(2) 0.0168(2) 0.00050(16) 0.00259(16) 0.00009(17) Cl2 0.0260(3) 0.0213(3) 0.0583(4) 0.0025(2) 0.0005(2) -0.00765(19) P1 0.0154(2) 0.0153(2) 0.0162(2) -0.00020(16) -0.00029(16) 0.00171(16) P2 0.0148(2) 0.0167(2) 0.0154(2) -0.00001(16) 0.00129(16) 0.00186(16) N1 0.0155(7) 0.0148(8) 0.0178(7) -0.0018(6) -0.0016(6) 0.0013(5) N2 0.0145(7) 0.0169(8) 0.0165(7) -0.0026(6) 0.0003(6) 0.0018(6) C1 0.0166(8) 0.0138(8) 0.0144(8) 0.0007(6) 0.0021(6) -0.0007(6) C2 0.0155(8) 0.0170(9) 0.0138(8) -0.0003(6) 0.0018(6) -0.0012(6) C3 0.0203(9) 0.0187(9) 0.0188(9) -0.0032(7) 0.0018(7) 0.0018(7) C4 0.0248(10) 0.0177(9) 0.0200(9) -0.0049(7) 0.0012(7) -0.0036(7) C5 0.0200(9) 0.0224(10) 0.0163(8) -0.0004(7) -0.0024(7) -0.0051(7) C6 0.0171(9) 0.0216(9) 0.0177(8) 0.0006(7) 0.0003(7) 0.0010(7) C7 0.0178(9) 0.0175(9) 0.0244(9) -0.0037(7) -0.0027(7) 0.0056(7) C8 0.0209(10) 0.0239(11) 0.0343(11) -0.0050(8) 0.0024(8) -0.0012(8) C9 0.0223(11) 0.0281(12) 0.0532(15) -0.0108(10) -0.0034(10) -0.0037(8) C10 0.0304(12) 0.0317(13) 0.0495(15) -0.0192(11) -0.0174(10) 0.0074(9) C11 0.0483(15) 0.0307(12) 0.0276(11) -0.0066(9) -0.0159(10) 0.0117(10) C12 0.0392(12) 0.0199(10) 0.0241(10) -0.0008(8) -0.0072(9) 0.0078(8) C13 0.0176(9) 0.0195(9) 0.0203(9) -0.0018(7) 0.0020(7) 0.0013(7) C14 0.0205(10) 0.0261(11) 0.0245(10) 0.0026(8) 0.0010(7) 0.0012(8) C15 0.0297(11) 0.0286(11) 0.0310(11) 0.0059(9) 0.0066(9) -0.0020(9) C16 0.0242(11) 0.0340(13) 0.0430(13) 0.0040(10) 0.0084(9) -0.0056(9) C17 0.0156(10) 0.0406(13) 0.0444(13) 0.0044(10) 0.0012(9) 0.0011(9) C18 0.0206(10) 0.0283(11) 0.0282(10) 0.0047(8) 0.0000(8) 0.0016(8) C19 0.0184(9) 0.0180(9) 0.0196(9) 0.0028(7) -0.0015(7) -0.0007(7) C20 0.0217(10) 0.0219(10) 0.0297(10) 0.0051(8) 0.0001(8) 0.0022(7) C21 0.0244(11) 0.0243(11) 0.0437(13) 0.0130(9) -0.0050(9) 0.0002(8) C22 0.0370(13) 0.0380(13) 0.0286(11) 0.0158(10) -0.0095(9) -0.0071(10) C23 0.0405(13) 0.0345(12) 0.0217(10) 0.0040(9) 0.0024(9) -0.0047(10) C24 0.0264(10) 0.0240(10) 0.0224(10) 0.0026(8) 0.0015(8) -0.0001(8) C25 0.0214(9) 0.0193(9) 0.0185(9) 0.0014(7) -0.0020(7) 0.0007(7) C26 0.0268(11) 0.0219(10) 0.0259(10) -0.0009(8) 0.0010(8) 0.0037(8) C27 0.0389(13) 0.0201(10) 0.0317(11) 0.0011(8) -0.0014(9) 0.0067(9) C28 0.0434(13) 0.0229(11) 0.0263(11) 0.0053(8) -0.0036(9) -0.0037(9) C29 0.0349(12) 0.0273(11) 0.0300(11) 0.0043(9) 0.0070(9) -0.0049(9) C30 0.0263(10) 0.0222(10) 0.0276(10) 0.0021(8) 0.0044(8) 0.0013(8) C31 0.0161(9) 0.0193(9) 0.0207(9) -0.0009(7) -0.0008(7) 0.0034(7) C32 0.0275(11) 0.0382(13) 0.0263(11) -0.0073(9) 0.0066(9) -0.0089(9) C33 0.0268(12) 0.0498(16) 0.0434(14) -0.0154(11) 0.0080(10) -0.0151(10) C34 0.0288(12) 0.0458(14) 0.0357(13) -0.0142(11) -0.0055(9) -0.0053(10) C35 0.0372(13) 0.0385(13) 0.0213(10) -0.0033(9) -0.0034(9) -0.0021(10) C36 0.0264(10) 0.0289(11) 0.0216(10) 0.0003(8) -0.0005(8) -0.0016(8) C37 0.0195(9) 0.0184(9) 0.0197(9) -0.0016(7) 0.0037(7) 0.0005(7) C38 0.0253(10) 0.0275(11) 0.0206(9) 0.0013(8) 0.0033(8) 0.0009(8) C39 0.0361(12) 0.0372(13) 0.0211(10) 0.0026(9) 0.0043(9) -0.0045(10) C40 0.0381(12) 0.0296(12) 0.0272(11) -0.0080(9) 0.0178(9) -0.0081(9) C41 0.0264(11) 0.0280(11) 0.0409(13) -0.0069(9) 0.0155(9) 0.0017(8) C42 0.0234(10) 0.0258(11) 0.0325(11) 0.0014(8) 0.0075(8) 0.0040(8) _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 Cl3 C43 1.766(4) . ? Cl4 C43 1.750(3) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C46 1.375(10) 3_656 ? C44 C49 1.567(11) . ? C44 C47 1.743(12) . ? C44 C47 1.809(11) 3_656 ? C44 C45 2.023(10) . ? C45 C49 0.571(7) . ? C45 C47 0.792(9) . ? C45 C46 1.511(7) . ? C45 C51 1.838(9) . ? C46 C47 1.050(8) . ? C46 C44 1.375(10) 3_656 ? C46 C49 1.389(8) . ? C46 C51 1.400(8) 3_656 ? C47 C51 1.442(9) . ? C47 C51 1.581(9) 3_656 ? C47 C44 1.809(11) 3_656 ? C49 C51 1.326(10) . ? C49 C51 1.920(10) 3_656 ? C51 C46 1.400(8) 3_656 ? C51 C47 1.581(9) 3_656 ? C51 C49 1.920(10) 3_656 ? Ni1 N2 1.9960(15) . ? Ni1 N1 2.0141(16) . ? Ni1 Cl2 2.2178(6) . ? Ni1 Cl1 2.2811(5) . ? P1 N1 1.6185(16) . ? P1 C7 1.796(2) . ? P1 C19 1.8079(19) . ? P1 C13 1.815(2) . ? P2 N2 1.6117(16) . ? P2 C31 1.799(2) . ? P2 C37 1.8076(19) . ? P2 C25 1.818(2) . ? N1 C1 1.414(2) . ? N2 C2 1.413(2) . ? C1 C6 1.399(3) . ? C1 C2 1.423(2) . ? C2 C3 1.397(3) . ? C3 C4 1.395(3) . ? C3 H3 0.9300 . ? C4 C5 1.382(3) . ? C4 H4 0.9300 . ? C5 C6 1.386(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.393(3) . ? C7 C8 1.399(3) . ? C8 C9 1.392(3) . ? C8 H8 0.9300 . ? C9 C10 1.384(4) . ? C9 H9 0.9300 . ? C10 C11 1.382(4) . ? C10 H10 0.9300 . ? C11 C12 1.393(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.398(3) . ? C13 C18 1.399(3) . ? C14 C15 1.392(3) . ? C14 H14 0.9300 . ? C15 C16 1.383(3) . ? C15 H15 0.9300 . ? C16 C17 1.379(3) . ? C16 H16 0.9300 . ? C17 C18 1.394(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.390(3) . ? C19 C20 1.401(3) . ? C20 C21 1.388(3) . ? C20 H20 0.9300 . ? C21 C22 1.386(4) . ? C21 H21 0.9300 . ? C22 C23 1.384(4) . ? C22 H22 0.9300 . ? C23 C24 1.393(3) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.396(3) . ? C25 C26 1.400(3) . ? C26 C27 1.388(3) . ? C26 H26 0.9300 . ? C27 C28 1.384(3) . ? C27 H27 0.9300 . ? C28 C29 1.391(3) . ? C28 H28 0.9300 . ? C29 C30 1.389(3) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.392(3) . ? C31 C36 1.395(3) . ? C32 C33 1.389(3) . ? C32 H32 0.9300 . ? C33 C34 1.379(4) . ? C33 H33 0.9300 . ? C34 C35 1.382(4) . ? C34 H34 0.9300 . ? C35 C36 1.388(3) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.395(3) . ? C37 C42 1.401(3) . ? C38 C39 1.388(3) . ? C38 H38 0.9300 . ? C39 C40 1.388(3) . ? C39 H39 0.9300 . ? C40 C41 1.380(4) . ? C40 H40 0.9300 . ? C41 C42 1.391(3) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? 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 Cl4 C43 Cl3 111.95(18) . . ? Cl4 C43 H43A 109.2 . . ? Cl3 C43 H43A 109.2 . . ? Cl4 C43 H43B 109.2 . . ? Cl3 C43 H43B 109.2 . . ? H43A C43 H43B 107.9 . . ? C46 C44 C49 113.2(7) 3_656 . ? C46 C44 C47 103.0(6) 3_656 . ? C49 C44 C47 11.7(4) . . ? C46 C44 C47 35.3(4) 3_656 3_656 ? C49 C44 C47 82.5(5) . 3_656 ? C47 C44 C47 71.0(5) . 3_656 ? C46 C44 C45 122.2(6) 3_656 . ? C49 C44 C45 11.0(4) . . ? C47 C44 C45 22.8(3) . . ? C47 C44 C45 93.1(5) 3_656 . ? C49 C45 C47 26.6(9) . . ? C49 C45 C46 66.9(10) . . ? C47 C45 C46 40.9(6) . . ? C49 C45 C51 22.1(10) . . ? C47 C45 C51 48.6(7) . . ? C46 C45 C51 87.9(4) . . ? C49 C45 C44 31.7(10) . . ? C47 C45 C44 58.3(7) . . ? C46 C45 C44 98.3(4) . . ? C51 C45 C44 10.7(3) . . ? C47 C46 C44 95.6(7) . 3_656 ? C47 C46 C49 8.2(6) . . ? C44 C46 C49 103.7(6) 3_656 . ? C47 C46 C51 79.0(6) . 3_656 ? C44 C46 C51 16.8(4) 3_656 3_656 ? C49 C46 C51 87.0(5) . 3_656 ? C47 C46 C45 29.6(5) . . ? C44 C46 C45 121.5(6) 3_656 . ? C49 C46 C45 22.2(3) . . ? C51 C46 C45 104.9(5) 3_656 . ? C45 C47 C46 109.4(9) . . ? C45 C47 C51 107.1(9) . . ? C46 C47 C51 138.9(7) . . ? C45 C47 C51 151.6(9) . 3_656 ? C46 C47 C51 60.4(5) . 3_656 ? C51 C47 C51 94.0(5) . 3_656 ? C45 C47 C44 98.9(8) . . ? C46 C47 C44 148.6(7) . . ? C51 C47 C44 9.8(4) . . ? C51 C47 C44 99.7(6) 3_656 . ? C45 C47 C44 148.6(9) . 3_656 ? C46 C47 C44 49.2(5) . 3_656 ? C51 C47 C44 102.3(6) . 3_656 ? C51 C47 C44 11.4(4) 3_656 3_656 ? C44 C47 C44 109.0(5) . 3_656 ? C45 C49 C51 148.6(14) . . ? C45 C49 C46 91.0(11) . . ? C51 C49 C46 118.7(7) . . ? C45 C49 C44 137.2(13) . . ? C51 C49 C44 13.0(4) . . ? C46 C49 C44 131.4(7) . . ? C45 C49 C51 126.9(12) . 3_656 ? C51 C49 C51 83.7(5) . 3_656 ? C46 C49 C51 46.7(4) . 3_656 ? C44 C49 C51 93.0(6) . 3_656 ? C49 C51 C46 128.8(6) . 3_656 ? C49 C51 C47 15.1(4) . . ? C46 C51 C47 119.1(5) 3_656 . ? C49 C51 C47 100.0(5) . 3_656 ? C46 C51 C47 40.7(4) 3_656 3_656 ? C47 C51 C47 86.0(5) . 3_656 ? C49 C51 C45 9.3(4) . . ? C46 C51 C45 134.7(5) 3_656 . ? C47 C51 C45 24.3(3) . . ? C47 C51 C45 109.0(5) 3_656 . ? C49 C51 C49 96.3(5) . 3_656 ? C46 C51 C49 46.3(3) 3_656 3_656 ? C47 C51 C49 81.9(4) . 3_656 ? C47 C51 C49 5.6(4) 3_656 3_656 ? C45 C51 C49 105.4(4) . 3_656 ? N2 Ni1 N1 83.60(6) . . ? N2 Ni1 Cl2 113.51(5) . . ? N1 Ni1 Cl2 116.55(5) . . ? N2 Ni1 Cl1 101.27(5) . . ? N1 Ni1 Cl1 104.15(5) . . ? Cl2 Ni1 Cl1 128.09(2) . . ? N1 P1 C7 106.32(8) . . ? N1 P1 C19 114.83(9) . . ? C7 P1 C19 106.81(9) . . ? N1 P1 C13 111.41(9) . . ? C7 P1 C13 110.56(9) . . ? C19 P1 C13 106.83(9) . . ? N2 P2 C31 108.03(8) . . ? N2 P2 C37 111.90(9) . . ? C31 P2 C37 106.75(9) . . ? N2 P2 C25 111.84(9) . . ? C31 P2 C25 105.98(9) . . ? C37 P2 C25 111.94(9) . . ? C1 N1 P1 123.48(13) . . ? C1 N1 Ni1 110.29(11) . . ? P1 N1 Ni1 124.04(9) . . ? C2 N2 P2 123.14(13) . . ? C2 N2 Ni1 111.01(11) . . ? P2 N2 Ni1 125.68(9) . . ? C6 C1 N1 125.25(17) . . ? C6 C1 C2 118.51(17) . . ? N1 C1 C2 116.23(16) . . ? C3 C2 N2 124.78(17) . . ? C3 C2 C1 118.98(17) . . ? N2 C2 C1 116.23(16) . . ? C4 C3 C2 121.21(18) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 119.74(18) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.01(18) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 121.55(18) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? C12 C7 C8 119.73(19) . . ? C12 C7 P1 120.50(16) . . ? C8 C7 P1 119.66(16) . . ? C9 C8 C7 119.4(2) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C8 120.6(2) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C11 C10 C9 120.1(2) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.0(2) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C7 120.1(2) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C14 C13 C18 119.44(18) . . ? C14 C13 P1 117.25(15) . . ? C18 C13 P1 123.19(15) . . ? C15 C14 C13 120.03(19) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.1(2) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 120.3(2) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.5(2) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 119.7(2) . . ? C17 C18 H18 120.2 . . ? C13 C18 H18 120.2 . . ? C24 C19 C20 119.43(18) . . ? C24 C19 P1 119.75(15) . . ? C20 C19 P1 120.81(15) . . ? C21 C20 C19 119.9(2) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 120.3(2) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 120.0(2) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.1(2) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C19 C24 C23 120.2(2) . . ? C19 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C30 C25 C26 119.27(19) . . ? C30 C25 P2 115.99(15) . . ? C26 C25 P2 124.56(16) . . ? C27 C26 C25 119.7(2) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C28 C27 C26 120.9(2) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 119.8(2) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C30 C29 C28 119.9(2) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C25 120.5(2) . . ? C29 C30 H30 119.7 . . ? C25 C30 H30 119.7 . . ? C32 C31 C36 119.71(19) . . ? C32 C31 P2 120.84(16) . . ? C36 C31 P2 119.39(15) . . ? C33 C32 C31 119.7(2) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C34 C33 C32 120.5(2) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 120.1(2) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C36 120.2(2) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 119.9(2) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C38 C37 C42 119.45(18) . . ? C38 C37 P2 117.54(15) . . ? C42 C37 P2 122.64(15) . . ? C39 C38 C37 120.2(2) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C40 C39 C38 120.2(2) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C41 C40 C39 119.8(2) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C42 120.8(2) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C41 C42 C37 119.5(2) . . ? C41 C42 H42 120.2 . . ? C37 C42 H42 120.2 . . ? 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 C46 C44 C45 C49 -37.1(17) 3_656 . . . ? C47 C44 C45 C49 -1.9(17) . . . . ? C47 C44 C45 C49 -15.9(15) 3_656 . . . ? C46 C44 C45 C47 -35.2(8) 3_656 . . . ? C49 C44 C45 C47 1.9(17) . . . . ? C47 C44 C45 C47 -14.0(8) 3_656 . . . ? C46 C44 C45 C46 -44.2(8) 3_656 . . . ? C49 C44 C45 C46 -7.1(15) . . . . ? C47 C44 C45 C46 -9.0(6) . . . . ? C47 C44 C45 C46 -23.0(5) 3_656 . . . ? C46 C44 C45 C51 -58.5(19) 3_656 . . . ? C49 C44 C45 C51 -21(2) . . . . ? C47 C44 C45 C51 -23(2) . . . . ? C47 C44 C45 C51 -37.3(19) 3_656 . . . ? C49 C45 C46 C47 7.7(13) . . . . ? C51 C45 C46 C47 14.4(8) . . . . ? C44 C45 C46 C47 11.7(8) . . . . ? C49 C45 C46 C44 39.7(11) . . . 3_656 ? C47 C45 C46 C44 32.0(9) . . . 3_656 ? C51 C45 C46 C44 46.4(6) . . . 3_656 ? C44 C45 C46 C44 43.8(8) . . . 3_656 ? C47 C45 C46 C49 -7.7(13) . . . . ? C51 C45 C46 C49 6.7(8) . . . . ? C44 C45 C46 C49 4.0(9) . . . . ? C49 C45 C46 C51 37.4(10) . . . 3_656 ? C47 C45 C46 C51 29.7(8) . . . 3_656 ? C51 C45 C46 C51 44.1(5) . . . 3_656 ? C44 C45 C46 C51 41.4(4) . . . 3_656 ? C49 C45 C47 C46 -164(3) . . . . ? C51 C45 C47 C46 -160.7(10) . . . . ? C44 C45 C47 C46 -166.3(9) . . . . ? C49 C45 C47 C51 -3.4(19) . . . . ? C46 C45 C47 C51 160.7(10) . . . . ? C44 C45 C47 C51 -5.6(5) . . . . ? C49 C45 C47 C51 133(3) . . . 3_656 ? C46 C45 C47 C51 -63.3(17) . . . 3_656 ? C51 C45 C47 C51 136(2) . . . 3_656 ? C44 C45 C47 C51 130.4(19) . . . 3_656 ? C49 C45 C47 C44 2(2) . . . . ? C46 C45 C47 C44 166.3(9) . . . . ? C51 C45 C47 C44 5.6(5) . . . . ? C49 C45 C47 C44 155(3) . . . 3_656 ? C46 C45 C47 C44 -41.2(12) . . . 3_656 ? C51 C45 C47 C44 158.1(17) . . . 3_656 ? C44 C45 C47 C44 152.5(15) . . . 3_656 ? C44 C46 C47 C45 -153.0(8) 3_656 . . . ? C49 C46 C47 C45 21(4) . . . . ? C51 C46 C47 C45 -150.8(8) 3_656 . . . ? C44 C46 C47 C51 55.7(10) 3_656 . . . ? C49 C46 C47 C51 -130(4) . . . . ? C51 C46 C47 C51 57.9(10) 3_656 . . . ? C45 C46 C47 C51 -151.3(15) . . . . ? C44 C46 C47 C51 -2.2(6) 3_656 . . 3_656 ? C49 C46 C47 C51 172(4) . . . 3_656 ? C45 C46 C47 C51 150.8(8) . . . 3_656 ? C44 C46 C47 C44 53.6(14) 3_656 . . . ? C49 C46 C47 C44 -132(5) . . . . ? C51 C46 C47 C44 55.9(12) 3_656 . . . ? C45 C46 C47 C44 -153.4(17) . . . . ? C49 C46 C47 C44 174(4) . . . 3_656 ? C51 C46 C47 C44 2.2(6) 3_656 . . 3_656 ? C45 C46 C47 C44 153.0(8) . . . 3_656 ? C46 C44 C47 C45 150.0(7) 3_656 . . . ? C49 C44 C47 C45 -1.8(16) . . . . ? C47 C44 C47 C45 165.2(8) 3_656 . . . ? C46 C44 C47 C46 -55.3(15) 3_656 . . . ? C49 C44 C47 C46 153(3) . . . . ? C47 C44 C47 C46 -40.1(12) 3_656 . . . ? C45 C44 C47 C46 154.7(16) . . . . ? C46 C44 C47 C51 -63(3) 3_656 . . . ? C49 C44 C47 C51 145(4) . . . . ? C47 C44 C47 C51 -48(3) 3_656 . . . ? C45 C44 C47 C51 147(3) . . . . ? C46 C44 C47 C51 -8.5(7) 3_656 . . 3_656 ? C49 C44 C47 C51 -160(2) . . . 3_656 ? C47 C44 C47 C51 6.8(4) 3_656 . . 3_656 ? C45 C44 C47 C51 -158.5(8) . . . 3_656 ? C46 C44 C47 C44 -15.2(5) 3_656 . . 3_656 ? C49 C44 C47 C44 -167(2) . . . 3_656 ? C47 C44 C47 C44 0.0 3_656 . . 3_656 ? C45 C44 C47 C44 -165.2(8) . . . 3_656 ? C47 C45 C49 C51 173(4) . . . . ? C46 C45 C49 C51 162(2) . . . . ? C44 C45 C49 C51 -10.4(11) . . . . ? C47 C45 C49 C46 11.3(18) . . . . ? C51 C45 C49 C46 -162(2) . . . . ? C44 C45 C49 C46 -172.4(16) . . . . ? C47 C45 C49 C44 -176(3) . . . . ? C46 C45 C49 C44 172.4(16) . . . . ? C51 C45 C49 C44 10.4(11) . . . . ? C47 C45 C49 C51 -21.1(15) . . . 3_656 ? C46 C45 C49 C51 -32.3(8) . . . 3_656 ? C51 C45 C49 C51 166(3) . . . 3_656 ? C44 C45 C49 C51 155(2) . . . 3_656 ? C47 C46 C49 C45 -152(5) . . . . ? C44 C46 C49 C45 -145.9(10) 3_656 . . . ? C51 C46 C49 C45 -144.0(10) 3_656 . . . ? C47 C46 C49 C51 38(4) . . . . ? C44 C46 C49 C51 44.7(7) 3_656 . . . ? C51 C46 C49 C51 46.6(7) 3_656 . . . ? C45 C46 C49 C51 -169.4(13) . . . . ? C47 C46 C49 C44 35(4) . . . . ? C44 C46 C49 C44 41.0(10) 3_656 . . . ? C51 C46 C49 C44 42.9(7) 3_656 . . . ? C45 C46 C49 C44 -173.1(15) . . . . ? C47 C46 C49 C51 -8(4) . . . 3_656 ? C44 C46 C49 C51 -1.9(6) 3_656 . . 3_656 ? C45 C46 C49 C51 144.0(10) . . . 3_656 ? C46 C44 C49 C45 146.3(15) 3_656 . . . ? C47 C44 C49 C45 176(3) . . . . ? C47 C44 C49 C45 164.0(15) 3_656 . . . ? C46 C44 C49 C51 -59(2) 3_656 . . . ? C47 C44 C49 C51 -28(3) . . . . ? C47 C44 C49 C51 -41(2) 3_656 . . . ? C45 C44 C49 C51 155(3) . . . . ? C46 C44 C49 C46 -43.9(11) 3_656 . . . ? C47 C44 C49 C46 -13.8(15) . . . . ? C47 C44 C49 C46 -26.2(9) 3_656 . . . ? C45 C44 C49 C46 170(2) . . . . ? C46 C44 C49 C51 -14.2(7) 3_656 . . 3_656 ? C47 C44 C49 C51 15.9(17) . . . 3_656 ? C47 C44 C49 C51 3.6(5) 3_656 . . 3_656 ? C45 C44 C49 C51 -160.4(18) . . . 3_656 ? C45 C49 C51 C46 132(2) . . . 3_656 ? C46 C49 C51 C46 -68.6(9) . . . 3_656 ? C44 C49 C51 C46 99(2) . . . 3_656 ? C51 C49 C51 C46 -36.5(6) 3_656 . . 3_656 ? C45 C49 C51 C47 -174(4) . . . . ? C46 C49 C51 C47 -14.3(14) . . . . ? C44 C49 C51 C47 153(3) . . . . ? C51 C49 C51 C47 17.9(16) 3_656 . . . ? C45 C49 C51 C47 164(2) . . . 3_656 ? C46 C49 C51 C47 -36.4(8) . . . 3_656 ? C44 C49 C51 C47 131(2) . . . 3_656 ? C51 C49 C51 C47 -4.2(4) 3_656 . . 3_656 ? C46 C49 C51 C45 159(3) . . . . ? C44 C49 C51 C45 -33(3) . . . . ? C51 C49 C51 C45 -169(2) 3_656 . . . ? C45 C49 C51 C49 169(2) . . . 3_656 ? C46 C49 C51 C49 -32.1(5) . . . 3_656 ? C44 C49 C51 C49 135(2) . . . 3_656 ? C51 C49 C51 C49 0.0 3_656 . . 3_656 ? C45 C47 C51 C49 2.5(14) . . . . ? C46 C47 C51 C49 154(2) . . . . ? C51 C47 C51 C49 -158(2) 3_656 . . . ? C44 C47 C51 C49 -32(3) . . . . ? C44 C47 C51 C49 -166(2) 3_656 . . . ? C45 C47 C51 C46 136.1(7) . . . 3_656 ? C46 C47 C51 C46 -72.3(12) . . . 3_656 ? C51 C47 C51 C46 -24.6(5) 3_656 . . 3_656 ? C44 C47 C51 C46 101(3) . . . 3_656 ? C44 C47 C51 C46 -32.5(7) 3_656 . . 3_656 ? C45 C47 C51 C47 160.7(8) . . . 3_656 ? C46 C47 C51 C47 -47.6(9) . . . 3_656 ? C51 C47 C51 C47 0.0 3_656 . . 3_656 ? C44 C47 C51 C47 126(3) . . . 3_656 ? C44 C47 C51 C47 -7.8(4) 3_656 . . 3_656 ? C46 C47 C51 C45 151.7(14) . . . . ? C51 C47 C51 C45 -160.7(8) 3_656 . . . ? C44 C47 C51 C45 -35(3) . . . . ? C44 C47 C51 C45 -168.5(9) 3_656 . . . ? C45 C47 C51 C49 164.6(6) . . . 3_656 ? C46 C47 C51 C49 -43.7(11) . . . 3_656 ? C51 C47 C51 C49 3.9(3) 3_656 . . 3_656 ? C44 C47 C51 C49 130(3) . . . 3_656 ? C44 C47 C51 C49 -4.0(5) 3_656 . . 3_656 ? C47 C45 C51 C49 -4(2) . . . . ? C46 C45 C51 C49 -17(2) . . . . ? C44 C45 C51 C49 149(3) . . . . ? C49 C45 C51 C46 -54(2) . . . 3_656 ? C47 C45 C51 C46 -58.4(9) . . . 3_656 ? C46 C45 C51 C46 -71.0(8) . . . 3_656 ? C44 C45 C51 C46 95(2) . . . 3_656 ? C49 C45 C51 C47 4(2) . . . . ? C46 C45 C51 C47 -12.5(7) . . . . ? C44 C45 C51 C47 153(2) . . . . ? C49 C45 C51 C47 -16(2) . . . 3_656 ? C47 C45 C51 C47 -20.4(9) . . . 3_656 ? C46 C45 C51 C47 -32.9(5) . . . 3_656 ? C44 C45 C51 C47 133(2) . . . 3_656 ? C49 C45 C51 C49 -12(2) . . . 3_656 ? C47 C45 C51 C49 -15.9(6) . . . 3_656 ? C46 C45 C51 C49 -28.4(4) . . . 3_656 ? C44 C45 C51 C49 137(2) . . . 3_656 ? C7 P1 N1 C1 172.93(15) . . . . ? C19 P1 N1 C1 -69.20(17) . . . . ? C13 P1 N1 C1 52.41(17) . . . . ? C7 P1 N1 Ni1 11.37(13) . . . . ? C19 P1 N1 Ni1 129.24(10) . . . . ? C13 P1 N1 Ni1 -109.15(11) . . . . ? N2 Ni1 N1 C1 14.20(12) . . . . ? Cl2 Ni1 N1 C1 127.32(11) . . . . ? Cl1 Ni1 N1 C1 -85.84(11) . . . . ? N2 Ni1 N1 P1 177.87(11) . . . . ? Cl2 Ni1 N1 P1 -69.01(11) . . . . ? Cl1 Ni1 N1 P1 77.82(10) . . . . ? C31 P2 N2 C2 -175.37(14) . . . . ? C37 P2 N2 C2 67.40(17) . . . . ? C25 P2 N2 C2 -59.11(17) . . . . ? C31 P2 N2 Ni1 -0.50(14) . . . . ? C37 P2 N2 Ni1 -117.72(11) . . . . ? C25 P2 N2 Ni1 115.76(11) . . . . ? N1 Ni1 N2 C2 -13.63(12) . . . . ? Cl2 Ni1 N2 C2 -129.84(11) . . . . ? Cl1 Ni1 N2 C2 89.57(12) . . . . ? N1 Ni1 N2 P2 170.96(12) . . . . ? Cl2 Ni1 N2 P2 54.76(12) . . . . ? Cl1 Ni1 N2 P2 -85.83(11) . . . . ? P1 N1 C1 C6 5.2(3) . . . . ? Ni1 N1 C1 C6 168.97(15) . . . . ? P1 N1 C1 C2 -176.15(13) . . . . ? Ni1 N1 C1 C2 -12.38(19) . . . . ? P2 N2 C2 C3 5.1(3) . . . . ? Ni1 N2 C2 C3 -170.41(15) . . . . ? P2 N2 C2 C1 -173.78(13) . . . . ? Ni1 N2 C2 C1 10.68(19) . . . . ? C6 C1 C2 C3 1.0(3) . . . . ? N1 C1 C2 C3 -177.71(16) . . . . ? C6 C1 C2 N2 -179.99(16) . . . . ? N1 C1 C2 N2 1.3(2) . . . . ? N2 C2 C3 C4 -179.14(18) . . . . ? C1 C2 C3 C4 -0.3(3) . . . . ? C2 C3 C4 C5 -0.5(3) . . . . ? C3 C4 C5 C6 0.4(3) . . . . ? C4 C5 C6 C1 0.4(3) . . . . ? N1 C1 C6 C5 177.49(17) . . . . ? C2 C1 C6 C5 -1.1(3) . . . . ? N1 P1 C7 C12 -82.58(18) . . . . ? C19 P1 C7 C12 154.36(16) . . . . ? C13 P1 C7 C12 38.49(19) . . . . ? N1 P1 C7 C8 93.58(17) . . . . ? C19 P1 C7 C8 -29.48(18) . . . . ? C13 P1 C7 C8 -145.35(16) . . . . ? C12 C7 C8 C9 -0.1(3) . . . . ? P1 C7 C8 C9 -176.25(16) . . . . ? C7 C8 C9 C10 1.2(3) . . . . ? C8 C9 C10 C11 -1.5(4) . . . . ? C9 C10 C11 C12 0.6(4) . . . . ? C10 C11 C12 C7 0.5(3) . . . . ? C8 C7 C12 C11 -0.8(3) . . . . ? P1 C7 C12 C11 175.38(17) . . . . ? N1 P1 C13 C14 34.66(18) . . . . ? C7 P1 C13 C14 -83.33(17) . . . . ? C19 P1 C13 C14 160.81(16) . . . . ? N1 P1 C13 C18 -141.36(17) . . . . ? C7 P1 C13 C18 100.65(18) . . . . ? C19 P1 C13 C18 -15.2(2) . . . . ? C18 C13 C14 C15 -0.4(3) . . . . ? P1 C13 C14 C15 -176.60(17) . . . . ? C13 C14 C15 C16 -0.4(3) . . . . ? C14 C15 C16 C17 0.7(4) . . . . ? C15 C16 C17 C18 -0.2(4) . . . . ? C16 C17 C18 C13 -0.6(4) . . . . ? C14 C13 C18 C17 0.9(3) . . . . ? P1 C13 C18 C17 176.89(18) . . . . ? N1 P1 C19 C24 9.1(2) . . . . ? C7 P1 C19 C24 126.67(17) . . . . ? C13 P1 C19 C24 -114.99(17) . . . . ? N1 P1 C19 C20 -171.56(15) . . . . ? C7 P1 C19 C20 -53.96(18) . . . . ? C13 P1 C19 C20 64.37(18) . . . . ? C24 C19 C20 C21 2.7(3) . . . . ? P1 C19 C20 C21 -176.63(16) . . . . ? C19 C20 C21 C22 -1.8(3) . . . . ? C20 C21 C22 C23 -0.3(4) . . . . ? C21 C22 C23 C24 1.5(4) . . . . ? C20 C19 C24 C23 -1.6(3) . . . . ? P1 C19 C24 C23 177.77(17) . . . . ? C22 C23 C24 C19 -0.5(3) . . . . ? N2 P2 C25 C30 -31.36(19) . . . . ? C31 P2 C25 C30 86.14(17) . . . . ? C37 P2 C25 C30 -157.85(16) . . . . ? N2 P2 C25 C26 153.48(17) . . . . ? C31 P2 C25 C26 -89.02(19) . . . . ? C37 P2 C25 C26 27.0(2) . . . . ? C30 C25 C26 C27 -1.5(3) . . . . ? P2 C25 C26 C27 173.54(16) . . . . ? C25 C26 C27 C28 0.8(3) . . . . ? C26 C27 C28 C29 0.7(4) . . . . ? C27 C28 C29 C30 -1.3(4) . . . . ? C28 C29 C30 C25 0.6(3) . . . . ? C26 C25 C30 C29 0.8(3) . . . . ? P2 C25 C30 C29 -174.63(17) . . . . ? N2 P2 C31 C32 -103.73(18) . . . . ? C37 P2 C31 C32 16.8(2) . . . . ? C25 P2 C31 C32 136.25(18) . . . . ? N2 P2 C31 C36 73.50(18) . . . . ? C37 P2 C31 C36 -166.00(16) . . . . ? C25 P2 C31 C36 -46.51(18) . . . . ? C36 C31 C32 C33 0.9(3) . . . . ? P2 C31 C32 C33 178.1(2) . . . . ? C31 C32 C33 C34 -0.6(4) . . . . ? C32 C33 C34 C35 -0.6(4) . . . . ? C33 C34 C35 C36 1.5(4) . . . . ? C34 C35 C36 C31 -1.2(4) . . . . ? C32 C31 C36 C35 0.0(3) . . . . ? P2 C31 C36 C35 -177.23(17) . . . . ? N2 P2 C37 C38 3.52(19) . . . . ? C31 P2 C37 C38 -114.48(17) . . . . ? C25 P2 C37 C38 129.97(16) . . . . ? N2 P2 C37 C42 176.53(17) . . . . ? C31 P2 C37 C42 58.53(19) . . . . ? C25 P2 C37 C42 -57.0(2) . . . . ? C42 C37 C38 C39 0.2(3) . . . . ? P2 C37 C38 C39 173.43(17) . . . . ? C37 C38 C39 C40 -0.3(3) . . . . ? C38 C39 C40 C41 0.5(4) . . . . ? C39 C40 C41 C42 -0.7(4) . . . . ? C40 C41 C42 C37 0.6(3) . . . . ? C38 C37 C42 C41 -0.4(3) . . . . ? P2 C37 C42 C41 -173.23(17) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.715 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.066 data_fl _database_code_CSD 182856 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H34 Cl2 N2 Ni P2' _chemical_formula_weight 710.22 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 Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.921(4) _cell_length_b 16.112(4) _cell_length_c 17.597(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.71(2) _cell_angle_gamma 90.00 _cell_volume 4322.5(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.091 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.670 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9734 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0980 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.97 _reflns_number_total 9418 _reflns_number_gt 4968 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1837P)^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 SHELXL _refine_ls_extinction_coef 0.0008(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9418 _refine_ls_number_parameters 431 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1551 _refine_ls_R_factor_gt 0.0943 _refine_ls_wR_factor_ref 0.3083 _refine_ls_wR_factor_gt 0.2803 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 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 0.73358(5) -0.00722(5) 0.21789(5) 0.0381(3) Uani 1 1 d . . . Cl1 Cl 0.74066(13) 0.10511(12) 0.14531(14) 0.0650(6) Uani 1 1 d . . . Cl2 Cl 0.66122(14) -0.12436(12) 0.15553(13) 0.0621(5) Uani 1 1 d . . . P1 P 0.94596(11) -0.03563(11) 0.29845(11) 0.0392(4) Uani 1 1 d . . . P2 P 0.61606(11) 0.02457(10) 0.32209(11) 0.0388(4) Uani 1 1 d . . . N1 N 0.8563(3) -0.0302(4) 0.3064(3) 0.0434(13) Uani 1 1 d . . . N2 N 0.7058(3) 0.0206(3) 0.3136(3) 0.0431(13) Uani 1 1 d . . . C1 C 0.8554(5) -0.0325(5) 0.3901(4) 0.0553(19) Uani 1 1 d . . . H1A H 0.9132 -0.0191 0.4337 0.066 Uiso 1 1 calc R . . H1B H 0.8401 -0.0879 0.4010 0.066 Uiso 1 1 calc R . . C2 C 0.7891(4) 0.0295(5) 0.3920(4) 0.0554(19) Uani 1 1 d . . . H2A H 0.7783 0.0197 0.4410 0.066 Uiso 1 1 calc R . . H2B H 0.8118 0.0854 0.3957 0.066 Uiso 1 1 calc R . . C3 C 0.6036(4) -0.0606(4) 0.3829(4) 0.0448(16) Uani 1 1 d . . . C4 C 0.6302(5) -0.1398(5) 0.3699(5) 0.0573(19) Uani 1 1 d . . . H4 H 0.6542 -0.1461 0.3317 0.069 Uiso 1 1 calc R . . C5 C 0.6219(6) -0.2065(5) 0.4115(6) 0.072(2) Uani 1 1 d . . . H5 H 0.6370 -0.2588 0.3998 0.086 Uiso 1 1 calc R . . C6 C 0.5905(7) -0.1971(6) 0.4722(7) 0.091(3) Uani 1 1 d . . . H6 H 0.5877 -0.2429 0.5031 0.109 Uiso 1 1 calc R . . C7 C 0.5632(7) -0.1196(7) 0.4870(7) 0.096(3) Uani 1 1 d . . . H7 H 0.5422 -0.1129 0.5275 0.115 Uiso 1 1 calc R . . C8 C 0.5683(6) -0.0534(6) 0.4399(6) 0.075(3) Uani 1 1 d . . . H8 H 0.5472 -0.0020 0.4468 0.090 Uiso 1 1 calc R . . C9 C 0.5279(4) 0.0204(4) 0.2166(4) 0.0453(16) Uani 1 1 d . . . C10 C 0.4543(5) -0.0280(5) 0.1985(5) 0.063(2) Uani 1 1 d . . . H10 H 0.4497 -0.0596 0.2406 0.076 Uiso 1 1 calc R . . C11 C 0.3879(6) -0.0290(6) 0.1179(7) 0.084(3) Uani 1 1 d . . . H11 H 0.3386 -0.0618 0.1058 0.101 Uiso 1 1 calc R . . C12 C 0.3932(6) 0.0170(6) 0.0558(6) 0.070(2) Uani 1 1 d . . . H12 H 0.3471 0.0166 0.0019 0.084 Uiso 1 1 calc R . . C13 C 0.4666(6) 0.0644(6) 0.0723(5) 0.068(2) Uani 1 1 d . . . H13 H 0.4717 0.0936 0.0291 0.082 Uiso 1 1 calc R . . C14 C 0.5332(5) 0.0684(5) 0.1543(5) 0.0538(18) Uani 1 1 d . . . H14 H 0.5810 0.1033 0.1668 0.065 Uiso 1 1 calc R . . C15 C 0.6002(5) 0.1180(4) 0.3717(5) 0.0472(16) Uani 1 1 d . . . C16 C 0.5346(6) 0.1736(5) 0.3284(6) 0.072(2) Uani 1 1 d . . . H16 H 0.4951 0.1613 0.2733 0.086 Uiso 1 1 calc R . . C17 C 0.5254(7) 0.2461(6) 0.3634(7) 0.086(3) Uani 1 1 d . . . H17 H 0.4803 0.2825 0.3321 0.103 Uiso 1 1 calc R . . C18 C 0.5832(7) 0.2656(6) 0.4453(7) 0.078(3) Uani 1 1 d . . . H18 H 0.5762 0.3145 0.4698 0.094 Uiso 1 1 calc R . . C19 C 0.6508(6) 0.2126(7) 0.4904(7) 0.083(3) Uani 1 1 d . . . H19 H 0.6917 0.2265 0.5446 0.100 Uiso 1 1 calc R . . C20 C 0.6575(5) 0.1378(6) 0.4540(5) 0.070(2) Uani 1 1 d . . . H20 H 0.7012 0.1003 0.4856 0.084 Uiso 1 1 calc R . . C21 C 0.9229(5) -0.0322(5) 0.1880(4) 0.0482(17) Uani 1 1 d . . . C22 C 0.8598(5) -0.0862(5) 0.1327(5) 0.0557(19) Uani 1 1 d . . . H22 H 0.8318 -0.1239 0.1528 0.067 Uiso 1 1 calc R . . C23 C 0.8391(6) -0.0832(6) 0.0466(5) 0.066(2) Uani 1 1 d . . . H23 H 0.7959 -0.1181 0.0093 0.080 Uiso 1 1 calc R . . C24 C 0.8812(7) -0.0301(6) 0.0172(6) 0.082(3) Uani 1 1 d . . . H24 H 0.8677 -0.0290 -0.0400 0.098 Uiso 1 1 calc R . . C25 C 0.9450(8) 0.0231(7) 0.0730(6) 0.087(3) Uani 1 1 d . . . H25 H 0.9739 0.0601 0.0530 0.104 Uiso 1 1 calc R . . C26 C 0.9655(6) 0.0208(5) 0.1594(5) 0.064(2) Uani 1 1 d . . . H26 H 1.0084 0.0559 0.1968 0.077 Uiso 1 1 calc R . . C27 C 1.0208(4) 0.0489(4) 0.3509(4) 0.0444(16) Uani 1 1 d . . . C28 C 0.9869(6) 0.1236(5) 0.3601(5) 0.059(2) Uani 1 1 d . . . H28 H 0.9267 0.1298 0.3409 0.070 Uiso 1 1 calc R . . C29 C 1.0436(8) 0.1911(5) 0.3987(6) 0.079(3) Uani 1 1 d . . . H29 H 1.0200 0.2421 0.4029 0.095 Uiso 1 1 calc R . . C30 C 1.1330(7) 0.1823(6) 0.4301(6) 0.081(3) Uani 1 1 d . . . H30 H 1.1702 0.2260 0.4578 0.097 Uiso 1 1 calc R . . C31 C 1.1664(6) 0.1075(6) 0.4198(6) 0.074(3) Uani 1 1 d . . . H31 H 1.2266 0.1012 0.4383 0.089 Uiso 1 1 calc R . . C32 C 1.1106(5) 0.0421(5) 0.3819(5) 0.059(2) Uani 1 1 d . . . H32 H 1.1345 -0.0085 0.3771 0.071 Uiso 1 1 calc R . . C33 C 1.0112(4) -0.1281(4) 0.3430(4) 0.0389(14) Uani 1 1 d . . . C34 C 1.0385(6) -0.1785(6) 0.2978(5) 0.082(3) Uani 1 1 d . . . H34 H 1.0220 -0.1682 0.2410 0.098 Uiso 1 1 calc R . . C35 C 1.0930(8) -0.2479(7) 0.3383(7) 0.107(4) Uani 1 1 d . . . H35 H 1.1120 -0.2817 0.3067 0.128 Uiso 1 1 calc R . . C36 C 1.1177(5) -0.2662(5) 0.4181(6) 0.067(2) Uani 1 1 d . . . H36 H 1.1534 -0.3119 0.4426 0.080 Uiso 1 1 calc R . . C37 C 1.0902(6) -0.2177(6) 0.4630(6) 0.082(3) Uani 1 1 d . . . H37 H 1.1057 -0.2305 0.5192 0.098 Uiso 1 1 calc R . . C38 C 1.0372(6) -0.1460(5) 0.4261(5) 0.072(2) Uani 1 1 d . . . H38 H 1.0204 -0.1116 0.4590 0.086 Uiso 1 1 calc R . . Cl10 Cl 1.1893(8) -0.3334(8) 0.6696(8) 0.163(4) Uiso 0.40 1 d P . . Cl11 Cl 0.3534(10) -0.1941(10) 0.2859(10) 0.200(5) Uiso 0.40 1 d P . . C40 C 1.2714(14) -0.2657(13) 0.7000(14) 0.067(5) Uiso 0.40 1 d P . . Cl12 Cl 0.8468(10) -0.2866(9) 0.3507(9) 0.193(5) Uiso 0.40 1 d P . . Cl13 Cl 0.2902(10) 0.1357(10) 0.2079(10) 0.204(6) Uiso 0.40 1 d P . . C41 C 0.7683(15) -0.1884(14) -0.1326(14) 0.068(6) Uiso 0.40 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 0.0359(4) 0.0419(5) 0.0341(4) 0.0013(3) 0.0128(3) -0.0016(4) Cl1 0.0606(12) 0.0559(11) 0.0807(14) 0.0227(10) 0.0328(11) -0.0005(9) Cl2 0.0644(12) 0.0510(11) 0.0654(12) -0.0090(9) 0.0231(10) -0.0154(9) P1 0.0354(9) 0.0437(9) 0.0375(9) -0.0018(7) 0.0151(7) 0.0042(7) P2 0.0329(8) 0.0418(9) 0.0407(9) 0.0019(7) 0.0151(7) 0.0023(7) N1 0.035(3) 0.061(4) 0.035(3) 0.003(2) 0.016(2) 0.007(3) N2 0.033(3) 0.056(3) 0.037(3) 0.002(2) 0.012(2) 0.000(2) C1 0.038(4) 0.086(6) 0.040(4) 0.009(4) 0.015(3) 0.015(4) C2 0.037(4) 0.092(6) 0.033(4) -0.003(4) 0.012(3) 0.006(4) C3 0.039(4) 0.051(4) 0.046(4) 0.006(3) 0.020(3) -0.002(3) C4 0.057(5) 0.050(4) 0.061(5) 0.002(4) 0.022(4) -0.001(4) C5 0.084(6) 0.049(5) 0.091(7) 0.003(4) 0.046(6) -0.004(4) C6 0.088(7) 0.071(7) 0.109(8) 0.033(6) 0.038(7) -0.010(5) C7 0.116(9) 0.094(8) 0.115(9) 0.025(7) 0.084(8) 0.006(7) C8 0.083(6) 0.067(6) 0.100(7) 0.024(5) 0.063(6) 0.015(5) C9 0.034(3) 0.053(4) 0.041(4) -0.004(3) 0.009(3) 0.010(3) C10 0.049(5) 0.068(5) 0.058(5) 0.004(4) 0.010(4) -0.008(4) C11 0.048(5) 0.086(7) 0.088(7) -0.012(6) 0.002(5) -0.022(5) C12 0.057(5) 0.079(6) 0.053(5) -0.011(4) 0.003(4) 0.008(5) C13 0.062(5) 0.076(6) 0.058(5) 0.008(4) 0.019(4) 0.020(5) C14 0.040(4) 0.067(5) 0.050(4) 0.016(4) 0.015(3) 0.008(3) C15 0.047(4) 0.051(4) 0.052(4) -0.005(3) 0.029(4) -0.002(3) C16 0.069(6) 0.061(5) 0.078(6) -0.001(4) 0.024(5) 0.020(4) C17 0.085(7) 0.076(6) 0.091(8) 0.001(5) 0.033(6) 0.034(5) C18 0.103(8) 0.065(6) 0.094(8) -0.013(5) 0.068(7) -0.004(6) C19 0.070(6) 0.094(7) 0.091(7) -0.044(6) 0.040(6) -0.011(5) C20 0.052(5) 0.089(6) 0.061(5) -0.019(5) 0.018(4) 0.007(4) C21 0.047(4) 0.061(4) 0.036(4) -0.001(3) 0.018(3) 0.014(3) C22 0.060(5) 0.058(5) 0.051(4) -0.011(4) 0.025(4) -0.001(4) C23 0.069(5) 0.069(5) 0.050(5) -0.009(4) 0.016(4) 0.007(4) C24 0.105(8) 0.090(7) 0.050(5) 0.012(5) 0.033(6) 0.018(6) C25 0.117(9) 0.095(7) 0.062(6) -0.001(5) 0.051(6) -0.012(6) C26 0.076(6) 0.071(5) 0.060(5) -0.005(4) 0.044(5) -0.010(4) C27 0.046(4) 0.047(4) 0.037(3) 0.002(3) 0.015(3) -0.001(3) C28 0.067(5) 0.052(4) 0.058(5) 0.003(4) 0.028(4) 0.001(4) C29 0.115(9) 0.042(5) 0.079(7) -0.007(4) 0.042(6) -0.006(5) C30 0.091(8) 0.069(6) 0.064(6) 0.007(5) 0.016(5) -0.015(5) C31 0.056(5) 0.080(6) 0.066(6) 0.009(5) 0.006(4) -0.022(5) C32 0.049(4) 0.067(5) 0.048(4) 0.004(4) 0.008(4) -0.005(4) C33 0.033(3) 0.041(3) 0.041(4) -0.001(3) 0.015(3) 0.005(3) C34 0.103(7) 0.087(6) 0.047(5) 0.001(4) 0.024(5) 0.049(6) C35 0.121(9) 0.098(8) 0.098(8) -0.010(6) 0.044(7) 0.068(7) C36 0.056(5) 0.064(5) 0.066(6) 0.003(4) 0.014(4) 0.020(4) C37 0.077(6) 0.082(7) 0.071(6) 0.022(5) 0.018(5) 0.030(5) C38 0.086(6) 0.068(5) 0.056(5) 0.004(4) 0.025(5) 0.028(5) _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 1.987(6) . ? Ni1 N1 2.017(5) . ? Ni1 Cl1 2.248(2) . ? Ni1 Cl2 2.258(2) . ? P1 N1 1.585(5) . ? P1 C21 1.810(7) . ? P1 C27 1.815(7) . ? P1 C33 1.817(6) . ? P2 N2 1.590(6) . ? P2 C3 1.808(7) . ? P2 C9 1.809(7) . ? P2 C15 1.818(7) . ? N1 C1 1.481(8) . ? N2 C2 1.490(9) . ? C1 C2 1.514(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C8 1.376(10) . ? C3 C4 1.406(10) . ? C4 C5 1.341(11) . ? C4 H4 0.9300 . ? C5 C6 1.392(14) . ? C5 H5 0.9300 . ? C6 C7 1.394(14) . ? C6 H6 0.9300 . ? C7 C8 1.377(12) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C14 1.376(10) . ? C9 C10 1.384(10) . ? C10 C11 1.375(12) . ? C10 H10 0.9300 . ? C11 C12 1.355(14) . ? C11 H11 0.9300 . ? C12 C13 1.377(12) . ? C12 H12 0.9300 . ? C13 C14 1.395(11) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.370(10) . ? C15 C20 1.386(11) . ? C16 C17 1.360(12) . ? C16 H16 0.9300 . ? C17 C18 1.383(14) . ? C17 H17 0.9300 . ? C18 C19 1.371(14) . ? C18 H18 0.9300 . ? C19 C20 1.393(12) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C26 1.348(11) . ? C21 C22 1.394(10) . ? C22 C23 1.399(11) . ? C22 H22 0.9300 . ? C23 C24 1.353(13) . ? C23 H23 0.9300 . ? C24 C25 1.395(14) . ? C24 H24 0.9300 . ? C25 C26 1.407(12) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.372(10) . ? C27 C32 1.379(10) . ? C28 C29 1.413(12) . ? C28 H28 0.9300 . ? C29 C30 1.374(13) . ? C29 H29 0.9300 . ? C30 C31 1.375(13) . ? C30 H30 0.9300 . ? C31 C32 1.379(11) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.352(10) . ? C33 C38 1.362(10) . ? C34 C35 1.427(12) . ? C34 H34 0.9300 . ? C35 C36 1.314(13) . ? C35 H35 0.9300 . ? C36 C37 1.331(12) . ? C36 H36 0.9300 . ? C37 C38 1.435(11) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? Cl10 C40 1.66(2) . ? Cl11 C40 1.68(3) 4_455 ? C40 Cl11 1.68(3) 4_656 ? Cl12 C41 1.53(2) 4_556 ? Cl12 Cl13 2.44(2) 2_645 ? Cl13 C41 1.52(3) 3_655 ? Cl13 Cl12 2.44(2) 2_655 ? C41 Cl13 1.52(3) 3_655 ? C41 Cl12 1.53(2) 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 86.0(2) . . ? N2 Ni1 Cl1 113.01(18) . . ? N1 Ni1 Cl1 107.20(17) . . ? N2 Ni1 Cl2 108.82(17) . . ? N1 Ni1 Cl2 112.40(18) . . ? Cl1 Ni1 Cl2 123.23(9) . . ? N1 P1 C21 108.9(3) . . ? N1 P1 C27 113.4(3) . . ? C21 P1 C27 107.5(3) . . ? N1 P1 C33 115.6(3) . . ? C21 P1 C33 107.2(3) . . ? C27 P1 C33 103.7(3) . . ? N2 P2 C3 112.7(3) . . ? N2 P2 C9 107.4(3) . . ? C3 P2 C9 108.8(3) . . ? N2 P2 C15 115.1(3) . . ? C3 P2 C15 105.3(3) . . ? C9 P2 C15 107.2(3) . . ? C1 N1 P1 120.6(4) . . ? C1 N1 Ni1 108.7(4) . . ? P1 N1 Ni1 130.3(3) . . ? C2 N2 P2 117.9(4) . . ? C2 N2 Ni1 109.3(4) . . ? P2 N2 Ni1 132.5(3) . . ? N1 C1 C2 109.4(6) . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 109.2(6) . . ? N2 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? N2 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? C8 C3 C4 117.8(7) . . ? C8 C3 P2 124.5(6) . . ? C4 C3 P2 117.7(5) . . ? C5 C4 C3 121.4(8) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 119.8(9) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 120.6(9) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C8 C7 C6 117.9(9) . . ? C8 C7 H7 121.0 . . ? C6 C7 H7 121.0 . . ? C3 C8 C7 122.2(9) . . ? C3 C8 H8 118.9 . . ? C7 C8 H8 118.9 . . ? C14 C9 C10 119.7(7) . . ? C14 C9 P2 119.1(5) . . ? C10 C9 P2 121.1(6) . . ? C11 C10 C9 119.7(8) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C12 C11 C10 121.0(8) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 120.1(8) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C14 119.6(8) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C9 C14 C13 119.7(7) . . ? C9 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C16 C15 C20 117.4(7) . . ? C16 C15 P2 121.8(6) . . ? C20 C15 P2 120.7(6) . . ? C17 C16 C15 122.3(9) . . ? C17 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C16 C17 C18 120.0(9) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 119.8(9) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 119.1(9) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C15 C20 C19 121.4(9) . . ? C15 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C26 C21 C22 120.5(7) . . ? C26 C21 P1 121.3(6) . . ? C22 C21 P1 118.3(6) . . ? C21 C22 C23 119.4(8) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C24 C23 C22 120.7(9) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 119.7(9) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C24 C25 C26 119.9(9) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C21 C26 C25 119.9(9) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C32 117.9(7) . . ? C28 C27 P1 118.9(6) . . ? C32 C27 P1 123.2(6) . . ? C27 C28 C29 120.1(8) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.8(9) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 118.8(9) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? C30 C31 C32 119.9(9) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C31 C32 C27 122.5(9) . . ? C31 C32 H32 118.8 . . ? C27 C32 H32 118.8 . . ? C34 C33 C38 118.1(7) . . ? C34 C33 P1 122.6(6) . . ? C38 C33 P1 119.3(5) . . ? C33 C34 C35 119.3(8) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C36 C35 C34 123.2(9) . . ? C36 C35 H35 118.4 . . ? C34 C35 H35 118.4 . . ? C35 C36 C37 118.1(8) . . ? C35 C36 H36 120.9 . . ? C37 C36 H36 120.9 . . ? C36 C37 C38 121.1(9) . . ? C36 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? C33 C38 C37 120.2(8) . . ? C33 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? Cl10 C40 Cl11 106.6(14) . 4_656 ? C41 Cl12 Cl13 37.0(9) 4_556 2_645 ? C41 Cl13 Cl12 37.3(10) 3_655 2_655 ? Cl13 C41 Cl12 105.7(16) 3_655 4 ? 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 C21 P1 N1 C1 179.4(6) . . . . ? C27 P1 N1 C1 -61.0(7) . . . . ? C33 P1 N1 C1 58.6(7) . . . . ? C21 P1 N1 Ni1 -8.3(6) . . . . ? C27 P1 N1 Ni1 111.4(4) . . . . ? C33 P1 N1 Ni1 -129.1(4) . . . . ? N2 Ni1 N1 C1 12.0(5) . . . . ? Cl1 Ni1 N1 C1 124.8(5) . . . . ? Cl2 Ni1 N1 C1 -96.7(5) . . . . ? N2 Ni1 N1 P1 -161.0(5) . . . . ? Cl1 Ni1 N1 P1 -48.2(5) . . . . ? Cl2 Ni1 N1 P1 90.2(4) . . . . ? C3 P2 N2 C2 -64.7(6) . . . . ? C9 P2 N2 C2 175.4(5) . . . . ? C15 P2 N2 C2 56.2(6) . . . . ? C3 P2 N2 Ni1 107.3(5) . . . . ? C9 P2 N2 Ni1 -12.6(5) . . . . ? C15 P2 N2 Ni1 -131.9(4) . . . . ? N1 Ni1 N2 C2 13.3(5) . . . . ? Cl1 Ni1 N2 C2 -93.7(5) . . . . ? Cl2 Ni1 N2 C2 125.6(4) . . . . ? N1 Ni1 N2 P2 -159.2(5) . . . . ? Cl1 Ni1 N2 P2 93.8(4) . . . . ? Cl2 Ni1 N2 P2 -46.9(5) . . . . ? P1 N1 C1 C2 139.3(6) . . . . ? Ni1 N1 C1 C2 -34.5(8) . . . . ? P2 N2 C2 C1 138.2(6) . . . . ? Ni1 N2 C2 C1 -35.5(7) . . . . ? N1 C1 C2 N2 46.5(9) . . . . ? N2 P2 C3 C8 140.5(7) . . . . ? C9 P2 C3 C8 -100.5(7) . . . . ? C15 P2 C3 C8 14.1(8) . . . . ? N2 P2 C3 C4 -40.8(7) . . . . ? C9 P2 C3 C4 78.2(6) . . . . ? C15 P2 C3 C4 -167.1(6) . . . . ? C8 C3 C4 C5 0.0(12) . . . . ? P2 C3 C4 C5 -178.9(7) . . . . ? C3 C4 C5 C6 -3.4(14) . . . . ? C4 C5 C6 C7 3.4(16) . . . . ? C5 C6 C7 C8 0.0(17) . . . . ? C4 C3 C8 C7 3.7(14) . . . . ? P2 C3 C8 C7 -177.5(8) . . . . ? C6 C7 C8 C3 -3.6(17) . . . . ? N2 P2 C9 C14 -44.8(6) . . . . ? C3 P2 C9 C14 -167.1(6) . . . . ? C15 P2 C9 C14 79.4(6) . . . . ? N2 P2 C9 C10 137.5(6) . . . . ? C3 P2 C9 C10 15.2(7) . . . . ? C15 P2 C9 C10 -98.3(7) . . . . ? C14 C9 C10 C11 1.4(12) . . . . ? P2 C9 C10 C11 179.2(7) . . . . ? C9 C10 C11 C12 -0.4(15) . . . . ? C10 C11 C12 C13 1.4(15) . . . . ? C11 C12 C13 C14 -3.6(14) . . . . ? C10 C9 C14 C13 -3.6(11) . . . . ? P2 C9 C14 C13 178.7(6) . . . . ? C12 C13 C14 C9 4.7(12) . . . . ? N2 P2 C15 C16 115.1(7) . . . . ? C3 P2 C15 C16 -120.1(7) . . . . ? C9 P2 C15 C16 -4.2(8) . . . . ? N2 P2 C15 C20 -61.4(7) . . . . ? C3 P2 C15 C20 63.4(7) . . . . ? C9 P2 C15 C20 179.2(7) . . . . ? C20 C15 C16 C17 0.6(13) . . . . ? P2 C15 C16 C17 -176.0(8) . . . . ? C15 C16 C17 C18 -0.2(16) . . . . ? C16 C17 C18 C19 1.5(16) . . . . ? C17 C18 C19 C20 -3.1(15) . . . . ? C16 C15 C20 C19 -2.4(13) . . . . ? P2 C15 C20 C19 174.3(7) . . . . ? C18 C19 C20 C15 3.6(15) . . . . ? N1 P1 C21 C26 129.7(7) . . . . ? C27 P1 C21 C26 6.4(8) . . . . ? C33 P1 C21 C26 -104.5(7) . . . . ? N1 P1 C21 C22 -50.4(7) . . . . ? C27 P1 C21 C22 -173.7(6) . . . . ? C33 P1 C21 C22 75.4(6) . . . . ? C26 C21 C22 C23 -1.9(12) . . . . ? P1 C21 C22 C23 178.3(6) . . . . ? C21 C22 C23 C24 1.7(13) . . . . ? C22 C23 C24 C25 -1.0(15) . . . . ? C23 C24 C25 C26 0.4(16) . . . . ? C22 C21 C26 C25 1.3(13) . . . . ? P1 C21 C26 C25 -178.8(7) . . . . ? C24 C25 C26 C21 -0.6(15) . . . . ? N1 P1 C27 C28 -27.1(7) . . . . ? C21 P1 C27 C28 93.3(6) . . . . ? C33 P1 C27 C28 -153.3(6) . . . . ? N1 P1 C27 C32 153.2(6) . . . . ? C21 P1 C27 C32 -86.4(7) . . . . ? C33 P1 C27 C32 27.0(7) . . . . ? C32 C27 C28 C29 1.4(11) . . . . ? P1 C27 C28 C29 -178.3(6) . . . . ? C27 C28 C29 C30 -2.3(13) . . . . ? C28 C29 C30 C31 3.1(14) . . . . ? C29 C30 C31 C32 -2.9(14) . . . . ? C30 C31 C32 C27 2.1(13) . . . . ? C28 C27 C32 C31 -1.3(11) . . . . ? P1 C27 C32 C31 178.4(7) . . . . ? N1 P1 C33 C34 125.1(7) . . . . ? C21 P1 C33 C34 3.4(8) . . . . ? C27 P1 C33 C34 -110.1(7) . . . . ? N1 P1 C33 C38 -57.8(7) . . . . ? C21 P1 C33 C38 -179.5(7) . . . . ? C27 P1 C33 C38 67.0(7) . . . . ? C38 C33 C34 C35 -0.1(14) . . . . ? P1 C33 C34 C35 177.1(8) . . . . ? C33 C34 C35 C36 0.8(19) . . . . ? C34 C35 C36 C37 0.2(19) . . . . ? C35 C36 C37 C38 -1.7(16) . . . . ? C34 C33 C38 C37 -1.5(13) . . . . ? P1 C33 C38 C37 -178.7(7) . . . . ? C36 C37 C38 C33 2.4(16) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.97 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.726 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.163