# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Zhong-Xia Wang' _publ_contact_author_address ; Chemistry University of Science and Technology of China 96 Jinzhai Road Hefei 230026 CHINA ; _publ_contact_author_email ZXWANG@USTC.EDU.CN _publ_section_title ; Amido Pincer Complex of Nickel-Catalysed Kumada Cross-Coupling Reactions ; loop_ _publ_author_name 'Zhong-Xia Wang.' 'Li Wang.' data_51225h _database_code_depnum_ccdc_archive 'CCDC 632195' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H39 N Ni P2' _chemical_formula_weight 630.35 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3992(18) _cell_length_b 9.5847(18) _cell_length_c 19.157(4) _cell_angle_alpha 98.680(3) _cell_angle_beta 98.408(3) _cell_angle_gamma 94.569(3) _cell_volume 1678.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5359 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 26.50 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.875174 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 8543 _diffrn_reflns_av_R_equivalents 0.0142 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5864 _reflns_number_gt 4858 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.4658P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5864 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0866 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.004 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.16233(3) 0.31238(3) 0.270809(12) 0.03396(9) Uani 1 1 d . . . P1 P 0.10341(5) 0.21326(5) 0.16032(2) 0.03273(12) Uani 1 1 d . . . P2 P 0.24778(6) 0.40326(6) 0.38151(3) 0.04082(14) Uani 1 1 d . . . N1 N 0.29872(18) 0.17037(17) 0.27995(8) 0.0365(4) Uani 1 1 d . . . C1 C 0.0241(2) 0.4456(2) 0.26088(11) 0.0436(5) Uani 1 1 d . . . C2 C -0.1080(3) 0.4230(3) 0.28456(14) 0.0674(7) Uani 1 1 d . . . H2 H -0.1244 0.3456 0.3074 0.081 Uiso 1 1 calc R . . C3 C -0.2153(4) 0.5123(5) 0.27500(18) 0.1096(15) Uani 1 1 d . . . H3 H -0.3028 0.4932 0.2907 0.131 Uiso 1 1 calc R . . C4 C -0.1941(6) 0.6285(6) 0.2427(2) 0.129(2) Uani 1 1 d . . . H4 H -0.2664 0.6884 0.2362 0.155 Uiso 1 1 calc R . . C5 C -0.0644(6) 0.6553(3) 0.21995(18) 0.1044(14) Uani 1 1 d . . . H5 H -0.0483 0.7351 0.1989 0.125 Uiso 1 1 calc R . . C6 C 0.0439(3) 0.5643(3) 0.22795(13) 0.0634(7) Uani 1 1 d . . . H6 H 0.1301 0.5833 0.2111 0.076 Uiso 1 1 calc R . . C7 C -0.0855(2) 0.1471(2) 0.12751(10) 0.0382(5) Uani 1 1 d . . . C8 C -0.1353(3) 0.0037(2) 0.11735(13) 0.0539(6) Uani 1 1 d . . . H8 H -0.0698 -0.0631 0.1229 0.065 Uiso 1 1 calc R . . C9 C -0.2821(3) -0.0401(3) 0.09890(16) 0.0715(8) Uani 1 1 d . . . H9 H -0.3142 -0.1362 0.0923 0.086 Uiso 1 1 calc R . . C10 C -0.3798(3) 0.0562(3) 0.09029(15) 0.0687(8) Uani 1 1 d . . . H10 H -0.4779 0.0258 0.0779 0.082 Uiso 1 1 calc R . . C11 C -0.3328(3) 0.1982(3) 0.09991(14) 0.0628(7) Uani 1 1 d . . . H11 H -0.3994 0.2639 0.0939 0.075 Uiso 1 1 calc R . . C12 C -0.1868(2) 0.2440(3) 0.11845(12) 0.0497(5) Uani 1 1 d . . . H12 H -0.1561 0.3404 0.1249 0.060 Uiso 1 1 calc R . . C13 C 0.1634(2) 0.3111(2) 0.09362(11) 0.0381(5) Uani 1 1 d . . . C14 C 0.2998(3) 0.3870(3) 0.11146(15) 0.0584(6) Uani 1 1 d . . . H14 H 0.3545 0.3885 0.1562 0.070 Uiso 1 1 calc R . . C15 C 0.3536(3) 0.4604(3) 0.0622(2) 0.0782(9) Uani 1 1 d . . . H15 H 0.4451 0.5105 0.0737 0.094 Uiso 1 1 calc R . . C16 C 0.2714(4) 0.4593(3) -0.00392(19) 0.0809(10) Uani 1 1 d . . . H16 H 0.3081 0.5081 -0.0369 0.097 Uiso 1 1 calc R . . C17 C 0.1375(4) 0.3873(3) -0.02095(15) 0.0745(8) Uani 1 1 d . . . H17 H 0.0825 0.3878 -0.0654 0.089 Uiso 1 1 calc R . . C18 C 0.0824(3) 0.3133(3) 0.02743(12) 0.0530(6) Uani 1 1 d . . . H18 H -0.0097 0.2647 0.0154 0.064 Uiso 1 1 calc R . . C19 C 0.2057(2) 0.0615(2) 0.15877(10) 0.0351(4) Uani 1 1 d . . . C20 C 0.2026(2) -0.0427(2) 0.09893(11) 0.0428(5) Uani 1 1 d . . . H20 H 0.1554 -0.0300 0.0545 0.051 Uiso 1 1 calc R . . C21 C 0.2688(2) -0.1640(2) 0.10521(12) 0.0498(6) Uani 1 1 d . . . H21 H 0.2691 -0.2324 0.0653 0.060 Uiso 1 1 calc R . . C22 C 0.3349(3) -0.1820(2) 0.17237(13) 0.0521(6) Uani 1 1 d . . . H22 H 0.3750 -0.2662 0.1775 0.062 Uiso 1 1 calc R . . C23 C 0.3432(2) -0.0786(2) 0.23186(12) 0.0461(5) Uani 1 1 d . . . H23 H 0.3864 -0.0952 0.2763 0.055 Uiso 1 1 calc R . . C24 C 0.2867(2) 0.0519(2) 0.22600(10) 0.0356(4) Uani 1 1 d . . . C25 C 0.4016(2) 0.1917(2) 0.34124(10) 0.0381(5) Uani 1 1 d . . . C26 C 0.5319(2) 0.1119(2) 0.34857(11) 0.0413(5) Uani 1 1 d . . . C27 C 0.6246(3) 0.1048(3) 0.29853(13) 0.0544(6) Uani 1 1 d . . . H27 H 0.6060 0.1498 0.2589 0.065 Uiso 1 1 calc R . . C28 C 0.7450(3) 0.0308(3) 0.30738(18) 0.0756(8) Uani 1 1 d . . . H28 H 0.8071 0.0267 0.2737 0.091 Uiso 1 1 calc R . . C29 C 0.7735(3) -0.0366(3) 0.3657(2) 0.0829(10) Uani 1 1 d . . . H29 H 0.8532 -0.0879 0.3707 0.099 Uiso 1 1 calc R . . C30 C 0.6846(3) -0.0280(3) 0.41593(17) 0.0752(8) Uani 1 1 d . . . H30 H 0.7051 -0.0717 0.4559 0.090 Uiso 1 1 calc R . . C31 C 0.5642(3) 0.0454(3) 0.40789(13) 0.0564(6) Uani 1 1 d . . . H31 H 0.5040 0.0504 0.4425 0.068 Uiso 1 1 calc R . . C32 C 0.3924(2) 0.2975(2) 0.39574(11) 0.0460(5) Uani 1 1 d . . . H32 H 0.4582 0.3134 0.4381 0.055 Uiso 1 1 calc R . . C33 C 0.3327(3) 0.5883(3) 0.40124(13) 0.0581(6) Uani 1 1 d . . . H33 H 0.3993 0.5988 0.4466 0.070 Uiso 1 1 calc R . . C34 C 0.4232(3) 0.6137(3) 0.34351(17) 0.0765(8) Uani 1 1 d . . . H34A H 0.3604 0.6110 0.2989 0.115 Uiso 1 1 calc R . . H34B H 0.4875 0.5412 0.3383 0.115 Uiso 1 1 calc R . . H34C H 0.4785 0.7049 0.3570 0.115 Uiso 1 1 calc R . . C35 C 0.2252(4) 0.6985(3) 0.41048(18) 0.0881(10) Uani 1 1 d . . . H35A H 0.2760 0.7920 0.4197 0.132 Uiso 1 1 calc R . . H35B H 0.1765 0.6845 0.4500 0.132 Uiso 1 1 calc R . . H35C H 0.1556 0.6883 0.3676 0.132 Uiso 1 1 calc R . . C36 C 0.1349(3) 0.3831(3) 0.45091(12) 0.0598(7) Uani 1 1 d . . . H36 H 0.0570 0.4446 0.4451 0.072 Uiso 1 1 calc R . . C37 C 0.0664(3) 0.2298(4) 0.43825(17) 0.0887(10) Uani 1 1 d . . . H37A H 0.1410 0.1674 0.4424 0.133 Uiso 1 1 calc R . . H37B H 0.0103 0.2075 0.3912 0.133 Uiso 1 1 calc R . . H37C H 0.0048 0.2181 0.4732 0.133 Uiso 1 1 calc R . . C38 C 0.2182(3) 0.4253(4) 0.52712(13) 0.0867(10) Uani 1 1 d . . . H38A H 0.1564 0.4045 0.5607 0.130 Uiso 1 1 calc R . . H38B H 0.2497 0.5250 0.5359 0.130 Uiso 1 1 calc R . . H38C H 0.3008 0.3728 0.5326 0.130 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.03641(15) 0.03699(15) 0.02579(14) 0.00214(10) -0.00173(10) 0.00574(10) P1 0.0357(3) 0.0343(3) 0.0257(2) 0.0035(2) -0.0019(2) 0.0043(2) P2 0.0403(3) 0.0502(3) 0.0275(3) -0.0026(2) -0.0017(2) 0.0080(2) N1 0.0414(9) 0.0373(9) 0.0276(8) 0.0028(7) -0.0038(7) 0.0064(7) C1 0.0486(13) 0.0478(12) 0.0309(11) -0.0024(9) -0.0007(9) 0.0134(10) C2 0.0557(15) 0.098(2) 0.0490(14) 0.0051(14) 0.0072(12) 0.0275(15) C3 0.076(2) 0.188(4) 0.066(2) -0.006(2) 0.0080(17) 0.077(3) C4 0.156(4) 0.154(4) 0.073(2) -0.017(2) -0.016(3) 0.122(4) C5 0.180(4) 0.0634(19) 0.062(2) 0.0021(15) -0.021(2) 0.061(2) C6 0.091(2) 0.0482(14) 0.0471(14) 0.0048(11) -0.0045(13) 0.0170(13) C7 0.0388(11) 0.0454(12) 0.0286(10) 0.0075(9) -0.0008(8) 0.0017(9) C8 0.0492(13) 0.0485(13) 0.0622(15) 0.0119(11) 0.0027(11) -0.0004(11) C9 0.0545(16) 0.0642(17) 0.089(2) 0.0101(15) 0.0044(15) -0.0169(13) C10 0.0393(14) 0.092(2) 0.0689(17) 0.0121(15) 0.0003(12) -0.0097(14) C11 0.0423(13) 0.0821(19) 0.0636(16) 0.0151(14) -0.0002(12) 0.0131(13) C12 0.0443(12) 0.0528(13) 0.0493(13) 0.0100(11) -0.0036(10) 0.0059(10) C13 0.0445(12) 0.0351(10) 0.0360(11) 0.0052(8) 0.0092(9) 0.0086(9) C14 0.0485(14) 0.0614(15) 0.0671(16) 0.0122(13) 0.0147(12) 0.0035(12) C15 0.0638(18) 0.0629(17) 0.121(3) 0.0250(18) 0.0475(19) 0.0073(14) C16 0.107(3) 0.0727(19) 0.093(2) 0.0480(18) 0.062(2) 0.0411(19) C17 0.103(2) 0.083(2) 0.0522(16) 0.0325(15) 0.0275(16) 0.0336(18) C18 0.0668(16) 0.0557(14) 0.0371(12) 0.0116(10) 0.0046(11) 0.0082(12) C19 0.0376(10) 0.0339(10) 0.0317(10) 0.0036(8) -0.0002(8) 0.0043(8) C20 0.0460(12) 0.0448(12) 0.0325(11) -0.0006(9) -0.0033(9) 0.0045(9) C21 0.0544(14) 0.0397(12) 0.0483(13) -0.0076(10) 0.0003(11) 0.0068(10) C22 0.0567(14) 0.0346(11) 0.0599(15) 0.0031(10) -0.0041(12) 0.0085(10) C23 0.0519(13) 0.0378(11) 0.0443(12) 0.0075(9) -0.0066(10) 0.0047(10) C24 0.0370(10) 0.0348(10) 0.0330(10) 0.0054(8) -0.0002(8) 0.0025(8) C25 0.0392(11) 0.0437(11) 0.0303(10) 0.0079(9) -0.0008(8) 0.0059(9) C26 0.0412(11) 0.0423(11) 0.0357(11) 0.0027(9) -0.0054(9) 0.0033(9) C27 0.0509(14) 0.0607(15) 0.0492(13) 0.0052(11) 0.0036(11) 0.0067(11) C28 0.0507(16) 0.085(2) 0.086(2) -0.0082(17) 0.0141(15) 0.0142(14) C29 0.0596(18) 0.0730(19) 0.104(3) -0.0061(18) -0.0184(18) 0.0285(15) C30 0.077(2) 0.0683(18) 0.0738(19) 0.0157(15) -0.0226(16) 0.0252(15) C31 0.0607(15) 0.0620(15) 0.0449(13) 0.0137(11) -0.0053(11) 0.0133(12) C32 0.0432(12) 0.0592(13) 0.0302(11) -0.0004(10) -0.0078(9) 0.0119(10) C33 0.0565(15) 0.0553(14) 0.0500(14) -0.0106(11) -0.0114(12) 0.0034(12) C34 0.0667(18) 0.0706(18) 0.087(2) 0.0154(16) 0.0028(16) -0.0092(14) C35 0.097(2) 0.0633(18) 0.089(2) -0.0231(16) -0.0040(18) 0.0219(17) C36 0.0478(13) 0.097(2) 0.0353(12) 0.0096(12) 0.0058(10) 0.0169(13) C37 0.073(2) 0.127(3) 0.0692(19) 0.0379(19) 0.0090(16) -0.0121(19) C38 0.079(2) 0.147(3) 0.0324(13) 0.0055(16) 0.0054(13) 0.028(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 C1 1.903(2) . ? Ni1 N1 1.9521(16) . ? Ni1 P1 2.1577(6) . ? Ni1 P2 2.1758(6) . ? P1 C19 1.805(2) . ? P1 C13 1.821(2) . ? P1 C7 1.823(2) . ? P2 C32 1.773(2) . ? P2 C36 1.841(2) . ? P2 C33 1.846(2) . ? N1 C25 1.386(2) . ? N1 C24 1.400(2) . ? C1 C6 1.394(3) . ? C1 C2 1.395(3) . ? C2 C3 1.384(4) . ? C2 H2 0.9300 . ? C3 C4 1.369(7) . ? C3 H3 0.9300 . ? C4 C5 1.371(6) . ? C4 H4 0.9300 . ? C5 C6 1.399(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.391(3) . ? C7 C12 1.394(3) . ? C8 C9 1.388(3) . ? C8 H8 0.9300 . ? C9 C10 1.363(4) . ? C9 H9 0.9300 . ? C10 C11 1.373(4) . ? C10 H10 0.9300 . ? C11 C12 1.384(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.384(3) . ? C13 C14 1.392(3) . ? C14 C15 1.387(4) . ? C14 H14 0.9300 . ? C15 C16 1.382(4) . ? C15 H15 0.9300 . ? C16 C17 1.356(5) . ? C16 H16 0.9300 . ? C17 C18 1.382(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.398(3) . ? C19 C24 1.417(3) . ? C20 C21 1.374(3) . ? C20 H20 0.9300 . ? C21 C22 1.386(3) . ? C21 H21 0.9300 . ? C22 C23 1.381(3) . ? C22 H22 0.9300 . ? C23 C24 1.411(3) . ? C23 H23 0.9300 . ? C25 C32 1.359(3) . ? C25 C26 1.495(3) . ? C26 C27 1.384(3) . ? C26 C31 1.392(3) . ? C27 C28 1.386(4) . ? C27 H27 0.9300 . ? C28 C29 1.376(4) . ? C28 H28 0.9300 . ? C29 C30 1.362(5) . ? C29 H29 0.9300 . ? C30 C31 1.382(4) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.526(4) . ? C33 C35 1.529(4) . ? C33 H33 0.9800 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.526(4) . ? C36 C38 1.532(3) . ? C36 H36 0.9800 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ni1 N1 178.03(8) . . ? C1 Ni1 P1 92.37(6) . . ? N1 Ni1 P1 86.59(5) . . ? C1 Ni1 P2 93.94(6) . . ? N1 Ni1 P2 87.19(5) . . ? P1 Ni1 P2 172.95(2) . . ? C19 P1 C13 105.60(9) . . ? C19 P1 C7 107.36(9) . . ? C13 P1 C7 106.54(9) . . ? C19 P1 Ni1 101.06(6) . . ? C13 P1 Ni1 116.81(7) . . ? C7 P1 Ni1 118.24(7) . . ? C32 P2 C36 107.10(11) . . ? C32 P2 C33 105.21(11) . . ? C36 P2 C33 106.52(13) . . ? C32 P2 Ni1 98.83(7) . . ? C36 P2 Ni1 119.05(8) . . ? C33 P2 Ni1 118.38(8) . . ? C25 N1 C24 123.36(17) . . ? C25 N1 Ni1 117.35(13) . . ? C24 N1 Ni1 119.29(12) . . ? C6 C1 C2 116.7(2) . . ? C6 C1 Ni1 123.66(19) . . ? C2 C1 Ni1 119.60(19) . . ? C3 C2 C1 121.9(3) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C4 C3 C2 120.7(4) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 118.9(3) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 121.1(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C1 C6 C5 120.8(3) . . ? C1 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C8 C7 C12 118.1(2) . . ? C8 C7 P1 122.58(17) . . ? C12 C7 P1 119.04(16) . . ? C9 C8 C7 120.4(2) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 120.7(3) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 119.8(2) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 120.3(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 120.7(2) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? C18 C13 C14 119.1(2) . . ? C18 C13 P1 124.09(17) . . ? C14 C13 P1 116.80(17) . . ? C15 C14 C13 119.7(3) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C16 C15 C14 120.1(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 120.4(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.3(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 120.5(3) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? C20 C19 C24 121.50(18) . . ? C20 C19 P1 124.74(15) . . ? C24 C19 P1 113.68(14) . . ? C21 C20 C19 120.48(19) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 118.5(2) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? C23 C22 C21 122.0(2) . . ? C23 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C22 C23 C24 120.7(2) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? N1 C24 C23 126.93(18) . . ? N1 C24 C19 117.05(17) . . ? C23 C24 C19 115.99(18) . . ? C32 C25 N1 119.52(18) . . ? C32 C25 C26 117.09(18) . . ? N1 C25 C26 123.16(18) . . ? C27 C26 C31 118.5(2) . . ? C27 C26 C25 121.70(19) . . ? C31 C26 C25 119.8(2) . . ? C26 C27 C28 120.1(3) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 120.5(3) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C30 C29 C28 119.8(3) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 120.4(3) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C26 120.7(3) . . ? C30 C31 H31 119.7 . . ? C26 C31 H31 119.7 . . ? C25 C32 P2 116.20(15) . . ? C25 C32 H32 121.9 . . ? P2 C32 H32 121.9 . . ? C34 C33 C35 111.8(2) . . ? C34 C33 P2 109.10(17) . . ? C35 C33 P2 113.76(19) . . ? C34 C33 H33 107.3 . . ? C35 C33 H33 107.3 . . ? P2 C33 H33 107.3 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C38 111.0(2) . . ? C37 C36 P2 108.38(19) . . ? C38 C36 P2 113.27(19) . . ? C37 C36 H36 108.0 . . ? C38 C36 H36 108.0 . . ? P2 C36 H36 108.0 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ni1 P1 C19 -172.19(9) . . . . ? N1 Ni1 P1 C19 6.13(8) . . . . ? P2 Ni1 P1 C19 34.3(2) . . . . ? C1 Ni1 P1 C13 73.87(10) . . . . ? N1 Ni1 P1 C13 -107.82(9) . . . . ? P2 Ni1 P1 C13 -79.7(2) . . . . ? C1 Ni1 P1 C7 -55.44(10) . . . . ? N1 Ni1 P1 C7 122.88(9) . . . . ? P2 Ni1 P1 C7 151.04(19) . . . . ? C1 Ni1 P2 C32 -174.75(11) . . . . ? N1 Ni1 P2 C32 6.87(9) . . . . ? P1 Ni1 P2 C32 -21.3(2) . . . . ? C1 Ni1 P2 C36 69.99(13) . . . . ? N1 Ni1 P2 C36 -108.38(12) . . . . ? P1 Ni1 P2 C36 -136.5(2) . . . . ? C1 Ni1 P2 C33 -62.06(12) . . . . ? N1 Ni1 P2 C33 119.56(11) . . . . ? P1 Ni1 P2 C33 91.4(2) . . . . ? C1 Ni1 N1 C25 -134(2) . . . . ? P1 Ni1 N1 C25 167.33(14) . . . . ? P2 Ni1 N1 C25 -9.34(14) . . . . ? C1 Ni1 N1 C24 44(2) . . . . ? P1 Ni1 N1 C24 -13.99(14) . . . . ? P2 Ni1 N1 C24 169.33(14) . . . . ? N1 Ni1 C1 C6 -135(2) . . . . ? P1 Ni1 C1 C6 -76.97(18) . . . . ? P2 Ni1 C1 C6 99.89(18) . . . . ? N1 Ni1 C1 C2 42(2) . . . . ? P1 Ni1 C1 C2 100.13(18) . . . . ? P2 Ni1 C1 C2 -83.02(18) . . . . ? C6 C1 C2 C3 1.0(4) . . . . ? Ni1 C1 C2 C3 -176.3(2) . . . . ? C1 C2 C3 C4 -1.1(5) . . . . ? C2 C3 C4 C5 -0.1(6) . . . . ? C3 C4 C5 C6 1.4(6) . . . . ? C2 C1 C6 C5 0.3(3) . . . . ? Ni1 C1 C6 C5 177.5(2) . . . . ? C4 C5 C6 C1 -1.6(5) . . . . ? C19 P1 C7 C8 10.7(2) . . . . ? C13 P1 C7 C8 123.42(19) . . . . ? Ni1 P1 C7 C8 -102.66(18) . . . . ? C19 P1 C7 C12 -175.47(16) . . . . ? C13 P1 C7 C12 -62.71(18) . . . . ? Ni1 P1 C7 C12 71.20(18) . . . . ? C12 C7 C8 C9 -0.2(3) . . . . ? P1 C7 C8 C9 173.8(2) . . . . ? C7 C8 C9 C10 0.1(4) . . . . ? C8 C9 C10 C11 0.0(4) . . . . ? C9 C10 C11 C12 -0.1(4) . . . . ? C10 C11 C12 C7 0.1(4) . . . . ? C8 C7 C12 C11 0.0(3) . . . . ? P1 C7 C12 C11 -174.11(19) . . . . ? C19 P1 C13 C18 105.77(19) . . . . ? C7 P1 C13 C18 -8.2(2) . . . . ? Ni1 P1 C13 C18 -142.87(17) . . . . ? C19 P1 C13 C14 -73.96(18) . . . . ? C7 P1 C13 C14 172.08(17) . . . . ? Ni1 P1 C13 C14 37.40(19) . . . . ? C18 C13 C14 C15 -1.6(3) . . . . ? P1 C13 C14 C15 178.15(19) . . . . ? C13 C14 C15 C16 0.7(4) . . . . ? C14 C15 C16 C17 0.5(4) . . . . ? C15 C16 C17 C18 -0.6(4) . . . . ? C16 C17 C18 C13 -0.4(4) . . . . ? C14 C13 C18 C17 1.5(3) . . . . ? P1 C13 C18 C17 -178.27(19) . . . . ? C13 P1 C19 C20 -60.0(2) . . . . ? C7 P1 C19 C20 53.4(2) . . . . ? Ni1 P1 C19 C20 177.87(17) . . . . ? C13 P1 C19 C24 123.01(15) . . . . ? C7 P1 C19 C24 -123.60(15) . . . . ? Ni1 P1 C19 C24 0.88(16) . . . . ? C24 C19 C20 C21 5.5(3) . . . . ? P1 C19 C20 C21 -171.26(17) . . . . ? C19 C20 C21 C22 1.7(3) . . . . ? C20 C21 C22 C23 -3.7(4) . . . . ? C21 C22 C23 C24 -1.5(4) . . . . ? C25 N1 C24 C23 18.9(3) . . . . ? Ni1 N1 C24 C23 -159.65(17) . . . . ? C25 N1 C24 C19 -163.14(18) . . . . ? Ni1 N1 C24 C19 18.3(2) . . . . ? C22 C23 C24 N1 -173.8(2) . . . . ? C22 C23 C24 C19 8.2(3) . . . . ? C20 C19 C24 N1 171.59(18) . . . . ? P1 C19 C24 N1 -11.3(2) . . . . ? C20 C19 C24 C23 -10.3(3) . . . . ? P1 C19 C24 C23 166.83(16) . . . . ? C24 N1 C25 C32 -170.04(19) . . . . ? Ni1 N1 C25 C32 8.6(3) . . . . ? C24 N1 C25 C26 15.5(3) . . . . ? Ni1 N1 C25 C26 -165.84(15) . . . . ? C32 C25 C26 C27 -121.9(2) . . . . ? N1 C25 C26 C27 52.6(3) . . . . ? C32 C25 C26 C31 56.4(3) . . . . ? N1 C25 C26 C31 -129.0(2) . . . . ? C31 C26 C27 C28 1.1(3) . . . . ? C25 C26 C27 C28 179.4(2) . . . . ? C26 C27 C28 C29 0.2(4) . . . . ? C27 C28 C29 C30 -1.5(5) . . . . ? C28 C29 C30 C31 1.5(5) . . . . ? C29 C30 C31 C26 -0.2(4) . . . . ? C27 C26 C31 C30 -1.1(4) . . . . ? C25 C26 C31 C30 -179.5(2) . . . . ? N1 C25 C32 P2 -1.5(3) . . . . ? C26 C25 C32 P2 173.22(16) . . . . ? C36 P2 C32 C25 119.31(19) . . . . ? C33 P2 C32 C25 -127.61(19) . . . . ? Ni1 P2 C32 C25 -4.88(19) . . . . ? C32 P2 C33 C34 68.9(2) . . . . ? C36 P2 C33 C34 -177.61(18) . . . . ? Ni1 P2 C33 C34 -40.2(2) . . . . ? C32 P2 C33 C35 -165.6(2) . . . . ? C36 P2 C33 C35 -52.1(2) . . . . ? Ni1 P2 C33 C35 85.3(2) . . . . ? C32 P2 C36 C37 -65.8(2) . . . . ? C33 P2 C36 C37 -178.04(18) . . . . ? Ni1 P2 C36 C37 44.9(2) . . . . ? C32 P2 C36 C38 57.7(2) . . . . ? C33 P2 C36 C38 -54.5(2) . . . . ? Ni1 P2 C36 C38 168.49(19) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.249 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.041 #============================================================================== data___R60416E _database_code_depnum_ccdc_archive 'CCDC 632196' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C44 H52 Cl N2 Ni P2 ' _chemical_formula_moiety 'C44 H52 Cl N2 Ni P2 ' _chemical_formula_weight 765.01 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 9.7247(4) _cell_length_b 12.8570(5) _cell_length_c 17.4756(7) _cell_angle_alpha 79.579(13) _cell_angle_beta 79.548(14) _cell_angle_gamma 77.064(11) _cell_volume 2071.64(20) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4085 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.1 _cell_measurement_temperature 294.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 810.00 _exptl_absorpt_coefficient_mu 0.642 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8759 _exptl_special_details ; ? ; #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 14358 _diffrn_reflns_av_R_equivalents 0.067 _diffrn_reflns_theta_max 26.37 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8380 _reflns_number_gt 5690 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1640 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 8380 _refine_ls_number_parameters 452 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0699P)^2^+0.1702P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.41 _refine_diff_density_min -0.55 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ni(1) Ni 0.68807(4) 0.21649(3) 0.27100(2) 0.04174(14) Uani 1.00 1 d . . . Cl(1) Cl 0.89410(10) 0.22130(8) 0.30344(6) 0.0572(2) Uani 1.00 1 d . . . P(1) P 0.75500(10) 0.04389(6) 0.28308(6) 0.0475(2) Uani 1.00 1 d . . . P(2) P 0.45128(10) 0.41394(8) 0.27099(6) 0.0477(2) Uani 1.00 1 d . . . N(1) N 0.5180(2) 0.1921(2) 0.23766(16) 0.0459(6) Uani 1.00 1 d . . . N(2) N 0.6214(2) 0.3734(2) 0.26882(14) 0.0421(6) Uani 1.00 1 d . . . C(1) C 0.8264(4) -0.0291(2) 0.3712(2) 0.0566(9) Uani 1.00 1 d . . . C(2) C 0.7640(6) 0.0038(4) 0.4419(2) 0.0925(16) Uani 1.00 1 d . . . C(3) C 0.8169(8) -0.0483(5) 0.5116(3) 0.118(2) Uani 1.00 1 d . . . C(4) C 0.9342(8) -0.1309(5) 0.5082(4) 0.117(2) Uani 1.00 1 d . . . C(5) C 0.9933(6) -0.1640(5) 0.4383(4) 0.120(2) Uani 1.00 1 d . . . C(6) C 0.9428(5) -0.1142(4) 0.3690(3) 0.0890(15) Uani 1.00 1 d . . . C(7) C 0.8792(3) -0.0087(2) 0.2018(2) 0.0523(8) Uani 1.00 1 d . . . C(8) C 1.0071(4) 0.0269(3) 0.1781(2) 0.0710(11) Uani 1.00 1 d . . . C(9) C 1.1061(5) -0.0123(5) 0.1171(3) 0.0993(17) Uani 1.00 1 d . . . C(10) C 1.0776(7) -0.0885(5) 0.0795(3) 0.114(2) Uani 1.00 1 d . . . C(11) C 0.9542(7) -0.1260(5) 0.1021(3) 0.113(2) Uani 1.00 1 d . . . C(12) C 0.8542(5) -0.0855(4) 0.1623(2) 0.0851(14) Uani 1.00 1 d . . . C(13) C 0.5898(4) 0.0028(2) 0.2850(2) 0.0550(9) Uani 1.00 1 d . . . C(14) C 0.4855(3) 0.0882(2) 0.2578(2) 0.0475(8) Uani 1.00 1 d . . . C(15) C 0.3499(4) 0.0675(3) 0.2557(2) 0.0634(10) Uani 1.00 1 d . . . C(16) C 0.3229(5) -0.0354(4) 0.2808(2) 0.0812(14) Uani 1.00 1 d . . . C(17) C 0.4267(5) -0.1185(3) 0.3079(3) 0.0914(16) Uani 1.00 1 d . . . C(18) C 0.5597(4) -0.0996(3) 0.3106(2) 0.0774(13) Uani 1.00 1 d . . . C(19) C 0.4421(3) 0.2648(2) 0.1835(2) 0.0466(8) Uani 1.00 1 d . . . C(20) C 0.4228(4) 0.2284(2) 0.1103(2) 0.0515(8) Uani 1.00 1 d . . . C(21) C 0.3014(4) 0.2680(3) 0.0752(2) 0.0718(12) Uani 1.00 1 d . . . C(22) C 0.2903(6) 0.2395(4) 0.0043(3) 0.0855(15) Uani 1.00 1 d . . . C(23) C 0.4006(6) 0.1730(4) -0.0328(2) 0.0915(16) Uani 1.00 1 d . . . C(24) C 0.5226(5) 0.1320(4) 0.0015(2) 0.0857(14) Uani 1.00 1 d . . . C(25) C 0.5343(4) 0.1585(3) 0.0726(2) 0.0668(11) Uani 1.00 1 d . . . C(26) C 0.3979(3) 0.3696(2) 0.1929(2) 0.0533(9) Uani 1.00 1 d . . . C(27) C 0.3555(4) 0.3631(3) 0.3671(2) 0.0651(10) Uani 1.00 1 d . . . C(28) C 0.2096(5) 0.3412(4) 0.3586(3) 0.1006(17) Uani 1.00 1 d . . . C(29) C 0.4392(5) 0.2650(3) 0.4141(2) 0.0731(12) Uani 1.00 1 d . . . C(30) C 0.3962(4) 0.5618(2) 0.2594(2) 0.0584(9) Uani 1.00 1 d . . . C(31) C 0.2364(5) 0.6029(4) 0.2840(3) 0.1036(18) Uani 1.00 1 d . . . C(32) C 0.4428(5) 0.6190(3) 0.1780(3) 0.0918(15) Uani 1.00 1 d . . . C(33) C 0.7201(3) 0.4450(2) 0.2419(2) 0.0457(8) Uani 1.00 1 d . . . C(34) C 0.7512(4) 0.5047(2) 0.2949(2) 0.0577(9) Uani 1.00 1 d . . . C(35) C 0.8466(5) 0.5735(4) 0.2660(3) 0.0863(15) Uani 1.00 1 d . . . C(36) C 0.9118(5) 0.5829(4) 0.1895(3) 0.1009(18) Uani 1.00 1 d . . . C(37) C 0.8848(5) 0.5217(4) 0.1395(3) 0.0824(14) Uani 1.00 1 d . . . C(38) C 0.7893(3) 0.4515(3) 0.1633(2) 0.0573(9) Uani 1.00 1 d . . . C(39) C 0.6877(4) 0.4929(3) 0.3815(2) 0.0648(10) Uani 1.00 1 d . . . C(40) C 0.6215(6) 0.5995(4) 0.4111(3) 0.113(2) Uani 1.00 1 d . . . C(41) C 0.7976(6) 0.4294(4) 0.4332(2) 0.1060(19) Uani 1.00 1 d . . . C(42) C 0.7667(4) 0.3843(3) 0.1051(2) 0.0686(11) Uani 1.00 1 d . . . C(43) C 0.7088(6) 0.4512(5) 0.0326(2) 0.1075(19) Uani 1.00 1 d . . . C(44) C 0.9029(6) 0.3074(4) 0.0781(3) 0.112(2) Uani 1.00 1 d . . . H(2) H 0.6861 0.0609 0.4437 0.111 Uiso 1.00 1 c R . . H(3) H 0.7729 -0.0270 0.5597 0.141 Uiso 1.00 1 c R . . H(4) H 0.9727 -0.1638 0.5537 0.140 Uiso 1.00 1 c R . . H(5) H 1.0702 -0.2219 0.4367 0.144 Uiso 1.00 1 c R . . H(6) H 0.9864 -0.1375 0.3215 0.107 Uiso 1.00 1 c R . . H(8) H 1.0269 0.0780 0.2038 0.085 Uiso 1.00 1 c R . . H(9) H 1.1909 0.0129 0.1017 0.119 Uiso 1.00 1 c R . . H(10) H 1.1433 -0.1147 0.0383 0.137 Uiso 1.00 1 c R . . H(11) H 0.9368 -0.1788 0.0771 0.136 Uiso 1.00 1 c R . . H(12) H 0.7689 -0.1102 0.1764 0.102 Uiso 1.00 1 c R . . H(15) H 0.2787 0.1229 0.2374 0.076 Uiso 1.00 1 c R . . H(16) H 0.2332 -0.0485 0.2793 0.097 Uiso 1.00 1 c R . . H(17) H 0.4072 -0.1873 0.3243 0.110 Uiso 1.00 1 c R . . H(18) H 0.6295 -0.1556 0.3296 0.093 Uiso 1.00 1 c R . . H(21) H 0.2259 0.3147 0.0997 0.086 Uiso 1.00 1 c R . . H(22) H 0.2071 0.2658 -0.0179 0.103 Uiso 1.00 1 c R . . H(23) H 0.3941 0.1551 -0.0810 0.110 Uiso 1.00 1 c R . . H(24) H 0.5978 0.0859 -0.0238 0.103 Uiso 1.00 1 c R . . H(25) H 0.6166 0.1298 0.0953 0.080 Uiso 1.00 1 c R . . H(35) H 0.8668 0.6145 0.2998 0.104 Uiso 1.00 1 c R . . H(36) H 0.9740 0.6305 0.1716 0.121 Uiso 1.00 1 c R . . H(37) H 0.9317 0.5270 0.0880 0.099 Uiso 1.00 1 c R . . H(26A) H 0.2944 0.3854 0.1997 0.064 Uiso 1.00 1 c R . . H(26B) H 0.4307 0.4127 0.1443 0.064 Uiso 1.00 1 c R . . H(27) H 0.3351 0.4216 0.3991 0.078 Uiso 1.00 1 c R . . H(28A) H 0.1630 0.3994 0.3236 0.121 Uiso 1.00 1 c R . . H(28B) H 0.1513 0.3357 0.4092 0.121 Uiso 1.00 1 c R . . H(28C) H 0.2237 0.2749 0.3377 0.121 Uiso 1.00 1 c R . . H(29A) H 0.5323 0.2774 0.4157 0.088 Uiso 1.00 1 c R . . H(29B) H 0.4483 0.2024 0.3893 0.088 Uiso 1.00 1 c R . . H(29C) H 0.3896 0.2535 0.4667 0.088 Uiso 1.00 1 c R . . H(30) H 0.4451 0.5858 0.2953 0.070 Uiso 1.00 1 c R . . H(31A) H 0.2076 0.5691 0.3363 0.124 Uiso 1.00 1 c R . . H(31B) H 0.1834 0.5858 0.2483 0.124 Uiso 1.00 1 c R . . H(31C) H 0.2182 0.6797 0.2828 0.124 Uiso 1.00 1 c R . . H(32A) H 0.5431 0.5939 0.1627 0.110 Uiso 1.00 1 c R . . H(32B) H 0.4242 0.6954 0.1788 0.110 Uiso 1.00 1 c R . . H(32C) H 0.3907 0.6039 0.1409 0.110 Uiso 1.00 1 c R . . H(39) H 0.6118 0.4517 0.3881 0.078 Uiso 1.00 1 c R . . H(40A) H 0.5734 0.5861 0.4639 0.135 Uiso 1.00 1 c R . . H(40B) H 0.5543 0.6410 0.3777 0.135 Uiso 1.00 1 c R . . H(40C) H 0.6949 0.6388 0.4104 0.135 Uiso 1.00 1 c R . . H(41A) H 0.7525 0.4188 0.4869 0.127 Uiso 1.00 1 c R . . H(41B) H 0.8723 0.4687 0.4293 0.127 Uiso 1.00 1 c R . . H(41C) H 0.8373 0.3606 0.4162 0.127 Uiso 1.00 1 c R . . H(42) H 0.6967 0.3407 0.1322 0.082 Uiso 1.00 1 c R . . H(43A) H 0.6195 0.4972 0.0483 0.129 Uiso 1.00 1 c R . . H(43B) H 0.6948 0.4042 -0.0009 0.129 Uiso 1.00 1 c R . . H(43C) H 0.7757 0.4946 0.0046 0.129 Uiso 1.00 1 c R . . H(44A) H 0.8830 0.2633 0.0442 0.134 Uiso 1.00 1 c R . . H(44B) H 0.9391 0.2622 0.1230 0.134 Uiso 1.00 1 c R . . H(44C) H 0.9728 0.3481 0.0499 0.134 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0377(2) 0.0428(2) 0.0445(2) -0.00914(18) -0.00875(19) -0.00179(19) Cl(1) 0.0487(5) 0.0551(5) 0.0732(6) -0.0106(3) -0.0257(4) -0.0060(4) P(1) 0.0447(5) 0.0442(5) 0.0539(5) -0.0090(3) -0.0147(4) 0.0001(4) P(2) 0.0384(4) 0.0479(5) 0.0554(5) -0.0066(3) -0.0039(4) -0.0095(4) N(1) 0.0446(16) 0.0444(15) 0.0492(16) -0.0106(12) -0.0133(13) 0.0003(13) N(2) 0.0410(15) 0.0397(14) 0.0446(15) -0.0101(11) -0.0058(12) -0.0014(12) C(1) 0.064(2) 0.051(2) 0.056(2) -0.0209(18) -0.0205(19) 0.0110(18) C(2) 0.131(4) 0.075(3) 0.068(3) -0.016(3) -0.024(3) 0.002(2) C(3) 0.190(7) 0.110(4) 0.059(3) -0.052(5) -0.035(4) 0.018(3) C(4) 0.142(6) 0.126(5) 0.098(4) -0.072(4) -0.076(4) 0.055(4) C(5) 0.094(4) 0.125(5) 0.119(5) -0.010(3) -0.047(4) 0.056(4) C(6) 0.077(3) 0.087(3) 0.089(3) -0.003(2) -0.030(2) 0.026(2) C(7) 0.050(2) 0.052(2) 0.055(2) -0.0063(16) -0.0162(17) -0.0058(17) C(8) 0.062(2) 0.079(2) 0.080(2) -0.019(2) -0.001(2) -0.034(2) C(9) 0.075(3) 0.128(4) 0.106(3) -0.038(3) 0.020(2) -0.057(3) C(10) 0.103(4) 0.147(5) 0.112(4) -0.041(4) 0.017(3) -0.081(4) C(11) 0.107(4) 0.141(5) 0.118(4) -0.045(4) 0.003(3) -0.081(4) C(12) 0.073(3) 0.100(3) 0.100(3) -0.031(2) -0.006(2) -0.048(3) C(13) 0.050(2) 0.048(2) 0.068(2) -0.0167(16) -0.0156(18) 0.0025(18) C(14) 0.0459(19) 0.0486(19) 0.051(2) -0.0180(15) -0.0107(16) -0.0020(16) C(15) 0.051(2) 0.069(2) 0.073(2) -0.0202(19) -0.019(2) 0.004(2) C(16) 0.062(2) 0.083(3) 0.106(3) -0.041(2) -0.024(2) 0.011(2) C(17) 0.082(3) 0.064(2) 0.133(4) -0.038(2) -0.033(3) 0.019(2) C(18) 0.070(2) 0.056(2) 0.108(3) -0.026(2) -0.029(2) 0.015(2) C(19) 0.0357(17) 0.052(2) 0.053(2) -0.0072(14) -0.0109(15) -0.0077(16) C(20) 0.055(2) 0.0465(19) 0.056(2) -0.0134(16) -0.0181(18) -0.0003(17) C(21) 0.069(2) 0.068(2) 0.087(3) -0.005(2) -0.040(2) -0.016(2) C(22) 0.100(3) 0.082(3) 0.089(3) -0.014(2) -0.052(3) -0.017(2) C(23) 0.119(4) 0.108(4) 0.064(2) -0.044(3) -0.025(3) -0.017(2) C(24) 0.076(3) 0.110(4) 0.080(3) -0.027(2) 0.005(2) -0.042(3) C(25) 0.060(2) 0.080(2) 0.067(2) -0.015(2) -0.013(2) -0.024(2) C(26) 0.0379(18) 0.058(2) 0.062(2) -0.0072(15) -0.0095(17) -0.0065(18) C(27) 0.055(2) 0.075(2) 0.061(2) -0.017(2) 0.0112(19) -0.014(2) C(28) 0.065(3) 0.123(4) 0.113(4) -0.042(3) 0.024(2) -0.022(3) C(29) 0.085(3) 0.078(2) 0.049(2) -0.020(2) 0.012(2) -0.007(2) C(30) 0.049(2) 0.050(2) 0.076(2) -0.0038(16) -0.0113(19) -0.0138(19) C(31) 0.066(3) 0.080(3) 0.146(5) 0.014(2) -0.001(3) -0.018(3) C(32) 0.091(3) 0.060(2) 0.106(3) 0.005(2) -0.006(3) 0.004(2) C(33) 0.0353(17) 0.0426(18) 0.058(2) -0.0086(13) -0.0097(15) -0.0005(16) C(34) 0.053(2) 0.047(2) 0.077(2) -0.0113(16) -0.022(2) -0.0052(19) C(35) 0.095(3) 0.078(3) 0.106(3) -0.045(2) -0.042(3) -0.002(2) C(36) 0.091(3) 0.104(4) 0.117(4) -0.063(3) -0.027(3) 0.028(3) C(37) 0.067(2) 0.092(3) 0.088(3) -0.044(2) -0.011(2) 0.020(2) C(38) 0.043(2) 0.065(2) 0.058(2) -0.0136(17) -0.0043(17) 0.0073(19) C(39) 0.070(2) 0.060(2) 0.068(2) -0.003(2) -0.019(2) -0.024(2) C(40) 0.134(5) 0.081(3) 0.125(4) 0.015(3) -0.038(4) -0.046(3) C(41) 0.118(4) 0.113(4) 0.079(3) 0.028(3) -0.041(3) -0.028(3) C(42) 0.069(2) 0.078(2) 0.055(2) -0.021(2) 0.007(2) -0.005(2) C(43) 0.117(4) 0.131(5) 0.069(3) 0.001(3) -0.032(3) -0.013(3) C(44) 0.122(5) 0.115(4) 0.074(3) 0.016(3) 0.002(3) -0.012(3) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.7.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ni(1) Cl(1) 2.1954(11) ? . . Ni(1) P(1) 2.1509(9) ? . . Ni(1) N(1) 1.955(3) ? . . Ni(1) N(2) 1.972(2) ? . . P(1) C(1) 1.819(4) ? . . P(1) C(7) 1.815(3) ? . . P(1) C(13) 1.793(4) ? . . P(2) N(2) 1.615(2) ? . . P(2) C(26) 1.770(4) ? . . P(2) C(27) 1.851(3) ? . . P(2) C(30) 1.841(3) ? . . N(1) C(14) 1.409(4) ? . . N(1) C(19) 1.393(4) ? . . N(2) C(33) 1.438(4) ? . . C(1) C(2) 1.369(6) ? . . C(1) C(6) 1.388(5) ? . . C(2) C(3) 1.406(8) ? . . C(3) C(4) 1.374(9) ? . . C(4) C(5) 1.353(10) ? . . C(5) C(6) 1.382(8) ? . . C(7) C(8) 1.388(6) ? . . C(7) C(12) 1.388(7) ? . . C(8) C(9) 1.386(6) ? . . C(9) C(10) 1.375(10) ? . . C(10) C(11) 1.358(10) ? . . C(11) C(12) 1.387(7) ? . . C(13) C(14) 1.396(4) ? . . C(13) C(18) 1.390(6) ? . . C(14) C(15) 1.411(5) ? . . C(15) C(16) 1.383(6) ? . . C(16) C(17) 1.375(6) ? . . C(17) C(18) 1.379(7) ? . . C(19) C(20) 1.495(5) ? . . C(19) C(26) 1.349(5) ? . . C(20) C(21) 1.382(6) ? . . C(20) C(25) 1.392(5) ? . . C(21) C(22) 1.383(7) ? . . C(22) C(23) 1.356(7) ? . . C(23) C(24) 1.381(8) ? . . C(24) C(25) 1.376(7) ? . . C(27) C(28) 1.545(7) ? . . C(27) C(29) 1.528(5) ? . . C(30) C(31) 1.534(5) ? . . C(30) C(32) 1.519(6) ? . . C(33) C(34) 1.415(6) ? . . C(33) C(38) 1.412(5) ? . . C(34) C(35) 1.391(6) ? . . C(34) C(39) 1.520(5) ? . . C(35) C(36) 1.369(8) ? . . C(36) C(37) 1.371(9) ? . . C(37) C(38) 1.397(6) ? . . C(38) C(42) 1.520(6) ? . . C(39) C(40) 1.517(6) ? . . C(39) C(41) 1.523(6) ? . . C(42) C(43) 1.520(6) ? . . C(42) C(44) 1.521(6) ? . . C(2) H(2) 0.930 ? . . C(3) H(3) 0.930 ? . . C(4) H(4) 0.930 ? . . C(5) H(5) 0.930 ? . . C(6) H(6) 0.930 ? . . C(8) H(8) 0.930 ? . . C(9) H(9) 0.930 ? . . C(10) H(10) 0.930 ? . . C(11) H(11) 0.930 ? . . C(12) H(12) 0.930 ? . . C(15) H(15) 0.930 ? . . C(16) H(16) 0.930 ? . . C(17) H(17) 0.930 ? . . C(18) H(18) 0.930 ? . . C(21) H(21) 0.930 ? . . C(22) H(22) 0.930 ? . . C(23) H(23) 0.930 ? . . C(24) H(24) 0.930 ? . . C(25) H(25) 0.930 ? . . C(26) H(26A) 0.970 ? . . C(26) H(26B) 0.970 ? . . C(27) H(27) 0.980 ? . . C(28) H(28A) 0.960 ? . . C(28) H(28B) 0.960 ? . . C(28) H(28C) 0.960 ? . . C(29) H(29A) 0.960 ? . . C(29) H(29B) 0.960 ? . . C(29) H(29C) 0.960 ? . . C(30) H(30) 0.980 ? . . C(31) H(31A) 0.960 ? . . C(31) H(31B) 0.960 ? . . C(31) H(31C) 0.960 ? . . C(32) H(32A) 0.960 ? . . C(32) H(32B) 0.960 ? . . C(32) H(32C) 0.960 ? . . C(35) H(35) 0.930 ? . . C(36) H(36) 0.930 ? . . C(37) H(37) 0.930 ? . . C(39) H(39) 0.980 ? . . C(40) H(40A) 0.960 ? . . C(40) H(40B) 0.960 ? . . C(40) H(40C) 0.960 ? . . C(41) H(41A) 0.960 ? . . C(41) H(41B) 0.960 ? . . C(41) H(41C) 0.960 ? . . C(42) H(42) 0.980 ? . . C(43) H(43A) 0.960 ? . . C(43) H(43B) 0.960 ? . . C(43) H(43C) 0.960 ? . . C(44) H(44A) 0.960 ? . . C(44) H(44B) 0.960 ? . . C(44) H(44C) 0.960 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Ni(1) P(1) 87.35(4) ? . . . Cl(1) Ni(1) N(1) 171.78(8) ? . . . Cl(1) Ni(1) N(2) 92.31(9) ? . . . P(1) Ni(1) N(1) 85.05(8) ? . . . P(1) Ni(1) N(2) 175.53(7) ? . . . N(1) Ni(1) N(2) 95.51(11) ? . . . Ni(1) P(1) C(1) 119.59(14) ? . . . Ni(1) P(1) C(7) 115.99(12) ? . . . Ni(1) P(1) C(13) 101.42(11) ? . . . C(1) P(1) C(7) 105.16(16) ? . . . C(1) P(1) C(13) 106.20(18) ? . . . C(7) P(1) C(13) 107.49(19) ? . . . N(2) P(2) C(26) 109.08(15) ? . . . N(2) P(2) C(27) 110.38(16) ? . . . N(2) P(2) C(30) 112.84(17) ? . . . C(26) P(2) C(27) 111.2(2) ? . . . C(26) P(2) C(30) 107.49(18) ? . . . C(27) P(2) C(30) 105.84(18) ? . . . Ni(1) N(1) C(14) 118.2(2) ? . . . Ni(1) N(1) C(19) 123.5(2) ? . . . C(14) N(1) C(19) 117.2(3) ? . . . Ni(1) N(2) P(2) 114.45(16) ? . . . Ni(1) N(2) C(33) 120.13(18) ? . . . P(2) N(2) C(33) 122.4(2) ? . . . P(1) C(1) C(2) 118.0(3) ? . . . P(1) C(1) C(6) 122.6(3) ? . . . C(2) C(1) C(6) 119.3(4) ? . . . C(1) C(2) C(3) 120.4(4) ? . . . C(2) C(3) C(4) 119.5(5) ? . . . C(3) C(4) C(5) 119.5(6) ? . . . C(4) C(5) C(6) 121.9(5) ? . . . C(1) C(6) C(5) 119.3(4) ? . . . P(1) C(7) C(8) 119.4(3) ? . . . P(1) C(7) C(12) 123.0(3) ? . . . C(8) C(7) C(12) 117.5(3) ? . . . C(7) C(8) C(9) 121.4(5) ? . . . C(8) C(9) C(10) 119.4(5) ? . . . C(9) C(10) C(11) 120.6(5) ? . . . C(10) C(11) C(12) 120.0(6) ? . . . C(7) C(12) C(11) 121.1(5) ? . . . P(1) C(13) C(14) 112.1(2) ? . . . P(1) C(13) C(18) 127.2(3) ? . . . C(14) C(13) C(18) 120.7(3) ? . . . N(1) C(14) C(13) 118.6(3) ? . . . N(1) C(14) C(15) 123.0(3) ? . . . C(13) C(14) C(15) 118.3(3) ? . . . C(14) C(15) C(16) 119.9(3) ? . . . C(15) C(16) C(17) 120.9(4) ? . . . C(16) C(17) C(18) 119.9(4) ? . . . C(13) C(18) C(17) 120.2(3) ? . . . N(1) C(19) C(20) 119.2(2) ? . . . N(1) C(19) C(26) 120.7(3) ? . . . C(20) C(19) C(26) 119.8(3) ? . . . C(19) C(20) C(21) 122.1(3) ? . . . C(19) C(20) C(25) 119.4(3) ? . . . C(21) C(20) C(25) 118.3(4) ? . . . C(20) C(21) C(22) 121.2(4) ? . . . C(21) C(22) C(23) 120.1(5) ? . . . C(22) C(23) C(24) 119.7(5) ? . . . C(23) C(24) C(25) 120.8(4) ? . . . C(20) C(25) C(24) 119.9(4) ? . . . P(2) C(26) C(19) 118.2(2) ? . . . P(2) C(27) C(28) 111.5(3) ? . . . P(2) C(27) C(29) 115.5(2) ? . . . C(28) C(27) C(29) 110.2(4) ? . . . P(2) C(30) C(31) 114.5(3) ? . . . P(2) C(30) C(32) 114.4(2) ? . . . C(31) C(30) C(32) 109.4(3) ? . . . N(2) C(33) C(34) 119.8(3) ? . . . N(2) C(33) C(38) 119.3(3) ? . . . C(34) C(33) C(38) 120.8(3) ? . . . C(33) C(34) C(35) 117.8(4) ? . . . C(33) C(34) C(39) 122.2(3) ? . . . C(35) C(34) C(39) 120.0(4) ? . . . C(34) C(35) C(36) 122.1(5) ? . . . C(35) C(36) C(37) 119.5(5) ? . . . C(36) C(37) C(38) 122.1(4) ? . . . C(33) C(38) C(37) 117.6(4) ? . . . C(33) C(38) C(42) 123.1(3) ? . . . C(37) C(38) C(42) 119.3(3) ? . . . C(34) C(39) C(40) 113.8(3) ? . . . C(34) C(39) C(41) 111.6(3) ? . . . C(40) C(39) C(41) 109.0(4) ? . . . C(38) C(42) C(43) 113.7(4) ? . . . C(38) C(42) C(44) 112.0(4) ? . . . C(43) C(42) C(44) 108.2(3) ? . . . C(1) C(2) H(2) 119.8 ? . . . C(3) C(2) H(2) 119.8 ? . . . C(2) C(3) H(3) 120.2 ? . . . C(4) C(3) H(3) 120.2 ? . . . C(3) C(4) H(4) 120.3 ? . . . C(5) C(4) H(4) 120.3 ? . . . C(4) C(5) H(5) 119.1 ? . . . C(6) C(5) H(5) 119.0 ? . . . C(1) C(6) H(6) 120.4 ? . . . C(5) C(6) H(6) 120.4 ? . . . C(7) C(8) H(8) 119.3 ? . . . C(9) C(8) H(8) 119.3 ? . . . C(8) C(9) H(9) 120.3 ? . . . C(10) C(9) H(9) 120.3 ? . . . C(9) C(10) H(10) 119.7 ? . . . C(11) C(10) H(10) 119.7 ? . . . C(10) C(11) H(11) 120.0 ? . . . C(12) C(11) H(11) 120.0 ? . . . C(7) C(12) H(12) 119.4 ? . . . C(11) C(12) H(12) 119.5 ? . . . C(14) C(15) H(15) 120.0 ? . . . C(16) C(15) H(15) 120.0 ? . . . C(15) C(16) H(16) 119.5 ? . . . C(17) C(16) H(16) 119.5 ? . . . C(16) C(17) H(17) 120.0 ? . . . C(18) C(17) H(17) 120.0 ? . . . C(13) C(18) H(18) 119.9 ? . . . C(17) C(18) H(18) 119.9 ? . . . C(20) C(21) H(21) 119.4 ? . . . C(22) C(21) H(21) 119.4 ? . . . C(21) C(22) H(22) 120.0 ? . . . C(23) C(22) H(22) 119.9 ? . . . C(22) C(23) H(23) 120.2 ? . . . C(24) C(23) H(23) 120.2 ? . . . C(23) C(24) H(24) 119.6 ? . . . C(25) C(24) H(24) 119.6 ? . . . C(20) C(25) H(25) 120.1 ? . . . C(24) C(25) H(25) 120.0 ? . . . P(2) C(26) H(26A) 107.8 ? . . . P(2) C(26) H(26B) 107.8 ? . . . C(19) C(26) H(26A) 107.8 ? . . . C(19) C(26) H(26B) 107.8 ? . . . H(26A) C(26) H(26B) 107.1 ? . . . P(2) C(27) H(27) 106.4 ? . . . C(28) C(27) H(27) 106.4 ? . . . C(29) C(27) H(27) 106.4 ? . . . C(27) C(28) H(28A) 109.5 ? . . . C(27) C(28) H(28B) 109.5 ? . . . C(27) C(28) H(28C) 109.5 ? . . . H(28A) C(28) H(28B) 109.5 ? . . . H(28A) C(28) H(28C) 109.5 ? . . . H(28B) C(28) H(28C) 109.5 ? . . . C(27) C(29) H(29A) 109.5 ? . . . C(27) C(29) H(29B) 109.5 ? . . . C(27) C(29) H(29C) 109.5 ? . . . H(29A) C(29) H(29B) 109.5 ? . . . H(29A) C(29) H(29C) 109.5 ? . . . H(29B) C(29) H(29C) 109.5 ? . . . P(2) C(30) H(30) 105.9 ? . . . C(31) C(30) H(30) 105.9 ? . . . C(32) C(30) H(30) 105.9 ? . . . C(30) C(31) H(31A) 109.5 ? . . . C(30) C(31) H(31B) 109.5 ? . . . C(30) C(31) H(31C) 109.5 ? . . . H(31A) C(31) H(31B) 109.5 ? . . . H(31A) C(31) H(31C) 109.5 ? . . . H(31B) C(31) H(31C) 109.5 ? . . . C(30) C(32) H(32A) 109.5 ? . . . C(30) C(32) H(32B) 109.5 ? . . . C(30) C(32) H(32C) 109.5 ? . . . H(32A) C(32) H(32B) 109.5 ? . . . H(32A) C(32) H(32C) 109.5 ? . . . H(32B) C(32) H(32C) 109.5 ? . . . C(34) C(35) H(35) 118.9 ? . . . C(36) C(35) H(35) 118.9 ? . . . C(35) C(36) H(36) 120.3 ? . . . C(37) C(36) H(36) 120.2 ? . . . C(36) C(37) H(37) 118.9 ? . . . C(38) C(37) H(37) 118.9 ? . . . C(34) C(39) H(39) 107.4 ? . . . C(40) C(39) H(39) 107.4 ? . . . C(41) C(39) H(39) 107.4 ? . . . C(39) C(40) H(40A) 109.5 ? . . . C(39) C(40) H(40B) 109.5 ? . . . C(39) C(40) H(40C) 109.5 ? . . . H(40A) C(40) H(40B) 109.5 ? . . . H(40A) C(40) H(40C) 109.5 ? . . . H(40B) C(40) H(40C) 109.5 ? . . . C(39) C(41) H(41A) 109.5 ? . . . C(39) C(41) H(41B) 109.5 ? . . . C(39) C(41) H(41C) 109.5 ? . . . H(41A) C(41) H(41B) 109.5 ? . . . H(41A) C(41) H(41C) 109.5 ? . . . H(41B) C(41) H(41C) 109.5 ? . . . C(38) C(42) H(42) 107.6 ? . . . C(43) C(42) H(42) 107.6 ? . . . C(44) C(42) H(42) 107.6 ? . . . C(42) C(43) H(43A) 109.5 ? . . . C(42) C(43) H(43B) 109.5 ? . . . C(42) C(43) H(43C) 109.5 ? . . . H(43A) C(43) H(43B) 109.5 ? . . . H(43A) C(43) H(43C) 109.5 ? . . . H(43B) C(43) H(43C) 109.5 ? . . . C(42) C(44) H(44A) 109.5 ? . . . C(42) C(44) H(44B) 109.5 ? . . . C(42) C(44) H(44C) 109.5 ? . . . H(44A) C(44) H(44B) 109.5 ? . . . H(44A) C(44) H(44C) 109.5 ? . . . H(44B) C(44) H(44C) 109.5 ? . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl(1) Ni(1) P(1) C(1) 49.42(15) ? . . . . Cl(1) Ni(1) P(1) C(7) -78.26(15) ? . . . . Cl(1) Ni(1) P(1) C(13) 165.66(13) ? . . . . Cl(1) Ni(1) N(1) C(14) 41.9(7) ? . . . . Cl(1) Ni(1) N(1) C(19) -126.0(5) ? . . . . Cl(1) Ni(1) N(2) P(2) -163.55(13) ? . . . . Cl(1) Ni(1) N(2) C(33) 35.5(2) ? . . . . P(1) Ni(1) N(1) C(14) 19.5(2) ? . . . . P(1) Ni(1) N(1) C(19) -148.4(2) ? . . . . N(1) Ni(1) P(1) C(1) -133.71(17) ? . . . . N(1) Ni(1) P(1) C(7) 98.61(17) ? . . . . N(1) Ni(1) P(1) C(13) -17.47(15) ? . . . . P(1) Ni(1) N(2) P(2) -78.0(12) ? . . . . P(1) Ni(1) N(2) C(33) 121.0(11) ? . . . . N(2) Ni(1) P(1) C(1) -36.3(12) ? . . . . N(2) Ni(1) P(1) C(7) -164.0(11) ? . . . . N(2) Ni(1) P(1) C(13) 80.0(12) ? . . . . N(1) Ni(1) N(2) P(2) 18.98(16) ? . . . . N(1) Ni(1) N(2) C(33) -142.0(2) ? . . . . N(2) Ni(1) N(1) C(14) -156.0(2) ? . . . . N(2) Ni(1) N(1) C(19) 36.1(2) ? . . . . Ni(1) P(1) C(1) C(2) 39.2(4) ? . . . . Ni(1) P(1) C(1) C(6) -139.1(3) ? . . . . Ni(1) P(1) C(7) C(8) 56.1(3) ? . . . . Ni(1) P(1) C(7) C(12) -125.3(3) ? . . . . Ni(1) P(1) C(13) C(14) 16.1(3) ? . . . . Ni(1) P(1) C(13) C(18) -163.1(3) ? . . . . C(1) P(1) C(7) C(8) -78.4(3) ? . . . . C(1) P(1) C(7) C(12) 100.2(3) ? . . . . C(7) P(1) C(1) C(2) 171.7(4) ? . . . . C(7) P(1) C(1) C(6) -6.6(4) ? . . . . C(1) P(1) C(13) C(14) 141.8(2) ? . . . . C(1) P(1) C(13) C(18) -37.4(4) ? . . . . C(13) P(1) C(1) C(2) -74.5(4) ? . . . . C(13) P(1) C(1) C(6) 107.1(4) ? . . . . C(7) P(1) C(13) C(14) -106.1(2) ? . . . . C(7) P(1) C(13) C(18) 74.7(4) ? . . . . C(13) P(1) C(7) C(8) 168.7(3) ? . . . . C(13) P(1) C(7) C(12) -12.7(3) ? . . . . N(2) P(2) C(26) C(19) 49.5(3) ? . . . . C(26) P(2) N(2) Ni(1) -55.14(19) ? . . . . C(26) P(2) N(2) C(33) 105.3(2) ? . . . . N(2) P(2) C(27) C(28) -147.4(3) ? . . . . N(2) P(2) C(27) C(29) -20.8(4) ? . . . . C(27) P(2) N(2) Ni(1) 67.3(2) ? . . . . C(27) P(2) N(2) C(33) -132.2(2) ? . . . . N(2) P(2) C(30) C(31) -163.5(3) ? . . . . N(2) P(2) C(30) C(32) 69.2(3) ? . . . . C(30) P(2) N(2) Ni(1) -174.53(17) ? . . . . C(30) P(2) N(2) C(33) -14.0(3) ? . . . . C(26) P(2) C(27) C(28) -26.3(3) ? . . . . C(26) P(2) C(27) C(29) 100.4(3) ? . . . . C(27) P(2) C(26) C(19) -72.5(3) ? . . . . C(26) P(2) C(30) C(31) 76.2(3) ? . . . . C(26) P(2) C(30) C(32) -51.1(3) ? . . . . C(30) P(2) C(26) C(19) 172.1(2) ? . . . . C(27) P(2) C(30) C(31) -42.7(4) ? . . . . C(27) P(2) C(30) C(32) -170.0(3) ? . . . . C(30) P(2) C(27) C(28) 90.1(3) ? . . . . C(30) P(2) C(27) C(29) -143.2(3) ? . . . . Ni(1) N(1) C(14) C(13) -13.6(4) ? . . . . Ni(1) N(1) C(14) C(15) 162.9(2) ? . . . . Ni(1) N(1) C(19) C(20) 122.0(3) ? . . . . Ni(1) N(1) C(19) C(26) -51.7(3) ? . . . . C(14) N(1) C(19) C(20) -46.0(4) ? . . . . C(14) N(1) C(19) C(26) 140.3(3) ? . . . . C(19) N(1) C(14) C(13) 155.1(3) ? . . . . C(19) N(1) C(14) C(15) -28.4(4) ? . . . . Ni(1) N(2) C(33) C(34) -114.5(2) ? . . . . Ni(1) N(2) C(33) C(38) 63.0(3) ? . . . . P(2) N(2) C(33) C(34) 86.1(3) ? . . . . P(2) N(2) C(33) C(38) -96.4(3) ? . . . . P(1) C(1) C(2) C(3) -178.6(5) ? . . . . P(1) C(1) C(6) C(5) 178.3(4) ? . . . . C(2) C(1) C(6) C(5) 0.0(8) ? . . . . C(6) C(1) C(2) C(3) -0.2(7) ? . . . . C(1) C(2) C(3) C(4) 1.6(11) ? . . . . C(2) C(3) C(4) C(5) -2.8(12) ? . . . . C(3) C(4) C(5) C(6) 2.7(12) ? . . . . C(4) C(5) C(6) C(1) -1.3(10) ? . . . . P(1) C(7) C(8) C(9) 179.0(3) ? . . . . P(1) C(7) C(12) C(11) -177.9(3) ? . . . . C(8) C(7) C(12) C(11) 0.7(6) ? . . . . C(12) C(7) C(8) C(9) 0.4(6) ? . . . . C(7) C(8) C(9) C(10) -0.5(7) ? . . . . C(8) C(9) C(10) C(11) -0.4(8) ? . . . . C(9) C(10) C(11) C(12) 1.5(9) ? . . . . C(10) C(11) C(12) C(7) -1.7(8) ? . . . . P(1) C(13) C(14) N(1) -3.6(4) ? . . . . P(1) C(13) C(14) C(15) 179.7(2) ? . . . . P(1) C(13) C(18) C(17) -179.6(3) ? . . . . C(14) C(13) C(18) C(17) 1.3(6) ? . . . . C(18) C(13) C(14) N(1) 175.6(3) ? . . . . C(18) C(13) C(14) C(15) -1.0(5) ? . . . . N(1) C(14) C(15) C(16) -176.1(3) ? . . . . C(13) C(14) C(15) C(16) 0.5(5) ? . . . . C(14) C(15) C(16) C(17) -0.1(5) ? . . . . C(15) C(16) C(17) C(18) 0.3(6) ? . . . . C(16) C(17) C(18) C(13) -0.9(7) ? . . . . N(1) C(19) C(20) C(21) 146.9(3) ? . . . . N(1) C(19) C(20) C(25) -38.0(5) ? . . . . N(1) C(19) C(26) P(2) 5.0(4) ? . . . . C(20) C(19) C(26) P(2) -168.6(2) ? . . . . C(26) C(19) C(20) C(21) -39.3(5) ? . . . . C(26) C(19) C(20) C(25) 135.7(3) ? . . . . C(19) C(20) C(21) C(22) 175.0(4) ? . . . . C(19) C(20) C(25) C(24) -174.2(4) ? . . . . C(21) C(20) C(25) C(24) 1.0(6) ? . . . . C(25) C(20) C(21) C(22) -0.1(5) ? . . . . C(20) C(21) C(22) C(23) -1.2(7) ? . . . . C(21) C(22) C(23) C(24) 1.5(8) ? . . . . C(22) C(23) C(24) C(25) -0.6(8) ? . . . . C(23) C(24) C(25) C(20) -0.7(7) ? . . . . N(2) C(33) C(34) C(35) -179.5(3) ? . . . . N(2) C(33) C(34) C(39) 2.4(4) ? . . . . N(2) C(33) C(38) C(37) -179.8(3) ? . . . . N(2) C(33) C(38) C(42) -1.2(4) ? . . . . C(34) C(33) C(38) C(37) -2.3(5) ? . . . . C(34) C(33) C(38) C(42) 176.3(3) ? . . . . C(38) C(33) C(34) C(35) 3.0(5) ? . . . . C(38) C(33) C(34) C(39) -175.1(3) ? . . . . C(33) C(34) C(35) C(36) -1.3(6) ? . . . . C(33) C(34) C(39) C(40) -130.5(4) ? . . . . C(33) C(34) C(39) C(41) 105.7(4) ? . . . . C(35) C(34) C(39) C(40) 51.5(5) ? . . . . C(35) C(34) C(39) C(41) -72.3(5) ? . . . . C(39) C(34) C(35) C(36) 176.8(4) ? . . . . C(34) C(35) C(36) C(37) -1.0(7) ? . . . . C(35) C(36) C(37) C(38) 1.8(7) ? . . . . C(36) C(37) C(38) C(33) -0.2(5) ? . . . . C(36) C(37) C(38) C(42) -178.8(4) ? . . . . C(33) C(38) C(42) C(43) 120.5(4) ? . . . . C(33) C(38) C(42) C(44) -116.5(4) ? . . . . C(37) C(38) C(42) C(43) -61.0(5) ? . . . . C(37) C(38) C(42) C(44) 62.0(4) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 C(4) C(28) 3.594(9) ? . 65602 C(10) C(10) 3.588(8) ? . 75502 C(24) C(24) 3.529(8) ? . 65502 C(28) C(4) 3.594(9) ? . 65602 Cl(1) H(4) 2.922 ? . 75602 Cl(1) H(28C) 3.597 ? . 65501 C(3) H(28C) 3.598 ? . 65602 C(3) H(29C) 3.588 ? . 65602 C(4) H(28B) 2.980 ? . 65602 C(4) H(28C) 3.318 ? . 65602 C(4) H(41C) 3.481 ? . 75602 C(5) H(28B) 3.443 ? . 65602 C(5) H(41C) 3.592 ? . 75602 C(6) H(16) 3.182 ? . 65501 C(8) H(15) 3.534 ? . 65501 C(8) H(16) 2.956 ? . 65501 C(9) H(16) 3.213 ? . 65501 C(9) H(24) 3.079 ? . 75502 C(10) H(10) 3.581 ? . 75502 C(10) H(24) 3.136 ? . 75502 C(10) H(44A) 3.308 ? . 75502 C(11) H(22) 3.304 ? . 65502 C(11) H(23) 3.580 ? . 65502 C(11) H(36) 3.124 ? . 54501 C(11) H(44A) 3.328 ? . 75502 C(12) H(23) 3.364 ? . 65502 C(12) H(36) 3.559 ? . 54501 C(15) H(3) 3.222 ? . 65602 C(15) H(8) 3.392 ? . 45501 C(15) H(9) 3.578 ? . 45501 C(16) H(3) 2.969 ? . 65602 C(16) H(8) 3.322 ? . 45501 C(16) H(9) 3.496 ? . 45501 C(17) H(3) 3.306 ? . 65602 C(17) H(32B) 3.579 ? . 54501 C(17) H(40B) 3.172 ? . 54501 C(18) H(40B) 3.338 ? . 54501 C(18) H(40C) 3.579 ? . 54501 C(21) H(43A) 3.527 ? . 66502 C(21) H(43C) 3.104 ? . 66502 C(21) H(44B) 3.485 ? . 45501 C(21) H(44C) 3.216 ? . 45501 C(22) H(9) 3.345 ? . 45501 C(22) H(11) 3.135 ? . 65502 C(22) H(37) 3.590 ? . 66502 C(22) H(43C) 3.315 ? . 66502 C(22) H(44C) 3.115 ? . 45501 C(23) H(9) 3.509 ? . 45501 C(23) H(11) 3.488 ? . 65502 C(23) H(12) 3.536 ? . 65502 C(23) H(24) 3.293 ? . 65502 C(23) H(32A) 3.501 ? . 66502 C(23) H(32B) 3.230 ? . 66502 C(24) H(9) 3.399 ? . 75502 C(24) H(10) 3.162 ? . 75502 C(24) H(24) 3.206 ? . 65502 C(24) H(32B) 3.538 ? . 66502 C(25) H(10) 3.362 ? . 75502 C(27) H(40A) 3.357 ? . 66602 C(28) H(4) 3.202 ? . 65602 C(28) H(41B) 3.439 ? . 45501 C(28) H(41C) 3.542 ? . 45501 C(29) H(40A) 3.084 ? . 66602 C(29) H(40C) 3.442 ? . 66602 C(31) H(35) 3.526 ? . 45501 C(31) H(36) 3.414 ? . 45501 C(35) H(28A) 3.566 ? . 65501 C(35) H(31B) 3.269 ? . 65501 C(36) H(11) 3.360 ? . 56501 C(36) H(22) 3.500 ? . 66502 C(36) H(31B) 3.012 ? . 65501 C(37) H(22) 3.204 ? . 66502 C(39) H(40A) 3.529 ? . 66602 C(40) H(17) 3.353 ? . 56501 C(40) H(18) 3.225 ? . 56501 C(40) H(27) 3.375 ? . 66602 C(40) H(29A) 3.598 ? . 66602 C(40) H(29C) 3.072 ? . 66602 C(40) H(40A) 3.563 ? . 66602 C(41) H(5) 3.356 ? . 75602 C(41) H(28B) 3.356 ? . 65501 C(43) H(21) 3.551 ? . 66502 C(43) H(26B) 3.600 ? . 66502 C(43) H(32C) 3.577 ? . 66502 C(44) H(11) 3.385 ? . 75502 C(44) H(21) 3.254 ? . 65501 C(44) H(22) 3.109 ? . 65501 H(3) C(15) 3.222 ? . 65602 H(3) C(16) 2.969 ? . 65602 H(3) C(17) 3.306 ? . 65602 H(3) H(15) 3.520 ? . 65602 H(3) H(16) 3.124 ? . 65602 H(3) H(28C) 3.359 ? . 65602 H(3) H(29B) 3.356 ? . 65602 H(4) Cl(1) 2.922 ? . 75602 H(4) C(28) 3.202 ? . 65602 H(4) H(28B) 2.674 ? . 65602 H(4) H(28C) 2.867 ? . 65602 H(4) H(41C) 2.806 ? . 75602 H(5) C(41) 3.356 ? . 75602 H(5) H(16) 3.582 ? . 65501 H(5) H(17) 3.577 ? . 65501 H(5) H(28B) 3.451 ? . 65602 H(5) H(31A) 3.366 ? . 64501 H(5) H(31C) 3.149 ? . 64501 H(5) H(41A) 2.970 ? . 75602 H(5) H(41B) 3.586 ? . 75602 H(5) H(41C) 3.010 ? . 75602 H(6) H(16) 2.810 ? . 65501 H(6) H(31C) 2.951 ? . 64501 H(8) C(15) 3.392 ? . 65501 H(8) C(16) 3.322 ? . 65501 H(8) H(15) 2.820 ? . 65501 H(8) H(16) 2.672 ? . 65501 H(9) C(15) 3.578 ? . 65501 H(9) C(16) 3.496 ? . 65501 H(9) C(22) 3.345 ? . 65501 H(9) C(23) 3.509 ? . 65501 H(9) C(24) 3.399 ? . 75502 H(9) H(15) 3.293 ? . 65501 H(9) H(16) 3.140 ? . 65501 H(9) H(22) 3.553 ? . 65501 H(9) H(24) 2.476 ? . 75502 H(10) C(10) 3.581 ? . 75502 H(10) C(24) 3.162 ? . 75502 H(10) C(25) 3.362 ? . 75502 H(10) H(24) 2.587 ? . 75502 H(10) H(25) 2.987 ? . 75502 H(10) H(44A) 2.673 ? . 75502 H(11) C(22) 3.135 ? . 65502 H(11) C(23) 3.488 ? . 65502 H(11) C(36) 3.360 ? . 54501 H(11) C(44) 3.385 ? . 75502 H(11) H(22) 2.435 ? . 65502 H(11) H(23) 3.153 ? . 65502 H(11) H(36) 2.688 ? . 54501 H(11) H(44A) 2.717 ? . 75502 H(11) H(44C) 3.259 ? . 75502 H(12) C(23) 3.536 ? . 65502 H(12) H(23) 2.709 ? . 65502 H(12) H(36) 3.487 ? . 54501 H(15) C(8) 3.534 ? . 45501 H(15) H(3) 3.520 ? . 65602 H(15) H(8) 2.820 ? . 45501 H(15) H(9) 3.293 ? . 45501 H(16) C(6) 3.182 ? . 45501 H(16) C(8) 2.956 ? . 45501 H(16) C(9) 3.213 ? . 45501 H(16) H(3) 3.124 ? . 65602 H(16) H(5) 3.582 ? . 45501 H(16) H(6) 2.810 ? . 45501 H(16) H(8) 2.672 ? . 45501 H(16) H(9) 3.140 ? . 45501 H(16) H(31C) 3.519 ? . 54501 H(17) C(40) 3.353 ? . 54501 H(17) H(5) 3.577 ? . 45501 H(17) H(30) 2.981 ? . 54501 H(17) H(31C) 3.028 ? . 54501 H(17) H(32B) 3.145 ? . 54501 H(17) H(40B) 2.473 ? . 54501 H(17) H(40C) 3.550 ? . 54501 H(18) C(40) 3.225 ? . 54501 H(18) H(35) 3.377 ? . 54501 H(18) H(29C) 3.541 ? . 65602 H(18) H(40B) 2.814 ? . 54501 H(18) H(40C) 2.759 ? . 54501 H(21) C(43) 3.551 ? . 66502 H(21) C(44) 3.254 ? . 45501 H(21) H(37) 3.492 ? . 45501 H(21) H(43A) 3.571 ? . 66502 H(21) H(43C) 2.776 ? . 66502 H(21) H(44B) 2.955 ? . 45501 H(21) H(44C) 2.678 ? . 45501 H(22) C(11) 3.304 ? . 65502 H(22) C(36) 3.500 ? . 66502 H(22) C(37) 3.204 ? . 66502 H(22) C(44) 3.109 ? . 45501 H(22) H(9) 3.553 ? . 45501 H(22) H(11) 2.435 ? . 65502 H(22) H(36) 3.385 ? . 66502 H(22) H(37) 2.867 ? . 66502 H(22) H(43C) 3.174 ? . 66502 H(22) H(44A) 3.148 ? . 45501 H(22) H(44B) 3.248 ? . 45501 H(22) H(44C) 2.472 ? . 45501 H(23) C(11) 3.580 ? . 65502 H(23) C(12) 3.364 ? . 65502 H(23) H(11) 3.153 ? . 65502 H(23) H(12) 2.709 ? . 65502 H(23) H(24) 3.294 ? . 65502 H(23) H(32A) 3.424 ? . 66502 H(23) H(32B) 2.995 ? . 66502 H(24) C(9) 3.079 ? . 75502 H(24) C(10) 3.136 ? . 75502 H(24) C(23) 3.293 ? . 65502 H(24) C(24) 3.206 ? . 65502 H(24) H(9) 2.476 ? . 75502 H(24) H(10) 2.587 ? . 75502 H(24) H(23) 3.294 ? . 65502 H(24) H(24) 3.135 ? . 65502 H(24) H(32B) 3.533 ? . 66502 H(25) H(10) 2.987 ? . 75502 H(35) C(31) 3.526 ? . 65501 H(35) H(18) 3.377 ? . 56501 H(35) H(28A) 3.545 ? . 65501 H(35) H(31A) 3.391 ? . 65501 H(35) H(31B) 3.005 ? . 65501 H(36) C(11) 3.124 ? . 56501 H(36) C(12) 3.559 ? . 56501 H(36) C(31) 3.414 ? . 65501 H(36) H(11) 2.688 ? . 56501 H(36) H(12) 3.487 ? . 56501 H(36) H(22) 3.385 ? . 66502 H(36) H(31B) 2.542 ? . 65501 H(36) H(31C) 3.551 ? . 65501 H(37) C(22) 3.590 ? . 66502 H(37) H(21) 3.492 ? . 65501 H(37) H(22) 2.867 ? . 66502 H(37) H(37) 3.253 ? . 76502 H(37) H(43C) 2.988 ? . 76502 H(37) H(44C) 2.776 ? . 76502 H(26B) C(43) 3.600 ? . 66502 H(26B) H(43A) 3.441 ? . 66502 H(26B) H(43B) 3.317 ? . 66502 H(26B) H(43C) 3.452 ? . 66502 H(27) C(40) 3.375 ? . 66602 H(27) H(40A) 2.681 ? . 66602 H(27) H(40C) 3.255 ? . 66602 H(27) H(41A) 2.998 ? . 66602 H(28A) C(35) 3.566 ? . 45501 H(28A) H(35) 3.545 ? . 45501 H(28A) H(41B) 3.125 ? . 45501 H(28A) H(41C) 3.384 ? . 45501 H(28B) C(4) 2.980 ? . 65602 H(28B) C(5) 3.443 ? . 65602 H(28B) C(41) 3.356 ? . 45501 H(28B) H(4) 2.674 ? . 65602 H(28B) H(5) 3.451 ? . 65602 H(28B) H(41B) 2.865 ? . 45501 H(28B) H(41C) 2.981 ? . 45501 H(28C) Cl(1) 3.597 ? . 45501 H(28C) C(3) 3.598 ? . 65602 H(28C) C(4) 3.318 ? . 65602 H(28C) H(3) 3.359 ? . 65602 H(28C) H(4) 2.867 ? . 65602 H(29A) C(40) 3.598 ? . 66602 H(29A) H(40A) 2.883 ? . 66602 H(29B) H(3) 3.356 ? . 65602 H(29C) C(3) 3.588 ? . 65602 H(29C) C(40) 3.072 ? . 66602 H(29C) H(18) 3.541 ? . 65602 H(29C) H(40A) 2.693 ? . 66602 H(29C) H(40B) 3.426 ? . 66602 H(29C) H(40C) 2.671 ? . 66602 H(30) H(17) 2.981 ? . 56501 H(31A) H(5) 3.366 ? . 46501 H(31A) H(35) 3.391 ? . 45501 H(31A) H(41A) 3.218 ? . 66602 H(31B) C(35) 3.269 ? . 45501 H(31B) C(36) 3.012 ? . 45501 H(31B) H(35) 3.005 ? . 45501 H(31B) H(36) 2.542 ? . 45501 H(31C) H(5) 3.149 ? . 46501 H(31C) H(6) 2.951 ? . 46501 H(31C) H(16) 3.519 ? . 56501 H(31C) H(17) 3.028 ? . 56501 H(31C) H(36) 3.551 ? . 45501 H(32A) C(23) 3.501 ? . 66502 H(32A) H(23) 3.424 ? . 66502 H(32B) C(17) 3.579 ? . 56501 H(32B) C(23) 3.230 ? . 66502 H(32B) C(24) 3.538 ? . 66502 H(32B) H(17) 3.145 ? . 56501 H(32B) H(23) 2.995 ? . 66502 H(32B) H(24) 3.533 ? . 66502 H(32C) C(43) 3.577 ? . 66502 H(32C) H(43B) 2.750 ? . 66502 H(39) H(40A) 2.901 ? . 66602 H(40A) C(27) 3.357 ? . 66602 H(40A) C(29) 3.084 ? . 66602 H(40A) C(39) 3.529 ? . 66602 H(40A) C(40) 3.563 ? . 66602 H(40A) H(27) 2.681 ? . 66602 H(40A) H(29A) 2.883 ? . 66602 H(40A) H(29C) 2.693 ? . 66602 H(40A) H(39) 2.901 ? . 66602 H(40A) H(40A) 2.878 ? . 66602 H(40A) H(41A) 3.142 ? . 66602 H(40B) C(17) 3.172 ? . 56501 H(40B) C(18) 3.338 ? . 56501 H(40B) H(17) 2.473 ? . 56501 H(40B) H(18) 2.814 ? . 56501 H(40B) H(29C) 3.426 ? . 66602 H(40B) H(41A) 3.591 ? . 66602 H(40C) C(18) 3.579 ? . 56501 H(40C) C(29) 3.442 ? . 66602 H(40C) H(17) 3.550 ? . 56501 H(40C) H(18) 2.759 ? . 56501 H(40C) H(27) 3.255 ? . 66602 H(40C) H(29C) 2.671 ? . 66602 H(41A) H(5) 2.970 ? . 75602 H(41A) H(27) 2.998 ? . 66602 H(41A) H(31A) 3.218 ? . 66602 H(41A) H(40A) 3.142 ? . 66602 H(41A) H(40B) 3.591 ? . 66602 H(41B) C(28) 3.439 ? . 65501 H(41B) H(5) 3.586 ? . 75602 H(41B) H(28A) 3.125 ? . 65501 H(41B) H(28B) 2.865 ? . 65501 H(41C) C(4) 3.481 ? . 75602 H(41C) C(5) 3.592 ? . 75602 H(41C) C(28) 3.542 ? . 65501 H(41C) H(4) 2.806 ? . 75602 H(41C) H(5) 3.010 ? . 75602 H(41C) H(28A) 3.384 ? . 65501 H(41C) H(28B) 2.981 ? . 65501 H(43A) C(21) 3.527 ? . 66502 H(43A) H(21) 3.571 ? . 66502 H(43A) H(26B) 3.441 ? . 66502 H(43A) H(43A) 3.093 ? . 66502 H(43A) H(43B) 3.231 ? . 66502 H(43B) H(26B) 3.317 ? . 66502 H(43B) H(32C) 2.750 ? . 66502 H(43B) H(43A) 3.231 ? . 66502 H(43C) C(21) 3.104 ? . 66502 H(43C) C(22) 3.315 ? . 66502 H(43C) H(21) 2.776 ? . 66502 H(43C) H(22) 3.174 ? . 66502 H(43C) H(37) 2.988 ? . 76502 H(43C) H(26B) 3.452 ? . 66502 H(43C) H(44C) 3.414 ? . 76502 H(44A) C(10) 3.308 ? . 75502 H(44A) C(11) 3.328 ? . 75502 H(44A) H(10) 2.673 ? . 75502 H(44A) H(11) 2.717 ? . 75502 H(44A) H(22) 3.148 ? . 65501 H(44B) C(21) 3.485 ? . 65501 H(44B) H(21) 2.955 ? . 65501 H(44B) H(22) 3.248 ? . 65501 H(44C) C(21) 3.216 ? . 65501 H(44C) C(22) 3.115 ? . 65501 H(44C) H(11) 3.259 ? . 75502 H(44C) H(21) 2.678 ? . 65501 H(44C) H(22) 2.472 ? . 65501 H(44C) H(37) 2.776 ? . 76502 H(44C) H(43C) 3.414 ? . 76502 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment '3c.cif' data_r60922e _database_code_depnum_ccdc_archive 'CCDC 632197' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H51 Cl N2 Ni P2' _chemical_formula_weight 763.97 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 11.861(2) _cell_length_b 12.509(3) _cell_length_c 14.959(3) _cell_angle_alpha 84.58(3) _cell_angle_beta 77.35(3) _cell_angle_gamma 64.29(3) _cell_volume 1951.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 5371 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.6 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8872 _exptl_absorpt_correction_T_max 0.9227 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 12038 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6834 _reflns_number_gt 5789 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0525P)^2^+0.0832P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6834 _refine_ls_number_parameters 459 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0881 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.21680(2) 0.14777(2) 0.289502(18) 0.01312(9) Uani 1 1 d . . . P1 P -0.02607(5) 0.24516(4) 0.21390(4) 0.01175(12) Uani 1 1 d . . . P2 P 0.40112(5) 0.01199(4) 0.30078(4) 0.01344(13) Uani 1 1 d . . . Cl1 Cl 0.22179(5) 0.22210(5) 0.41364(4) 0.02223(13) Uani 1 1 d . . . N1 N 0.04184(15) 0.26919(14) 0.28644(12) 0.0131(4) Uani 1 1 d . . . N2 N 0.23472(15) 0.06548(14) 0.18012(12) 0.0122(4) Uani 1 1 d . . . C1 C -0.00567(18) 0.38963(17) 0.31798(14) 0.0133(4) Uani 1 1 d . . . C2 C -0.11229(19) 0.43440(18) 0.38962(14) 0.0164(4) Uani 1 1 d . . . C3 C -0.1565(2) 0.55094(18) 0.41810(15) 0.0203(5) Uani 1 1 d . . . H3 H -0.2266 0.5812 0.4660 0.024 Uiso 1 1 calc R . . C4 C -0.0984(2) 0.62243(18) 0.37665(16) 0.0221(5) Uani 1 1 d . . . H4 H -0.1300 0.7005 0.3958 0.027 Uiso 1 1 calc R . . C5 C 0.0065(2) 0.57739(18) 0.30669(15) 0.0195(5) Uani 1 1 d . . . H5 H 0.0448 0.6263 0.2786 0.023 Uiso 1 1 calc R . . C6 C 0.05685(19) 0.46080(17) 0.27693(14) 0.0157(4) Uani 1 1 d . . . C7 C 0.17947(18) 0.41497(18) 0.20468(15) 0.0171(5) Uani 1 1 d . . . H7 H 0.2082 0.3294 0.1980 0.021 Uiso 1 1 calc R . . C8 C 0.1608(2) 0.4723(2) 0.11114(16) 0.0237(5) Uani 1 1 d . . . H8A H 0.0949 0.4602 0.0921 0.036 Uiso 1 1 calc R . . H8B H 0.2392 0.4369 0.0672 0.036 Uiso 1 1 calc R . . H8C H 0.1366 0.5558 0.1152 0.036 Uiso 1 1 calc R . . C9 C 0.2848(2) 0.4341(2) 0.23524(17) 0.0253(5) Uani 1 1 d . . . H9A H 0.2603 0.5176 0.2398 0.038 Uiso 1 1 calc R . . H9B H 0.3630 0.3992 0.1911 0.038 Uiso 1 1 calc R . . H9C H 0.2968 0.3975 0.2939 0.038 Uiso 1 1 calc R . . C10 C -0.17826(19) 0.35877(19) 0.43937(15) 0.0196(5) Uani 1 1 d . . . H10 H -0.1668 0.2994 0.3958 0.023 Uiso 1 1 calc R . . C11 C -0.3228(2) 0.4293(2) 0.47421(19) 0.0319(6) Uani 1 1 d . . . H11A H -0.3370 0.4771 0.5256 0.048 Uiso 1 1 calc R . . H11B H -0.3614 0.3751 0.4926 0.048 Uiso 1 1 calc R . . H11C H -0.3602 0.4795 0.4261 0.048 Uiso 1 1 calc R . . C12 C -0.1133(2) 0.2925(2) 0.51760(19) 0.0366(6) Uani 1 1 d . . . H12A H -0.0242 0.2457 0.4941 0.055 Uiso 1 1 calc R . . H12B H -0.1520 0.2415 0.5467 0.055 Uiso 1 1 calc R . . H12C H -0.1225 0.3485 0.5615 0.055 Uiso 1 1 calc R . . C13 C -0.18091(18) 0.36513(17) 0.20659(14) 0.0130(4) Uani 1 1 d . . . C14 C -0.1916(2) 0.47522(18) 0.17133(15) 0.0185(5) Uani 1 1 d . . . H14 H -0.1186 0.4875 0.1490 0.022 Uiso 1 1 calc R . . C15 C -0.3108(2) 0.56661(19) 0.16931(17) 0.0239(5) Uani 1 1 d . . . H15 H -0.3174 0.6395 0.1443 0.029 Uiso 1 1 calc R . . C16 C -0.4202(2) 0.54993(19) 0.20445(17) 0.0248(5) Uani 1 1 d . . . H16 H -0.5001 0.6116 0.2031 0.030 Uiso 1 1 calc R . . C17 C -0.41041(19) 0.44224(19) 0.24124(16) 0.0227(5) Uani 1 1 d . . . H17 H -0.4840 0.4316 0.2657 0.027 Uiso 1 1 calc R . . C18 C -0.29155(19) 0.34905(18) 0.24222(15) 0.0183(5) Uani 1 1 d . . . H18 H -0.2856 0.2760 0.2666 0.022 Uiso 1 1 calc R . . C19 C -0.05578(18) 0.11485(17) 0.23922(15) 0.0144(4) Uani 1 1 d . . . C20 C -0.0390(2) 0.05223(18) 0.32044(16) 0.0213(5) Uani 1 1 d . . . H20 H -0.0106 0.0763 0.3647 0.026 Uiso 1 1 calc R . . C21 C -0.0651(2) -0.0473(2) 0.33512(19) 0.0325(6) Uani 1 1 d . . . H21 H -0.0541 -0.0898 0.3895 0.039 Uiso 1 1 calc R . . C22 C -0.1069(2) -0.0827(2) 0.2698(2) 0.0320(6) Uani 1 1 d . . . H22 H -0.1234 -0.1495 0.2801 0.038 Uiso 1 1 calc R . . C23 C -0.1247(2) -0.02042(19) 0.18897(19) 0.0264(5) Uani 1 1 d . . . H23 H -0.1532 -0.0449 0.1451 0.032 Uiso 1 1 calc R . . C24 C -0.09994(19) 0.07826(18) 0.17390(16) 0.0187(5) Uani 1 1 d . . . H24 H -0.1127 0.1210 0.1198 0.022 Uiso 1 1 calc R . . C25 C 0.07543(18) 0.21797(17) 0.10276(14) 0.0129(4) Uani 1 1 d . . . C26 C 0.04059(19) 0.28008(17) 0.02327(14) 0.0146(4) Uani 1 1 d . . . H26 H -0.0423 0.3381 0.0258 0.018 Uiso 1 1 calc R . . C27 C 0.12688(19) 0.25688(17) -0.05901(14) 0.0167(4) Uani 1 1 d . . . H27 H 0.1029 0.2987 -0.1116 0.020 Uiso 1 1 calc R . . C28 C 0.25086(19) 0.16937(18) -0.06169(15) 0.0162(4) Uani 1 1 d . . . H28 H 0.3100 0.1532 -0.1167 0.019 Uiso 1 1 calc R . . C29 C 0.28711(19) 0.10648(17) 0.01580(15) 0.0150(4) Uani 1 1 d . . . H29 H 0.3703 0.0485 0.0120 0.018 Uiso 1 1 calc R . . C30 C 0.20101(18) 0.12801(17) 0.10059(14) 0.0133(4) Uani 1 1 d . . . C31 C 0.33185(18) -0.05110(17) 0.16736(14) 0.0141(4) Uani 1 1 d . . . C32 C 0.32633(19) -0.13307(17) 0.10378(14) 0.0141(4) Uani 1 1 d . . . C33 C 0.2097(2) -0.13481(19) 0.10370(16) 0.0220(5) Uani 1 1 d . . . H33 H 0.1351 -0.0783 0.1373 0.026 Uiso 1 1 calc R . . C34 C 0.2035(2) -0.2190(2) 0.05456(17) 0.0270(5) Uani 1 1 d . . . H34 H 0.1248 -0.2186 0.0550 0.032 Uiso 1 1 calc R . . C35 C 0.3132(2) -0.30433(19) 0.00442(16) 0.0233(5) Uani 1 1 d . . . H35 H 0.3090 -0.3619 -0.0280 0.028 Uiso 1 1 calc R . . C36 C 0.4292(2) -0.30245(18) 0.00342(15) 0.0212(5) Uani 1 1 d . . . H36 H 0.5035 -0.3589 -0.0306 0.025 Uiso 1 1 calc R . . C37 C 0.4362(2) -0.21798(18) 0.05219(15) 0.0170(4) Uani 1 1 d . . . H37 H 0.5150 -0.2178 0.0505 0.020 Uiso 1 1 calc R . . C38 C 0.42017(19) -0.09291(18) 0.22055(14) 0.0159(4) Uani 1 1 d . . . H38 H 0.4850 -0.1696 0.2156 0.019 Uiso 1 1 calc R . . C39 C 0.4179(2) -0.06684(18) 0.41017(15) 0.0189(5) Uani 1 1 d . . . H39 H 0.4107 -0.0112 0.4554 0.023 Uiso 1 1 calc R . . C40 C 0.3072(2) -0.1026(2) 0.44220(18) 0.0315(6) Uani 1 1 d . . . H40A H 0.3147 -0.1608 0.4010 0.047 Uiso 1 1 calc R . . H40B H 0.2277 -0.0339 0.4429 0.047 Uiso 1 1 calc R . . H40C H 0.3098 -0.1354 0.5028 0.047 Uiso 1 1 calc R . . C41 C 0.5471(2) -0.1734(2) 0.40566(16) 0.0285(5) Uani 1 1 d . . . H41A H 0.5497 -0.2130 0.4638 0.043 Uiso 1 1 calc R . . H41B H 0.6138 -0.1468 0.3912 0.043 Uiso 1 1 calc R . . H41C H 0.5590 -0.2273 0.3591 0.043 Uiso 1 1 calc R . . C42 C 0.53919(19) 0.04881(18) 0.26631(15) 0.0172(5) Uani 1 1 d . . . H42 H 0.6162 -0.0262 0.2557 0.021 Uiso 1 1 calc R . . C43 C 0.5305(2) 0.11549(19) 0.17534(15) 0.0224(5) Uani 1 1 d . . . H43A H 0.4574 0.1908 0.1840 0.034 Uiso 1 1 calc R . . H43B H 0.5222 0.0698 0.1312 0.034 Uiso 1 1 calc R . . H43C H 0.6064 0.1277 0.1537 0.034 Uiso 1 1 calc R . . C44 C 0.5539(2) 0.1173(2) 0.33851(16) 0.0243(5) Uani 1 1 d . . . H44A H 0.6287 0.1314 0.3168 0.036 Uiso 1 1 calc R . . H44B H 0.5623 0.0718 0.3941 0.036 Uiso 1 1 calc R . . H44C H 0.4800 0.1917 0.3502 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01212(15) 0.01203(15) 0.01398(16) -0.00227(11) -0.00458(10) -0.00263(11) P1 0.0113(3) 0.0095(3) 0.0145(3) 0.0001(2) -0.0041(2) -0.0038(2) P2 0.0127(3) 0.0133(3) 0.0133(3) -0.0006(2) -0.0043(2) -0.0037(2) Cl1 0.0197(3) 0.0229(3) 0.0205(3) -0.0090(2) -0.0084(2) -0.0020(2) N1 0.0121(8) 0.0117(8) 0.0158(9) -0.0031(7) -0.0044(7) -0.0040(7) N2 0.0100(8) 0.0100(8) 0.0144(9) -0.0015(7) -0.0037(7) -0.0015(6) C1 0.0111(10) 0.0119(10) 0.0156(11) -0.0011(8) -0.0053(8) -0.0022(8) C2 0.0157(11) 0.0175(11) 0.0171(11) 0.0009(9) -0.0074(9) -0.0060(8) C3 0.0184(11) 0.0189(11) 0.0170(12) -0.0041(9) -0.0001(9) -0.0028(9) C4 0.0250(12) 0.0120(10) 0.0251(13) -0.0055(9) -0.0031(10) -0.0039(9) C5 0.0234(12) 0.0148(10) 0.0218(12) -0.0008(9) -0.0048(9) -0.0093(9) C6 0.0145(11) 0.0149(10) 0.0167(11) -0.0005(8) -0.0059(8) -0.0039(8) C7 0.0140(11) 0.0153(11) 0.0209(12) -0.0021(9) -0.0014(9) -0.0056(8) C8 0.0217(12) 0.0285(12) 0.0218(13) 0.0000(10) -0.0034(9) -0.0119(10) C9 0.0203(12) 0.0283(13) 0.0278(13) -0.0029(10) -0.0042(10) -0.0107(10) C10 0.0185(11) 0.0197(11) 0.0191(12) -0.0009(9) -0.0015(9) -0.0076(9) C11 0.0220(13) 0.0309(13) 0.0385(16) -0.0045(12) 0.0035(11) -0.0110(10) C12 0.0323(14) 0.0510(17) 0.0341(16) 0.0213(13) -0.0132(12) -0.0259(12) C13 0.0126(10) 0.0118(10) 0.0142(11) -0.0029(8) -0.0028(8) -0.0041(8) C14 0.0163(11) 0.0197(11) 0.0202(12) 0.0005(9) -0.0032(9) -0.0086(9) C15 0.0190(12) 0.0133(11) 0.0352(14) 0.0039(10) -0.0052(10) -0.0038(9) C16 0.0158(11) 0.0186(11) 0.0333(14) 0.0005(10) -0.0064(10) -0.0005(9) C17 0.0096(11) 0.0250(12) 0.0328(14) -0.0018(10) -0.0037(9) -0.0065(9) C18 0.0172(11) 0.0147(10) 0.0236(12) 0.0013(9) -0.0060(9) -0.0068(8) C19 0.0094(10) 0.0097(10) 0.0208(12) -0.0002(8) 0.0006(8) -0.0025(8) C20 0.0183(11) 0.0172(11) 0.0261(13) 0.0038(9) -0.0059(9) -0.0053(9) C21 0.0248(13) 0.0226(12) 0.0430(16) 0.0145(11) -0.0053(11) -0.0070(10) C22 0.0193(12) 0.0160(12) 0.0595(19) 0.0002(12) -0.0021(12) -0.0091(9) C23 0.0166(11) 0.0177(11) 0.0467(16) -0.0052(11) -0.0055(10) -0.0081(9) C24 0.0129(11) 0.0166(11) 0.0252(12) -0.0013(9) -0.0043(9) -0.0044(8) C25 0.0143(10) 0.0120(10) 0.0155(11) -0.0015(8) -0.0043(8) -0.0076(8) C26 0.0162(11) 0.0100(10) 0.0191(11) -0.0024(8) -0.0054(8) -0.0056(8) C27 0.0237(12) 0.0157(10) 0.0153(11) 0.0034(9) -0.0087(9) -0.0112(9) C28 0.0188(11) 0.0178(11) 0.0141(11) -0.0026(9) -0.0009(8) -0.0104(9) C29 0.0134(10) 0.0120(10) 0.0198(11) -0.0022(8) -0.0041(8) -0.0048(8) C30 0.0149(10) 0.0117(10) 0.0167(11) -0.0017(8) -0.0046(8) -0.0076(8) C31 0.0132(10) 0.0135(10) 0.0155(11) -0.0014(8) -0.0004(8) -0.0065(8) C32 0.0173(11) 0.0113(10) 0.0142(11) 0.0022(8) -0.0063(8) -0.0054(8) C33 0.0154(11) 0.0184(11) 0.0304(13) -0.0057(10) -0.0053(9) -0.0041(9) C34 0.0228(12) 0.0262(12) 0.0369(15) -0.0057(11) -0.0104(11) -0.0118(10) C35 0.0329(13) 0.0192(11) 0.0221(13) -0.0026(9) -0.0078(10) -0.0133(10) C36 0.0241(12) 0.0160(11) 0.0181(12) -0.0053(9) -0.0007(9) -0.0042(9) C37 0.0148(10) 0.0173(11) 0.0171(11) 0.0005(9) -0.0047(8) -0.0045(8) C38 0.0134(10) 0.0138(10) 0.0178(11) -0.0020(9) -0.0050(9) -0.0021(8) C39 0.0244(12) 0.0184(11) 0.0139(11) 0.0022(9) -0.0062(9) -0.0083(9) C40 0.0380(15) 0.0376(14) 0.0254(14) 0.0092(11) -0.0060(11) -0.0241(12) C41 0.0342(14) 0.0227(12) 0.0216(13) 0.0040(10) -0.0125(10) -0.0030(10) C42 0.0128(11) 0.0166(10) 0.0201(12) -0.0018(9) -0.0040(9) -0.0036(8) C43 0.0203(12) 0.0224(12) 0.0214(12) 0.0037(10) -0.0026(9) -0.0078(9) C44 0.0266(13) 0.0278(12) 0.0237(13) -0.0026(10) -0.0062(10) -0.0153(10) _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 1.9386(17) . ? Ni1 N1 1.9773(18) . ? Ni1 P2 2.1399(10) . ? Ni1 Cl1 2.1769(8) . ? P1 N1 1.6035(17) . ? P1 C25 1.790(2) . ? P1 C19 1.802(2) . ? P1 C13 1.817(2) . ? P2 C38 1.771(2) . ? P2 C39 1.832(2) . ? P2 C42 1.844(2) . ? N1 C1 1.446(3) . ? N2 C30 1.396(3) . ? N2 C31 1.410(3) . ? C1 C2 1.402(3) . ? C1 C6 1.411(3) . ? C2 C3 1.392(3) . ? C2 C10 1.521(3) . ? C3 C4 1.379(3) . ? C3 H3 0.9300 . ? C4 C5 1.377(3) . ? C4 H4 0.9300 . ? C5 C6 1.390(3) . ? C5 H5 0.9300 . ? C6 C7 1.522(3) . ? C7 C8 1.526(3) . ? C7 C9 1.535(3) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C12 1.519(3) . ? C10 C11 1.541(3) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.390(3) . ? C13 C18 1.396(3) . ? C14 C15 1.384(3) . ? C14 H14 0.9300 . ? C15 C16 1.386(3) . ? C15 H15 0.9300 . ? C16 C17 1.372(3) . ? C16 H16 0.9300 . ? C17 C18 1.388(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.386(3) . ? C19 C24 1.398(3) . ? C20 C21 1.395(3) . ? C20 H20 0.9300 . ? C21 C22 1.371(4) . ? C21 H21 0.9300 . ? C22 C23 1.381(4) . ? C22 H22 0.9300 . ? C23 C24 1.376(3) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.397(3) . ? C25 C30 1.420(3) . ? C26 C27 1.380(3) . ? C26 H26 0.9300 . ? C27 C28 1.396(3) . ? C27 H27 0.9300 . ? C28 C29 1.378(3) . ? C28 H28 0.9300 . ? C29 C30 1.408(3) . ? C29 H29 0.9300 . ? C31 C38 1.347(3) . ? C31 C32 1.493(3) . ? C32 C37 1.391(3) . ? C32 C33 1.393(3) . ? C33 C34 1.376(3) . ? C33 H33 0.9300 . ? C34 C35 1.383(3) . ? C34 H34 0.9300 . ? C35 C36 1.383(3) . ? C35 H35 0.9300 . ? C36 C37 1.380(3) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C41 1.526(3) . ? C39 C40 1.532(3) . ? C39 H39 0.9800 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C44 1.522(3) . ? C42 C43 1.527(3) . ? C42 H42 0.9800 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? 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 95.26(7) . . ? N2 Ni1 P2 86.21(6) . . ? N1 Ni1 P2 176.29(5) . . ? N2 Ni1 Cl1 172.39(5) . . ? N1 Ni1 Cl1 92.34(6) . . ? P2 Ni1 Cl1 86.18(4) . . ? N1 P1 C25 110.13(9) . . ? N1 P1 C19 113.49(10) . . ? C25 P1 C19 104.85(9) . . ? N1 P1 C13 113.60(9) . . ? C25 P1 C13 109.34(10) . . ? C19 P1 C13 104.95(9) . . ? C38 P2 C39 106.06(10) . . ? C38 P2 C42 106.86(10) . . ? C39 P2 C42 106.31(10) . . ? C38 P2 Ni1 100.87(8) . . ? C39 P2 Ni1 117.61(8) . . ? C42 P2 Ni1 117.88(7) . . ? C1 N1 P1 117.79(13) . . ? C1 N1 Ni1 123.09(13) . . ? P1 N1 Ni1 115.23(9) . . ? C30 N2 C31 116.04(17) . . ? C30 N2 Ni1 120.90(13) . . ? C31 N2 Ni1 116.77(14) . . ? C2 C1 C6 120.49(18) . . ? C2 C1 N1 119.98(18) . . ? C6 C1 N1 119.53(18) . . ? C3 C2 C1 118.72(19) . . ? C3 C2 C10 118.95(19) . . ? C1 C2 C10 122.29(18) . . ? C4 C3 C2 121.3(2) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 119.51(19) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.7(2) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 118.20(19) . . ? C5 C6 C7 118.40(18) . . ? C1 C6 C7 123.35(18) . . ? C6 C7 C8 112.68(17) . . ? C6 C7 C9 110.71(18) . . ? C8 C7 C9 109.58(18) . . ? C6 C7 H7 107.9 . . ? C8 C7 H7 107.9 . . ? C9 C7 H7 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C2 109.68(18) . . ? C12 C10 C11 110.7(2) . . ? C2 C10 C11 113.81(18) . . ? C12 C10 H10 107.5 . . ? C2 C10 H10 107.5 . . ? C11 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 119.25(18) . . ? C14 C13 P1 121.10(15) . . ? C18 C13 P1 119.53(16) . . ? C15 C14 C13 120.16(19) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.3(2) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 119.85(19) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.5(2) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C13 119.9(2) . . ? C17 C18 H18 120.1 . . ? C13 C18 H18 120.1 . . ? C20 C19 C24 119.60(19) . . ? C20 C19 P1 122.80(17) . . ? C24 C19 P1 117.59(16) . . ? C19 C20 C21 119.3(2) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C22 C21 C20 120.3(2) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.8(2) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 119.4(2) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C19 120.6(2) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? C26 C25 C30 120.55(18) . . ? C26 C25 P1 125.03(15) . . ? C30 C25 P1 114.38(15) . . ? C27 C26 C25 121.23(18) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 118.7(2) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? C29 C28 C27 121.10(19) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C30 121.47(18) . . ? C28 C29 H29 119.3 . . ? C30 C29 H29 119.3 . . ? N2 C30 C29 122.80(18) . . ? N2 C30 C25 120.21(17) . . ? C29 C30 C25 116.99(19) . . ? C38 C31 N2 120.01(19) . . ? C38 C31 C32 119.80(18) . . ? N2 C31 C32 119.67(17) . . ? C37 C32 C33 118.29(19) . . ? C37 C32 C31 121.90(18) . . ? C33 C32 C31 119.37(18) . . ? C34 C33 C32 120.8(2) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 120.7(2) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C36 C35 C34 118.8(2) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? C37 C36 C35 120.9(2) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C36 C37 C32 120.5(2) . . ? C36 C37 H37 119.8 . . ? C32 C37 H37 119.8 . . ? C31 C38 P2 113.60(15) . . ? C31 C38 H38 123.2 . . ? P2 C38 H38 123.2 . . ? C41 C39 C40 111.69(19) . . ? C41 C39 P2 112.84(15) . . ? C40 C39 P2 109.19(16) . . ? C41 C39 H39 107.6 . . ? C40 C39 H39 107.6 . . ? P2 C39 H39 107.6 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C44 C42 C43 111.46(18) . . ? C44 C42 P2 113.95(15) . . ? C43 C42 P2 108.92(15) . . ? C44 C42 H42 107.4 . . ? C43 C42 H42 107.4 . . ? P2 C42 H42 107.4 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 P2 C38 -12.75(9) . . . . ? N1 Ni1 P2 C38 100.7(8) . . . . ? Cl1 Ni1 P2 C38 167.40(7) . . . . ? N2 Ni1 P2 C39 -127.47(10) . . . . ? N1 Ni1 P2 C39 -14.0(8) . . . . ? Cl1 Ni1 P2 C39 52.67(8) . . . . ? N2 Ni1 P2 C42 103.09(10) . . . . ? N1 Ni1 P2 C42 -143.5(8) . . . . ? Cl1 Ni1 P2 C42 -76.77(8) . . . . ? C25 P1 N1 C1 106.55(16) . . . . ? C19 P1 N1 C1 -136.27(14) . . . . ? C13 P1 N1 C1 -16.48(18) . . . . ? C25 P1 N1 Ni1 -51.97(12) . . . . ? C19 P1 N1 Ni1 65.21(12) . . . . ? C13 P1 N1 Ni1 -175.00(9) . . . . ? N2 Ni1 N1 C1 -147.23(15) . . . . ? P2 Ni1 N1 C1 99.6(8) . . . . ? Cl1 Ni1 N1 C1 33.08(15) . . . . ? N2 Ni1 N1 P1 10.02(11) . . . . ? P2 Ni1 N1 P1 -103.1(8) . . . . ? Cl1 Ni1 N1 P1 -169.67(9) . . . . ? N1 Ni1 N2 C30 47.09(15) . . . . ? P2 Ni1 N2 C30 -136.33(14) . . . . ? Cl1 Ni1 N2 C30 -135.3(3) . . . . ? N1 Ni1 N2 C31 -161.86(14) . . . . ? P2 Ni1 N2 C31 14.72(13) . . . . ? Cl1 Ni1 N2 C31 15.8(5) . . . . ? P1 N1 C1 C2 83.2(2) . . . . ? Ni1 N1 C1 C2 -120.09(18) . . . . ? P1 N1 C1 C6 -97.5(2) . . . . ? Ni1 N1 C1 C6 59.2(2) . . . . ? C6 C1 C2 C3 1.2(3) . . . . ? N1 C1 C2 C3 -179.51(18) . . . . ? C6 C1 C2 C10 -176.59(19) . . . . ? N1 C1 C2 C10 2.7(3) . . . . ? C1 C2 C3 C4 0.7(3) . . . . ? C10 C2 C3 C4 178.6(2) . . . . ? C2 C3 C4 C5 -1.0(3) . . . . ? C3 C4 C5 C6 -0.6(3) . . . . ? C4 C5 C6 C1 2.5(3) . . . . ? C4 C5 C6 C7 -175.0(2) . . . . ? C2 C1 C6 C5 -2.8(3) . . . . ? N1 C1 C6 C5 177.96(18) . . . . ? C2 C1 C6 C7 174.59(19) . . . . ? N1 C1 C6 C7 -4.7(3) . . . . ? C5 C6 C7 C8 -69.0(3) . . . . ? C1 C6 C7 C8 113.6(2) . . . . ? C5 C6 C7 C9 54.1(3) . . . . ? C1 C6 C7 C9 -123.3(2) . . . . ? C3 C2 C10 C12 -90.9(2) . . . . ? C1 C2 C10 C12 86.9(3) . . . . ? C3 C2 C10 C11 33.7(3) . . . . ? C1 C2 C10 C11 -148.5(2) . . . . ? N1 P1 C13 C14 67.6(2) . . . . ? C25 P1 C13 C14 -55.9(2) . . . . ? C19 P1 C13 C14 -167.91(18) . . . . ? N1 P1 C13 C18 -108.36(18) . . . . ? C25 P1 C13 C18 128.18(17) . . . . ? C19 P1 C13 C18 16.17(19) . . . . ? C18 C13 C14 C15 -1.8(3) . . . . ? P1 C13 C14 C15 -177.76(17) . . . . ? C13 C14 C15 C16 1.6(3) . . . . ? C14 C15 C16 C17 -0.1(4) . . . . ? C15 C16 C17 C18 -1.1(4) . . . . ? C16 C17 C18 C13 0.8(3) . . . . ? C14 C13 C18 C17 0.6(3) . . . . ? P1 C13 C18 C17 176.63(17) . . . . ? N1 P1 C19 C20 9.1(2) . . . . ? C25 P1 C19 C20 129.28(17) . . . . ? C13 P1 C19 C20 -115.55(18) . . . . ? N1 P1 C19 C24 -172.19(15) . . . . ? C25 P1 C19 C24 -51.97(17) . . . . ? C13 P1 C19 C24 63.21(18) . . . . ? C24 C19 C20 C21 0.7(3) . . . . ? P1 C19 C20 C21 179.47(16) . . . . ? C19 C20 C21 C22 0.0(3) . . . . ? C20 C21 C22 C23 -0.5(4) . . . . ? C21 C22 C23 C24 0.1(3) . . . . ? C22 C23 C24 C19 0.7(3) . . . . ? C20 C19 C24 C23 -1.1(3) . . . . ? P1 C19 C24 C23 -179.91(15) . . . . ? N1 P1 C25 C26 -125.17(17) . . . . ? C19 P1 C25 C26 112.40(18) . . . . ? C13 P1 C25 C26 0.3(2) . . . . ? N1 P1 C25 C30 52.62(16) . . . . ? C19 P1 C25 C30 -69.82(16) . . . . ? C13 P1 C25 C30 178.10(14) . . . . ? C30 C25 C26 C27 -0.6(3) . . . . ? P1 C25 C26 C27 177.03(15) . . . . ? C25 C26 C27 C28 0.1(3) . . . . ? C26 C27 C28 C29 0.3(3) . . . . ? C27 C28 C29 C30 -0.2(3) . . . . ? C31 N2 C30 C29 -28.4(3) . . . . ? Ni1 N2 C30 C29 122.90(17) . . . . ? C31 N2 C30 C25 151.77(17) . . . . ? Ni1 N2 C30 C25 -57.0(2) . . . . ? C28 C29 C30 N2 179.72(19) . . . . ? C28 C29 C30 C25 -0.4(3) . . . . ? C26 C25 C30 N2 -179.33(18) . . . . ? P1 C25 C30 N2 2.8(2) . . . . ? C26 C25 C30 C29 0.8(3) . . . . ? P1 C25 C30 C29 -177.11(14) . . . . ? C30 N2 C31 C38 141.2(2) . . . . ? Ni1 N2 C31 C38 -11.3(2) . . . . ? C30 N2 C31 C32 -47.0(2) . . . . ? Ni1 N2 C31 C32 160.52(14) . . . . ? C38 C31 C32 C37 -41.8(3) . . . . ? N2 C31 C32 C37 146.4(2) . . . . ? C38 C31 C32 C33 130.4(2) . . . . ? N2 C31 C32 C33 -41.4(3) . . . . ? C37 C32 C33 C34 0.6(3) . . . . ? C31 C32 C33 C34 -171.9(2) . . . . ? C32 C33 C34 C35 0.3(4) . . . . ? C33 C34 C35 C36 -1.0(4) . . . . ? C34 C35 C36 C37 0.7(4) . . . . ? C35 C36 C37 C32 0.3(3) . . . . ? C33 C32 C37 C36 -0.9(3) . . . . ? C31 C32 C37 C36 171.4(2) . . . . ? N2 C31 C38 P2 -1.3(3) . . . . ? C32 C31 C38 P2 -173.09(14) . . . . ? C39 P2 C38 C31 134.18(17) . . . . ? C42 P2 C38 C31 -112.71(17) . . . . ? Ni1 P2 C38 C31 11.05(17) . . . . ? C38 P2 C39 C41 59.44(18) . . . . ? C42 P2 C39 C41 -54.05(18) . . . . ? Ni1 P2 C39 C41 171.29(13) . . . . ? C38 P2 C39 C40 -65.39(17) . . . . ? C42 P2 C39 C40 -178.89(15) . . . . ? Ni1 P2 C39 C40 46.45(17) . . . . ? C38 P2 C42 C44 -167.56(15) . . . . ? C39 P2 C42 C44 -54.62(17) . . . . ? Ni1 P2 C42 C44 79.90(16) . . . . ? C38 P2 C42 C43 67.31(16) . . . . ? C39 P2 C42 C43 -179.75(14) . . . . ? Ni1 P2 C42 C43 -45.23(16) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.365 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.061 # Attachment '4b.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 632198' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H53 N3 Ni P2' _chemical_formula_sum 'C48 H53 N3 Ni P2' _chemical_formula_weight 792.58 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9490(16) _cell_length_b 10.3142(17) _cell_length_c 20.637(4) _cell_angle_alpha 81.768(5) _cell_angle_beta 87.185(7) _cell_angle_gamma 81.643(6) _cell_volume 2072.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 6366 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.582 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9024 _exptl_absorpt_correction_T_max 0.9441 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22994 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 26.02 _reflns_number_total 8156 _reflns_number_gt 6881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0478P)^2^+0.1246P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0080(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8156 _refine_ls_number_parameters 494 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0854 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.55160(2) 0.17195(2) 0.763522(10) 0.01309(8) Uani 1 1 d . . . P1 P 0.48312(5) -0.03354(5) 0.68038(2) 0.01416(11) Uani 1 1 d . . . P2 P 0.72106(4) 0.21813(4) 0.87229(2) 0.01281(11) Uani 1 1 d . . . N1 N 0.53214(15) 0.10747(14) 0.68086(7) 0.0152(3) Uani 1 1 d . . . N2 N 0.64863(14) -0.00448(14) 0.79609(7) 0.0133(3) Uani 1 1 d . . . N3 N 0.56848(14) 0.22937(14) 0.84682(7) 0.0136(3) Uani 1 1 d . . . C1 C 0.57924(18) 0.18474(17) 0.62345(8) 0.0154(4) Uani 1 1 d . . . C2 C 0.71003(19) 0.21705(18) 0.62273(9) 0.0200(4) Uani 1 1 d . . . H2 H 0.7672 0.1818 0.6584 0.024 Uiso 1 1 calc R . . C3 C 0.7585(2) 0.2999(2) 0.57082(10) 0.0269(5) Uani 1 1 d . . . H3 H 0.8481 0.3214 0.5711 0.032 Uiso 1 1 calc R . . C4 C 0.6759(2) 0.3512(2) 0.51844(10) 0.0293(5) Uani 1 1 d . . . H4 H 0.7082 0.4090 0.4829 0.035 Uiso 1 1 calc R . . C5 C 0.5471(2) 0.31810(19) 0.51816(9) 0.0267(5) Uani 1 1 d . . . H5 H 0.4911 0.3524 0.4819 0.032 Uiso 1 1 calc R . . C6 C 0.4975(2) 0.23513(18) 0.57011(9) 0.0205(4) Uani 1 1 d . . . H6 H 0.4083 0.2129 0.5693 0.025 Uiso 1 1 calc R . . C7 C 0.31705(18) -0.02748(18) 0.64656(9) 0.0170(4) Uani 1 1 d . . . C8 C 0.20790(19) 0.0490(2) 0.67457(10) 0.0256(5) Uani 1 1 d . . . H8 H 0.2233 0.0973 0.7087 0.031 Uiso 1 1 calc R . . C9 C 0.0779(2) 0.0546(2) 0.65283(11) 0.0309(5) Uani 1 1 d . . . H9 H 0.0043 0.1073 0.6719 0.037 Uiso 1 1 calc R . . C10 C 0.0541(2) -0.0161(2) 0.60334(10) 0.0297(5) Uani 1 1 d . . . H10 H -0.0356 -0.0126 0.5888 0.036 Uiso 1 1 calc R . . C11 C 0.1610(2) -0.0913(2) 0.57536(10) 0.0281(5) Uani 1 1 d . . . H11 H 0.1446 -0.1392 0.5412 0.034 Uiso 1 1 calc R . . C12 C 0.2925(2) -0.09795(19) 0.59654(9) 0.0231(4) Uani 1 1 d . . . H12 H 0.3656 -0.1504 0.5770 0.028 Uiso 1 1 calc R . . C13 C 0.59842(18) -0.14628(18) 0.63590(9) 0.0172(4) Uani 1 1 d . . . C14 C 0.6650(2) -0.1019(2) 0.57737(9) 0.0235(4) Uani 1 1 d . . . H14 H 0.6490 -0.0111 0.5595 0.028 Uiso 1 1 calc R . . C15 C 0.7539(2) -0.1894(2) 0.54529(10) 0.0277(5) Uani 1 1 d . . . H15 H 0.7995 -0.1579 0.5059 0.033 Uiso 1 1 calc R . . C16 C 0.7770(2) -0.3219(2) 0.57008(10) 0.0294(5) Uani 1 1 d . . . H16 H 0.8389 -0.3812 0.5481 0.035 Uiso 1 1 calc R . . C17 C 0.7096(2) -0.3680(2) 0.62695(10) 0.0337(5) Uani 1 1 d . . . H17 H 0.7241 -0.4595 0.6436 0.040 Uiso 1 1 calc R . . C18 C 0.6211(2) -0.2815(2) 0.65993(10) 0.0274(5) Uani 1 1 d . . . H18 H 0.5755 -0.3141 0.6991 0.033 Uiso 1 1 calc R . . C19 C 0.46957(18) -0.11426(17) 0.76257(8) 0.0150(4) Uani 1 1 d . . . C20 C 0.56694(17) -0.10381(17) 0.80862(8) 0.0135(4) Uani 1 1 d . . . C21 C 0.56661(18) -0.18714(17) 0.86886(8) 0.0153(4) Uani 1 1 d . . . H21 H 0.6312 -0.1824 0.9006 0.018 Uiso 1 1 calc R . . C22 C 0.47403(18) -0.27567(18) 0.88274(9) 0.0181(4) Uani 1 1 d . . . H22 H 0.4765 -0.3314 0.9236 0.022 Uiso 1 1 calc R . . C23 C 0.37739(19) -0.28440(19) 0.83777(9) 0.0212(4) Uani 1 1 d . . . H23 H 0.3137 -0.3451 0.8479 0.025 Uiso 1 1 calc R . . C24 C 0.37500(18) -0.20392(18) 0.77824(9) 0.0195(4) Uani 1 1 d . . . H24 H 0.3087 -0.2091 0.7474 0.023 Uiso 1 1 calc R . . C25 C 0.77235(17) -0.02186(17) 0.82423(8) 0.0133(4) Uani 1 1 d . . . C26 C 0.82159(17) 0.07683(17) 0.84940(8) 0.0149(4) Uani 1 1 d . . . H26 H 0.9169 0.0683 0.8549 0.018 Uiso 1 1 calc R . . C27 C 0.86515(17) -0.14870(17) 0.81978(8) 0.0147(4) Uani 1 1 d . . . C28 C 0.88821(19) -0.19430(18) 0.75937(9) 0.0199(4) Uani 1 1 d . . . H28 H 0.8406 -0.1482 0.7222 0.024 Uiso 1 1 calc R . . C29 C 0.98077(19) -0.30722(19) 0.75309(10) 0.0235(4) Uani 1 1 d . . . H29 H 0.9980 -0.3365 0.7115 0.028 Uiso 1 1 calc R . . C30 C 1.04755(19) -0.37677(19) 0.80723(10) 0.0250(4) Uani 1 1 d . . . H30 H 1.1102 -0.4541 0.8030 0.030 Uiso 1 1 calc R . . C31 C 1.02283(19) -0.33329(19) 0.86780(10) 0.0249(4) Uani 1 1 d . . . H31 H 1.0674 -0.3818 0.9052 0.030 Uiso 1 1 calc R . . C32 C 0.93295(18) -0.21883(18) 0.87393(9) 0.0189(4) Uani 1 1 d . . . H32 H 0.9179 -0.1885 0.9154 0.023 Uiso 1 1 calc R . . C33 C 0.72089(18) 0.20060(18) 0.96196(8) 0.0160(4) Uani 1 1 d . . . H33 H 0.6631 0.2800 0.9760 0.019 Uiso 1 1 calc R . . C34 C 0.6559(2) 0.07865(19) 0.99044(9) 0.0239(4) Uani 1 1 d . . . H34A H 0.7113 -0.0008 0.9777 0.036 Uiso 1 1 calc R . . H34B H 0.5643 0.0863 0.9736 0.036 Uiso 1 1 calc R . . H34C H 0.6504 0.0723 1.0383 0.036 Uiso 1 1 calc R . . C35 C 0.8621(2) 0.1933(2) 0.98901(10) 0.0311(5) Uani 1 1 d . . . H35A H 0.8563 0.1799 1.0370 0.047 Uiso 1 1 calc R . . H35B H 0.8985 0.2761 0.9737 0.047 Uiso 1 1 calc R . . H35C H 0.9225 0.1193 0.9737 0.047 Uiso 1 1 calc R . . C36 C 0.81078(18) 0.35766(17) 0.83965(8) 0.0165(4) Uani 1 1 d . . . H36 H 0.9007 0.3449 0.8610 0.020 Uiso 1 1 calc R . . C37 C 0.7318(2) 0.48937(18) 0.85435(10) 0.0249(4) Uani 1 1 d . . . H37A H 0.7804 0.5620 0.8345 0.037 Uiso 1 1 calc R . . H37B H 0.7235 0.4895 0.9019 0.037 Uiso 1 1 calc R . . H37C H 0.6410 0.5010 0.8362 0.037 Uiso 1 1 calc R . . C38 C 0.8362(2) 0.3597(2) 0.76570(9) 0.0253(4) Uani 1 1 d . . . H38A H 0.7497 0.3623 0.7445 0.038 Uiso 1 1 calc R . . H38B H 0.8973 0.2798 0.7574 0.038 Uiso 1 1 calc R . . H38C H 0.8780 0.4381 0.7479 0.038 Uiso 1 1 calc R . . C39 C 0.44750(17) 0.26933(17) 0.88142(8) 0.0144(4) Uani 1 1 d . . . C40 C 0.42935(18) 0.37267(18) 0.91961(9) 0.0182(4) Uani 1 1 d . . . H40 H 0.5022 0.4213 0.9231 0.022 Uiso 1 1 calc R . . C41 C 0.3065(2) 0.40524(19) 0.95254(9) 0.0230(4) Uani 1 1 d . . . H41 H 0.2971 0.4746 0.9789 0.028 Uiso 1 1 calc R . . C42 C 0.19818(19) 0.3383(2) 0.94744(10) 0.0250(5) Uani 1 1 d . . . H42 H 0.1147 0.3605 0.9704 0.030 Uiso 1 1 calc R . . C43 C 0.21248(19) 0.2380(2) 0.90844(9) 0.0243(4) Uani 1 1 d . . . H43 H 0.1378 0.1925 0.9039 0.029 Uiso 1 1 calc R . . C44 C 0.33529(18) 0.20369(18) 0.87606(9) 0.0196(4) Uani 1 1 d . . . H44 H 0.3436 0.1344 0.8497 0.024 Uiso 1 1 calc R . . C45 C 0.46375(19) 0.34902(17) 0.72895(8) 0.0178(4) Uani 1 1 d . . . H45A H 0.4577 0.4053 0.7643 0.021 Uiso 1 1 calc R . . H45B H 0.5232 0.3869 0.6935 0.021 Uiso 1 1 calc R . . C46 C 0.32242(19) 0.35785(18) 0.70220(9) 0.0208(4) Uani 1 1 d . . . H46A H 0.2581 0.3390 0.7393 0.025 Uiso 1 1 calc R . . H46B H 0.3235 0.2883 0.6736 0.025 Uiso 1 1 calc R . . C47 C 0.2696(2) 0.4917(2) 0.66317(9) 0.0256(5) Uani 1 1 d . . . H47A H 0.2528 0.5594 0.6932 0.031 Uiso 1 1 calc R . . H47B H 0.3400 0.5180 0.6303 0.031 Uiso 1 1 calc R . . C48 C 0.1388(2) 0.4877(2) 0.62839(10) 0.0326(5) Uani 1 1 d . . . H48A H 0.1567 0.4260 0.5961 0.049 Uiso 1 1 calc R . . H48B H 0.1057 0.5763 0.6062 0.049 Uiso 1 1 calc R . . H48C H 0.0699 0.4584 0.6606 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01502(13) 0.01165(13) 0.01259(13) -0.00233(9) -0.00282(9) -0.00042(9) P1 0.0143(2) 0.0145(2) 0.0142(2) -0.00352(18) -0.00345(18) -0.00120(18) P2 0.0117(2) 0.0134(2) 0.0142(2) -0.00378(18) -0.00066(17) -0.00292(17) N1 0.0184(8) 0.0139(8) 0.0139(8) -0.0025(6) -0.0026(6) -0.0028(6) N2 0.0128(8) 0.0122(8) 0.0158(8) -0.0026(6) -0.0043(6) -0.0023(6) N3 0.0114(7) 0.0164(8) 0.0134(7) -0.0034(6) -0.0002(6) -0.0021(6) C1 0.0212(10) 0.0117(9) 0.0130(9) -0.0031(7) -0.0014(7) 0.0006(7) C2 0.0205(10) 0.0204(10) 0.0192(10) -0.0046(8) -0.0023(8) -0.0009(8) C3 0.0283(11) 0.0270(11) 0.0281(11) -0.0095(9) 0.0063(9) -0.0094(9) C4 0.0460(14) 0.0221(11) 0.0193(10) -0.0010(8) 0.0077(9) -0.0077(10) C5 0.0404(13) 0.0216(11) 0.0156(10) -0.0004(8) -0.0052(9) 0.0030(9) C6 0.0229(10) 0.0198(10) 0.0185(10) -0.0037(8) -0.0037(8) 0.0000(8) C7 0.0171(9) 0.0155(10) 0.0189(9) -0.0015(7) -0.0039(7) -0.0037(7) C8 0.0209(11) 0.0270(11) 0.0311(11) -0.0110(9) -0.0047(8) -0.0023(8) C9 0.0170(10) 0.0336(12) 0.0429(13) -0.0117(10) -0.0051(9) 0.0018(9) C10 0.0202(11) 0.0351(13) 0.0352(12) -0.0028(10) -0.0101(9) -0.0073(9) C11 0.0290(11) 0.0328(12) 0.0261(11) -0.0083(9) -0.0118(9) -0.0081(9) C12 0.0222(10) 0.0254(11) 0.0224(10) -0.0063(8) -0.0059(8) -0.0014(8) C13 0.0167(9) 0.0180(10) 0.0182(9) -0.0064(7) -0.0057(7) -0.0007(7) C14 0.0260(11) 0.0195(10) 0.0264(11) -0.0069(8) 0.0023(8) -0.0053(8) C15 0.0262(11) 0.0286(12) 0.0303(12) -0.0119(9) 0.0083(9) -0.0061(9) C16 0.0265(11) 0.0286(12) 0.0323(12) -0.0139(9) -0.0070(9) 0.0099(9) C17 0.0523(15) 0.0198(11) 0.0248(11) -0.0030(9) -0.0048(10) 0.0105(10) C18 0.0376(13) 0.0231(11) 0.0190(10) -0.0031(8) -0.0011(9) 0.0038(9) C19 0.0156(9) 0.0146(9) 0.0149(9) -0.0037(7) -0.0013(7) -0.0010(7) C20 0.0116(9) 0.0114(9) 0.0174(9) -0.0053(7) 0.0009(7) 0.0022(7) C21 0.0156(9) 0.0146(9) 0.0154(9) -0.0037(7) -0.0019(7) 0.0013(7) C22 0.0207(10) 0.0158(10) 0.0165(9) -0.0011(7) 0.0031(7) -0.0001(7) C23 0.0163(10) 0.0193(10) 0.0283(11) -0.0013(8) 0.0012(8) -0.0062(8) C24 0.0164(10) 0.0218(10) 0.0215(10) -0.0034(8) -0.0025(8) -0.0054(8) C25 0.0134(9) 0.0151(9) 0.0112(9) -0.0008(7) 0.0010(7) -0.0021(7) C26 0.0101(9) 0.0165(9) 0.0188(9) -0.0053(7) 0.0001(7) -0.0013(7) C27 0.0109(9) 0.0137(9) 0.0208(9) -0.0037(7) -0.0003(7) -0.0043(7) C28 0.0185(10) 0.0198(10) 0.0216(10) -0.0034(8) -0.0003(8) -0.0030(8) C29 0.0191(10) 0.0231(11) 0.0300(11) -0.0115(9) 0.0048(8) -0.0033(8) C30 0.0137(10) 0.0191(10) 0.0431(13) -0.0101(9) -0.0007(9) 0.0001(8) C31 0.0189(10) 0.0194(11) 0.0353(12) -0.0020(9) -0.0093(8) 0.0018(8) C32 0.0161(9) 0.0195(10) 0.0220(10) -0.0058(8) -0.0041(7) -0.0009(7) C33 0.0159(9) 0.0188(10) 0.0139(9) -0.0041(7) 0.0000(7) -0.0027(7) C34 0.0270(11) 0.0265(11) 0.0176(10) 0.0016(8) -0.0009(8) -0.0064(9) C35 0.0231(11) 0.0536(15) 0.0194(10) -0.0064(10) -0.0054(8) -0.0120(10) C36 0.0156(9) 0.0172(10) 0.0182(9) -0.0053(7) 0.0020(7) -0.0050(7) C37 0.0249(11) 0.0175(10) 0.0335(12) -0.0059(8) 0.0078(9) -0.0077(8) C38 0.0320(12) 0.0240(11) 0.0216(10) -0.0035(8) 0.0059(8) -0.0116(9) C39 0.0139(9) 0.0152(9) 0.0118(9) 0.0033(7) -0.0014(7) 0.0006(7) C40 0.0172(10) 0.0171(10) 0.0200(10) -0.0017(8) 0.0002(7) -0.0024(7) C41 0.0249(11) 0.0204(10) 0.0215(10) -0.0034(8) 0.0034(8) 0.0032(8) C42 0.0154(10) 0.0285(11) 0.0273(11) 0.0011(9) 0.0066(8) 0.0029(8) C43 0.0135(10) 0.0276(11) 0.0311(11) 0.0003(9) 0.0006(8) -0.0048(8) C44 0.0193(10) 0.0191(10) 0.0204(10) -0.0023(8) -0.0011(8) -0.0028(8) C45 0.0251(10) 0.0150(10) 0.0130(9) -0.0019(7) -0.0013(7) -0.0012(8) C46 0.0235(10) 0.0198(10) 0.0174(10) -0.0017(8) -0.0004(8) 0.0021(8) C47 0.0240(11) 0.0261(11) 0.0222(11) 0.0024(8) 0.0009(8) 0.0050(8) C48 0.0275(12) 0.0402(14) 0.0251(11) 0.0007(10) -0.0027(9) 0.0074(10) _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 N3 1.9190(14) . ? Ni1 N1 1.9453(15) . ? Ni1 C45 1.9577(17) . ? Ni1 N2 1.9743(14) . ? P1 N1 1.6012(15) . ? P1 C19 1.7871(18) . ? P1 C7 1.8144(18) . ? P1 C13 1.8236(18) . ? P2 N3 1.6137(15) . ? P2 C26 1.7535(18) . ? P2 C36 1.8326(18) . ? P2 C33 1.8332(18) . ? N1 C1 1.429(2) . ? N2 C25 1.364(2) . ? N2 C20 1.387(2) . ? N3 C39 1.409(2) . ? C1 C2 1.388(3) . ? C1 C6 1.394(2) . ? C2 C3 1.384(3) . ? C2 H2 0.9500 . ? C3 C4 1.386(3) . ? C3 H3 0.9500 . ? C4 C5 1.374(3) . ? C4 H4 0.9500 . ? C5 C6 1.390(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.394(3) . ? C7 C8 1.398(3) . ? C8 C9 1.380(3) . ? C8 H8 0.9500 . ? C9 C10 1.385(3) . ? C9 H9 0.9500 . ? C10 C11 1.376(3) . ? C10 H10 0.9500 . ? C11 C12 1.389(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.399(3) . ? C13 C18 1.401(3) . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 C16 1.379(3) . ? C15 H15 0.9500 . ? C16 C17 1.381(3) . ? C16 H16 0.9500 . ? C17 C18 1.386(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.408(2) . ? C19 C20 1.415(2) . ? C20 C21 1.407(2) . ? C21 C22 1.381(2) . ? C21 H21 0.9500 . ? C22 C23 1.389(3) . ? C22 H22 0.9500 . ? C23 C24 1.380(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.367(2) . ? C25 C27 1.499(2) . ? C26 H26 0.9500 . ? C27 C32 1.388(2) . ? C27 C28 1.392(2) . ? C28 C29 1.393(3) . ? C28 H28 0.9500 . ? C29 C30 1.382(3) . ? C29 H29 0.9500 . ? C30 C31 1.387(3) . ? C30 H30 0.9500 . ? C31 C32 1.391(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C35 1.525(2) . ? C33 C34 1.527(3) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.529(2) . ? C36 C38 1.533(2) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.400(2) . ? C39 C44 1.404(2) . ? C40 C41 1.391(3) . ? C40 H40 0.9500 . ? C41 C42 1.378(3) . ? C41 H41 0.9500 . ? C42 C43 1.386(3) . ? C42 H42 0.9500 . ? C43 C44 1.388(3) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.521(3) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.531(2) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.525(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ni1 N1 177.77(6) . . ? N3 Ni1 C45 90.20(7) . . ? N1 Ni1 C45 91.40(7) . . ? N3 Ni1 N2 90.39(6) . . ? N1 Ni1 N2 88.09(6) . . ? C45 Ni1 N2 177.15(7) . . ? N1 P1 C19 109.49(8) . . ? N1 P1 C7 115.03(8) . . ? C19 P1 C7 105.18(8) . . ? N1 P1 C13 114.16(8) . . ? C19 P1 C13 106.59(8) . . ? C7 P1 C13 105.68(8) . . ? N3 P2 C26 110.46(8) . . ? N3 P2 C36 114.55(8) . . ? C26 P2 C36 105.83(8) . . ? N3 P2 C33 110.69(8) . . ? C26 P2 C33 106.65(8) . . ? C36 P2 C33 108.25(8) . . ? C1 N1 P1 123.34(12) . . ? C1 N1 Ni1 116.10(11) . . ? P1 N1 Ni1 120.13(8) . . ? C25 N2 C20 119.38(14) . . ? C25 N2 Ni1 122.67(12) . . ? C20 N2 Ni1 114.70(11) . . ? C39 N3 P2 126.34(12) . . ? C39 N3 Ni1 117.36(11) . . ? P2 N3 Ni1 116.18(8) . . ? C2 C1 C6 118.82(17) . . ? C2 C1 N1 118.02(15) . . ? C6 C1 N1 123.05(16) . . ? C3 C2 C1 121.05(18) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 119.80(19) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 119.61(18) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.98(18) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 119.72(18) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? C12 C7 C8 119.04(17) . . ? C12 C7 P1 123.77(14) . . ? C8 C7 P1 117.15(14) . . ? C9 C8 C7 120.37(19) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.31(19) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 119.72(19) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 120.74(19) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C7 119.82(18) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C14 C13 C18 118.35(17) . . ? C14 C13 P1 121.76(14) . . ? C18 C13 P1 119.88(14) . . ? C15 C14 C13 120.49(18) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 120.52(19) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 119.77(19) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 120.41(19) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 120.43(19) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? C24 C19 C20 120.06(16) . . ? C24 C19 P1 119.36(14) . . ? C20 C19 P1 119.86(13) . . ? N2 C20 C21 122.32(16) . . ? N2 C20 C19 119.62(15) . . ? C21 C20 C19 117.71(16) . . ? C22 C21 C20 121.16(17) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 120.98(17) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C24 C23 C22 119.26(17) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C19 120.82(17) . . ? C23 C24 H24 119.6 . . ? C19 C24 H24 119.6 . . ? N2 C25 C26 122.74(16) . . ? N2 C25 C27 118.44(15) . . ? C26 C25 C27 118.35(15) . . ? C25 C26 P2 124.52(14) . . ? C25 C26 H26 117.7 . . ? P2 C26 H26 117.7 . . ? C32 C27 C28 119.22(16) . . ? C32 C27 C25 121.55(16) . . ? C28 C27 C25 119.17(15) . . ? C27 C28 C29 120.27(17) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 120.17(18) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 119.77(18) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C30 C31 C32 120.19(18) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C27 C32 C31 120.34(18) . . ? C27 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C35 C33 C34 110.61(16) . . ? C35 C33 P2 113.18(13) . . ? C34 C33 P2 109.31(12) . . ? C35 C33 H33 107.9 . . ? C34 C33 H33 107.9 . . ? P2 C33 H33 107.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C38 110.47(15) . . ? C37 C36 P2 111.61(12) . . ? C38 C36 P2 109.72(13) . . ? C37 C36 H36 108.3 . . ? C38 C36 H36 108.3 . . ? P2 C36 H36 108.3 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C44 117.19(16) . . ? C40 C39 N3 124.77(16) . . ? C44 C39 N3 118.02(16) . . ? C41 C40 C39 121.06(18) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C42 C41 C40 120.83(19) . . ? C42 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C41 C42 C43 119.17(17) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C42 C43 C44 120.39(19) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C39 121.33(18) . . ? C43 C44 H44 119.3 . . ? C39 C44 H44 119.3 . . ? C46 C45 Ni1 116.39(13) . . ? C46 C45 H45A 108.2 . . ? Ni1 C45 H45A 108.2 . . ? C46 C45 H45B 108.2 . . ? Ni1 C45 H45B 108.2 . . ? H45A C45 H45B 107.3 . . ? C45 C46 C47 114.62(16) . . ? C45 C46 H46A 108.6 . . ? C47 C46 H46A 108.6 . . ? C45 C46 H46B 108.6 . . ? C47 C46 H46B 108.6 . . ? H46A C46 H46B 107.6 . . ? C48 C47 C46 112.16(17) . . ? C48 C47 H47A 109.2 . . ? C46 C47 H47A 109.2 . . ? C48 C47 H47B 109.2 . . ? C46 C47 H47B 109.2 . . ? H47A C47 H47B 107.9 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C19 P1 N1 C1 166.85(13) . . . . ? C7 P1 N1 C1 -74.99(15) . . . . ? C13 P1 N1 C1 47.46(16) . . . . ? C19 P1 N1 Ni1 -5.32(12) . . . . ? C7 P1 N1 Ni1 112.84(10) . . . . ? C13 P1 N1 Ni1 -124.71(9) . . . . ? N3 Ni1 N1 C1 -173.5(15) . . . . ? C45 Ni1 N1 C1 50.79(13) . . . . ? N2 Ni1 N1 C1 -126.40(12) . . . . ? N3 Ni1 N1 P1 -0.8(16) . . . . ? C45 Ni1 N1 P1 -136.49(10) . . . . ? N2 Ni1 N1 P1 46.32(10) . . . . ? N3 Ni1 N2 C25 -53.07(14) . . . . ? N1 Ni1 N2 C25 128.56(14) . . . . ? C45 Ni1 N2 C25 48.8(14) . . . . ? N3 Ni1 N2 C20 106.41(12) . . . . ? N1 Ni1 N2 C20 -71.95(12) . . . . ? C45 Ni1 N2 C20 -151.7(13) . . . . ? C26 P2 N3 C39 140.06(14) . . . . ? C36 P2 N3 C39 -100.56(15) . . . . ? C33 P2 N3 C39 22.16(17) . . . . ? C26 P2 N3 Ni1 -35.81(11) . . . . ? C36 P2 N3 Ni1 83.57(10) . . . . ? C33 P2 N3 Ni1 -153.71(9) . . . . ? N1 Ni1 N3 C39 -72.0(16) . . . . ? C45 Ni1 N3 C39 63.74(13) . . . . ? N2 Ni1 N3 C39 -119.05(12) . . . . ? N1 Ni1 N3 P2 104.2(15) . . . . ? C45 Ni1 N3 P2 -120.01(10) . . . . ? N2 Ni1 N3 P2 57.21(9) . . . . ? P1 N1 C1 C2 -120.88(16) . . . . ? Ni1 N1 C1 C2 51.58(19) . . . . ? P1 N1 C1 C6 62.9(2) . . . . ? Ni1 N1 C1 C6 -124.59(16) . . . . ? C6 C1 C2 C3 1.3(3) . . . . ? N1 C1 C2 C3 -175.07(16) . . . . ? C1 C2 C3 C4 -0.3(3) . . . . ? C2 C3 C4 C5 -0.8(3) . . . . ? C3 C4 C5 C6 0.9(3) . . . . ? C4 C5 C6 C1 0.1(3) . . . . ? C2 C1 C6 C5 -1.2(3) . . . . ? N1 C1 C6 C5 174.96(16) . . . . ? N1 P1 C7 C12 126.71(16) . . . . ? C19 P1 C7 C12 -112.74(16) . . . . ? C13 P1 C7 C12 -0.19(18) . . . . ? N1 P1 C7 C8 -55.73(17) . . . . ? C19 P1 C7 C8 64.82(16) . . . . ? C13 P1 C7 C8 177.37(15) . . . . ? C12 C7 C8 C9 -0.1(3) . . . . ? P1 C7 C8 C9 -177.82(16) . . . . ? C7 C8 C9 C10 0.4(3) . . . . ? C8 C9 C10 C11 -0.6(3) . . . . ? C9 C10 C11 C12 0.5(3) . . . . ? C10 C11 C12 C7 -0.2(3) . . . . ? C8 C7 C12 C11 0.0(3) . . . . ? P1 C7 C12 C11 177.54(15) . . . . ? N1 P1 C13 C14 -38.92(18) . . . . ? C19 P1 C13 C14 -159.94(15) . . . . ? C7 P1 C13 C14 88.50(16) . . . . ? N1 P1 C13 C18 141.75(15) . . . . ? C19 P1 C13 C18 20.73(18) . . . . ? C7 P1 C13 C18 -90.83(17) . . . . ? C18 C13 C14 C15 -1.9(3) . . . . ? P1 C13 C14 C15 178.78(15) . . . . ? C13 C14 C15 C16 0.9(3) . . . . ? C14 C15 C16 C17 0.7(3) . . . . ? C15 C16 C17 C18 -1.3(3) . . . . ? C16 C17 C18 C13 0.2(3) . . . . ? C14 C13 C18 C17 1.3(3) . . . . ? P1 C13 C18 C17 -179.30(17) . . . . ? N1 P1 C19 C24 151.18(14) . . . . ? C7 P1 C19 C24 27.04(16) . . . . ? C13 P1 C19 C24 -84.87(15) . . . . ? N1 P1 C19 C20 -38.56(16) . . . . ? C7 P1 C19 C20 -162.70(14) . . . . ? C13 P1 C19 C20 85.40(15) . . . . ? C25 N2 C20 C21 32.4(2) . . . . ? Ni1 N2 C20 C21 -127.85(14) . . . . ? C25 N2 C20 C19 -154.54(16) . . . . ? Ni1 N2 C20 C19 45.25(19) . . . . ? C24 C19 C20 N2 -172.18(16) . . . . ? P1 C19 C20 N2 17.6(2) . . . . ? C24 C19 C20 C21 1.2(2) . . . . ? P1 C19 C20 C21 -168.96(12) . . . . ? N2 C20 C21 C22 172.91(16) . . . . ? C19 C20 C21 C22 -0.3(2) . . . . ? C20 C21 C22 C23 -0.6(3) . . . . ? C21 C22 C23 C24 0.5(3) . . . . ? C22 C23 C24 C19 0.4(3) . . . . ? C20 C19 C24 C23 -1.3(3) . . . . ? P1 C19 C24 C23 168.92(14) . . . . ? C20 N2 C25 C26 -139.13(17) . . . . ? Ni1 N2 C25 C26 19.4(2) . . . . ? C20 N2 C25 C27 48.8(2) . . . . ? Ni1 N2 C25 C27 -152.64(12) . . . . ? N2 C25 C26 P2 20.3(2) . . . . ? C27 C25 C26 P2 -167.67(13) . . . . ? N3 P2 C26 C25 -10.94(18) . . . . ? C36 P2 C26 C25 -135.47(16) . . . . ? C33 P2 C26 C25 109.40(16) . . . . ? N2 C25 C27 C32 -134.12(17) . . . . ? C26 C25 C27 C32 53.4(2) . . . . ? N2 C25 C27 C28 48.6(2) . . . . ? C26 C25 C27 C28 -123.86(19) . . . . ? C32 C27 C28 C29 -1.5(3) . . . . ? C25 C27 C28 C29 175.82(16) . . . . ? C27 C28 C29 C30 1.8(3) . . . . ? C28 C29 C30 C31 -0.4(3) . . . . ? C29 C30 C31 C32 -1.1(3) . . . . ? C28 C27 C32 C31 0.0(3) . . . . ? C25 C27 C32 C31 -177.30(17) . . . . ? C30 C31 C32 C27 1.3(3) . . . . ? N3 P2 C33 C35 -178.40(14) . . . . ? C26 P2 C33 C35 61.40(16) . . . . ? C36 P2 C33 C35 -52.09(16) . . . . ? N3 P2 C33 C34 57.83(14) . . . . ? C26 P2 C33 C34 -62.37(14) . . . . ? C36 P2 C33 C34 -175.85(12) . . . . ? N3 P2 C36 C37 56.38(15) . . . . ? C26 P2 C36 C37 178.32(13) . . . . ? C33 P2 C36 C37 -67.65(15) . . . . ? N3 P2 C36 C38 -66.41(15) . . . . ? C26 P2 C36 C38 55.53(15) . . . . ? C33 P2 C36 C38 169.56(13) . . . . ? P2 N3 C39 C40 40.3(2) . . . . ? Ni1 N3 C39 C40 -143.83(15) . . . . ? P2 N3 C39 C44 -141.50(14) . . . . ? Ni1 N3 C39 C44 34.33(19) . . . . ? C44 C39 C40 C41 2.2(3) . . . . ? N3 C39 C40 C41 -179.64(16) . . . . ? C39 C40 C41 C42 -1.3(3) . . . . ? C40 C41 C42 C43 -0.5(3) . . . . ? C41 C42 C43 C44 1.4(3) . . . . ? C42 C43 C44 C39 -0.4(3) . . . . ? C40 C39 C44 C43 -1.4(3) . . . . ? N3 C39 C44 C43 -179.67(16) . . . . ? N3 Ni1 C45 C46 -122.18(13) . . . . ? N1 Ni1 C45 C46 56.26(14) . . . . ? N2 Ni1 C45 C46 136.0(13) . . . . ? Ni1 C45 C46 C47 -167.98(13) . . . . ? C45 C46 C47 C48 170.64(16) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.314 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.057