# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Zhong-Xia Wang' _publ_contact_author_email zxwang@ustc.edu.cn _publ_author_name 'Zhong-Xia Wang' data_110101b _database_code_depnum_ccdc_archive 'CCDC 878348' #TrackingRef '- 2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H26 Cl4 N3 Ni P' _chemical_formula_weight 648.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.1681(11) _cell_length_b 16.3886(15) _cell_length_c 14.9929(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.7500(10) _cell_angle_gamma 90.00 _cell_volume 2979.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2560 _cell_measurement_theta_min 2.418 _cell_measurement_theta_max 20.409 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 1.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7362 _exptl_absorpt_correction_T_max 0.7959 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 15435 _diffrn_reflns_av_R_equivalents 0.0826 _diffrn_reflns_av_sigmaI/netI 0.0931 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5256 _reflns_number_gt 2827 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5256 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1249 _refine_ls_wR_factor_gt 0.1108 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.31456(5) 0.59167(3) 0.60908(4) 0.0467(2) Uani 1 1 d . . . Cl1 Cl 0.26538(11) 0.59683(7) 0.46358(8) 0.0623(4) Uani 1 1 d . . . Cl2 Cl 0.28096(13) 0.47595(8) 0.68011(11) 0.0909(5) Uani 1 1 d . . . Cl3 Cl 0.4610(7) 0.541(2) 0.8745(13) 0.185(9) Uani 0.54(4) 1 d P A 1 Cl4 Cl 0.6342(14) 0.4321(14) 0.8354(19) 0.186(6) Uani 0.54(4) 1 d P A 1 Cl3' Cl 0.602(2) 0.4233(12) 0.8779(19) 0.180(8) Uani 0.46(4) 1 d P A 2 Cl4' Cl 0.498(3) 0.5839(11) 0.8923(7) 0.174(8) Uani 0.46(4) 1 d P A 2 N1 N 0.4744(3) 0.6122(2) 0.6352(3) 0.0501(10) Uani 1 1 d . . . N2 N 0.2998(3) 0.69643(19) 0.6750(2) 0.0428(9) Uani 1 1 d . . . N3 N 0.1946(3) 0.8419(2) 0.6500(3) 0.0506(10) Uani 1 1 d . . . H3 H 0.1618 0.8780 0.6798 0.061 Uiso 1 1 calc R . . P1 P 0.18842(9) 0.74677(7) 0.68347(8) 0.0437(3) Uani 1 1 d . . . C1 C 0.5585(4) 0.5682(3) 0.6131(3) 0.0617(14) Uani 1 1 d . . . H1 H 0.5443 0.5204 0.5808 0.074 Uiso 1 1 calc R . . C2 C 0.6674(4) 0.5901(3) 0.6357(4) 0.0678(15) Uani 1 1 d . . . H2 H 0.7243 0.5570 0.6189 0.081 Uiso 1 1 calc R . . C3 C 0.6905(4) 0.6586(3) 0.6817(4) 0.0653(15) Uani 1 1 d . . . H3A H 0.7636 0.6736 0.6958 0.078 Uiso 1 1 calc R . . C4 C 0.6049(4) 0.7085(3) 0.7089(3) 0.0539(13) Uani 1 1 d . . . C5 C 0.4966(4) 0.6832(3) 0.6831(3) 0.0468(12) Uani 1 1 d . . . C6 C 0.4040(4) 0.7281(3) 0.7063(3) 0.0453(11) Uani 1 1 d . . . C7 C 0.4251(4) 0.7978(3) 0.7574(3) 0.0552(13) Uani 1 1 d . . . H7 H 0.3664 0.8287 0.7747 0.066 Uiso 1 1 calc R . . C8 C 0.5324(4) 0.8224(3) 0.7830(3) 0.0629(15) Uani 1 1 d . . . H8 H 0.5439 0.8697 0.8169 0.075 Uiso 1 1 calc R . . C9 C 0.6209(4) 0.7790(3) 0.7599(3) 0.0625(15) Uani 1 1 d . . . H9 H 0.6920 0.7964 0.7781 0.075 Uiso 1 1 calc R . . C10 C 0.0802(4) 0.6941(3) 0.6189(3) 0.0482(12) Uani 1 1 d . . . C11 C 0.0170(4) 0.7322(3) 0.5516(4) 0.0608(14) Uani 1 1 d . . . H11 H 0.0295 0.7866 0.5381 0.073 Uiso 1 1 calc R . . C12 C -0.0660(4) 0.6885(4) 0.5036(4) 0.0744(16) Uani 1 1 d . . . H12 H -0.1087 0.7141 0.4574 0.089 Uiso 1 1 calc R . . C13 C -0.0858(5) 0.6099(4) 0.5227(4) 0.0750(17) Uani 1 1 d . . . H13 H -0.1411 0.5815 0.4892 0.090 Uiso 1 1 calc R . . C14 C -0.0262(4) 0.5724(3) 0.5898(4) 0.0687(15) Uani 1 1 d . . . H14 H -0.0410 0.5183 0.6032 0.082 Uiso 1 1 calc R . . C15 C 0.0572(4) 0.6137(3) 0.6393(3) 0.0572(13) Uani 1 1 d . . . H15 H 0.0978 0.5876 0.6863 0.069 Uiso 1 1 calc R . . C16 C 0.1488(4) 0.7508(3) 0.7951(3) 0.0538(13) Uani 1 1 d . . . C17 C 0.2033(4) 0.7034(3) 0.8600(4) 0.0670(15) Uani 1 1 d . . . H17 H 0.2639 0.6726 0.8464 0.080 Uiso 1 1 calc R . . C18 C 0.1684(5) 0.7009(4) 0.9460(4) 0.0832(18) Uani 1 1 d . . . H18 H 0.2055 0.6691 0.9902 0.100 Uiso 1 1 calc R . . C19 C 0.0800(6) 0.7454(4) 0.9641(4) 0.0846(19) Uani 1 1 d . . . H19 H 0.0563 0.7429 1.0215 0.102 Uiso 1 1 calc R . . C20 C 0.0245(5) 0.7931(4) 0.9031(5) 0.0842(18) Uani 1 1 d . . . H20 H -0.0356 0.8237 0.9182 0.101 Uiso 1 1 calc R . . C21 C 0.0583(4) 0.7959(3) 0.8173(4) 0.0706(16) Uani 1 1 d . . . H21 H 0.0201 0.8282 0.7742 0.085 Uiso 1 1 calc R . . C22 C 0.2497(4) 0.8693(3) 0.5758(4) 0.0508(12) Uani 1 1 d . . . C23 C 0.2608(4) 0.8201(3) 0.5019(4) 0.0577(13) Uani 1 1 d . . . H23 H 0.2316 0.7677 0.5000 0.069 Uiso 1 1 calc R . . C24 C 0.3152(4) 0.8491(3) 0.4308(4) 0.0662(15) Uani 1 1 d . . . H24 H 0.3232 0.8147 0.3825 0.079 Uiso 1 1 calc R . . C25 C 0.3572(4) 0.9252(4) 0.4287(4) 0.0691(15) Uani 1 1 d . . . C26 C 0.3469(4) 0.9736(3) 0.5036(4) 0.0732(16) Uani 1 1 d . . . H26 H 0.3769 1.0259 0.5049 0.088 Uiso 1 1 calc R . . C27 C 0.2936(4) 0.9469(3) 0.5762(4) 0.0646(15) Uani 1 1 d . . . H27 H 0.2875 0.9811 0.6251 0.078 Uiso 1 1 calc R . . C28 C 0.4147(5) 0.9574(4) 0.3506(4) 0.099(2) Uani 1 1 d . . . H28A H 0.4717 0.9201 0.3369 0.148 Uiso 1 1 calc R . . H28B H 0.4467 1.0096 0.3658 0.148 Uiso 1 1 calc R . . H28C H 0.3623 0.9630 0.2995 0.148 Uiso 1 1 calc R . . C29 C 0.595(3) 0.521(2) 0.887(3) 0.170(13) Uani 0.54(4) 1 d P A 1 H29A H 0.6175 0.5178 0.9507 0.204 Uiso 0.54(4) 1 calc PR A 1 H29B H 0.6342 0.5670 0.8634 0.204 Uiso 0.54(4) 1 calc PR A 1 C29' C 0.558(5) 0.512(3) 0.833(4) 0.175(16) Uani 0.46(4) 1 d P A 2 H29C H 0.6210 0.5380 0.8096 0.210 Uiso 0.46(4) 1 calc PR A 2 H29D H 0.5063 0.4994 0.7825 0.210 Uiso 0.46(4) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0473(4) 0.0434(4) 0.0493(4) -0.0051(3) 0.0029(3) 0.0006(3) Cl1 0.0715(9) 0.0664(8) 0.0487(8) -0.0031(6) 0.0035(6) 0.0026(7) Cl2 0.0930(12) 0.0728(9) 0.1054(14) 0.0407(9) -0.0004(9) -0.0002(9) Cl3 0.113(6) 0.235(18) 0.199(10) 0.065(11) -0.040(5) -0.061(6) Cl4 0.215(9) 0.159(9) 0.179(13) -0.036(8) -0.012(8) -0.066(6) Cl3' 0.207(14) 0.156(7) 0.165(12) 0.043(8) -0.059(10) -0.070(8) Cl4' 0.201(17) 0.145(8) 0.166(7) 0.008(5) -0.052(7) -0.040(8) N1 0.046(2) 0.055(2) 0.049(3) -0.006(2) 0.0042(19) 0.006(2) N2 0.039(2) 0.044(2) 0.045(2) -0.0033(18) 0.0013(17) 0.0003(18) N3 0.052(2) 0.043(2) 0.058(3) -0.006(2) 0.009(2) 0.0096(19) P1 0.0406(7) 0.0455(7) 0.0452(8) -0.0044(6) 0.0043(6) 0.0025(6) C1 0.053(3) 0.068(3) 0.064(4) -0.014(3) 0.006(3) 0.008(3) C2 0.049(3) 0.079(4) 0.077(4) -0.014(3) 0.007(3) 0.013(3) C3 0.044(3) 0.080(4) 0.072(4) -0.006(3) 0.002(3) 0.003(3) C4 0.044(3) 0.063(3) 0.054(3) -0.007(3) 0.003(2) 0.000(3) C5 0.042(3) 0.054(3) 0.045(3) -0.003(2) 0.003(2) 0.001(3) C6 0.044(3) 0.047(3) 0.044(3) -0.004(2) 0.004(2) 0.001(2) C7 0.052(3) 0.054(3) 0.059(3) -0.013(3) 0.001(2) -0.001(3) C8 0.058(4) 0.063(3) 0.066(4) -0.015(3) -0.004(3) -0.006(3) C9 0.048(3) 0.072(4) 0.065(4) -0.007(3) -0.007(3) -0.010(3) C10 0.043(3) 0.055(3) 0.048(3) -0.005(2) 0.011(2) -0.002(2) C11 0.050(3) 0.072(3) 0.061(4) 0.000(3) 0.007(3) 0.000(3) C12 0.058(4) 0.101(5) 0.064(4) -0.003(4) -0.004(3) 0.003(4) C13 0.056(4) 0.097(5) 0.072(4) -0.023(4) 0.005(3) -0.013(4) C14 0.057(4) 0.075(4) 0.075(4) -0.013(3) 0.013(3) -0.012(3) C15 0.048(3) 0.067(3) 0.057(3) -0.010(3) 0.009(3) -0.003(3) C16 0.052(3) 0.058(3) 0.053(3) -0.012(3) 0.012(3) -0.004(3) C17 0.069(4) 0.077(4) 0.056(4) -0.002(3) 0.011(3) -0.009(3) C18 0.088(5) 0.097(5) 0.064(5) -0.001(4) 0.005(4) -0.012(4) C19 0.090(5) 0.102(5) 0.065(5) -0.018(4) 0.024(4) -0.023(4) C20 0.082(5) 0.094(5) 0.082(5) -0.025(4) 0.034(4) 0.000(4) C21 0.069(4) 0.077(4) 0.068(4) -0.014(3) 0.020(3) 0.002(3) C22 0.049(3) 0.049(3) 0.055(3) 0.001(3) 0.007(3) 0.005(3) C23 0.063(3) 0.050(3) 0.062(4) 0.002(3) 0.010(3) 0.003(3) C24 0.074(4) 0.068(4) 0.057(4) 0.007(3) 0.010(3) 0.005(3) C25 0.069(4) 0.078(4) 0.061(4) 0.011(3) 0.012(3) -0.008(3) C26 0.077(4) 0.062(4) 0.080(5) 0.010(3) 0.009(3) -0.017(3) C27 0.069(4) 0.059(3) 0.066(4) -0.008(3) 0.007(3) -0.008(3) C28 0.097(5) 0.117(5) 0.084(5) 0.021(4) 0.022(4) -0.029(4) C29 0.17(3) 0.17(3) 0.17(3) 0.01(2) -0.045(19) -0.06(2) C29' 0.17(4) 0.17(4) 0.17(4) 0.03(3) -0.04(3) -0.05(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.981(4) . ? Ni1 N2 1.996(3) . ? Ni1 Cl1 2.2154(14) . ? Ni1 Cl2 2.2294(15) . ? Cl3 C29 1.66(4) . ? Cl4 C29 1.74(5) . ? Cl3' C29' 1.67(5) . ? Cl4' C29' 1.67(6) . ? N1 C1 1.316(5) . ? N1 C5 1.383(5) . ? N2 C6 1.413(5) . ? N2 P1 1.601(3) . ? N3 C22 1.419(6) . ? N3 P1 1.641(4) . ? N3 H3 0.8600 . ? P1 C16 1.781(5) . ? P1 C10 1.791(5) . ? C1 C2 1.387(6) . ? C1 H1 0.9300 . ? C2 C3 1.336(6) . ? C2 H2 0.9300 . ? C3 C4 1.411(6) . ? C3 H3A 0.9300 . ? C4 C9 1.391(6) . ? C4 C5 1.404(6) . ? C5 C6 1.413(6) . ? C6 C7 1.388(6) . ? C7 C8 1.389(6) . ? C7 H7 0.9300 . ? C8 C9 1.360(6) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.367(6) . ? C10 C15 1.386(6) . ? C11 C12 1.389(7) . ? C11 H11 0.9300 . ? C12 C13 1.346(7) . ? C12 H12 0.9300 . ? C13 C14 1.340(7) . ? C13 H13 0.9300 . ? C14 C15 1.384(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.372(6) . ? C16 C21 1.390(6) . ? C17 C18 1.391(7) . ? C17 H17 0.9300 . ? C18 C19 1.345(8) . ? C18 H18 0.9300 . ? C19 C20 1.344(8) . ? C19 H19 0.9300 . ? C20 C21 1.382(8) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.380(6) . ? C22 C23 1.385(6) . ? C23 C24 1.384(7) . ? C23 H23 0.9300 . ? C24 C25 1.348(7) . ? C24 H24 0.9300 . ? C25 C26 1.389(7) . ? C25 C28 1.507(7) . ? C26 C27 1.385(7) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29' H29C 0.9700 . ? C29' H29D 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 83.30(15) . . ? N1 Ni1 Cl1 111.67(12) . . ? N2 Ni1 Cl1 115.24(10) . . ? N1 Ni1 Cl2 105.39(11) . . ? N2 Ni1 Cl2 117.89(11) . . ? Cl1 Ni1 Cl2 117.23(6) . . ? C1 N1 C5 118.0(4) . . ? C1 N1 Ni1 128.9(3) . . ? C5 N1 Ni1 113.1(3) . . ? C6 N2 P1 121.8(3) . . ? C6 N2 Ni1 111.4(3) . . ? P1 N2 Ni1 126.44(19) . . ? C22 N3 P1 125.2(3) . . ? C22 N3 H3 117.4 . . ? P1 N3 H3 117.4 . . ? N2 P1 N3 113.87(19) . . ? N2 P1 C16 113.0(2) . . ? N3 P1 C16 106.0(2) . . ? N2 P1 C10 107.34(19) . . ? N3 P1 C10 110.0(2) . . ? C16 P1 C10 106.4(2) . . ? N1 C1 C2 123.0(5) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 119.9(5) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.5(5) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C9 C4 C5 118.8(5) . . ? C9 C4 C3 124.5(5) . . ? C5 C4 C3 116.7(5) . . ? N1 C5 C4 122.0(4) . . ? N1 C5 C6 116.1(4) . . ? C4 C5 C6 121.9(4) . . ? C7 C6 C5 116.6(4) . . ? C7 C6 N2 127.3(4) . . ? C5 C6 N2 116.1(4) . . ? C6 C7 C8 121.3(5) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 C7 121.5(5) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C4 119.8(5) . . ? C8 C9 H9 120.1 . . ? C4 C9 H9 120.1 . . ? C11 C10 C15 119.1(4) . . ? C11 C10 P1 121.5(4) . . ? C15 C10 P1 119.4(4) . . ? C10 C11 C12 119.2(5) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 121.2(5) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C14 C13 C12 120.2(5) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.4(5) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C10 119.9(5) . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? C17 C16 C21 118.5(5) . . ? C17 C16 P1 119.5(4) . . ? C21 C16 P1 121.8(4) . . ? C16 C17 C18 120.5(6) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 118.8(6) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C20 C19 C18 122.9(6) . . ? C20 C19 H19 118.6 . . ? C18 C19 H19 118.6 . . ? C19 C20 C21 118.8(6) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C20 C21 C16 120.5(6) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? C27 C22 C23 118.5(5) . . ? C27 C22 N3 119.7(5) . . ? C23 C22 N3 121.8(4) . . ? C24 C23 C22 120.0(5) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 122.8(6) . . ? C25 C24 H24 118.6 . . ? C23 C24 H24 118.6 . . ? C24 C25 C26 116.7(5) . . ? C24 C25 C28 122.9(6) . . ? C26 C25 C28 120.4(6) . . ? C27 C26 C25 122.3(5) . . ? C27 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? C22 C27 C26 119.6(5) . . ? C22 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Cl3 C29 Cl4 114(3) . . ? Cl3 C29 H29A 108.7 . . ? Cl4 C29 H29A 108.7 . . ? Cl3 C29 H29B 108.7 . . ? Cl4 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? Cl4' C29' Cl3' 123(4) . . ? Cl4' C29' H29C 106.7 . . ? Cl3' C29' H29C 106.7 . . ? Cl4' C29' H29D 106.7 . . ? Cl3' C29' H29D 106.7 . . ? H29C C29' H29D 106.6 . . ? 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 N1 C1 -179.3(4) . . . . ? Cl1 Ni1 N1 C1 -64.8(4) . . . . ? Cl2 Ni1 N1 C1 63.5(4) . . . . ? N2 Ni1 N1 C5 0.3(3) . . . . ? Cl1 Ni1 N1 C5 114.9(3) . . . . ? Cl2 Ni1 N1 C5 -116.8(3) . . . . ? N1 Ni1 N2 C6 -1.5(3) . . . . ? Cl1 Ni1 N2 C6 -112.3(3) . . . . ? Cl2 Ni1 N2 C6 102.4(3) . . . . ? N1 Ni1 N2 P1 171.5(3) . . . . ? Cl1 Ni1 N2 P1 60.7(3) . . . . ? Cl2 Ni1 N2 P1 -84.6(2) . . . . ? C6 N2 P1 N3 47.8(4) . . . . ? Ni1 N2 P1 N3 -124.5(2) . . . . ? C6 N2 P1 C16 -73.2(4) . . . . ? Ni1 N2 P1 C16 114.5(3) . . . . ? C6 N2 P1 C10 169.9(3) . . . . ? Ni1 N2 P1 C10 -2.5(3) . . . . ? C22 N3 P1 N2 37.7(4) . . . . ? C22 N3 P1 C16 162.5(4) . . . . ? C22 N3 P1 C10 -82.9(4) . . . . ? C5 N1 C1 C2 0.1(7) . . . . ? Ni1 N1 C1 C2 179.8(4) . . . . ? N1 C1 C2 C3 -0.3(8) . . . . ? C1 C2 C3 C4 1.1(8) . . . . ? C2 C3 C4 C9 177.3(5) . . . . ? C2 C3 C4 C5 -1.6(7) . . . . ? C1 N1 C5 C4 -0.7(7) . . . . ? Ni1 N1 C5 C4 179.6(3) . . . . ? C1 N1 C5 C6 -179.4(4) . . . . ? Ni1 N1 C5 C6 0.9(5) . . . . ? C9 C4 C5 N1 -177.6(4) . . . . ? C3 C4 C5 N1 1.4(7) . . . . ? C9 C4 C5 C6 1.1(7) . . . . ? C3 C4 C5 C6 -179.9(4) . . . . ? N1 C5 C6 C7 177.6(4) . . . . ? C4 C5 C6 C7 -1.2(7) . . . . ? N1 C5 C6 N2 -2.2(6) . . . . ? C4 C5 C6 N2 179.1(4) . . . . ? P1 N2 C6 C7 9.2(6) . . . . ? Ni1 N2 C6 C7 -177.4(4) . . . . ? P1 N2 C6 C5 -171.0(3) . . . . ? Ni1 N2 C6 C5 2.4(5) . . . . ? C5 C6 C7 C8 0.8(7) . . . . ? N2 C6 C7 C8 -179.4(4) . . . . ? C6 C7 C8 C9 -0.5(8) . . . . ? C7 C8 C9 C4 0.4(8) . . . . ? C5 C4 C9 C8 -0.7(7) . . . . ? C3 C4 C9 C8 -179.6(5) . . . . ? N2 P1 C10 C11 -123.4(4) . . . . ? N3 P1 C10 C11 1.0(5) . . . . ? C16 P1 C10 C11 115.3(4) . . . . ? N2 P1 C10 C15 58.8(4) . . . . ? N3 P1 C10 C15 -176.8(4) . . . . ? C16 P1 C10 C15 -62.4(4) . . . . ? C15 C10 C11 C12 -2.1(7) . . . . ? P1 C10 C11 C12 -179.9(4) . . . . ? C10 C11 C12 C13 0.6(8) . . . . ? C11 C12 C13 C14 1.0(9) . . . . ? C12 C13 C14 C15 -0.9(9) . . . . ? C13 C14 C15 C10 -0.7(8) . . . . ? C11 C10 C15 C14 2.2(7) . . . . ? P1 C10 C15 C14 -180.0(4) . . . . ? N2 P1 C16 C17 -9.3(5) . . . . ? N3 P1 C16 C17 -134.6(4) . . . . ? C10 P1 C16 C17 108.3(4) . . . . ? N2 P1 C16 C21 175.9(4) . . . . ? N3 P1 C16 C21 50.6(4) . . . . ? C10 P1 C16 C21 -66.5(4) . . . . ? C21 C16 C17 C18 -0.2(8) . . . . ? P1 C16 C17 C18 -175.1(4) . . . . ? C16 C17 C18 C19 0.5(8) . . . . ? C17 C18 C19 C20 -0.9(9) . . . . ? C18 C19 C20 C21 1.1(9) . . . . ? C19 C20 C21 C16 -0.7(8) . . . . ? C17 C16 C21 C20 0.3(7) . . . . ? P1 C16 C21 C20 175.1(4) . . . . ? P1 N3 C22 C27 -150.2(4) . . . . ? P1 N3 C22 C23 30.0(6) . . . . ? C27 C22 C23 C24 0.2(7) . . . . ? N3 C22 C23 C24 -179.9(4) . . . . ? C22 C23 C24 C25 -1.5(8) . . . . ? C23 C24 C25 C26 2.2(8) . . . . ? C23 C24 C25 C28 -178.8(5) . . . . ? C24 C25 C26 C27 -1.8(8) . . . . ? C28 C25 C26 C27 179.2(5) . . . . ? C23 C22 C27 C26 0.1(7) . . . . ? N3 C22 C27 C26 -179.7(4) . . . . ? C25 C26 C27 C22 0.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.398 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.072 # Attachment '- 4.cif' data_100321d _database_code_depnum_ccdc_archive 'CCDC 878349' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H33 Cl N3 Ni O P' _chemical_formula_weight 564.71 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1230(10) _cell_length_b 11.83510(12) _cell_length_c 12.17190(13) _cell_angle_alpha 99.2830(10) _cell_angle_beta 111.966(2) _cell_angle_gamma 92.9710(10) _cell_volume 1324.64(13) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1663 _cell_measurement_theta_min 2.283 _cell_measurement_theta_max 21.631 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.922 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8300 _exptl_absorpt_correction_T_max 0.9135 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 7006 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0793 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4591 _reflns_number_gt 2824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0103P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4591 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.81117(5) 0.29010(4) 0.15042(4) 0.04516(15) Uani 1 1 d . . . Cl1 Cl 0.93866(12) 0.28418(9) 0.04106(11) 0.0918(4) Uani 1 1 d . . . N1 N 0.7506(3) 0.4402(2) 0.1179(2) 0.0452(7) Uani 1 1 d . . . N2 N 0.7003(2) 0.3045(2) 0.2460(2) 0.0410(7) Uani 1 1 d . . . N3 N 0.5409(3) 0.1387(2) 0.3036(2) 0.0457(7) Uani 1 1 d . A . H3 H 0.5028 0.1759 0.3485 0.055 Uiso 1 1 d R . . O1 O 0.6215(3) 0.7481(2) 0.5577(3) 0.0799(8) Uani 1 1 d . . . P1 P 0.69422(9) 0.20765(7) 0.32324(8) 0.0411(2) Uani 1 1 d . . . C1 C 0.6571(3) 0.4750(3) 0.1704(3) 0.0442(9) Uani 1 1 d . . . C2 C 0.6282(3) 0.4016(3) 0.2406(3) 0.0429(9) Uani 1 1 d . . . C3 C 0.5338(3) 0.4307(3) 0.2947(3) 0.0518(10) Uani 1 1 d . . . H3A H 0.5139 0.3841 0.3426 0.062 Uiso 1 1 calc R . . C4 C 0.4678(4) 0.5316(3) 0.2768(3) 0.0599(11) Uani 1 1 d . . . H4 H 0.4027 0.5499 0.3122 0.072 Uiso 1 1 calc R . . C5 C 0.4957(4) 0.6025(3) 0.2102(3) 0.0622(11) Uani 1 1 d . . . H5 H 0.4497 0.6683 0.2001 0.075 Uiso 1 1 calc R . . C6 C 0.5939(4) 0.5776(3) 0.1558(3) 0.0520(10) Uani 1 1 d . . . C7 C 0.6353(4) 0.6462(3) 0.0890(3) 0.0660(12) Uani 1 1 d . . . H7 H 0.5976 0.7154 0.0782 0.079 Uiso 1 1 calc R . . C8 C 0.7297(4) 0.6133(3) 0.0396(3) 0.0648(11) Uani 1 1 d . . . H8 H 0.7587 0.6600 -0.0037 0.078 Uiso 1 1 calc R . . C9 C 0.7830(4) 0.5081(3) 0.0546(3) 0.0542(10) Uani 1 1 d . . . H9 H 0.8451 0.4849 0.0175 0.065 Uiso 1 1 calc R . . C10 C 0.8050(3) 0.1144(3) 0.2811(3) 0.0437(9) Uani 1 1 d . . . C11 C 0.8534(3) 0.1469(3) 0.1955(3) 0.0421(9) Uani 1 1 d . . . C12 C 0.9303(3) 0.0667(3) 0.1543(3) 0.0529(10) Uani 1 1 d . . . H12 H 0.9646 0.0827 0.0968 0.064 Uiso 1 1 calc R . . C13 C 0.9564(4) -0.0341(3) 0.1956(4) 0.0606(11) Uani 1 1 d . . . H13 H 1.0048 -0.0859 0.1635 0.073 Uiso 1 1 calc R . . C14 C 0.9123(4) -0.0606(3) 0.2842(4) 0.0665(12) Uani 1 1 d . . . H14 H 0.9343 -0.1275 0.3145 0.080 Uiso 1 1 calc R . . C15 C 0.8352(3) 0.0145(3) 0.3261(3) 0.0572(11) Uani 1 1 d . . . H15 H 0.8033 -0.0018 0.3849 0.069 Uiso 1 1 calc R . . C16 C 0.7651(3) 0.2666(3) 0.4819(3) 0.0402(8) Uani 1 1 d . . . C17 C 0.8548(3) 0.3699(3) 0.5256(3) 0.0545(10) Uani 1 1 d . . . H17 H 0.8750 0.4088 0.4721 0.065 Uiso 1 1 calc R . . C18 C 0.9143(4) 0.4155(3) 0.6476(4) 0.0696(12) Uani 1 1 d . . . H18 H 0.9739 0.4853 0.6761 0.084 Uiso 1 1 calc R . . C19 C 0.8855(4) 0.3583(4) 0.7265(4) 0.0669(12) Uani 1 1 d . . . H19 H 0.9252 0.3896 0.8087 0.080 Uiso 1 1 calc R . . C20 C 0.8000(4) 0.2565(3) 0.6861(3) 0.0621(11) Uani 1 1 d . . . H20 H 0.7822 0.2177 0.7407 0.075 Uiso 1 1 calc R . . C21 C 0.7394(3) 0.2102(3) 0.5645(3) 0.0531(10) Uani 1 1 d . . . H21 H 0.6804 0.1402 0.5375 0.064 Uiso 1 1 calc R . . C22 C 0.4328(4) 0.0664(3) 0.1911(3) 0.0527(10) Uani 1 1 d . . . C23 C 0.367(2) 0.1354(13) 0.1071(15) 0.096(6) Uani 0.52(2) 1 d P A 1 H23A H 0.4385 0.1749 0.0880 0.143 Uiso 0.52(2) 1 calc PR A 1 H23B H 0.3198 0.1908 0.1410 0.143 Uiso 0.52(2) 1 calc PR A 1 H23C H 0.2978 0.0876 0.0349 0.143 Uiso 0.52(2) 1 calc PR A 1 C24 C 0.5024(15) -0.0341(15) 0.1433(16) 0.081(5) Uani 0.52(2) 1 d P A 1 H24A H 0.4297 -0.0855 0.0763 0.122 Uiso 0.52(2) 1 calc PR A 1 H24B H 0.5472 -0.0755 0.2066 0.122 Uiso 0.52(2) 1 calc PR A 1 H24C H 0.5732 -0.0034 0.1176 0.122 Uiso 0.52(2) 1 calc PR A 1 C25 C 0.3284(16) 0.0029(15) 0.2336(12) 0.085(5) Uani 0.52(2) 1 d P A 1 H25A H 0.2813 0.0583 0.2676 0.127 Uiso 0.52(2) 1 calc PR A 1 H25B H 0.3813 -0.0393 0.2935 0.127 Uiso 0.52(2) 1 calc PR A 1 H25C H 0.2580 -0.0495 0.1659 0.127 Uiso 0.52(2) 1 calc PR A 1 C23' C 0.4324(17) 0.1138(15) 0.0772(14) 0.069(4) Uani 0.48(2) 1 d P A 2 H23D H 0.3552 0.0717 0.0062 0.103 Uiso 0.48(2) 1 calc PR A 2 H23E H 0.5221 0.1044 0.0688 0.103 Uiso 0.48(2) 1 calc PR A 2 H23F H 0.4198 0.1941 0.0872 0.103 Uiso 0.48(2) 1 calc PR A 2 C24' C 0.458(2) -0.0513(14) 0.1842(16) 0.081(5) Uani 0.48(2) 1 d P A 2 H24D H 0.3824 -0.0977 0.1148 0.122 Uiso 0.48(2) 1 calc PR A 2 H24E H 0.4591 -0.0762 0.2559 0.122 Uiso 0.48(2) 1 calc PR A 2 H24F H 0.5482 -0.0594 0.1772 0.122 Uiso 0.48(2) 1 calc PR A 2 C25' C 0.2804(12) 0.082(2) 0.1877(15) 0.095(7) Uani 0.48(2) 1 d P A 2 H25D H 0.2598 0.1586 0.1757 0.143 Uiso 0.48(2) 1 calc PR A 2 H25E H 0.2759 0.0714 0.2627 0.143 Uiso 0.48(2) 1 calc PR A 2 H25F H 0.2112 0.0266 0.1225 0.143 Uiso 0.48(2) 1 calc PR A 2 C26 C 0.7257(5) 0.6717(4) 0.5960(4) 0.0929(15) Uani 1 1 d . . . H26A H 0.6792 0.5933 0.5769 0.112 Uiso 1 1 calc R . . H26B H 0.7790 0.6927 0.6827 0.112 Uiso 1 1 calc R . . C27 C 0.8227(4) 0.6804(3) 0.5327(4) 0.0858(14) Uani 1 1 d . . . H27A H 0.9214 0.6787 0.5861 0.103 Uiso 1 1 calc R . . H27B H 0.7965 0.6180 0.4633 0.103 Uiso 1 1 calc R . . C28 C 0.8032(5) 0.7916(4) 0.4956(5) 0.1068(17) Uani 1 1 d . . . H28A H 0.8095 0.7880 0.4176 0.128 Uiso 1 1 calc R . . H28B H 0.8762 0.8512 0.5541 0.128 Uiso 1 1 calc R . . C29 C 0.6596(5) 0.8162(4) 0.4887(4) 0.0879(14) Uani 1 1 d . . . H29A H 0.6614 0.8972 0.5202 0.106 Uiso 1 1 calc R . . H29B H 0.5911 0.7976 0.4055 0.106 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 0.0434(3) 0.0523(3) 0.0436(3) 0.0114(2) 0.0204(2) 0.0054(2) Cl1 0.1204(10) 0.1016(9) 0.1100(10) 0.0527(8) 0.0908(8) 0.0458(8) N1 0.0417(18) 0.0517(18) 0.0377(18) 0.0112(16) 0.0104(15) -0.0012(15) N2 0.0398(16) 0.0438(16) 0.0433(18) 0.0090(15) 0.0195(15) 0.0125(14) N3 0.0441(17) 0.0493(17) 0.0463(18) -0.0005(15) 0.0252(15) -0.0019(14) O1 0.084(2) 0.087(2) 0.093(2) 0.0301(19) 0.0543(19) 0.0313(17) P1 0.0394(5) 0.0410(5) 0.0465(6) 0.0085(5) 0.0205(5) 0.0058(4) C1 0.043(2) 0.043(2) 0.040(2) 0.0070(19) 0.0098(19) 0.0038(18) C2 0.041(2) 0.044(2) 0.041(2) 0.0069(19) 0.0121(19) 0.0049(18) C3 0.052(2) 0.046(2) 0.064(3) 0.012(2) 0.029(2) 0.0118(19) C4 0.062(3) 0.058(2) 0.065(3) 0.009(2) 0.030(2) 0.021(2) C5 0.068(3) 0.046(2) 0.066(3) 0.007(2) 0.020(2) 0.016(2) C6 0.056(3) 0.046(2) 0.049(3) 0.009(2) 0.015(2) 0.005(2) C7 0.074(3) 0.053(2) 0.062(3) 0.016(2) 0.014(2) 0.005(2) C8 0.073(3) 0.059(3) 0.061(3) 0.027(2) 0.019(2) 0.000(2) C9 0.052(2) 0.061(3) 0.049(2) 0.018(2) 0.016(2) 0.001(2) C10 0.043(2) 0.042(2) 0.054(2) 0.0103(19) 0.0279(19) 0.0070(17) C11 0.0312(19) 0.052(2) 0.040(2) 0.0025(18) 0.0136(17) 0.0028(17) C12 0.047(2) 0.058(2) 0.063(3) 0.008(2) 0.032(2) 0.008(2) C13 0.055(3) 0.057(3) 0.080(3) 0.009(2) 0.039(2) 0.015(2) C14 0.067(3) 0.055(2) 0.098(3) 0.023(2) 0.050(3) 0.021(2) C15 0.060(3) 0.055(2) 0.074(3) 0.020(2) 0.042(2) 0.016(2) C16 0.035(2) 0.045(2) 0.044(2) 0.0109(19) 0.0164(18) 0.0100(17) C17 0.047(2) 0.061(2) 0.053(3) 0.008(2) 0.018(2) 0.000(2) C18 0.062(3) 0.069(3) 0.062(3) 0.001(3) 0.011(3) -0.001(2) C19 0.056(3) 0.088(3) 0.045(3) 0.002(3) 0.009(2) 0.015(2) C20 0.059(3) 0.082(3) 0.046(3) 0.021(2) 0.017(2) 0.015(2) C21 0.050(2) 0.057(2) 0.052(3) 0.013(2) 0.018(2) 0.0067(19) C22 0.050(2) 0.054(2) 0.050(3) 0.000(2) 0.020(2) -0.007(2) C23 0.089(13) 0.079(8) 0.080(11) 0.012(8) -0.007(8) -0.018(8) C24 0.069(8) 0.084(9) 0.076(11) -0.031(8) 0.032(6) -0.009(6) C25 0.060(8) 0.096(10) 0.084(8) -0.016(7) 0.030(7) -0.037(7) C23' 0.063(9) 0.080(9) 0.053(7) 0.008(6) 0.015(6) -0.008(7) C24' 0.093(13) 0.063(7) 0.075(11) 0.007(7) 0.024(8) -0.010(8) C25' 0.041(6) 0.150(16) 0.075(10) -0.032(11) 0.026(6) -0.017(8) C26 0.103(4) 0.100(4) 0.117(4) 0.054(3) 0.071(3) 0.046(3) C27 0.078(3) 0.076(3) 0.122(4) 0.019(3) 0.059(3) 0.015(3) C28 0.104(4) 0.100(4) 0.140(5) 0.046(4) 0.065(4) 0.008(3) C29 0.118(4) 0.080(3) 0.080(3) 0.024(3) 0.047(3) 0.038(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C11 1.885(3) . ? Ni1 N2 1.891(2) . ? Ni1 N1 1.961(3) . ? Ni1 Cl1 2.1695(11) . ? N1 C9 1.307(4) . ? N1 C1 1.372(4) . ? N2 C2 1.390(4) . ? N2 P1 1.608(3) . ? N3 C22 1.486(4) . ? N3 P1 1.631(2) . ? N3 H3 0.8599 . ? O1 C29 1.390(4) . ? O1 C26 1.419(4) . ? P1 C10 1.765(3) . ? P1 C16 1.791(3) . ? C1 C2 1.404(4) . ? C1 C6 1.407(4) . ? C2 C3 1.377(4) . ? C3 C4 1.406(4) . ? C3 H3A 0.9300 . ? C4 C5 1.343(5) . ? C4 H4 0.9300 . ? C5 C6 1.405(4) . ? C5 H5 0.9300 . ? C6 C7 1.388(5) . ? C7 C8 1.348(4) . ? C7 H7 0.9300 . ? C8 C9 1.394(4) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C15 1.384(4) . ? C10 C11 1.402(4) . ? C11 C12 1.404(4) . ? C12 C13 1.369(4) . ? C12 H12 0.9300 . ? C13 C14 1.384(5) . ? C13 H13 0.9300 . ? C14 C15 1.371(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.385(4) . ? C16 C21 1.385(4) . ? C17 C18 1.377(4) . ? C17 H17 0.9300 . ? C18 C19 1.366(5) . ? C18 H18 0.9300 . ? C19 C20 1.350(4) . ? C19 H19 0.9300 . ? C20 C21 1.375(4) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.404(14) . ? C22 C24' 1.422(17) . ? C22 C25 1.548(10) . ? C22 C25' 1.549(11) . ? C22 C24 1.556(14) . ? C22 C23' 1.576(15) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C23' H23D 0.9600 . ? C23' H23E 0.9600 . ? C23' H23F 0.9600 . ? C24' H24D 0.9600 . ? C24' H24E 0.9600 . ? C24' H24F 0.9600 . ? C25' H25D 0.9600 . ? C25' H25E 0.9600 . ? C25' H25F 0.9600 . ? C26 C27 1.466(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.458(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.471(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? 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 C11 Ni1 N2 88.18(13) . . ? C11 Ni1 N1 171.69(14) . . ? N2 Ni1 N1 83.51(12) . . ? C11 Ni1 Cl1 94.96(11) . . ? N2 Ni1 Cl1 176.69(9) . . ? N1 Ni1 Cl1 93.34(9) . . ? C9 N1 C1 117.3(3) . . ? C9 N1 Ni1 130.6(3) . . ? C1 N1 Ni1 112.1(2) . . ? C2 N2 P1 125.8(2) . . ? C2 N2 Ni1 114.4(2) . . ? P1 N2 Ni1 119.79(14) . . ? C22 N3 P1 128.3(2) . . ? C22 N3 H3 112.8 . . ? P1 N3 H3 110.9 . . ? C29 O1 C26 109.5(3) . . ? N2 P1 N3 120.52(13) . . ? N2 P1 C10 99.01(14) . . ? N3 P1 C10 111.71(14) . . ? N2 P1 C16 111.60(15) . . ? N3 P1 C16 101.67(14) . . ? C10 P1 C16 112.83(15) . . ? N1 C1 C2 115.6(3) . . ? N1 C1 C6 122.7(3) . . ? C2 C1 C6 121.7(4) . . ? C3 C2 N2 127.2(3) . . ? C3 C2 C1 118.6(3) . . ? N2 C2 C1 114.2(3) . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 122.2(4) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C4 C5 C6 120.4(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 125.6(4) . . ? C7 C6 C1 116.7(4) . . ? C5 C6 C1 117.7(4) . . ? C8 C7 C6 120.7(4) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 119.0(4) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? N1 C9 C8 123.6(4) . . ? N1 C9 H9 118.2 . . ? C8 C9 H9 118.2 . . ? C15 C10 C11 123.3(3) . . ? C15 C10 P1 121.7(3) . . ? C11 C10 P1 114.9(3) . . ? C10 C11 C12 114.4(3) . . ? C10 C11 Ni1 117.8(3) . . ? C12 C11 Ni1 127.8(3) . . ? C13 C12 C11 122.5(3) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C12 C13 C14 121.3(3) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C15 C14 C13 118.3(4) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? C14 C15 C10 120.1(3) . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? C17 C16 C21 118.0(3) . . ? C17 C16 P1 119.3(3) . . ? C21 C16 P1 122.6(3) . . ? C18 C17 C16 120.6(4) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 119.9(4) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C20 C19 C18 120.6(4) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 120.2(4) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C16 120.8(3) . . ? C20 C21 H21 119.6 . . ? C16 C21 H21 119.6 . . ? C23 C22 C24' 135.3(9) . . ? C23 C22 N3 110.4(6) . . ? C24' C22 N3 110.5(7) . . ? C23 C22 C25 114.0(6) . . ? C24' C22 C25 71.7(6) . . ? N3 C22 C25 104.6(5) . . ? C23 C22 C25' 70.4(6) . . ? C24' C22 C25' 111.6(7) . . ? N3 C22 C25' 109.2(5) . . ? C25 C22 C25' 45.6(5) . . ? C23 C22 C24 114.7(8) . . ? C24' C22 C24 31.9(6) . . ? N3 C22 C24 109.9(6) . . ? C25 C22 C24 102.6(6) . . ? C25' C22 C24 134.9(7) . . ? C23 C22 C23' 34.4(7) . . ? C24' C22 C23' 112.2(8) . . ? N3 C22 C23' 110.4(6) . . ? C25 C22 C23' 139.8(7) . . ? C25' C22 C23' 102.8(8) . . ? C24 C22 C23' 83.7(7) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? C22 C23' H23D 109.5 . . ? C22 C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? C22 C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? C22 C24' H24D 109.5 . . ? C22 C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C22 C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? C22 C25' H25D 109.5 . . ? C22 C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? C22 C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? O1 C26 C27 107.8(4) . . ? O1 C26 H26A 110.1 . . ? C27 C26 H26A 110.1 . . ? O1 C26 H26B 110.1 . . ? C27 C26 H26B 110.1 . . ? H26A C26 H26B 108.5 . . ? C28 C27 C26 103.6(3) . . ? C28 C27 H27A 111.0 . . ? C26 C27 H27A 111.0 . . ? C28 C27 H27B 111.0 . . ? C26 C27 H27B 111.0 . . ? H27A C27 H27B 109.0 . . ? C27 C28 C29 106.1(4) . . ? C27 C28 H28A 110.5 . . ? C29 C28 H28A 110.5 . . ? C27 C28 H28B 110.5 . . ? C29 C28 H28B 110.5 . . ? H28A C28 H28B 108.7 . . ? O1 C29 C28 106.9(3) . . ? O1 C29 H29A 110.3 . . ? C28 C29 H29A 110.3 . . ? O1 C29 H29B 110.3 . . ? C28 C29 H29B 110.3 . . ? H29A C29 H29B 108.6 . . ? 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 C11 Ni1 N1 C9 178.1(7) . . . . ? N2 Ni1 N1 C9 177.5(3) . . . . ? Cl1 Ni1 N1 C9 -1.5(3) . . . . ? C11 Ni1 N1 C1 -3.1(10) . . . . ? N2 Ni1 N1 C1 -3.7(2) . . . . ? Cl1 Ni1 N1 C1 177.3(2) . . . . ? C11 Ni1 N2 C2 -176.0(2) . . . . ? N1 Ni1 N2 C2 4.0(2) . . . . ? Cl1 Ni1 N2 C2 22.3(16) . . . . ? C11 Ni1 N2 P1 3.29(17) . . . . ? N1 Ni1 N2 P1 -176.79(17) . . . . ? Cl1 Ni1 N2 P1 -158.5(14) . . . . ? C2 N2 P1 N3 56.4(3) . . . . ? Ni1 N2 P1 N3 -122.74(16) . . . . ? C2 N2 P1 C10 178.3(3) . . . . ? Ni1 N2 P1 C10 -0.85(19) . . . . ? C2 N2 P1 C16 -62.7(3) . . . . ? Ni1 N2 P1 C16 118.19(16) . . . . ? C22 N3 P1 N2 59.1(3) . . . . ? C22 N3 P1 C10 -56.4(3) . . . . ? C22 N3 P1 C16 -177.0(3) . . . . ? C9 N1 C1 C2 -178.2(3) . . . . ? Ni1 N1 C1 C2 2.8(3) . . . . ? C9 N1 C1 C6 1.7(5) . . . . ? Ni1 N1 C1 C6 -177.3(3) . . . . ? P1 N2 C2 C3 -3.2(5) . . . . ? Ni1 N2 C2 C3 176.0(3) . . . . ? P1 N2 C2 C1 177.3(2) . . . . ? Ni1 N2 C2 C1 -3.5(3) . . . . ? N1 C1 C2 C3 -179.2(3) . . . . ? C6 C1 C2 C3 0.9(5) . . . . ? N1 C1 C2 N2 0.3(4) . . . . ? C6 C1 C2 N2 -179.6(3) . . . . ? N2 C2 C3 C4 -178.5(3) . . . . ? C1 C2 C3 C4 1.0(5) . . . . ? C2 C3 C4 C5 -1.3(5) . . . . ? C3 C4 C5 C6 -0.3(6) . . . . ? C4 C5 C6 C7 -177.4(4) . . . . ? C4 C5 C6 C1 2.1(5) . . . . ? N1 C1 C6 C7 -2.7(5) . . . . ? C2 C1 C6 C7 177.1(3) . . . . ? N1 C1 C6 C5 177.7(3) . . . . ? C2 C1 C6 C5 -2.4(5) . . . . ? C5 C6 C7 C8 -179.3(3) . . . . ? C1 C6 C7 C8 1.2(5) . . . . ? C6 C7 C8 C9 1.3(6) . . . . ? C1 N1 C9 C8 1.0(5) . . . . ? Ni1 N1 C9 C8 179.7(2) . . . . ? C7 C8 C9 N1 -2.5(6) . . . . ? N2 P1 C10 C15 179.5(3) . . . . ? N3 P1 C10 C15 -52.4(3) . . . . ? C16 P1 C10 C15 61.4(3) . . . . ? N2 P1 C10 C11 -3.2(3) . . . . ? N3 P1 C10 C11 124.9(2) . . . . ? C16 P1 C10 C11 -121.3(3) . . . . ? C15 C10 C11 C12 2.9(5) . . . . ? P1 C10 C11 C12 -174.4(2) . . . . ? C15 C10 C11 Ni1 -176.6(3) . . . . ? P1 C10 C11 Ni1 6.1(3) . . . . ? N2 Ni1 C11 C10 -5.4(3) . . . . ? N1 Ni1 C11 C10 -6.0(10) . . . . ? Cl1 Ni1 C11 C10 173.5(2) . . . . ? N2 Ni1 C11 C12 175.1(3) . . . . ? N1 Ni1 C11 C12 174.6(7) . . . . ? Cl1 Ni1 C11 C12 -5.9(3) . . . . ? C10 C11 C12 C13 -0.6(5) . . . . ? Ni1 C11 C12 C13 178.8(3) . . . . ? C11 C12 C13 C14 -2.3(6) . . . . ? C12 C13 C14 C15 3.0(6) . . . . ? C13 C14 C15 C10 -0.8(5) . . . . ? C11 C10 C15 C14 -2.3(5) . . . . ? P1 C10 C15 C14 174.8(3) . . . . ? N2 P1 C16 C17 -20.1(3) . . . . ? N3 P1 C16 C17 -149.8(2) . . . . ? C10 P1 C16 C17 90.4(3) . . . . ? N2 P1 C16 C21 163.0(2) . . . . ? N3 P1 C16 C21 33.3(3) . . . . ? C10 P1 C16 C21 -86.5(3) . . . . ? C21 C16 C17 C18 -1.0(5) . . . . ? P1 C16 C17 C18 -178.1(3) . . . . ? C16 C17 C18 C19 0.4(6) . . . . ? C17 C18 C19 C20 0.6(6) . . . . ? C18 C19 C20 C21 -0.9(6) . . . . ? C19 C20 C21 C16 0.2(5) . . . . ? C17 C16 C21 C20 0.7(5) . . . . ? P1 C16 C21 C20 177.7(2) . . . . ? P1 N3 C22 C23 -69.0(11) . . . . ? P1 N3 C22 C24' 92.4(10) . . . . ? P1 N3 C22 C25 167.9(9) . . . . ? P1 N3 C22 C25' -144.5(12) . . . . ? P1 N3 C22 C24 58.4(9) . . . . ? P1 N3 C22 C23' -32.3(9) . . . . ? C29 O1 C26 C27 -8.8(5) . . . . ? O1 C26 C27 C28 20.7(5) . . . . ? C26 C27 C28 C29 -24.5(5) . . . . ? C26 O1 C29 C28 -6.9(5) . . . . ? C27 C28 C29 O1 20.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.333 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.050 # Attachment '- 7.cif' data_100725-s _database_code_depnum_ccdc_archive 'CCDC 878350' #TrackingRef '- 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H22 Cl2 N3 Ni P' _chemical_formula_weight 549.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.5863(13) _cell_length_b 11.5292(2) _cell_length_c 19.6821(5) _cell_angle_alpha 90.00 _cell_angle_beta 117.126(4) _cell_angle_gamma 90.00 _cell_volume 6985.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 7078 _cell_measurement_theta_min 2.2610 _cell_measurement_theta_max 62.6621 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 2.758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4723 _exptl_absorpt_correction_T_max 0.5574 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Gemini S Ultra, Oxford Diffraction' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9149 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13149 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 62.76 _reflns_number_total 5522 _reflns_number_gt 4373 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd.)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd.)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd.)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 (L. J. Farrugia, 2001)' _computing_publication_material SHELXL-97 _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^)+(0.0710P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5522 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 0.630018(12) 0.08132(3) 0.15993(2) 0.04440(14) Uani 1 1 d . . . P1 P 0.620896(19) 0.31014(5) 0.05815(4) 0.04247(17) Uani 1 1 d . . . Cl2 Cl 0.642193(19) -0.02483(5) 0.07101(4) 0.05100(17) Uani 1 1 d . . . Cl1 Cl 0.65442(2) -0.04933(6) 0.26210(4) 0.0613(2) Uani 1 1 d . . . N1 N 0.56542(6) 0.03718(16) 0.12521(11) 0.0426(5) Uani 1 1 d . . . N2 N 0.59826(6) 0.22358(16) 0.09319(12) 0.0437(5) Uani 1 1 d . . . C4 C 0.49128(8) 0.1090(2) 0.06041(15) 0.0484(6) Uani 1 1 d . . . C6 C 0.55342(7) 0.2244(2) 0.06803(14) 0.0440(6) Uani 1 1 d . . . N3 N 0.68867(6) 0.18242(18) 0.21374(13) 0.0508(5) Uani 1 1 d . . . C5 C 0.53643(7) 0.1216(2) 0.08533(14) 0.0415(5) Uani 1 1 d . . . C7 C 0.52452(8) 0.3117(2) 0.02986(17) 0.0540(7) Uani 1 1 d . . . H7 H 0.5349 0.3809 0.0200 0.065 Uiso 1 1 calc R . . C2 C 0.50608(9) -0.0802(2) 0.11625(17) 0.0580(7) Uani 1 1 d . . . H2 H 0.4968 -0.1501 0.1273 0.070 Uiso 1 1 calc R . . C3 C 0.47710(8) 0.0033(3) 0.07748(16) 0.0555(7) Uani 1 1 d . . . H3 H 0.4477 -0.0088 0.0620 0.067 Uiso 1 1 calc R . . C10 C 0.59642(8) 0.3101(2) -0.04460(15) 0.0515(6) Uani 1 1 d . . . C1 C 0.55068(9) -0.0605(2) 0.13993(16) 0.0517(6) Uani 1 1 d . . . H1 H 0.5704 -0.1185 0.1669 0.062 Uiso 1 1 calc R . . C17 C 0.61643(10) 0.4787(3) 0.15191(17) 0.0642(7) Uani 1 1 d . . . H17 H 0.6066 0.4194 0.1720 0.077 Uiso 1 1 calc R . . C9 C 0.46289(9) 0.2007(3) 0.01946(18) 0.0593(7) Uani 1 1 d . . . H9 H 0.4331 0.1938 0.0024 0.071 Uiso 1 1 calc R . . C22 C 0.67518(8) 0.2580(2) 0.08965(16) 0.0498(6) Uani 1 1 d . . . H22A H 0.6740 0.1798 0.0707 0.060 Uiso 1 1 calc R . . H22B H 0.6897 0.3064 0.0681 0.060 Uiso 1 1 calc R . . C11 C 0.60162(10) 0.2119(3) -0.08063(17) 0.0619(7) Uani 1 1 d . . . H11 H 0.6171 0.1487 -0.0515 0.074 Uiso 1 1 calc R . . C16 C 0.62524(8) 0.4565(2) 0.09195(15) 0.0477(6) Uani 1 1 d . . . C21 C 0.64009(9) 0.5464(2) 0.06268(19) 0.0608(7) Uani 1 1 d . . . H21 H 0.6464 0.5320 0.0224 0.073 Uiso 1 1 calc R . . C8 C 0.47990(9) 0.2987(2) 0.00549(19) 0.0613(7) Uani 1 1 d . . . H8 H 0.4613 0.3591 -0.0211 0.074 Uiso 1 1 calc R . . C23 C 0.70110(8) 0.2574(2) 0.17446(16) 0.0511(6) Uani 1 1 d . . . C26 C 0.74650(11) 0.2556(3) 0.3286(2) 0.0819(10) Uani 1 1 d . . . H26 H 0.7614 0.2532 0.3816 0.098 Uiso 1 1 calc R . . C15 C 0.57236(10) 0.4021(3) -0.08883(18) 0.0690(8) Uani 1 1 d . . . H15 H 0.5678 0.4676 -0.0658 0.083 Uiso 1 1 calc R . . C25 C 0.75877(10) 0.3297(3) 0.2896(2) 0.0815(10) Uani 1 1 d . . . H25 H 0.7823 0.3792 0.3150 0.098 Uiso 1 1 calc R . . C24 C 0.73587(9) 0.3311(3) 0.2112(2) 0.0664(8) Uani 1 1 d . . . H24 H 0.7439 0.3817 0.1830 0.080 Uiso 1 1 calc R . . C27 C 0.71141(10) 0.1827(3) 0.28945(18) 0.0685(8) Uani 1 1 d . . . H27 H 0.7034 0.1316 0.3174 0.082 Uiso 1 1 calc R . . C13 C 0.56044(13) 0.2990(4) -0.2028(2) 0.0849(10) Uani 1 1 d . . . H13 H 0.5481 0.2953 -0.2557 0.102 Uiso 1 1 calc R . . C14 C 0.55512(12) 0.3961(4) -0.1675(2) 0.0873(11) Uani 1 1 d . . . H14 H 0.5397 0.4590 -0.1971 0.105 Uiso 1 1 calc R . . C20 C 0.64542(10) 0.6556(3) 0.0927(2) 0.0751(10) Uani 1 1 d . . . H20 H 0.6550 0.7152 0.0724 0.090 Uiso 1 1 calc R . . C18 C 0.62216(12) 0.5893(3) 0.1827(2) 0.0840(11) Uani 1 1 d . . . H18 H 0.6163 0.6044 0.2235 0.101 Uiso 1 1 calc R . . C19 C 0.63675(12) 0.6772(3) 0.1521(3) 0.0846(11) Uani 1 1 d . . . H19 H 0.6406 0.7516 0.1724 0.102 Uiso 1 1 calc R . . C12 C 0.58412(12) 0.2073(3) -0.1591(2) 0.0790(9) Uani 1 1 d . . . H12 H 0.5884 0.1419 -0.1825 0.095 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 0.0352(2) 0.0389(2) 0.0528(3) 0.00264(17) 0.01456(19) -0.00055(16) P1 0.0382(3) 0.0345(3) 0.0513(4) -0.0016(3) 0.0174(3) -0.0043(2) Cl2 0.0466(3) 0.0417(3) 0.0607(4) -0.0019(3) 0.0210(3) 0.0013(3) Cl1 0.0579(4) 0.0566(4) 0.0578(4) 0.0087(3) 0.0164(3) 0.0005(3) N1 0.0382(10) 0.0394(11) 0.0483(11) 0.0024(9) 0.0180(9) -0.0020(8) N2 0.0347(10) 0.0367(10) 0.0554(12) 0.0015(9) 0.0168(9) -0.0021(8) C4 0.0382(13) 0.0501(14) 0.0549(15) -0.0028(12) 0.0195(12) -0.0034(11) C6 0.0383(12) 0.0397(13) 0.0522(14) -0.0023(11) 0.0191(11) -0.0013(10) N3 0.0386(11) 0.0485(12) 0.0566(13) -0.0017(10) 0.0142(10) -0.0030(9) C5 0.0370(12) 0.0389(12) 0.0472(13) -0.0032(10) 0.0180(11) -0.0022(10) C7 0.0452(14) 0.0397(13) 0.0711(18) 0.0033(12) 0.0213(13) -0.0001(11) C2 0.0525(15) 0.0533(15) 0.0687(18) 0.0038(14) 0.0281(14) -0.0131(13) C3 0.0392(13) 0.0629(16) 0.0650(17) 0.0018(14) 0.0243(12) -0.0085(13) C10 0.0488(14) 0.0497(14) 0.0541(15) -0.0025(12) 0.0217(12) -0.0096(12) C1 0.0480(14) 0.0443(14) 0.0597(16) 0.0055(12) 0.0219(13) -0.0019(11) C17 0.0682(18) 0.0537(16) 0.0676(18) -0.0087(14) 0.0282(15) -0.0045(14) C9 0.0362(13) 0.0623(17) 0.0740(19) -0.0007(14) 0.0203(13) 0.0024(12) C22 0.0429(13) 0.0430(13) 0.0664(16) -0.0013(12) 0.0274(12) -0.0041(11) C11 0.0676(18) 0.0558(16) 0.0636(18) -0.0052(14) 0.0311(15) -0.0073(14) C16 0.0416(13) 0.0367(12) 0.0565(15) -0.0025(11) 0.0151(12) -0.0034(10) C21 0.0550(16) 0.0432(15) 0.0781(19) -0.0005(13) 0.0249(15) -0.0064(12) C8 0.0443(15) 0.0480(15) 0.082(2) 0.0058(14) 0.0204(14) 0.0106(12) C23 0.0343(12) 0.0479(14) 0.0651(17) -0.0042(13) 0.0174(12) -0.0010(11) C26 0.0560(18) 0.095(2) 0.068(2) -0.0114(19) 0.0042(16) -0.0137(18) C15 0.0685(19) 0.0613(17) 0.0593(18) -0.0008(14) 0.0137(15) 0.0016(15) C25 0.0487(17) 0.079(2) 0.092(3) -0.016(2) 0.0107(18) -0.0204(16) C24 0.0422(15) 0.0622(18) 0.083(2) -0.0027(15) 0.0187(15) -0.0120(13) C27 0.0533(16) 0.073(2) 0.0616(19) -0.0017(15) 0.0113(15) -0.0056(14) C13 0.087(2) 0.104(3) 0.0558(19) -0.007(2) 0.0261(18) -0.020(2) C14 0.084(2) 0.087(2) 0.064(2) 0.0153(19) 0.0111(18) -0.0003(19) C20 0.0622(19) 0.0399(15) 0.107(3) -0.0040(17) 0.0250(19) -0.0066(13) C18 0.085(2) 0.077(2) 0.084(2) -0.0270(19) 0.034(2) 0.0052(19) C19 0.072(2) 0.0462(18) 0.112(3) -0.0219(19) 0.021(2) -0.0017(15) C12 0.087(2) 0.086(2) 0.067(2) -0.0199(19) 0.0373(19) -0.017(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 N2 2.0753(19) . ? Ni1 N1 2.0796(19) . ? Ni1 N3 2.153(2) . ? Ni1 Cl2 2.3260(8) . ? Ni1 Cl1 2.3403(8) . ? P1 N2 1.605(2) . ? P1 C22 1.792(2) . ? P1 C16 1.795(2) . ? P1 C10 1.801(3) . ? N1 C1 1.322(3) . ? N1 C5 1.361(3) . ? N2 C6 1.396(3) . ? C4 C3 1.410(4) . ? C4 C5 1.415(3) . ? C4 C9 1.417(4) . ? C6 C7 1.375(4) . ? C6 C5 1.431(3) . ? N3 C27 1.331(4) . ? N3 C23 1.354(3) . ? C7 C8 1.400(4) . ? C7 H7 0.9300 . ? C2 C3 1.348(4) . ? C2 C1 1.412(4) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C10 C15 1.384(4) . ? C10 C11 1.391(4) . ? C1 H1 0.9300 . ? C17 C16 1.371(4) . ? C17 C18 1.387(4) . ? C17 H17 0.9300 . ? C9 C8 1.359(4) . ? C9 H9 0.9300 . ? C22 C23 1.492(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C11 C12 1.378(4) . ? C11 H11 0.9300 . ? C16 C21 1.393(4) . ? C21 C20 1.368(4) . ? C21 H21 0.9300 . ? C8 H8 0.9300 . ? C23 C24 1.377(4) . ? C26 C25 1.340(5) . ? C26 C27 1.386(4) . ? C26 H26 0.9300 . ? C15 C14 1.385(5) . ? C15 H15 0.9300 . ? C25 C24 1.377(5) . ? C25 H25 0.9300 . ? C24 H24 0.9300 . ? C27 H27 0.9300 . ? C13 C12 1.373(5) . ? C13 C14 1.373(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C20 C19 1.354(6) . ? C20 H20 0.9300 . ? C18 C19 1.386(6) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C12 H12 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N1 78.82(7) . . ? N2 Ni1 N3 89.51(8) . . ? N1 Ni1 N3 157.53(8) . . ? N2 Ni1 Cl2 99.48(6) . . ? N1 Ni1 Cl2 99.20(6) . . ? N3 Ni1 Cl2 101.64(6) . . ? N2 Ni1 Cl1 158.76(6) . . ? N1 Ni1 Cl1 92.15(6) . . ? N3 Ni1 Cl1 92.06(6) . . ? Cl2 Ni1 Cl1 100.94(3) . . ? N2 P1 C22 106.38(11) . . ? N2 P1 C16 113.58(12) . . ? C22 P1 C16 106.85(12) . . ? N2 P1 C10 114.25(11) . . ? C22 P1 C10 105.69(13) . . ? C16 P1 C10 109.46(12) . . ? C1 N1 C5 118.7(2) . . ? C1 N1 Ni1 126.90(17) . . ? C5 N1 Ni1 114.40(14) . . ? C6 N2 P1 121.58(17) . . ? C6 N2 Ni1 114.31(15) . . ? P1 N2 Ni1 122.84(11) . . ? C3 C4 C5 117.1(2) . . ? C3 C4 C9 123.6(2) . . ? C5 C4 C9 119.3(2) . . ? C7 C6 N2 127.7(2) . . ? C7 C6 C5 117.4(2) . . ? N2 C6 C5 114.8(2) . . ? C27 N3 C23 117.3(2) . . ? C27 N3 Ni1 119.7(2) . . ? C23 N3 Ni1 122.55(17) . . ? N1 C5 C4 122.2(2) . . ? N1 C5 C6 117.1(2) . . ? C4 C5 C6 120.7(2) . . ? C6 C7 C8 121.5(2) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C3 C2 C1 119.4(2) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 120.2(2) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C15 C10 C11 118.9(3) . . ? C15 C10 P1 123.1(2) . . ? C11 C10 P1 117.9(2) . . ? N1 C1 C2 122.5(2) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C16 C17 C18 120.3(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C8 C9 C4 118.9(2) . . ? C8 C9 H9 120.5 . . ? C4 C9 H9 120.5 . . ? C23 C22 P1 112.88(18) . . ? C23 C22 H22A 109.0 . . ? P1 C22 H22A 109.0 . . ? C23 C22 H22B 109.0 . . ? P1 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C12 C11 C10 120.6(3) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C17 C16 C21 119.1(3) . . ? C17 C16 P1 118.8(2) . . ? C21 C16 P1 122.0(2) . . ? C20 C21 C16 120.6(3) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? C9 C8 C7 122.1(3) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? N3 C23 C24 121.5(3) . . ? N3 C23 C22 117.1(2) . . ? C24 C23 C22 121.4(3) . . ? C25 C26 C27 119.6(3) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C10 C15 C14 119.6(3) . . ? C10 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C26 C25 C24 118.6(3) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? N3 C27 C26 123.0(3) . . ? N3 C27 H27 118.5 . . ? C26 C27 H27 118.5 . . ? C12 C13 C14 119.4(3) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C13 C14 C15 121.1(3) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C19 C20 C21 120.2(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C19 C18 C17 119.3(4) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C20 C19 C18 120.6(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? 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 N1 C1 176.3(2) . . . . ? N3 Ni1 N1 C1 -123.7(3) . . . . ? Cl2 Ni1 N1 C1 78.4(2) . . . . ? Cl1 Ni1 N1 C1 -23.1(2) . . . . ? N2 Ni1 N1 C5 -5.90(16) . . . . ? N3 Ni1 N1 C5 54.1(3) . . . . ? Cl2 Ni1 N1 C5 -103.84(16) . . . . ? Cl1 Ni1 N1 C5 154.71(16) . . . . ? C22 P1 N2 C6 -167.04(19) . . . . ? C16 P1 N2 C6 75.7(2) . . . . ? C10 P1 N2 C6 -50.8(2) . . . . ? C22 P1 N2 Ni1 -0.68(17) . . . . ? C16 P1 N2 Ni1 -117.94(14) . . . . ? C10 P1 N2 Ni1 115.53(15) . . . . ? N1 Ni1 N2 C6 6.69(16) . . . . ? N3 Ni1 N2 C6 -153.99(17) . . . . ? Cl2 Ni1 N2 C6 104.29(16) . . . . ? Cl1 Ni1 N2 C6 -59.6(3) . . . . ? N1 Ni1 N2 P1 -160.57(15) . . . . ? N3 Ni1 N2 P1 38.74(14) . . . . ? Cl2 Ni1 N2 P1 -62.98(13) . . . . ? Cl1 Ni1 N2 P1 133.18(13) . . . . ? P1 N2 C6 C7 -19.7(4) . . . . ? Ni1 N2 C6 C7 172.9(2) . . . . ? P1 N2 C6 C5 160.92(18) . . . . ? Ni1 N2 C6 C5 -6.5(3) . . . . ? N2 Ni1 N3 C27 132.2(2) . . . . ? N1 Ni1 N3 C27 74.0(3) . . . . ? Cl2 Ni1 N3 C27 -128.2(2) . . . . ? Cl1 Ni1 N3 C27 -26.6(2) . . . . ? N2 Ni1 N3 C23 -39.8(2) . . . . ? N1 Ni1 N3 C23 -97.9(3) . . . . ? Cl2 Ni1 N3 C23 59.8(2) . . . . ? Cl1 Ni1 N3 C23 161.39(19) . . . . ? C1 N1 C5 C4 1.1(4) . . . . ? Ni1 N1 C5 C4 -176.85(18) . . . . ? C1 N1 C5 C6 -177.8(2) . . . . ? Ni1 N1 C5 C6 4.3(3) . . . . ? C3 C4 C5 N1 -1.1(4) . . . . ? C9 C4 C5 N1 179.7(2) . . . . ? C3 C4 C5 C6 177.7(2) . . . . ? C9 C4 C5 C6 -1.5(4) . . . . ? C7 C6 C5 N1 -178.0(2) . . . . ? N2 C6 C5 N1 1.5(3) . . . . ? C7 C6 C5 C4 3.1(4) . . . . ? N2 C6 C5 C4 -177.4(2) . . . . ? N2 C6 C7 C8 177.6(3) . . . . ? C5 C6 C7 C8 -3.0(4) . . . . ? C1 C2 C3 C4 0.4(4) . . . . ? C5 C4 C3 C2 0.3(4) . . . . ? C9 C4 C3 C2 179.5(3) . . . . ? N2 P1 C10 C15 109.2(2) . . . . ? C22 P1 C10 C15 -134.2(3) . . . . ? C16 P1 C10 C15 -19.5(3) . . . . ? N2 P1 C10 C11 -69.8(2) . . . . ? C22 P1 C10 C11 46.8(2) . . . . ? C16 P1 C10 C11 161.5(2) . . . . ? C5 N1 C1 C2 -0.4(4) . . . . ? Ni1 N1 C1 C2 177.3(2) . . . . ? C3 C2 C1 N1 -0.4(4) . . . . ? C3 C4 C9 C8 -179.5(3) . . . . ? C5 C4 C9 C8 -0.3(4) . . . . ? N2 P1 C22 C23 -60.8(2) . . . . ? C16 P1 C22 C23 60.8(2) . . . . ? C10 P1 C22 C23 177.36(18) . . . . ? C15 C10 C11 C12 1.8(4) . . . . ? P1 C10 C11 C12 -179.2(2) . . . . ? C18 C17 C16 C21 0.1(4) . . . . ? C18 C17 C16 P1 175.8(3) . . . . ? N2 P1 C16 C17 10.7(3) . . . . ? C22 P1 C16 C17 -106.2(2) . . . . ? C10 P1 C16 C17 139.8(2) . . . . ? N2 P1 C16 C21 -173.7(2) . . . . ? C22 P1 C16 C21 69.3(3) . . . . ? C10 P1 C16 C21 -44.7(3) . . . . ? C17 C16 C21 C20 -0.7(4) . . . . ? P1 C16 C21 C20 -176.2(2) . . . . ? C4 C9 C8 C7 0.4(5) . . . . ? C6 C7 C8 C9 1.3(5) . . . . ? C27 N3 C23 C24 0.1(4) . . . . ? Ni1 N3 C23 C24 172.2(2) . . . . ? C27 N3 C23 C22 -179.2(2) . . . . ? Ni1 N3 C23 C22 -7.1(3) . . . . ? P1 C22 C23 N3 67.0(3) . . . . ? P1 C22 C23 C24 -112.3(3) . . . . ? C11 C10 C15 C14 -1.9(5) . . . . ? P1 C10 C15 C14 179.1(3) . . . . ? C27 C26 C25 C24 0.1(6) . . . . ? C26 C25 C24 C23 0.1(5) . . . . ? N3 C23 C24 C25 -0.2(5) . . . . ? C22 C23 C24 C25 179.1(3) . . . . ? C23 N3 C27 C26 0.2(5) . . . . ? Ni1 N3 C27 C26 -172.2(3) . . . . ? C25 C26 C27 N3 -0.3(6) . . . . ? C12 C13 C14 C15 -1.6(6) . . . . ? C10 C15 C14 C13 1.9(6) . . . . ? C16 C21 C20 C19 0.8(5) . . . . ? C16 C17 C18 C19 0.2(5) . . . . ? C21 C20 C19 C18 -0.4(5) . . . . ? C17 C18 C19 C20 -0.1(5) . . . . ? C14 C13 C12 C11 1.3(5) . . . . ? C10 C11 C12 C13 -1.5(5) . . . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.009 -0.205 0.259 1409 251 ' ' 2 0.018 0.194 0.768 1409 251 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 62.76 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.265 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.058 # Attachment '- 9.cif' data_101231a _database_code_depnum_ccdc_archive 'CCDC 878351' #TrackingRef '- 9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H38 Cl4 N3 Ni O P' _chemical_formula_weight 808.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4343(15) _cell_length_b 11.6020(15) _cell_length_c 17.1801(19) _cell_angle_alpha 76.682(2) _cell_angle_beta 73.1970(10) _cell_angle_gamma 64.5420(10) _cell_volume 1955.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2195 _cell_measurement_theta_min 2.495 _cell_measurement_theta_max 26.086 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 0.846 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8424 _exptl_absorpt_correction_T_max 0.9354 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 10204 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.1121 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6709 _reflns_number_gt 3629 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6709 _refine_ls_number_parameters 507 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1415 _refine_ls_R_factor_gt 0.0858 _refine_ls_wR_factor_ref 0.2113 _refine_ls_wR_factor_gt 0.1953 _refine_ls_goodness_of_fit_ref 1.309 _refine_ls_restrained_S_all 1.309 _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 0.58843(9) 0.30658(8) 0.29714(6) 0.0407(3) Uani 1 1 d . . . Cl1 Cl 0.65645(18) 0.47284(17) 0.22908(12) 0.0520(5) Uani 1 1 d . . . Cl2 Cl 0.79756(18) 0.14786(18) 0.28989(13) 0.0585(6) Uani 1 1 d . . . Cl3 Cl 0.7876(5) 0.2920(5) -0.0034(3) 0.192(2) Uani 1 1 d . A . Cl4 Cl 1.0097(8) 0.3051(12) 0.0221(5) 0.212(6) Uani 0.620(13) 1 d P A 1 Cl4' Cl 1.0098(13) 0.129(2) 0.0484(8) 0.212(10) Uani 0.380(13) 1 d P A 2 N1 N 0.5600(6) 0.3235(5) 0.4182(4) 0.0478(15) Uani 1 1 d . . . N2 N 0.3874(5) 0.4104(5) 0.3233(3) 0.0439(14) Uani 1 1 d . . . N3 N 0.5536(6) 0.2313(5) 0.2052(3) 0.0446(14) Uani 1 1 d . . . O1 O 0.312(3) 0.074(3) 0.4921(17) 0.139(10) Uani 0.68(3) 1 d P B 1 O1' O 0.305(3) 0.185(3) 0.4949(17) 0.105(12) Uani 0.32(3) 1 d P B 2 P1 P 0.30503(18) 0.48463(17) 0.25300(12) 0.0422(5) Uani 1 1 d . . . C1 C 0.6536(8) 0.2786(7) 0.4612(5) 0.057(2) Uani 1 1 d . . . H1 H 0.7420 0.2373 0.4360 0.068 Uiso 1 1 calc R . . C2 C 0.6197(9) 0.2932(8) 0.5443(5) 0.061(2) Uani 1 1 d . . . H2 H 0.6860 0.2597 0.5740 0.073 Uiso 1 1 calc R . . C3 C 0.4939(9) 0.3543(8) 0.5819(5) 0.059(2) Uani 1 1 d . . . H3 H 0.4739 0.3643 0.6370 0.071 Uiso 1 1 calc R . . C4 C 0.3914(8) 0.4035(7) 0.5386(5) 0.056(2) Uani 1 1 d . . . C5 C 0.4302(7) 0.3865(7) 0.4545(4) 0.0465(18) Uani 1 1 d . . . C6 C 0.3372(8) 0.4330(7) 0.4054(5) 0.0489(19) Uani 1 1 d . . . C7 C 0.2073(8) 0.4974(7) 0.4424(5) 0.060(2) Uani 1 1 d . . . H7 H 0.1426 0.5305 0.4116 0.071 Uiso 1 1 calc R . . C8 C 0.1700(9) 0.5143(8) 0.5254(5) 0.066(2) Uani 1 1 d . . . H8 H 0.0811 0.5586 0.5482 0.079 Uiso 1 1 calc R . . C9 C 0.2556(9) 0.4700(8) 0.5713(5) 0.065(2) Uani 1 1 d . . . H9 H 0.2273 0.4821 0.6264 0.078 Uiso 1 1 calc R . . C10 C 0.4231(7) 0.4452(6) 0.1574(4) 0.0453(17) Uani 1 1 d . . . H10A H 0.3797 0.4893 0.1119 0.054 Uiso 1 1 calc R . . H10B H 0.4941 0.4730 0.1520 0.054 Uiso 1 1 calc R . . C11 C 0.4796(7) 0.3004(7) 0.1558(4) 0.0433(17) Uani 1 1 d . . . C12 C 0.4384(7) 0.2535(7) 0.0988(5) 0.053(2) Uani 1 1 d . . . C13 C 0.3849(8) 0.1628(8) 0.1235(5) 0.064(2) Uani 1 1 d . . . H13 H 0.3722 0.1275 0.1781 0.077 Uiso 1 1 calc R . . C14 C 0.3502(10) 0.1243(10) 0.0677(7) 0.085(3) Uani 1 1 d . . . H14 H 0.3182 0.0591 0.0853 0.102 Uiso 1 1 calc R . . C15 C 0.3591(11) 0.1737(11) -0.0093(7) 0.092(3) Uani 1 1 d . . . H15 H 0.3328 0.1455 -0.0452 0.111 Uiso 1 1 calc R . . C16 C 0.4092(11) 0.2698(10) -0.0361(6) 0.089(3) Uani 1 1 d . . . H16 H 0.4169 0.3068 -0.0904 0.107 Uiso 1 1 calc R . . C17 C 0.4463(9) 0.3087(9) 0.0175(5) 0.070(2) Uani 1 1 d . . . H17 H 0.4779 0.3741 -0.0003 0.084 Uiso 1 1 calc R . . C18 C 0.2381(7) 0.6568(7) 0.2478(5) 0.0528(19) Uani 1 1 d . . . C19 C 0.3217(8) 0.7126(8) 0.2416(5) 0.065(2) Uani 1 1 d . . . H19 H 0.4111 0.6616 0.2396 0.079 Uiso 1 1 calc R . . C20 C 0.2778(10) 0.8469(8) 0.2381(6) 0.083(3) Uani 1 1 d . . . H20 H 0.3360 0.8856 0.2339 0.099 Uiso 1 1 calc R . . C21 C 0.1430(11) 0.9191(9) 0.2411(7) 0.092(3) Uani 1 1 d . . . H21 H 0.1107 1.0080 0.2393 0.111 Uiso 1 1 calc R . . C22 C 0.0577(10) 0.8635(9) 0.2465(7) 0.087(3) Uani 1 1 d . . . H22 H -0.0315 0.9138 0.2475 0.104 Uiso 1 1 calc R . . C23 C 0.1044(9) 0.7329(8) 0.2505(6) 0.077(3) Uani 1 1 d . . . H23 H 0.0459 0.6943 0.2551 0.092 Uiso 1 1 calc R . . C24 C 0.1801(7) 0.4315(7) 0.2543(5) 0.0515(19) Uani 1 1 d . . . C25 C 0.1037(8) 0.4830(8) 0.1942(6) 0.067(2) Uani 1 1 d . . . H25 H 0.1169 0.5470 0.1532 0.080 Uiso 1 1 calc R . . C26 C 0.0096(9) 0.4381(10) 0.1968(6) 0.081(3) Uani 1 1 d . . . H26 H -0.0464 0.4774 0.1601 0.097 Uiso 1 1 calc R . . C27 C -0.0035(9) 0.3370(10) 0.2520(6) 0.075(3) Uani 1 1 d . . . H27 H -0.0650 0.3050 0.2511 0.089 Uiso 1 1 calc R . . C28 C 0.0746(9) 0.2823(9) 0.3091(6) 0.074(3) Uani 1 1 d . . . H28 H 0.0670 0.2124 0.3465 0.089 Uiso 1 1 calc R . . C29 C 0.1642(8) 0.3317(8) 0.3106(5) 0.060(2) Uani 1 1 d . . . H29 H 0.2146 0.2965 0.3504 0.072 Uiso 1 1 calc R . . C30 C 0.6059(8) 0.0940(7) 0.2126(5) 0.0511(19) Uani 1 1 d . . . C31 C 0.5591(10) 0.0298(8) 0.2829(6) 0.076(3) Uani 1 1 d . . . H31 H 0.4925 0.0750 0.3237 0.092 Uiso 1 1 calc R . . C32 C 0.6130(11) -0.1069(10) 0.2933(7) 0.095(3) Uani 1 1 d . . . H32 H 0.5802 -0.1511 0.3408 0.114 Uiso 1 1 calc R . . C33 C 0.7083(12) -0.1711(10) 0.2368(8) 0.095(3) Uani 1 1 d . . . H33 H 0.7413 -0.2605 0.2442 0.114 Uiso 1 1 calc R . . C34 C 0.7607(10) -0.1087(9) 0.1664(7) 0.082(3) Uani 1 1 d . . . H34 H 0.8304 -0.1554 0.1274 0.098 Uiso 1 1 calc R . . C35 C 0.7074(8) 0.0256(8) 0.1543(5) 0.064(2) Uani 1 1 d . . . H35 H 0.7409 0.0689 0.1066 0.077 Uiso 1 1 calc R . . C36 C 0.8733(16) 0.272(2) 0.0700(10) 0.195(8) Uani 1 1 d . . . H36A H 0.8176 0.3300 0.1109 0.234 Uiso 0.620(13) 1 calc PR A 1 H36B H 0.8994 0.1845 0.0972 0.234 Uiso 0.620(13) 1 calc PR A 1 H36C H 0.8213 0.2641 0.1252 0.234 Uiso 0.380(13) 1 d PR A 2 H36D H 0.8998 0.3435 0.0628 0.234 Uiso 0.380(13) 1 d PR A 2 C37 C 0.217(4) 0.161(5) 0.551(2) 0.135(12) Uani 0.68(3) 1 d P B 1 H37A H 0.2354 0.2376 0.5426 0.162 Uiso 0.68(3) 1 calc PR B 1 H37B H 0.2248 0.1193 0.6064 0.162 Uiso 0.68(3) 1 calc PR B 1 C38 C 0.077(3) 0.197(4) 0.5402(13) 0.134(13) Uani 0.68(3) 1 d P B 1 H38A H 0.0132 0.2152 0.5917 0.161 Uiso 0.68(3) 1 calc PR B 1 H38B H 0.0527 0.2721 0.5000 0.161 Uiso 0.68(3) 1 calc PR B 1 C39 C 0.083(3) 0.080(3) 0.5109(15) 0.132(11) Uani 0.68(3) 1 d P B 1 H39A H 0.0192 0.1030 0.4773 0.158 Uiso 0.68(3) 1 calc PR B 1 H39B H 0.0700 0.0156 0.5561 0.158 Uiso 0.68(3) 1 calc PR B 1 C40 C 0.229(3) 0.035(2) 0.4597(14) 0.131(10) Uani 0.68(3) 1 d P B 1 H40A H 0.2668 -0.0583 0.4614 0.157 Uiso 0.68(3) 1 calc PR B 1 H40B H 0.2296 0.0719 0.4030 0.157 Uiso 0.68(3) 1 calc PR B 1 C37' C 0.165(8) 0.223(6) 0.531(3) 0.092(16) Uani 0.32(3) 1 d P B 2 H37C H 0.1115 0.2907 0.4959 0.111 Uiso 0.32(3) 1 calc PR B 2 H37D H 0.1435 0.2532 0.5841 0.111 Uiso 0.32(3) 1 calc PR B 2 C38' C 0.144(8) 0.098(6) 0.541(4) 0.12(2) Uani 0.32(3) 1 d P B 2 H38C H 0.0850 0.0872 0.5932 0.140 Uiso 0.32(3) 1 calc PR B 2 H38D H 0.1055 0.0985 0.4974 0.140 Uiso 0.32(3) 1 calc PR B 2 C39' C 0.283(5) -0.010(5) 0.537(3) 0.13(2) Uani 0.32(3) 1 d P B 2 H39C H 0.2964 -0.0705 0.5013 0.158 Uiso 0.32(3) 1 calc PR B 2 H39D H 0.2916 -0.0562 0.5912 0.158 Uiso 0.32(3) 1 calc PR B 2 C40' C 0.387(7) 0.051(7) 0.503(4) 0.102(19) Uani 0.32(3) 1 d P B 2 H40C H 0.4431 0.0310 0.5417 0.122 Uiso 0.32(3) 1 calc PR B 2 H40D H 0.4423 0.0234 0.4510 0.122 Uiso 0.32(3) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0336(5) 0.0340(5) 0.0472(6) -0.0081(4) -0.0075(4) -0.0056(4) Cl1 0.0416(11) 0.0468(11) 0.0627(12) -0.0022(9) -0.0091(9) -0.0162(9) Cl2 0.0387(11) 0.0431(11) 0.0799(15) -0.0142(10) -0.0164(10) 0.0024(9) Cl3 0.200(5) 0.235(5) 0.148(4) 0.065(3) -0.070(3) -0.114(4) Cl4 0.138(7) 0.330(15) 0.180(8) -0.109(8) 0.012(5) -0.093(7) Cl4' 0.138(11) 0.33(3) 0.180(13) -0.108(14) 0.012(9) -0.093(13) N1 0.051(4) 0.043(4) 0.051(4) -0.007(3) -0.012(3) -0.019(3) N2 0.039(3) 0.042(4) 0.046(4) -0.010(3) -0.006(3) -0.011(3) N3 0.049(4) 0.037(4) 0.046(4) -0.006(3) -0.010(3) -0.015(3) O1 0.16(3) 0.102(18) 0.080(14) 0.026(12) -0.013(16) 0.00(2) O1' 0.11(2) 0.09(2) 0.075(19) 0.005(14) -0.008(15) -0.013(18) P1 0.0317(10) 0.0349(11) 0.0503(12) -0.0077(8) -0.0059(9) -0.0048(8) C1 0.057(5) 0.052(5) 0.055(5) -0.003(4) -0.019(4) -0.014(4) C2 0.069(6) 0.058(5) 0.062(6) -0.004(4) -0.028(5) -0.023(5) C3 0.073(6) 0.056(5) 0.050(5) -0.008(4) -0.014(5) -0.026(5) C4 0.066(6) 0.051(5) 0.052(5) -0.012(4) -0.005(4) -0.025(4) C5 0.048(5) 0.044(4) 0.049(5) -0.010(4) -0.004(4) -0.021(4) C6 0.050(5) 0.046(5) 0.053(5) -0.009(4) -0.005(4) -0.024(4) C7 0.051(5) 0.060(5) 0.059(5) -0.013(4) -0.003(4) -0.016(4) C8 0.054(5) 0.070(6) 0.059(6) -0.015(5) 0.003(5) -0.018(5) C9 0.068(6) 0.067(6) 0.051(5) -0.016(4) 0.003(5) -0.024(5) C10 0.046(4) 0.036(4) 0.046(4) 0.001(3) -0.013(3) -0.010(3) C11 0.042(4) 0.043(4) 0.044(4) -0.006(3) -0.009(3) -0.015(4) C12 0.053(5) 0.051(5) 0.052(5) -0.010(4) -0.012(4) -0.016(4) C13 0.071(6) 0.060(6) 0.067(6) -0.007(4) -0.026(5) -0.024(5) C14 0.094(8) 0.080(7) 0.088(8) -0.011(6) -0.031(6) -0.032(6) C15 0.099(8) 0.102(9) 0.087(8) -0.031(7) -0.035(7) -0.030(7) C16 0.100(8) 0.096(8) 0.066(7) -0.012(6) -0.022(6) -0.031(7) C17 0.079(7) 0.070(6) 0.058(6) -0.008(5) -0.018(5) -0.023(5) C18 0.044(5) 0.037(4) 0.067(5) -0.008(4) -0.013(4) -0.005(4) C19 0.053(5) 0.049(5) 0.086(6) -0.011(4) -0.021(5) -0.007(4) C20 0.077(7) 0.043(6) 0.124(9) -0.021(5) -0.024(6) -0.014(5) C21 0.074(7) 0.050(6) 0.124(9) -0.017(6) -0.022(6) 0.006(6) C22 0.052(6) 0.051(6) 0.133(9) -0.027(6) -0.022(6) 0.013(5) C23 0.054(6) 0.055(6) 0.108(8) -0.021(5) -0.013(5) -0.005(5) C24 0.044(5) 0.050(5) 0.058(5) -0.012(4) -0.008(4) -0.014(4) C25 0.051(5) 0.067(6) 0.081(6) -0.011(5) -0.019(5) -0.018(4) C26 0.054(6) 0.095(8) 0.096(8) -0.020(6) -0.033(5) -0.018(6) C27 0.053(6) 0.085(7) 0.092(7) -0.021(6) -0.010(5) -0.031(5) C28 0.067(6) 0.073(7) 0.082(7) -0.013(5) -0.004(5) -0.033(5) C29 0.058(5) 0.058(5) 0.064(5) -0.010(4) -0.011(4) -0.023(4) C30 0.058(5) 0.039(5) 0.054(5) -0.008(4) -0.018(4) -0.012(4) C31 0.085(7) 0.050(6) 0.078(7) 0.002(5) -0.012(5) -0.020(5) C32 0.106(9) 0.058(7) 0.095(8) 0.014(6) -0.017(7) -0.023(6) C33 0.109(9) 0.051(6) 0.107(9) -0.009(6) -0.032(7) -0.009(6) C34 0.088(7) 0.057(6) 0.086(7) -0.031(5) -0.024(6) 0.000(5) C35 0.071(6) 0.047(5) 0.067(6) -0.011(4) -0.018(5) -0.013(4) C36 0.134(14) 0.32(3) 0.160(15) -0.125(16) 0.004(12) -0.094(17) C37 0.14(3) 0.12(3) 0.09(2) 0.00(2) -0.01(2) -0.02(3) C38 0.13(3) 0.11(2) 0.066(12) 0.033(13) -0.015(15) 0.02(2) C39 0.13(2) 0.11(2) 0.074(16) 0.037(13) -0.031(14) 0.005(17) C40 0.14(2) 0.104(16) 0.084(15) 0.021(12) -0.018(15) -0.005(15) C37' 0.10(5) 0.08(4) 0.06(3) 0.02(2) -0.02(3) -0.01(3) C38' 0.13(5) 0.10(4) 0.07(4) 0.01(3) -0.02(3) -0.01(5) C39' 0.13(4) 0.11(4) 0.08(3) 0.02(3) -0.02(3) -0.01(3) C40' 0.12(5) 0.09(4) 0.06(3) 0.01(2) -0.02(3) -0.01(4) _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 2.052(5) . ? Ni1 N1 2.052(6) . ? Ni1 N3 2.171(6) . ? Ni1 Cl2 2.296(2) . ? Ni1 Cl1 2.328(2) . ? Cl3 C36 1.730(16) . ? Cl4 C36 1.698(18) . ? Cl4 H36D 1.1917 . ? Cl4' C36 1.75(2) . ? N1 C1 1.328(9) . ? N1 C5 1.367(9) . ? N2 C6 1.401(8) . ? N2 P1 1.602(6) . ? N3 C11 1.264(9) . ? N3 C30 1.430(9) . ? O1 C37 1.46(5) . ? O1 C40 1.49(4) . ? O1' C40' 1.43(8) . ? O1' C37' 1.44(8) . ? P1 C24 1.775(8) . ? P1 C18 1.796(7) . ? P1 C10 1.806(7) . ? C1 C2 1.396(10) . ? C1 H1 0.9300 . ? C2 C3 1.337(10) . ? C2 H2 0.9300 . ? C3 C4 1.409(11) . ? C3 H3 0.9300 . ? C4 C9 1.410(11) . ? C4 C5 1.417(10) . ? C5 C6 1.396(10) . ? C6 C7 1.374(10) . ? C7 C8 1.399(11) . ? C7 H7 0.9300 . ? C8 C9 1.292(11) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.523(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.485(10) . ? C12 C13 1.365(10) . ? C12 C17 1.391(11) . ? C13 C14 1.357(12) . ? C13 H13 0.9300 . ? C14 C15 1.309(13) . ? C14 H14 0.9300 . ? C15 C16 1.394(14) . ? C15 H15 0.9300 . ? C16 C17 1.345(12) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.337(10) . ? C18 C23 1.392(11) . ? C19 C20 1.409(11) . ? C19 H19 0.9300 . ? C20 C21 1.394(13) . ? C20 H20 0.9300 . ? C21 C22 1.355(13) . ? C21 H21 0.9300 . ? C22 C23 1.366(11) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.368(10) . ? C24 C25 1.405(11) . ? C25 C26 1.369(11) . ? C25 H25 0.9300 . ? C26 C27 1.362(13) . ? C26 H26 0.9300 . ? C27 C28 1.377(13) . ? C27 H27 0.9300 . ? C28 C29 1.380(11) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.362(11) . ? C30 C35 1.372(10) . ? C31 C32 1.421(12) . ? C31 H31 0.9300 . ? C32 C33 1.307(13) . ? C32 H32 0.9300 . ? C33 C34 1.377(14) . ? C33 H33 0.9300 . ? C34 C35 1.397(11) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C36 H36D 0.9700 . ? C37 C38 1.53(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.53(5) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.57(3) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C37' C38' 1.54(11) . ? C37' H37C 0.9700 . ? C37' H37D 0.9700 . ? C38' C39' 1.54(8) . ? C38' H38C 0.9700 . ? C38' H38D 0.9700 . ? C39' C40' 1.55(11) . ? C39' H39C 0.9700 . ? C39' H39D 0.9700 . ? C40' H40C 0.9700 . ? C40' H40D 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N1 80.0(2) . . ? N2 Ni1 N3 86.4(2) . . ? N1 Ni1 N3 149.0(2) . . ? N2 Ni1 Cl2 164.76(16) . . ? N1 Ni1 Cl2 94.59(19) . . ? N3 Ni1 Cl2 91.29(17) . . ? N2 Ni1 Cl1 98.92(16) . . ? N1 Ni1 Cl1 102.83(16) . . ? N3 Ni1 Cl1 106.75(16) . . ? Cl2 Ni1 Cl1 96.18(7) . . ? C36 Cl4 H36D 33.8 . . ? C1 N1 C5 120.2(7) . . ? C1 N1 Ni1 126.2(5) . . ? C5 N1 Ni1 113.6(5) . . ? C6 N2 P1 123.3(5) . . ? C6 N2 Ni1 112.9(5) . . ? P1 N2 Ni1 122.3(3) . . ? C11 N3 C30 121.7(6) . . ? C11 N3 Ni1 123.7(5) . . ? C30 N3 Ni1 114.1(5) . . ? C37 O1 C40 104(3) . . ? C40' O1' C37' 118(4) . . ? N2 P1 C24 114.4(3) . . ? N2 P1 C18 114.1(3) . . ? C24 P1 C18 110.3(4) . . ? N2 P1 C10 105.6(3) . . ? C24 P1 C10 105.2(3) . . ? C18 P1 C10 106.3(3) . . ? N1 C1 C2 120.2(8) . . ? N1 C1 H1 119.9 . . ? C2 C1 H1 119.9 . . ? C3 C2 C1 121.3(8) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 C4 120.4(8) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C9 125.7(8) . . ? C3 C4 C5 116.4(7) . . ? C9 C4 C5 117.9(8) . . ? N1 C5 C6 117.2(7) . . ? N1 C5 C4 121.5(7) . . ? C6 C5 C4 121.3(7) . . ? C7 C6 C5 116.6(7) . . ? C7 C6 N2 127.2(8) . . ? C5 C6 N2 116.2(7) . . ? C6 C7 C8 121.6(8) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C9 C8 C7 121.9(9) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C8 C9 C4 120.6(8) . . ? C8 C9 H9 119.7 . . ? C4 C9 H9 119.7 . . ? C11 C10 P1 109.2(5) . . ? C11 C10 H10A 109.8 . . ? P1 C10 H10A 109.8 . . ? C11 C10 H10B 109.8 . . ? P1 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? N3 C11 C12 126.2(7) . . ? N3 C11 C10 116.7(6) . . ? C12 C11 C10 117.0(6) . . ? C13 C12 C17 117.3(8) . . ? C13 C12 C11 123.0(7) . . ? C17 C12 C11 119.6(7) . . ? C14 C13 C12 119.6(9) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 123.7(10) . . ? C15 C14 H14 118.1 . . ? C13 C14 H14 118.1 . . ? C14 C15 C16 118.2(10) . . ? C14 C15 H15 120.9 . . ? C16 C15 H15 120.9 . . ? C17 C16 C15 119.4(10) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C12 121.7(9) . . ? C16 C17 H17 119.2 . . ? C12 C17 H17 119.2 . . ? C19 C18 C23 119.4(7) . . ? C19 C18 P1 117.7(6) . . ? C23 C18 P1 123.0(6) . . ? C18 C19 C20 121.6(8) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C21 C20 C19 117.0(9) . . ? C21 C20 H20 121.5 . . ? C19 C20 H20 121.5 . . ? C22 C21 C20 121.8(9) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 119.2(9) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C22 C23 C18 121.0(9) . . ? C22 C23 H23 119.5 . . ? C18 C23 H23 119.5 . . ? C29 C24 C25 118.7(7) . . ? C29 C24 P1 120.0(6) . . ? C25 C24 P1 121.2(6) . . ? C26 C25 C24 119.4(9) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C27 C26 C25 121.3(9) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 119.7(9) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C29 119.6(9) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C24 C29 C28 121.1(9) . . ? C24 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C31 C30 C35 119.4(8) . . ? C31 C30 N3 118.2(7) . . ? C35 C30 N3 122.2(7) . . ? C30 C31 C32 119.4(9) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C33 C32 C31 120.6(10) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 121.2(10) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C33 C34 C35 119.0(9) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? C30 C35 C34 120.3(9) . . ? C30 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? Cl4 C36 Cl3 107.8(11) . . ? Cl4 C36 Cl4' 70.6(9) . . ? Cl3 C36 Cl4' 101.2(9) . . ? Cl4 C36 H36A 110.1 . . ? Cl3 C36 H36A 110.1 . . ? Cl4' C36 H36A 146.1 . . ? Cl4 C36 H36B 110.1 . . ? Cl3 C36 H36B 110.1 . . ? Cl4' C36 H36B 46.1 . . ? H36A C36 H36B 108.5 . . ? Cl4 C36 H36C 138.5 . . ? Cl3 C36 H36C 111.9 . . ? Cl4' C36 H36C 111.6 . . ? H36A C36 H36C 44.4 . . ? H36B C36 H36C 66.4 . . ? Cl4 C36 H36D 43.1 . . ? Cl3 C36 H36D 110.7 . . ? Cl4' C36 H36D 111.9 . . ? H36A C36 H36D 69.1 . . ? H36B C36 H36D 136.9 . . ? H36C C36 H36D 109.3 . . ? O1 C37 C38 109(4) . . ? O1 C37 H37A 109.9 . . ? C38 C37 H37A 109.9 . . ? O1 C37 H37B 109.9 . . ? C38 C37 H37B 109.9 . . ? H37A C37 H37B 108.3 . . ? C39 C38 C37 105(3) . . ? C39 C38 H38A 110.7 . . ? C37 C38 H38A 110.7 . . ? C39 C38 H38B 110.7 . . ? C37 C38 H38B 110.7 . . ? H38A C38 H38B 108.8 . . ? C38 C39 C40 98(3) . . ? C38 C39 H39A 112.1 . . ? C40 C39 H39A 112.1 . . ? C38 C39 H39B 112.1 . . ? C40 C39 H39B 112.1 . . ? H39A C39 H39B 109.7 . . ? O1 C40 C39 111(2) . . ? O1 C40 H40A 109.4 . . ? C39 C40 H40A 109.4 . . ? O1 C40 H40B 109.4 . . ? C39 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? O1' C37' C38' 103(6) . . ? O1' C37' H37C 111.3 . . ? C38' C37' H37C 111.3 . . ? O1' C37' H37D 111.3 . . ? C38' C37' H37D 111.3 . . ? H37C C37' H37D 109.2 . . ? C39' C38' C37' 105(8) . . ? C39' C38' H38C 110.7 . . ? C37' C38' H38C 110.7 . . ? C39' C38' H38D 110.7 . . ? C37' C38' H38D 110.7 . . ? H38C C38' H38D 108.8 . . ? C38' C39' C40' 108(5) . . ? C38' C39' H39C 110.0 . . ? C40' C39' H39C 110.0 . . ? C38' C39' H39D 110.0 . . ? C40' C39' H39D 110.0 . . ? H39C C39' H39D 108.4 . . ? O1' C40' C39' 102(4) . . ? O1' C40' H40C 111.4 . . ? C39' C40' H40C 111.4 . . ? O1' C40' H40D 111.4 . . ? C39' C40' H40D 111.4 . . ? H40C C40' H40D 109.3 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.920 _refine_diff_density_min -0.751 _refine_diff_density_rms 0.116 # Attachment '- 11.cif' data_101217a _database_code_depnum_ccdc_archive 'CCDC 878352' #TrackingRef '- 11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 Cl2 N2 Ni P2' _chemical_formula_weight 656.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 14.7449(16) _cell_length_b 13.6940(14) _cell_length_c 16.1341(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3257.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2188 _cell_measurement_theta_min 2.763 _cell_measurement_theta_max 26.632 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.883 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8362 _exptl_absorpt_correction_T_max 0.8789 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 15728 _diffrn_reflns_av_R_equivalents 0.1945 _diffrn_reflns_av_sigmaI/netI 0.2969 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5668 _reflns_number_gt 2142 _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^)+(0.0095P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.07(5) _refine_ls_number_reflns 5668 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2389 _refine_ls_R_factor_gt 0.0984 _refine_ls_wR_factor_ref 0.1844 _refine_ls_wR_factor_gt 0.1595 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.48633(10) 0.43374(13) 0.43921(9) 0.0404(5) Uani 1 1 d . . . Cl1 Cl 0.6025(2) 0.4231(3) 0.5331(2) 0.0675(12) Uani 1 1 d . . . Cl2 Cl 0.5162(2) 0.3348(3) 0.32588(19) 0.0587(11) Uani 1 1 d . . . N1 N 0.4079(7) 0.3407(9) 0.5016(7) 0.047(3) Uani 1 1 d . . . N2 N 0.3595(7) 0.4933(7) 0.4110(6) 0.036(3) Uani 1 1 d . . . P1 P 0.3431(2) 0.5667(3) 0.3363(2) 0.0367(9) Uani 1 1 d . . . P2 P 0.54084(19) 0.5758(3) 0.36918(19) 0.0383(10) Uani 1 1 d . . . C1 C 0.4321(9) 0.2627(11) 0.5433(9) 0.049(4) Uani 1 1 d . . . H1 H 0.4934 0.2470 0.5452 0.059 Uiso 1 1 calc R . . C2 C 0.3692(10) 0.2000(10) 0.5863(8) 0.057(4) Uani 1 1 d . . . H2 H 0.3898 0.1463 0.6161 0.068 Uiso 1 1 calc R . . C3 C 0.2811(10) 0.2204(11) 0.5826(9) 0.056(4) Uani 1 1 d . . . H3 H 0.2405 0.1791 0.6093 0.067 Uiso 1 1 calc R . . C4 C 0.2480(10) 0.2996(11) 0.5411(9) 0.047(4) Uani 1 1 d . . . C5 C 0.3138(9) 0.3579(11) 0.4988(9) 0.045(4) Uani 1 1 d . . . C6 C 0.2884(8) 0.4395(11) 0.4510(8) 0.040(4) Uani 1 1 d . . . C7 C 0.1991(8) 0.4641(10) 0.4480(8) 0.050(4) Uani 1 1 d . . . H7 H 0.1803 0.5178 0.4172 0.060 Uiso 1 1 calc R . . C8 C 0.1355(9) 0.4079(11) 0.4919(8) 0.051(4) Uani 1 1 d . . . H8 H 0.0749 0.4268 0.4906 0.062 Uiso 1 1 calc R . . C9 C 0.1585(10) 0.3274(11) 0.5359(8) 0.054(4) Uani 1 1 d . . . H9 H 0.1140 0.2910 0.5626 0.065 Uiso 1 1 calc R . . C10 C 0.4514(7) 0.5849(10) 0.2886(7) 0.044(4) Uani 1 1 d . . . H10A H 0.4535 0.6487 0.2626 0.053 Uiso 1 1 calc R . . H10B H 0.4613 0.5358 0.2462 0.053 Uiso 1 1 calc R . . C11 C 0.3047(8) 0.6827(11) 0.3662(11) 0.047(4) Uani 1 1 d . . . C12 C 0.3001(9) 0.7583(13) 0.3094(10) 0.058(5) Uani 1 1 d . . . H12 H 0.3123 0.7465 0.2537 0.069 Uiso 1 1 calc R . . C13 C 0.2772(10) 0.8530(13) 0.3357(12) 0.064(5) Uani 1 1 d . . . H13 H 0.2744 0.9041 0.2978 0.077 Uiso 1 1 calc R . . C14 C 0.2592(10) 0.8691(13) 0.4167(13) 0.067(5) Uani 1 1 d . . . H14 H 0.2445 0.9320 0.4338 0.080 Uiso 1 1 calc R . . C15 C 0.2619(9) 0.7975(13) 0.4730(11) 0.064(5) Uani 1 1 d . . . H15 H 0.2465 0.8101 0.5279 0.077 Uiso 1 1 calc R . . C16 C 0.2884(8) 0.7028(12) 0.4484(10) 0.053(4) Uani 1 1 d . . . H16 H 0.2948 0.6538 0.4879 0.063 Uiso 1 1 calc R . . C17 C 0.2671(10) 0.5157(13) 0.2602(9) 0.054(4) Uani 1 1 d . . . C18 C 0.2853(9) 0.4264(14) 0.2308(9) 0.059(4) Uani 1 1 d . . . H18 H 0.3386 0.3962 0.2482 0.071 Uiso 1 1 calc R . . C19 C 0.2298(11) 0.3758(14) 0.1759(10) 0.079(6) Uani 1 1 d . . . H19 H 0.2438 0.3141 0.1556 0.094 Uiso 1 1 calc R . . C20 C 0.1501(11) 0.4269(16) 0.1539(9) 0.076(5) Uani 1 1 d . . . H20 H 0.1100 0.3964 0.1176 0.091 Uiso 1 1 calc R . . C21 C 0.1287(11) 0.5141(14) 0.1809(10) 0.070(5) Uani 1 1 d . . . H21 H 0.0756 0.5445 0.1635 0.084 Uiso 1 1 calc R . . C22 C 0.1890(9) 0.5619(14) 0.2381(8) 0.061(4) Uani 1 1 d . . . H22 H 0.1750 0.6231 0.2595 0.073 Uiso 1 1 calc R . . C23 C 0.6464(8) 0.5837(11) 0.3127(8) 0.043(4) Uani 1 1 d . . . C24 C 0.7231(8) 0.5484(11) 0.3479(9) 0.051(4) Uani 1 1 d . . . H24 H 0.7197 0.5150 0.3980 0.061 Uiso 1 1 calc R . . C25 C 0.8058(9) 0.5613(13) 0.3104(10) 0.064(5) Uani 1 1 d . . . H25 H 0.8573 0.5384 0.3374 0.077 Uiso 1 1 calc R . . C26 C 0.8159(11) 0.6046(12) 0.2383(11) 0.067(6) Uani 1 1 d . . . H26 H 0.8727 0.6095 0.2135 0.081 Uiso 1 1 calc R . . C27 C 0.7418(11) 0.6414(12) 0.2014(10) 0.067(5) Uani 1 1 d . . . H27 H 0.7481 0.6711 0.1499 0.081 Uiso 1 1 calc R . . C28 C 0.6545(10) 0.6370(11) 0.2376(9) 0.055(4) Uani 1 1 d . . . H28 H 0.6048 0.6675 0.2133 0.065 Uiso 1 1 calc R . . C29 C 0.5274(8) 0.6866(10) 0.4263(8) 0.041(4) Uani 1 1 d . . . C30 C 0.5235(9) 0.7789(12) 0.3941(9) 0.055(4) Uani 1 1 d . . . H30 H 0.5282 0.7860 0.3369 0.066 Uiso 1 1 calc R . . C31 C 0.5129(9) 0.8629(11) 0.4419(11) 0.066(4) Uani 1 1 d . . . H31 H 0.5053 0.9238 0.4173 0.079 Uiso 1 1 calc R . . C32 C 0.5142(9) 0.8524(12) 0.5268(10) 0.063(4) Uani 1 1 d . . . H32 H 0.5098 0.9073 0.5604 0.075 Uiso 1 1 calc R . . C33 C 0.5217(9) 0.7646(12) 0.5610(10) 0.059(4) Uani 1 1 d . . . H33 H 0.5200 0.7586 0.6184 0.071 Uiso 1 1 calc R . . C34 C 0.5319(8) 0.6832(11) 0.5134(9) 0.057(4) Uani 1 1 d . . . H34 H 0.5422 0.6235 0.5393 0.068 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 0.0325(10) 0.0468(11) 0.0417(9) -0.0001(11) -0.0002(8) 0.0023(11) Cl1 0.059(2) 0.069(3) 0.074(3) 0.010(3) -0.032(2) -0.010(2) Cl2 0.060(2) 0.061(3) 0.055(2) -0.010(2) -0.002(2) 0.010(2) N1 0.043(8) 0.039(8) 0.058(8) 0.003(7) -0.002(6) 0.001(7) N2 0.023(6) 0.035(7) 0.049(7) 0.007(6) 0.002(5) 0.003(5) P1 0.0213(18) 0.042(2) 0.047(2) 0.001(3) -0.0019(16) 0.001(2) P2 0.0201(19) 0.049(3) 0.046(2) 0.002(3) 0.0033(15) 0.000(2) C1 0.033(8) 0.040(10) 0.074(12) 0.008(10) 0.003(8) 0.006(8) C2 0.054(11) 0.043(11) 0.075(12) 0.006(9) 0.002(9) 0.011(9) C3 0.050(11) 0.047(12) 0.072(12) 0.002(10) 0.004(9) -0.004(9) C4 0.038(9) 0.042(10) 0.060(11) 0.003(9) 0.005(8) -0.004(8) C5 0.036(9) 0.042(10) 0.058(10) 0.001(9) 0.009(7) -0.001(8) C6 0.024(7) 0.035(9) 0.060(10) 0.000(10) 0.002(7) -0.007(8) C7 0.039(8) 0.049(11) 0.062(10) 0.005(9) 0.005(8) -0.005(8) C8 0.033(8) 0.048(11) 0.073(11) 0.003(10) 0.007(7) -0.004(8) C9 0.045(9) 0.049(11) 0.068(11) 0.002(10) 0.006(9) -0.007(9) C10 0.034(8) 0.046(10) 0.052(8) 0.004(9) 0.000(6) -0.001(8) C11 0.030(8) 0.050(12) 0.061(11) 0.005(10) 0.005(8) 0.000(8) C12 0.050(11) 0.052(12) 0.071(13) 0.006(12) 0.002(8) 0.002(10) C13 0.057(11) 0.054(14) 0.082(15) 0.009(12) 0.004(10) 0.009(10) C14 0.055(11) 0.054(13) 0.092(15) -0.002(13) 0.005(11) 0.006(9) C15 0.054(10) 0.061(14) 0.078(14) -0.003(12) 0.014(9) 0.003(10) C16 0.044(9) 0.047(12) 0.066(13) 0.002(11) 0.004(9) -0.001(8) C17 0.044(10) 0.053(12) 0.064(11) -0.001(10) -0.004(8) -0.003(9) C18 0.044(9) 0.061(13) 0.072(12) -0.009(13) -0.018(8) 0.000(11) C19 0.067(12) 0.084(15) 0.085(14) -0.011(12) -0.018(10) -0.005(12) C20 0.066(12) 0.086(15) 0.074(12) -0.006(14) -0.023(10) -0.007(14) C21 0.052(11) 0.082(15) 0.077(13) 0.004(12) -0.023(9) 0.006(11) C22 0.053(10) 0.063(12) 0.066(11) 0.000(12) -0.009(8) 0.002(11) C23 0.027(8) 0.051(11) 0.053(9) -0.012(9) 0.009(7) -0.008(9) C24 0.025(7) 0.065(13) 0.063(9) -0.003(10) 0.011(7) -0.005(9) C25 0.041(9) 0.078(14) 0.074(12) -0.003(13) 0.011(8) 0.001(11) C26 0.047(11) 0.074(16) 0.081(14) 0.001(11) 0.021(10) -0.001(10) C27 0.051(11) 0.080(14) 0.071(12) 0.000(11) 0.014(10) -0.006(11) C28 0.039(9) 0.068(12) 0.057(10) 0.003(10) 0.000(8) -0.002(9) C29 0.037(8) 0.040(10) 0.046(10) 0.000(8) 0.006(7) -0.011(8) C30 0.052(10) 0.052(11) 0.062(10) 0.000(10) 0.007(8) -0.007(9) C31 0.073(10) 0.049(11) 0.077(11) -0.006(11) 0.006(12) -0.008(9) C32 0.064(10) 0.050(11) 0.075(13) -0.010(10) 0.008(10) -0.013(10) C33 0.063(10) 0.053(10) 0.062(10) -0.022(11) 0.007(10) -0.014(10) C34 0.055(10) 0.050(11) 0.066(11) 0.000(10) 0.005(9) 0.003(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.993(11) . ? Ni1 N2 2.091(10) . ? Ni1 Cl1 2.291(3) . ? Ni1 Cl2 2.318(4) . ? Ni1 P2 2.389(4) . ? N1 C1 1.312(15) . ? N1 C5 1.409(15) . ? N2 C6 1.435(14) . ? N2 P1 1.588(10) . ? P1 C11 1.754(16) . ? P1 C10 1.789(10) . ? P1 C17 1.803(15) . ? P2 C29 1.787(13) . ? P2 C23 1.806(12) . ? P2 C10 1.856(11) . ? C1 C2 1.443(17) . ? C1 H1 0.9300 . ? C2 C3 1.330(17) . ? C2 H2 0.9300 . ? C3 C4 1.365(17) . ? C3 H3 0.9300 . ? C4 C9 1.376(17) . ? C4 C5 1.429(17) . ? C5 C6 1.408(17) . ? C6 C7 1.360(15) . ? C7 C8 1.404(15) . ? C7 H7 0.9300 . ? C8 C9 1.356(16) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.376(17) . ? C11 C12 1.384(18) . ? C12 C13 1.406(19) . ? C12 H12 0.9300 . ? C13 C14 1.351(18) . ? C13 H13 0.9300 . ? C14 C15 1.337(18) . ? C14 H14 0.9300 . ? C15 C16 1.412(17) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.339(19) . ? C17 C22 1.361(18) . ? C18 C19 1.392(18) . ? C18 H18 0.9300 . ? C19 C20 1.41(2) . ? C19 H19 0.9300 . ? C20 C21 1.31(2) . ? C20 H20 0.9300 . ? C21 C22 1.439(18) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.355(16) . ? C23 C28 1.420(16) . ? C24 C25 1.373(16) . ? C24 H24 0.9300 . ? C25 C26 1.314(18) . ? C25 H25 0.9300 . ? C26 C27 1.342(18) . ? C26 H26 0.9300 . ? C27 C28 1.415(17) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.368(15) . ? C29 C34 1.407(16) . ? C30 C31 1.393(16) . ? C30 H30 0.9300 . ? C31 C32 1.378(17) . ? C31 H31 0.9300 . ? C32 C33 1.328(17) . ? C32 H32 0.9300 . ? C33 C34 1.362(16) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 80.8(4) . . ? N1 Ni1 Cl1 93.4(3) . . ? N2 Ni1 Cl1 146.9(3) . . ? N1 Ni1 Cl2 97.8(3) . . ? N2 Ni1 Cl2 103.1(3) . . ? Cl1 Ni1 Cl2 110.00(15) . . ? N1 Ni1 P2 162.7(4) . . ? N2 Ni1 P2 83.1(3) . . ? Cl1 Ni1 P2 96.50(14) . . ? Cl2 Ni1 P2 92.22(13) . . ? C1 N1 C5 114.9(12) . . ? C1 N1 Ni1 128.4(9) . . ? C5 N1 Ni1 116.7(10) . . ? C6 N2 P1 123.8(9) . . ? C6 N2 Ni1 110.8(8) . . ? P1 N2 Ni1 123.2(6) . . ? N2 P1 C11 114.4(7) . . ? N2 P1 C10 106.2(6) . . ? C11 P1 C10 106.3(7) . . ? N2 P1 C17 111.4(7) . . ? C11 P1 C17 109.7(8) . . ? C10 P1 C17 108.4(6) . . ? C29 P2 C23 107.8(6) . . ? C29 P2 C10 103.0(7) . . ? C23 P2 C10 104.8(6) . . ? C29 P2 Ni1 114.2(5) . . ? C23 P2 Ni1 125.3(5) . . ? C10 P2 Ni1 98.4(4) . . ? N1 C1 C2 123.8(12) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C3 C2 C1 118.8(14) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 122.6(15) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C3 C4 C9 126.3(15) . . ? C3 C4 C5 115.8(13) . . ? C9 C4 C5 117.9(14) . . ? C6 C5 N1 114.3(12) . . ? C6 C5 C4 121.6(13) . . ? N1 C5 C4 124.0(14) . . ? C7 C6 C5 118.3(13) . . ? C7 C6 N2 124.3(14) . . ? C5 C6 N2 117.4(11) . . ? C6 C7 C8 119.6(13) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 C7 122.9(13) . . ? C9 C8 H8 118.6 . . ? C7 C8 H8 118.6 . . ? C8 C9 C4 119.8(14) . . ? C8 C9 H9 120.1 . . ? C4 C9 H9 120.1 . . ? P1 C10 P2 108.9(6) . . ? P1 C10 H10A 109.9 . . ? P2 C10 H10A 109.9 . . ? P1 C10 H10B 109.9 . . ? P2 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C16 C11 C12 118.7(15) . . ? C16 C11 P1 120.2(14) . . ? C12 C11 P1 120.7(13) . . ? C11 C12 C13 120.1(15) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 119.3(17) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C15 C14 C13 122.2(17) . . ? C15 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? C14 C15 C16 119.4(16) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C11 C16 C15 120.2(16) . . ? C11 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C22 120.1(15) . . ? C18 C17 P1 118.1(13) . . ? C22 C17 P1 121.6(14) . . ? C17 C18 C19 124.2(15) . . ? C17 C18 H18 117.9 . . ? C19 C18 H18 117.9 . . ? C18 C19 C20 113.8(16) . . ? C18 C19 H19 123.1 . . ? C20 C19 H19 123.1 . . ? C21 C20 C19 124.6(17) . . ? C21 C20 H20 117.7 . . ? C19 C20 H20 117.7 . . ? C20 C21 C22 118.6(16) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? C17 C22 C21 118.7(16) . . ? C17 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C24 C23 C28 118.1(12) . . ? C24 C23 P2 119.1(11) . . ? C28 C23 P2 122.2(11) . . ? C23 C24 C25 120.7(14) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 123.3(15) . . ? C26 C25 H25 118.3 . . ? C24 C25 H25 118.3 . . ? C25 C26 C27 118.0(15) . . ? C25 C26 H26 121.0 . . ? C27 C26 H26 121.0 . . ? C26 C27 C28 122.8(16) . . ? C26 C27 H27 118.6 . . ? C28 C27 H27 118.6 . . ? C27 C28 C23 116.8(14) . . ? C27 C28 H28 121.6 . . ? C23 C28 H28 121.6 . . ? C30 C29 C34 114.3(14) . . ? C30 C29 P2 126.4(11) . . ? C34 C29 P2 118.8(12) . . ? C29 C30 C31 123.9(13) . . ? C29 C30 H30 118.1 . . ? C31 C30 H30 118.1 . . ? C32 C31 C30 117.5(15) . . ? C32 C31 H31 121.2 . . ? C30 C31 H31 121.2 . . ? C33 C32 C31 120.6(16) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 121.0(15) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C33 C34 C29 122.1(14) . . ? C33 C34 H34 119.0 . . ? C29 C34 H34 119.0 . . ? 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 N1 C1 176.7(12) . . . . ? Cl1 Ni1 N1 C1 -36.2(12) . . . . ? Cl2 Ni1 N1 C1 74.6(12) . . . . ? P2 Ni1 N1 C1 -160.9(9) . . . . ? N2 Ni1 N1 C5 -0.9(9) . . . . ? Cl1 Ni1 N1 C5 146.3(9) . . . . ? Cl2 Ni1 N1 C5 -103.0(9) . . . . ? P2 Ni1 N1 C5 21.5(17) . . . . ? N1 Ni1 N2 C6 1.2(8) . . . . ? Cl1 Ni1 N2 C6 -80.9(10) . . . . ? Cl2 Ni1 N2 C6 97.1(7) . . . . ? P2 Ni1 N2 C6 -172.2(8) . . . . ? N1 Ni1 N2 P1 -162.4(7) . . . . ? Cl1 Ni1 N2 P1 115.5(6) . . . . ? Cl2 Ni1 N2 P1 -66.5(7) . . . . ? P2 Ni1 N2 P1 24.1(6) . . . . ? C6 N2 P1 C11 80.6(11) . . . . ? Ni1 N2 P1 C11 -117.9(7) . . . . ? C6 N2 P1 C10 -162.5(9) . . . . ? Ni1 N2 P1 C10 -1.0(8) . . . . ? C6 N2 P1 C17 -44.6(12) . . . . ? Ni1 N2 P1 C17 116.9(8) . . . . ? N1 Ni1 P2 C29 50.4(12) . . . . ? N2 Ni1 P2 C29 72.7(5) . . . . ? Cl1 Ni1 P2 C29 -74.0(5) . . . . ? Cl2 Ni1 P2 C29 175.6(5) . . . . ? N1 Ni1 P2 C23 -173.0(11) . . . . ? N2 Ni1 P2 C23 -150.6(6) . . . . ? Cl1 Ni1 P2 C23 62.7(6) . . . . ? Cl2 Ni1 P2 C23 -47.7(5) . . . . ? N1 Ni1 P2 C10 -58.1(11) . . . . ? N2 Ni1 P2 C10 -35.8(5) . . . . ? Cl1 Ni1 P2 C10 177.6(4) . . . . ? Cl2 Ni1 P2 C10 67.1(4) . . . . ? C5 N1 C1 C2 -2.3(19) . . . . ? Ni1 N1 C1 C2 -179.9(9) . . . . ? N1 C1 C2 C3 1(2) . . . . ? C1 C2 C3 C4 -1(2) . . . . ? C2 C3 C4 C9 -178.2(14) . . . . ? C2 C3 C4 C5 2(2) . . . . ? C1 N1 C5 C6 -177.5(12) . . . . ? Ni1 N1 C5 C6 0.4(15) . . . . ? C1 N1 C5 C4 3.3(19) . . . . ? Ni1 N1 C5 C4 -178.8(10) . . . . ? C3 C4 C5 C6 177.5(13) . . . . ? C9 C4 C5 C6 -2(2) . . . . ? C3 C4 C5 N1 -3(2) . . . . ? C9 C4 C5 N1 177.1(12) . . . . ? N1 C5 C6 C7 -177.0(12) . . . . ? C4 C5 C6 C7 2(2) . . . . ? N1 C5 C6 N2 0.7(17) . . . . ? C4 C5 C6 N2 180.0(12) . . . . ? P1 N2 C6 C7 -20.3(18) . . . . ? Ni1 N2 C6 C7 176.2(11) . . . . ? P1 N2 C6 C5 162.1(10) . . . . ? Ni1 N2 C6 C5 -1.4(14) . . . . ? C5 C6 C7 C8 0(2) . . . . ? N2 C6 C7 C8 -177.8(11) . . . . ? C6 C7 C8 C9 -2(2) . . . . ? C7 C8 C9 C4 2(2) . . . . ? C3 C4 C9 C8 -179.6(13) . . . . ? C5 C4 C9 C8 0(2) . . . . ? N2 P1 C10 P2 -31.8(9) . . . . ? C11 P1 C10 P2 90.4(9) . . . . ? C17 P1 C10 P2 -151.7(8) . . . . ? C29 P2 C10 P1 -72.6(8) . . . . ? C23 P2 C10 P1 174.8(7) . . . . ? Ni1 P2 C10 P1 44.8(7) . . . . ? N2 P1 C11 C16 -2.0(13) . . . . ? C10 P1 C11 C16 -118.9(11) . . . . ? C17 P1 C11 C16 124.0(11) . . . . ? N2 P1 C11 C12 170.5(10) . . . . ? C10 P1 C11 C12 53.6(12) . . . . ? C17 P1 C11 C12 -63.4(12) . . . . ? C16 C11 C12 C13 -2(2) . . . . ? P1 C11 C12 C13 -174.2(10) . . . . ? C11 C12 C13 C14 0(2) . . . . ? C12 C13 C14 C15 0(2) . . . . ? C13 C14 C15 C16 3(2) . . . . ? C12 C11 C16 C15 4(2) . . . . ? P1 C11 C16 C15 176.7(10) . . . . ? C14 C15 C16 C11 -5(2) . . . . ? N2 P1 C17 C18 -51.5(14) . . . . ? C11 P1 C17 C18 -179.3(12) . . . . ? C10 P1 C17 C18 65.0(14) . . . . ? N2 P1 C17 C22 122.9(13) . . . . ? C11 P1 C17 C22 -4.9(15) . . . . ? C10 P1 C17 C22 -120.6(13) . . . . ? C22 C17 C18 C19 1(2) . . . . ? P1 C17 C18 C19 175.9(11) . . . . ? C17 C18 C19 C20 -1(2) . . . . ? C18 C19 C20 C21 1(2) . . . . ? C19 C20 C21 C22 -1(3) . . . . ? C18 C17 C22 C21 -2(2) . . . . ? P1 C17 C22 C21 -176.1(11) . . . . ? C20 C21 C22 C17 2(2) . . . . ? C29 P2 C23 C24 92.1(14) . . . . ? C10 P2 C23 C24 -158.6(13) . . . . ? Ni1 P2 C23 C24 -46.8(14) . . . . ? C29 P2 C23 C28 -79.3(12) . . . . ? C10 P2 C23 C28 29.9(13) . . . . ? Ni1 P2 C23 C28 141.8(10) . . . . ? C28 C23 C24 C25 -2(2) . . . . ? P2 C23 C24 C25 -173.8(13) . . . . ? C23 C24 C25 C26 -2(3) . . . . ? C24 C25 C26 C27 3(3) . . . . ? C25 C26 C27 C28 1(3) . . . . ? C26 C27 C28 C23 -5(2) . . . . ? C24 C23 C28 C27 6(2) . . . . ? P2 C23 C28 C27 177.1(11) . . . . ? C23 P2 C29 C30 59.3(14) . . . . ? C10 P2 C29 C30 -51.2(13) . . . . ? Ni1 P2 C29 C30 -156.8(11) . . . . ? C23 P2 C29 C34 -112.4(11) . . . . ? C10 P2 C29 C34 137.2(10) . . . . ? Ni1 P2 C29 C34 31.6(12) . . . . ? C34 C29 C30 C31 -8(2) . . . . ? P2 C29 C30 C31 -180.0(11) . . . . ? C29 C30 C31 C32 6(2) . . . . ? C30 C31 C32 C33 -3(2) . . . . ? C31 C32 C33 C34 3(2) . . . . ? C32 C33 C34 C29 -5(2) . . . . ? C30 C29 C34 C33 8(2) . . . . ? P2 C29 C34 C33 -179.6(10) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.397 0.056 0.452 20.6 1.2 2 0.506 0.154 0.726 64.5 1.2 3 1.006 0.346 0.274 64.5 1.3 4 0.897 0.443 0.548 20.5 1.2 5 0.603 0.556 0.048 20.6 1.9 6 0.494 0.654 0.774 64.5 0.9 7 -0.006 0.846 0.226 64.5 1.3 8 0.103 0.943 0.951 20.6 1.5 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.641 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.118 # Attachment '- 13.cif' data_090720a _database_code_depnum_ccdc_archive 'CCDC 878353' #TrackingRef '- 13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C107 H90 Cl2 N8 Ni2 P4' _chemical_formula_weight 1800.07 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 11.7609(14) _cell_length_b 12.4767(16) _cell_length_c 17.3590(18) _cell_angle_alpha 82.3720(10) _cell_angle_beta 85.171(2) _cell_angle_gamma 79.2300(10) _cell_volume 2475.6(5) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4055 _cell_measurement_theta_min 3.488 _cell_measurement_theta_max 23.858 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 938 _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8842 _exptl_absorpt_correction_T_max 0.8982 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 13056 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8566 _reflns_number_gt 5412 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1197P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8566 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0945 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1936 _refine_ls_wR_factor_gt 0.1716 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 0.67787(5) 0.79721(4) 0.62602(3) 0.0452(2) Uani 1 1 d . . . P1 P 0.91030(9) 0.67143(9) 0.70175(6) 0.0416(3) Uani 1 1 d . . . P2 P 0.69608(10) 0.56490(9) 0.73216(7) 0.0440(3) Uani 1 1 d . . . Cl1 Cl 0.58993(15) 0.74931(12) 0.52460(8) 0.0845(5) Uani 1 1 d . . . N1 N 0.7352(3) 0.9278(3) 0.5578(2) 0.0528(9) Uani 1 1 d . . . N2 N 0.8357(3) 0.7904(3) 0.6710(2) 0.0466(9) Uani 1 1 d . . . N3 N 0.5401(3) 0.8957(3) 0.6772(2) 0.0542(10) Uani 1 1 d . . . N4 N 0.6180(3) 0.6834(3) 0.7084(2) 0.0460(8) Uani 1 1 d . . . C1 C 0.6822(5) 0.9930(4) 0.4999(3) 0.0675(14) Uani 1 1 d . . . H1 H 0.6194 0.9726 0.4801 0.081 Uiso 1 1 calc R . . C2 C 0.7172(5) 1.0914(4) 0.4673(3) 0.0719(15) Uani 1 1 d . . . H2 H 0.6776 1.1353 0.4270 0.086 Uiso 1 1 calc R . . C3 C 0.8076(5) 1.1220(4) 0.4945(3) 0.0699(15) Uani 1 1 d . . . H3 H 0.8306 1.1875 0.4729 0.084 Uiso 1 1 calc R . . C4 C 0.8687(4) 1.0564(4) 0.5552(3) 0.0553(12) Uani 1 1 d . . . C5 C 0.8281(4) 0.9576(3) 0.5857(3) 0.0488(11) Uani 1 1 d . . . C6 C 0.8856(4) 0.8824(3) 0.6465(3) 0.0475(10) Uani 1 1 d . . . C7 C 0.9825(4) 0.9104(4) 0.6721(3) 0.0559(12) Uani 1 1 d . . . H7 H 1.0236 0.8630 0.7102 0.067 Uiso 1 1 calc R . . C8 C 1.0210(5) 1.0085(4) 0.6423(3) 0.0669(14) Uani 1 1 d . . . H8 H 1.0861 1.0250 0.6619 0.080 Uiso 1 1 calc R . . C9 C 0.9661(5) 1.0795(4) 0.5860(3) 0.0638(13) Uani 1 1 d . . . H9 H 0.9933 1.1441 0.5677 0.077 Uiso 1 1 calc R . . C10 C 0.5080(5) 1.0041(4) 0.6621(3) 0.0710(15) Uani 1 1 d . . . H10 H 0.5586 1.0438 0.6318 0.085 Uiso 1 1 calc R . . C11 C 0.4033(6) 1.0602(5) 0.6895(4) 0.0844(18) Uani 1 1 d . . . H11 H 0.3832 1.1358 0.6767 0.101 Uiso 1 1 calc R . . C12 C 0.3299(5) 1.0034(5) 0.7353(4) 0.0790(17) Uani 1 1 d . . . H12 H 0.2604 1.0407 0.7558 0.095 Uiso 1 1 calc R . . C13 C 0.3582(4) 0.8886(4) 0.7519(3) 0.0646(13) Uani 1 1 d . . . C14 C 0.4670(4) 0.8378(4) 0.7224(3) 0.0503(11) Uani 1 1 d . . . C15 C 0.5075(4) 0.7212(4) 0.7391(3) 0.0498(11) Uani 1 1 d . . . C16 C 0.4313(4) 0.6598(4) 0.7818(3) 0.0623(13) Uani 1 1 d . . . H16 H 0.4525 0.5839 0.7915 0.075 Uiso 1 1 calc R . . C17 C 0.3213(5) 0.7126(5) 0.8105(3) 0.0741(15) Uani 1 1 d . . . H17 H 0.2721 0.6701 0.8397 0.089 Uiso 1 1 calc R . . C18 C 0.2858(5) 0.8223(5) 0.7970(3) 0.0745(15) Uani 1 1 d . . . H18 H 0.2136 0.8544 0.8172 0.089 Uiso 1 1 calc R . . C19 C 0.8344(4) 0.5680(3) 0.6976(3) 0.0467(10) Uani 1 1 d . . . H19 H 0.8731 0.5075 0.6741 0.056 Uiso 1 1 calc R . . C20 C 0.9574(4) 0.6705(4) 0.7994(3) 0.0511(11) Uani 1 1 d . . . C21 C 1.0218(4) 0.5751(4) 0.8356(3) 0.0636(13) Uani 1 1 d . . . H21 H 1.0422 0.5133 0.8094 0.076 Uiso 1 1 calc R . . C22 C 1.0553(6) 0.5716(6) 0.9094(3) 0.0821(18) Uani 1 1 d . . . H22 H 1.0993 0.5077 0.9329 0.098 Uiso 1 1 calc R . . C23 C 1.0253(6) 0.6596(6) 0.9483(4) 0.091(2) Uani 1 1 d . . . H23 H 1.0493 0.6558 0.9984 0.110 Uiso 1 1 calc R . . C24 C 0.9603(6) 0.7545(6) 0.9159(4) 0.0899(19) Uani 1 1 d . . . H24 H 0.9390 0.8144 0.9441 0.108 Uiso 1 1 calc R . . C25 C 0.9256(5) 0.7609(5) 0.8392(3) 0.0697(14) Uani 1 1 d . . . H25 H 0.8820 0.8252 0.8159 0.084 Uiso 1 1 calc R . . C26 C 1.0403(4) 0.6390(3) 0.6400(3) 0.0500(11) Uani 1 1 d . . . C27 C 1.1513(4) 0.6350(4) 0.6620(3) 0.0681(14) Uani 1 1 d . . . H27 H 1.1626 0.6513 0.7113 0.082 Uiso 1 1 calc R . . C28 C 1.2450(5) 0.6071(5) 0.6114(4) 0.089(2) Uani 1 1 d . . . H28 H 1.3197 0.6058 0.6259 0.107 Uiso 1 1 calc R . . C29 C 1.2278(7) 0.5812(5) 0.5393(5) 0.098(2) Uani 1 1 d . . . H29 H 1.2918 0.5589 0.5062 0.118 Uiso 1 1 calc R . . C30 C 1.1211(7) 0.5874(5) 0.5155(4) 0.0883(19) Uani 1 1 d . . . H30 H 1.1113 0.5720 0.4658 0.106 Uiso 1 1 calc R . . C31 C 1.0254(5) 0.6168(4) 0.5652(3) 0.0688(14) Uani 1 1 d . . . H31 H 0.9512 0.6217 0.5488 0.083 Uiso 1 1 calc R . . C32 C 0.6535(4) 0.4545(3) 0.6900(3) 0.0482(11) Uani 1 1 d . . . C33 C 0.5623(4) 0.4787(4) 0.6414(3) 0.0525(11) Uani 1 1 d . . . H33 H 0.5220 0.5503 0.6326 0.063 Uiso 1 1 calc R . . C34 C 0.5311(4) 0.3963(4) 0.6060(3) 0.0595(12) Uani 1 1 d . . . H34 H 0.4683 0.4126 0.5746 0.071 Uiso 1 1 calc R . . C35 C 0.5914(5) 0.2915(4) 0.6166(3) 0.0651(14) Uani 1 1 d . . . H35 H 0.5701 0.2370 0.5921 0.078 Uiso 1 1 calc R . . C36 C 0.6843(5) 0.2658(4) 0.6637(3) 0.0722(15) Uani 1 1 d . . . H36 H 0.7258 0.1944 0.6707 0.087 Uiso 1 1 calc R . . C37 C 0.7151(4) 0.3476(4) 0.7005(3) 0.0628(13) Uani 1 1 d . . . H37 H 0.7772 0.3307 0.7324 0.075 Uiso 1 1 calc R . . C38 C 0.6784(4) 0.5340(4) 0.8383(3) 0.0591(12) Uani 1 1 d . . . C39 C 0.6893(5) 0.6139(5) 0.8813(3) 0.0784(16) Uani 1 1 d . . . H39 H 0.7034 0.6811 0.8561 0.094 Uiso 1 1 calc R . . C40 C 0.6800(7) 0.5983(7) 0.9626(4) 0.103(2) Uani 1 1 d . . . H40 H 0.6875 0.6544 0.9911 0.123 Uiso 1 1 calc R . . C41 C 0.6603(7) 0.5032(9) 0.9982(5) 0.113(3) Uani 1 1 d . . . H41 H 0.6545 0.4927 1.0523 0.136 Uiso 1 1 calc R . . C42 C 0.6484(7) 0.4207(7) 0.9588(5) 0.115(3) Uani 1 1 d . . . H42 H 0.6341 0.3543 0.9853 0.138 Uiso 1 1 calc R . . C43 C 0.6581(6) 0.4358(6) 0.8763(4) 0.0902(19) Uani 1 1 d . . . H43 H 0.6505 0.3793 0.8482 0.108 Uiso 1 1 calc R . . C44 C 0.250(2) 0.3198(16) 0.785(2) 0.232(12) Uani 1 1 d . . . C45 C 0.241(2) 0.3313(16) 0.7089(19) 0.233(11) Uani 1 1 d . . . H45 H 0.2984 0.3555 0.6746 0.279 Uiso 1 1 calc R . . C46 C 0.141(2) 0.3061(12) 0.6814(15) 0.231(10) Uani 1 1 d . . . H46 H 0.1273 0.3163 0.6287 0.277 Uiso 1 1 calc R . . C47 C 0.066(2) 0.2663(17) 0.736(2) 0.241(10) Uani 1 1 d . . . H47 H -0.0008 0.2516 0.7179 0.289 Uiso 1 1 calc R . . C48 C 0.079(3) 0.2445(18) 0.816(2) 0.259(13) Uani 1 1 d . . . H48 H 0.0232 0.2166 0.8502 0.311 Uiso 1 1 calc R . . C49 C 0.182(2) 0.2680(14) 0.8423(13) 0.236(9) Uani 1 1 d . . . H49 H 0.2029 0.2500 0.8936 0.283 Uiso 1 1 calc R . . C50 C 0.3641(16) 0.3391(13) 0.8026(12) 0.280(10) Uani 1 1 d . . . H50A H 0.4123 0.3454 0.7553 0.420 Uiso 1 1 calc R . . H50B H 0.4000 0.2788 0.8378 0.420 Uiso 1 1 calc R . . H50C H 0.3546 0.4059 0.8262 0.420 Uiso 1 1 calc R . . C51 C 0.687(7) 0.015(6) 0.895(5) 0.16(3) Uani 0.27(3) 1 d P A 1 C52 C 0.682(4) -0.006(4) 0.978(3) 0.179(11) Uani 0.50 1 d P . . H52 H 0.6242 -0.0403 1.0048 0.214 Uiso 0.27(3) 1 calc PR A 1 H52' H 0.6737 -0.0105 1.0319 0.214 Uiso 0.23(3) 1 d PR A 2 C53 C 0.765(7) 0.025(5) 1.017(4) 0.17(3) Uani 0.27(3) 1 d P A 1 H53 H 0.7641 0.0121 1.0708 0.201 Uiso 0.27(3) 1 calc PR A 1 C54 C 0.850(8) 0.075(7) 0.975(6) 0.16(2) Uani 0.27(3) 1 d P A 1 H54 H 0.9051 0.0967 1.0018 0.196 Uiso 0.27(3) 1 calc PR A 1 C55 C 0.854(7) 0.093(4) 0.895(5) 0.17(2) Uani 0.27(3) 1 d P A 1 H55 H 0.9130 0.1241 0.8678 0.203 Uiso 0.27(3) 1 calc PR A 1 C56 C 0.769(5) 0.065(3) 0.857(3) 0.162(11) Uani 0.50 1 d P . . H56 H 0.7681 0.0817 0.8037 0.195 Uiso 0.27(3) 1 calc PR A 1 H56' H 0.8206 0.1065 0.8303 0.195 Uiso 0.23(3) 1 d PR A 2 C57 C 0.597(9) -0.020(8) 0.856(6) 0.17(3) Uani 0.27(3) 1 d P A 1 H57A H 0.5225 0.0231 0.8681 0.255 Uiso 0.27(3) 1 calc PR A 1 H57B H 0.5948 -0.0963 0.8724 0.255 Uiso 0.27(3) 1 calc PR A 1 H57C H 0.6135 -0.0101 0.8003 0.255 Uiso 0.27(3) 1 calc PR A 1 C51' C 0.753(11) 0.061(7) 0.936(6) 0.17(3) Uani 0.23(3) 1 d P A 2 C53' C 0.624(7) -0.067(6) 0.938(5) 0.17(3) Uani 0.23(3) 1 d P A 2 H53' H 0.5768 -0.1132 0.9656 0.200 Uiso 0.23(3) 1 calc PR A 2 C54' C 0.638(14) -0.059(9) 0.859(9) 0.17(4) Uani 0.23(3) 1 d P A 2 H54' H 0.5997 -0.0997 0.8320 0.204 Uiso 0.23(3) 1 calc PR A 2 C55' C 0.708(8) 0.008(7) 0.819(5) 0.16(3) Uani 0.23(3) 1 d P A 2 H55' H 0.7149 0.0154 0.7648 0.196 Uiso 0.23(3) 1 calc PR A 2 C57' C 0.812(9) 0.124(6) 0.980(6) 0.16(3) Uani 0.23(3) 1 d P A 2 H57D H 0.8742 0.1500 0.9476 0.247 Uiso 0.23(3) 1 calc PR A 2 H57E H 0.8436 0.0784 1.0251 0.247 Uiso 0.23(3) 1 calc PR A 2 H57F H 0.7583 0.1860 0.9965 0.247 Uiso 0.23(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0388(3) 0.0453(3) 0.0526(4) -0.0063(2) -0.0105(3) -0.0065(2) P1 0.0355(6) 0.0407(6) 0.0498(6) -0.0056(5) -0.0086(5) -0.0066(5) P2 0.0392(6) 0.0422(6) 0.0521(7) -0.0057(5) -0.0071(5) -0.0092(5) Cl1 0.1066(12) 0.0866(10) 0.0728(9) -0.0110(7) -0.0390(9) -0.0327(9) N1 0.049(2) 0.051(2) 0.057(2) 0.0006(18) -0.0114(19) -0.0084(18) N2 0.041(2) 0.0418(19) 0.058(2) -0.0047(16) -0.0120(17) -0.0082(16) N3 0.055(2) 0.047(2) 0.062(2) -0.0140(18) -0.007(2) -0.0056(18) N4 0.039(2) 0.046(2) 0.055(2) -0.0070(16) -0.0047(17) -0.0082(16) C1 0.061(3) 0.070(3) 0.068(3) 0.007(3) -0.017(3) -0.007(3) C2 0.074(4) 0.066(3) 0.067(3) 0.015(3) -0.012(3) -0.003(3) C3 0.076(4) 0.049(3) 0.080(4) 0.004(3) 0.002(3) -0.009(3) C4 0.060(3) 0.039(2) 0.065(3) -0.008(2) 0.002(2) -0.005(2) C5 0.047(3) 0.042(2) 0.057(3) -0.010(2) 0.001(2) -0.006(2) C6 0.045(3) 0.042(2) 0.058(3) -0.010(2) -0.005(2) -0.008(2) C7 0.053(3) 0.049(3) 0.068(3) -0.003(2) -0.015(2) -0.012(2) C8 0.059(3) 0.058(3) 0.090(4) -0.012(3) -0.007(3) -0.024(3) C9 0.067(3) 0.043(3) 0.086(4) -0.010(2) -0.001(3) -0.020(2) C10 0.071(4) 0.049(3) 0.090(4) -0.014(3) -0.001(3) 0.000(3) C11 0.084(4) 0.059(3) 0.105(5) -0.022(3) -0.001(4) 0.008(3) C12 0.068(4) 0.071(4) 0.092(4) -0.029(3) -0.008(3) 0.020(3) C13 0.051(3) 0.074(3) 0.068(3) -0.022(3) -0.005(3) 0.002(3) C14 0.044(3) 0.054(3) 0.054(3) -0.017(2) -0.008(2) -0.004(2) C15 0.043(3) 0.056(3) 0.054(3) -0.012(2) -0.006(2) -0.010(2) C16 0.047(3) 0.069(3) 0.071(3) -0.007(3) -0.004(3) -0.011(2) C17 0.050(3) 0.096(4) 0.078(4) -0.010(3) 0.004(3) -0.018(3) C18 0.049(3) 0.090(4) 0.081(4) -0.026(3) 0.004(3) 0.004(3) C19 0.042(2) 0.040(2) 0.059(3) -0.0110(19) -0.005(2) -0.0068(19) C20 0.047(3) 0.058(3) 0.051(3) -0.004(2) -0.010(2) -0.015(2) C21 0.060(3) 0.070(3) 0.058(3) 0.006(2) -0.013(3) -0.011(3) C22 0.081(4) 0.098(5) 0.066(4) 0.014(3) -0.020(3) -0.024(4) C23 0.097(5) 0.124(6) 0.060(4) 0.006(4) -0.026(4) -0.040(5) C24 0.102(5) 0.109(5) 0.070(4) -0.033(4) -0.013(4) -0.031(4) C25 0.071(4) 0.078(4) 0.062(3) -0.014(3) -0.009(3) -0.014(3) C26 0.045(3) 0.045(2) 0.060(3) -0.004(2) -0.003(2) -0.008(2) C27 0.047(3) 0.075(3) 0.075(3) 0.011(3) -0.004(3) -0.006(3) C28 0.047(3) 0.092(4) 0.109(5) 0.022(4) 0.009(4) 0.007(3) C29 0.086(5) 0.075(4) 0.112(6) 0.009(4) 0.046(5) 0.007(4) C30 0.106(5) 0.077(4) 0.083(4) -0.023(3) 0.028(4) -0.026(4) C31 0.072(4) 0.071(3) 0.069(3) -0.018(3) 0.011(3) -0.025(3) C32 0.041(2) 0.046(2) 0.060(3) -0.010(2) -0.003(2) -0.013(2) C33 0.045(3) 0.048(3) 0.065(3) -0.011(2) -0.005(2) -0.008(2) C34 0.053(3) 0.060(3) 0.072(3) -0.018(2) -0.008(3) -0.016(2) C35 0.069(3) 0.058(3) 0.075(3) -0.015(3) -0.006(3) -0.025(3) C36 0.079(4) 0.043(3) 0.094(4) -0.010(3) -0.004(3) -0.009(3) C37 0.060(3) 0.049(3) 0.081(3) -0.008(2) -0.018(3) -0.008(2) C38 0.048(3) 0.069(3) 0.060(3) -0.001(3) -0.007(2) -0.011(2) C39 0.079(4) 0.097(4) 0.065(4) -0.015(3) -0.006(3) -0.026(3) C40 0.105(6) 0.136(7) 0.072(4) -0.019(4) -0.013(4) -0.025(5) C41 0.115(6) 0.146(8) 0.071(5) -0.004(5) -0.015(4) -0.007(6) C42 0.122(7) 0.117(6) 0.089(5) 0.034(5) 0.003(5) -0.013(5) C43 0.098(5) 0.088(4) 0.075(4) 0.013(3) -0.004(4) -0.010(4) C44 0.187(18) 0.123(11) 0.38(3) -0.085(19) 0.10(3) -0.024(11) C45 0.21(2) 0.114(10) 0.36(3) -0.068(18) 0.07(3) 0.006(12) C46 0.172(15) 0.104(9) 0.39(3) -0.041(12) 0.10(2) 0.003(10) C47 0.192(19) 0.143(14) 0.37(3) -0.09(2) 0.05(3) 0.016(13) C48 0.21(2) 0.170(15) 0.38(4) -0.08(2) 0.09(3) -0.005(15) C49 0.193(17) 0.154(13) 0.35(3) -0.084(15) 0.10(2) -0.022(13) C50 0.225(18) 0.242(18) 0.40(3) -0.144(17) 0.046(19) -0.071(15) C51 0.18(6) 0.13(5) 0.15(7) -0.03(5) -0.05(6) 0.05(4) C52 0.19(3) 0.15(3) 0.17(3) -0.02(3) -0.04(3) 0.05(2) C53 0.19(6) 0.13(4) 0.16(5) -0.03(4) -0.04(5) 0.04(4) C54 0.19(7) 0.12(5) 0.17(6) -0.02(5) -0.05(5) 0.03(5) C55 0.19(6) 0.12(3) 0.17(6) -0.01(3) -0.04(6) 0.04(4) C56 0.20(4) 0.11(2) 0.15(3) 0.00(2) -0.05(3) 0.04(2) C57 0.19(8) 0.13(6) 0.16(5) -0.03(4) -0.05(6) 0.06(4) C51' 0.19(9) 0.12(6) 0.17(9) -0.02(6) -0.04(9) 0.04(5) C53' 0.19(6) 0.12(5) 0.17(6) -0.03(5) -0.04(5) 0.05(4) C54' 0.19(9) 0.13(7) 0.16(7) -0.03(6) -0.05(7) 0.06(6) C55' 0.19(8) 0.12(5) 0.16(6) -0.02(4) -0.04(5) 0.05(4) C57' 0.19(7) 0.11(5) 0.17(6) -0.02(5) -0.03(5) 0.06(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N4 2.055(3) . ? Ni1 N3 2.056(4) . ? Ni1 N2 2.056(3) . ? Ni1 N1 2.068(4) . ? Ni1 Cl1 2.3115(13) . ? P1 N2 1.625(3) . ? P1 C19 1.713(4) . ? P1 C26 1.805(5) . ? P1 C20 1.825(4) . ? P2 N4 1.611(4) . ? P2 C19 1.691(4) . ? P2 C32 1.809(4) . ? P2 C38 1.834(5) . ? N1 C1 1.327(6) . ? N1 C5 1.361(5) . ? N2 C6 1.387(5) . ? N3 C10 1.331(6) . ? N3 C14 1.358(6) . ? N4 C15 1.384(6) . ? C1 C2 1.401(7) . ? C1 H1 0.9300 . ? C2 C3 1.335(8) . ? C2 H2 0.9300 . ? C3 C4 1.406(7) . ? C3 H3 0.9300 . ? C4 C9 1.397(7) . ? C4 C5 1.425(6) . ? C5 C6 1.439(6) . ? C6 C7 1.376(6) . ? C7 C8 1.404(6) . ? C7 H7 0.9300 . ? C8 C9 1.348(7) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.378(8) . ? C10 H10 0.9300 . ? C11 C12 1.358(8) . ? C11 H11 0.9300 . ? C12 C13 1.405(7) . ? C12 H12 0.9300 . ? C13 C14 1.406(7) . ? C13 C18 1.415(8) . ? C14 C15 1.442(6) . ? C15 C16 1.390(6) . ? C16 C17 1.420(7) . ? C16 H16 0.9300 . ? C17 C18 1.350(8) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C25 1.377(7) . ? C20 C21 1.389(6) . ? C21 C22 1.364(7) . ? C21 H21 0.9300 . ? C22 C23 1.341(9) . ? C22 H22 0.9300 . ? C23 C24 1.364(9) . ? C23 H23 0.9300 . ? C24 C25 1.414(7) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.382(7) . ? C26 C31 1.393(7) . ? C27 C28 1.371(8) . ? C27 H27 0.9300 . ? C28 C29 1.374(10) . ? C28 H28 0.9300 . ? C29 C30 1.340(10) . ? C29 H29 0.9300 . ? C30 C31 1.382(8) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.384(6) . ? C32 C37 1.390(6) . ? C33 C34 1.385(6) . ? C33 H33 0.9300 . ? C34 C35 1.363(7) . ? C34 H34 0.9300 . ? C35 C36 1.384(7) . ? C35 H35 0.9300 . ? C36 C37 1.390(7) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.353(7) . ? C38 C43 1.364(8) . ? C39 C40 1.395(8) . ? C39 H39 0.9300 . ? C40 C41 1.314(10) . ? C40 H40 0.9300 . ? C41 C42 1.344(11) . ? C41 H41 0.9300 . ? C42 C43 1.417(9) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 C45 1.32(3) . ? C44 C49 1.39(3) . ? C44 C50 1.47(3) . ? C45 C46 1.41(3) . ? C45 H45 0.9300 . ? C46 C47 1.34(3) . ? C46 H46 0.9300 . ? C47 C48 1.40(3) . ? C47 H47 0.9300 . ? C48 C49 1.43(3) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C56 1.32(10) . ? C51 C52 1.42(9) . ? C51 C57 1.48(15) . ? C52 C53 1.37(9) . ? C52 C51' 1.38(13) . ? C52 C53' 1.39(9) . ? C52 H52 0.9300 . ? C52 H52' 0.9300 . ? C53 C54 1.37(11) . ? C53 H52' 1.2314 . ? C53 H53 0.9300 . ? C54 C55 1.37(11) . ? C54 H54 0.9300 . ? C55 C56 1.36(8) . ? C55 H55 0.9300 . ? C55 H56' 1.2065 . ? C56 C51' 1.36(11) . ? C56 C55' 1.36(11) . ? C56 H56 0.9300 . ? C56 H56' 0.9300 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C51' C57' 1.47(15) . ? C53' C54' 1.37(16) . ? C53' H53' 0.9300 . ? C54' C55' 1.37(18) . ? C54' H54' 0.9300 . ? C55' H55' 0.9300 . ? C57' H57D 0.9600 . ? C57' H57E 0.9600 . ? C57' H57F 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 N4 Ni1 N3 79.73(15) . . ? N4 Ni1 N2 97.27(14) . . ? N3 Ni1 N2 115.41(15) . . ? N4 Ni1 N1 170.52(14) . . ? N3 Ni1 N1 93.63(15) . . ? N2 Ni1 N1 79.37(14) . . ? N4 Ni1 Cl1 94.73(10) . . ? N3 Ni1 Cl1 100.62(11) . . ? N2 Ni1 Cl1 143.46(12) . . ? N1 Ni1 Cl1 93.14(11) . . ? N2 P1 C19 111.23(19) . . ? N2 P1 C26 111.0(2) . . ? C19 P1 C26 105.1(2) . . ? N2 P1 C20 111.1(2) . . ? C19 P1 C20 111.6(2) . . ? C26 P1 C20 106.5(2) . . ? N4 P2 C19 108.8(2) . . ? N4 P2 C32 113.7(2) . . ? C19 P2 C32 105.5(2) . . ? N4 P2 C38 107.4(2) . . ? C19 P2 C38 114.2(2) . . ? C32 P2 C38 107.3(2) . . ? C1 N1 C5 118.4(4) . . ? C1 N1 Ni1 127.4(3) . . ? C5 N1 Ni1 113.3(3) . . ? C6 N2 P1 123.1(3) . . ? C6 N2 Ni1 113.7(3) . . ? P1 N2 Ni1 119.10(18) . . ? C10 N3 C14 118.6(4) . . ? C10 N3 Ni1 127.6(4) . . ? C14 N3 Ni1 113.1(3) . . ? C15 N4 P2 126.1(3) . . ? C15 N4 Ni1 112.6(3) . . ? P2 N4 Ni1 121.3(2) . . ? N1 C1 C2 122.5(5) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 119.7(5) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 120.8(5) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C9 C4 C3 125.2(5) . . ? C9 C4 C5 118.4(4) . . ? C3 C4 C5 116.4(5) . . ? N1 C5 C4 122.1(4) . . ? N1 C5 C6 116.5(4) . . ? C4 C5 C6 121.4(4) . . ? C7 C6 N2 128.7(4) . . ? C7 C6 C5 116.3(4) . . ? N2 C6 C5 115.0(4) . . ? C6 C7 C8 121.9(4) . . ? C6 C7 H7 119.1 . . ? C8 C7 H7 119.1 . . ? C9 C8 C7 121.7(5) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C4 120.3(4) . . ? C8 C9 H9 119.8 . . ? C4 C9 H9 119.8 . . ? N3 C10 C11 123.0(6) . . ? N3 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C12 C11 C10 119.0(6) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 120.4(5) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C14 117.0(5) . . ? C12 C13 C18 124.4(5) . . ? C14 C13 C18 118.6(5) . . ? N3 C14 C13 121.9(4) . . ? N3 C14 C15 116.4(4) . . ? C13 C14 C15 121.7(5) . . ? N4 C15 C16 127.7(4) . . ? N4 C15 C14 115.2(4) . . ? C16 C15 C14 117.1(4) . . ? C15 C16 C17 120.3(5) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 122.2(5) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C17 C18 C13 120.0(5) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? P2 C19 P1 126.4(3) . . ? P2 C19 H19 116.8 . . ? P1 C19 H19 116.8 . . ? C25 C20 C21 119.4(4) . . ? C25 C20 P1 121.1(4) . . ? C21 C20 P1 119.4(4) . . ? C22 C21 C20 120.4(6) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 120.5(6) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 121.5(6) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C23 C24 C25 119.3(6) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C20 C25 C24 118.9(5) . . ? C20 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C27 C26 C31 118.9(5) . . ? C27 C26 P1 124.4(4) . . ? C31 C26 P1 116.7(4) . . ? C28 C27 C26 120.1(6) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 119.6(6) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 121.5(6) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C31 119.8(6) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C30 C31 C26 120.0(6) . . ? C30 C31 H31 120.0 . . ? C26 C31 H31 120.0 . . ? C33 C32 C37 119.2(4) . . ? C33 C32 P2 118.9(3) . . ? C37 C32 P2 121.7(3) . . ? C32 C33 C34 120.0(4) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.7(5) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 120.3(5) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C37 119.4(5) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C36 C37 C32 120.4(5) . . ? C36 C37 H37 119.8 . . ? C32 C37 H37 119.8 . . ? C39 C38 C43 118.3(5) . . ? C39 C38 P2 117.1(4) . . ? C43 C38 P2 124.6(4) . . ? C38 C39 C40 121.9(6) . . ? C38 C39 H39 119.1 . . ? C40 C39 H39 119.1 . . ? C41 C40 C39 119.0(7) . . ? C41 C40 H40 120.5 . . ? C39 C40 H40 120.5 . . ? C40 C41 C42 122.0(8) . . ? C40 C41 H41 119.0 . . ? C42 C41 H41 119.0 . . ? C41 C42 C43 119.3(7) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C38 C43 C42 119.5(7) . . ? C38 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C45 C44 C49 127(3) . . ? C45 C44 C50 110(3) . . ? C49 C44 C50 120(4) . . ? C44 C45 C46 118(3) . . ? C44 C45 H45 121.0 . . ? C46 C45 H45 121.0 . . ? C47 C46 C45 116(3) . . ? C47 C46 H46 121.9 . . ? C45 C46 H46 121.9 . . ? C46 C47 C48 127(3) . . ? C46 C47 H47 116.4 . . ? C48 C47 H47 116.4 . . ? C47 C48 C49 116(3) . . ? C47 C48 H48 122.2 . . ? C49 C48 H48 122.2 . . ? C44 C49 C48 115(3) . . ? C44 C49 H49 122.7 . . ? C48 C49 H49 122.7 . . ? C44 C50 H50A 109.5 . . ? C44 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C44 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C56 C51 C52 121(8) . . ? C56 C51 C57 123(9) . . ? C52 C51 C57 116(10) . . ? C53 C52 C51' 62(6) . . ? C53 C52 C53' 162(4) . . ? C51' C52 C53' 119(7) . . ? C53 C52 C51 118(8) . . ? C51' C52 C51 57(6) . . ? C53' C52 C51 63(6) . . ? C53 C52 H52 121.0 . . ? C51' C52 H52 169.8 . . ? C53' C52 H52 61.1 . . ? C51 C52 H52 121.0 . . ? C53 C52 H52' 61.3 . . ? C51' C52 H52' 120.4 . . ? C53' C52 H52' 120.3 . . ? C51 C52 H52' 172.3 . . ? H52 C52 H52' 60.3 . . ? C52 C53 C54 120(7) . . ? C52 C53 H52' 41.5 . . ? C54 C53 H52' 159.9 . . ? C52 C53 H53 120.2 . . ? C54 C53 H53 120.2 . . ? H52' C53 H53 79.2 . . ? C55 C54 C53 121(9) . . ? C55 C54 H54 119.4 . . ? C53 C54 H54 119.4 . . ? C56 C55 C54 119(9) . . ? C56 C55 H55 120.6 . . ? C54 C55 H55 120.6 . . ? C56 C55 H56' 42.0 . . ? C54 C55 H56' 159.1 . . ? H55 C55 H56' 79.2 . . ? C51 C56 C51' 60(7) . . ? C51 C56 C55' 60(6) . . ? C51' C56 C55' 119(10) . . ? C51 C56 C55 122(6) . . ? C51' C56 C55 63(6) . . ? C55' C56 C55 162(4) . . ? C51 C56 H56 119.2 . . ? C51' C56 H56 168.0 . . ? C55' C56 H56 62.4 . . ? C55 C56 H56 119.2 . . ? C51 C56 H56' 174.5 . . ? C51' C56 H56' 120.4 . . ? C55' C56 H56' 120.3 . . ? C55 C56 H56' 60.1 . . ? H56 C56 H56' 59.4 . . ? C51 C57 H57A 109.5 . . ? C51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C51' C52 121(10) . . ? C56 C51' C57' 121(10) . . ? C52 C51' C57' 118(9) . . ? C54' C53' C52 119(10) . . ? C54' C53' H53' 120.5 . . ? C52 C53' H53' 120.5 . . ? C53' C54' C55' 121(10) . . ? C53' C54' H54' 119.7 . . ? C55' C54' H54' 119.7 . . ? C56 C55' C54' 121(9) . . ? C56 C55' H55' 119.7 . . ? C54' C55' H55' 119.7 . . ? C51' C57' H57D 109.5 . . ? C51' C57' H57E 109.5 . . ? H57D C57' H57E 109.5 . . ? C51' C57' H57F 109.5 . . ? H57D C57' H57F 109.5 . . ? H57E C57' H57F 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 N4 Ni1 N1 C1 -111.9(9) . . . . ? N3 Ni1 N1 C1 -66.8(4) . . . . ? N2 Ni1 N1 C1 178.1(4) . . . . ? Cl1 Ni1 N1 C1 34.1(4) . . . . ? N4 Ni1 N1 C5 56.8(10) . . . . ? N3 Ni1 N1 C5 102.0(3) . . . . ? N2 Ni1 N1 C5 -13.2(3) . . . . ? Cl1 Ni1 N1 C5 -157.1(3) . . . . ? C19 P1 N2 C6 -160.5(4) . . . . ? C26 P1 N2 C6 -43.8(4) . . . . ? C20 P1 N2 C6 74.5(4) . . . . ? C19 P1 N2 Ni1 -4.9(3) . . . . ? C26 P1 N2 Ni1 111.8(2) . . . . ? C20 P1 N2 Ni1 -129.9(2) . . . . ? N4 Ni1 N2 C6 -159.1(3) . . . . ? N3 Ni1 N2 C6 -77.1(3) . . . . ? N1 Ni1 N2 C6 11.9(3) . . . . ? Cl1 Ni1 N2 C6 92.7(3) . . . . ? N4 Ni1 N2 P1 43.1(2) . . . . ? N3 Ni1 N2 P1 125.2(2) . . . . ? N1 Ni1 N2 P1 -145.9(3) . . . . ? Cl1 Ni1 N2 P1 -65.1(3) . . . . ? N4 Ni1 N3 C10 175.9(4) . . . . ? N2 Ni1 N3 C10 82.7(4) . . . . ? N1 Ni1 N3 C10 2.8(4) . . . . ? Cl1 Ni1 N3 C10 -91.1(4) . . . . ? N4 Ni1 N3 C14 -14.5(3) . . . . ? N2 Ni1 N3 C14 -107.8(3) . . . . ? N1 Ni1 N3 C14 172.3(3) . . . . ? Cl1 Ni1 N3 C14 78.4(3) . . . . ? C19 P2 N4 C15 -165.5(3) . . . . ? C32 P2 N4 C15 77.2(4) . . . . ? C38 P2 N4 C15 -41.4(4) . . . . ? C19 P2 N4 Ni1 14.3(3) . . . . ? C32 P2 N4 Ni1 -103.0(2) . . . . ? C38 P2 N4 Ni1 138.4(2) . . . . ? N3 Ni1 N4 C15 15.3(3) . . . . ? N2 Ni1 N4 C15 130.0(3) . . . . ? N1 Ni1 N4 C15 61.4(9) . . . . ? Cl1 Ni1 N4 C15 -84.6(3) . . . . ? N3 Ni1 N4 P2 -164.5(2) . . . . ? N2 Ni1 N4 P2 -49.9(2) . . . . ? N1 Ni1 N4 P2 -118.5(8) . . . . ? Cl1 Ni1 N4 P2 95.5(2) . . . . ? C5 N1 C1 C2 -0.9(8) . . . . ? Ni1 N1 C1 C2 167.4(4) . . . . ? N1 C1 C2 C3 0.4(9) . . . . ? C1 C2 C3 C4 0.2(9) . . . . ? C2 C3 C4 C9 178.0(5) . . . . ? C2 C3 C4 C5 -0.4(8) . . . . ? C1 N1 C5 C4 0.7(7) . . . . ? Ni1 N1 C5 C4 -169.2(3) . . . . ? C1 N1 C5 C6 -177.7(4) . . . . ? Ni1 N1 C5 C6 12.4(5) . . . . ? C9 C4 C5 N1 -178.6(4) . . . . ? C3 C4 C5 N1 0.0(7) . . . . ? C9 C4 C5 C6 -0.3(7) . . . . ? C3 C4 C5 C6 178.3(4) . . . . ? P1 N2 C6 C7 -31.7(7) . . . . ? Ni1 N2 C6 C7 171.5(4) . . . . ? P1 N2 C6 C5 147.8(3) . . . . ? Ni1 N2 C6 C5 -9.0(5) . . . . ? N1 C5 C6 C7 177.2(4) . . . . ? C4 C5 C6 C7 -1.2(6) . . . . ? N1 C5 C6 N2 -2.3(6) . . . . ? C4 C5 C6 N2 179.3(4) . . . . ? N2 C6 C7 C8 -178.6(5) . . . . ? C5 C6 C7 C8 1.9(7) . . . . ? C6 C7 C8 C9 -1.2(8) . . . . ? C7 C8 C9 C4 -0.4(8) . . . . ? C3 C4 C9 C8 -177.3(5) . . . . ? C5 C4 C9 C8 1.1(7) . . . . ? C14 N3 C10 C11 -0.8(8) . . . . ? Ni1 N3 C10 C11 168.2(4) . . . . ? N3 C10 C11 C12 1.5(9) . . . . ? C10 C11 C12 C13 -2.6(9) . . . . ? C11 C12 C13 C14 3.1(8) . . . . ? C11 C12 C13 C18 -177.9(6) . . . . ? C10 N3 C14 C13 1.4(7) . . . . ? Ni1 N3 C14 C13 -169.2(4) . . . . ? C10 N3 C14 C15 -178.0(4) . . . . ? Ni1 N3 C14 C15 11.4(5) . . . . ? C12 C13 C14 N3 -2.5(7) . . . . ? C18 C13 C14 N3 178.5(4) . . . . ? C12 C13 C14 C15 176.9(4) . . . . ? C18 C13 C14 C15 -2.2(7) . . . . ? P2 N4 C15 C16 -15.9(7) . . . . ? Ni1 N4 C15 C16 164.3(4) . . . . ? P2 N4 C15 C14 165.9(3) . . . . ? Ni1 N4 C15 C14 -13.9(5) . . . . ? N3 C14 C15 N4 1.7(6) . . . . ? C13 C14 C15 N4 -177.7(4) . . . . ? N3 C14 C15 C16 -176.7(4) . . . . ? C13 C14 C15 C16 3.9(7) . . . . ? N4 C15 C16 C17 178.5(5) . . . . ? C14 C15 C16 C17 -3.3(7) . . . . ? C15 C16 C17 C18 1.0(8) . . . . ? C16 C17 C18 C13 0.8(9) . . . . ? C12 C13 C18 C17 -179.2(5) . . . . ? C14 C13 C18 C17 -0.2(8) . . . . ? N4 P2 C19 P1 43.7(4) . . . . ? C32 P2 C19 P1 166.1(3) . . . . ? C38 P2 C19 P1 -76.2(4) . . . . ? N2 P1 C19 P2 -49.2(4) . . . . ? C26 P1 C19 P2 -169.4(3) . . . . ? C20 P1 C19 P2 75.5(3) . . . . ? N2 P1 C20 C25 2.6(5) . . . . ? C19 P1 C20 C25 -122.2(4) . . . . ? C26 P1 C20 C25 123.6(4) . . . . ? N2 P1 C20 C21 179.5(4) . . . . ? C19 P1 C20 C21 54.7(4) . . . . ? C26 P1 C20 C21 -59.5(4) . . . . ? C25 C20 C21 C22 -1.3(8) . . . . ? P1 C20 C21 C22 -178.2(4) . . . . ? C20 C21 C22 C23 0.9(9) . . . . ? C21 C22 C23 C24 0.4(10) . . . . ? C22 C23 C24 C25 -1.1(10) . . . . ? C21 C20 C25 C24 0.5(8) . . . . ? P1 C20 C25 C24 177.4(4) . . . . ? C23 C24 C25 C20 0.7(9) . . . . ? N2 P1 C26 C27 110.6(4) . . . . ? C19 P1 C26 C27 -129.1(4) . . . . ? C20 P1 C26 C27 -10.5(5) . . . . ? N2 P1 C26 C31 -69.4(4) . . . . ? C19 P1 C26 C31 50.9(4) . . . . ? C20 P1 C26 C31 169.5(4) . . . . ? C31 C26 C27 C28 -1.5(7) . . . . ? P1 C26 C27 C28 178.6(4) . . . . ? C26 C27 C28 C29 -1.2(9) . . . . ? C27 C28 C29 C30 3.1(10) . . . . ? C28 C29 C30 C31 -2.3(10) . . . . ? C29 C30 C31 C26 -0.5(9) . . . . ? C27 C26 C31 C30 2.4(7) . . . . ? P1 C26 C31 C30 -177.7(4) . . . . ? N4 P2 C32 C33 1.0(4) . . . . ? C19 P2 C32 C33 -118.2(4) . . . . ? C38 P2 C32 C33 119.6(4) . . . . ? N4 P2 C32 C37 176.4(4) . . . . ? C19 P2 C32 C37 57.2(5) . . . . ? C38 P2 C32 C37 -65.0(5) . . . . ? C37 C32 C33 C34 2.0(7) . . . . ? P2 C32 C33 C34 177.5(4) . . . . ? C32 C33 C34 C35 -1.8(8) . . . . ? C33 C34 C35 C36 0.6(8) . . . . ? C34 C35 C36 C37 0.4(8) . . . . ? C35 C36 C37 C32 -0.3(8) . . . . ? C33 C32 C37 C36 -0.9(8) . . . . ? P2 C32 C37 C36 -176.3(4) . . . . ? N4 P2 C38 C39 -47.9(5) . . . . ? C19 P2 C38 C39 72.8(5) . . . . ? C32 P2 C38 C39 -170.6(4) . . . . ? N4 P2 C38 C43 133.7(5) . . . . ? C19 P2 C38 C43 -105.6(5) . . . . ? C32 P2 C38 C43 11.0(6) . . . . ? C43 C38 C39 C40 -0.2(9) . . . . ? P2 C38 C39 C40 -178.6(5) . . . . ? C38 C39 C40 C41 0.2(11) . . . . ? C39 C40 C41 C42 -0.3(13) . . . . ? C40 C41 C42 C43 0.5(13) . . . . ? C39 C38 C43 C42 0.3(9) . . . . ? P2 C38 C43 C42 178.6(5) . . . . ? C41 C42 C43 C38 -0.4(12) . . . . ? C49 C44 C45 C46 12(4) . . . . ? C50 C44 C45 C46 174.4(13) . . . . ? C44 C45 C46 C47 -4(3) . . . . ? C45 C46 C47 C48 -2(3) . . . . ? C46 C47 C48 C49 0(3) . . . . ? C45 C44 C49 C48 -13(3) . . . . ? C50 C44 C49 C48 -174.3(17) . . . . ? C47 C48 C49 C44 6(3) . . . . ? C56 C51 C52 C53 -1(6) . . . . ? C57 C51 C52 C53 180(4) . . . . ? C56 C51 C52 C51' 11(5) . . . . ? C57 C51 C52 C51' -168(6) . . . . ? C56 C51 C52 C53' -161(5) . . . . ? C57 C51 C52 C53' 20(5) . . . . ? C51' C52 C53 C54 -11(6) . . . . ? C53' C52 C53 C54 89(26) . . . . ? C51 C52 C53 C54 0(7) . . . . ? C52 C53 C54 C55 -1(10) . . . . ? C53 C54 C55 C56 3(9) . . . . ? C52 C51 C56 C51' -11(4) . . . . ? C57 C51 C56 C51' 169(7) . . . . ? C52 C51 C56 C55' 163(6) . . . . ? C57 C51 C56 C55' -18(6) . . . . ? C52 C51 C56 C55 3(7) . . . . ? C57 C51 C56 C55 -178(5) . . . . ? C54 C55 C56 C51 -4(7) . . . . ? C54 C55 C56 C51' 9(5) . . . . ? C54 C55 C56 C55' -94(29) . . . . ? C51 C56 C51' C52 11(5) . . . . ? C55' C56 C51' C52 4(8) . . . . ? C55 C56 C51' C52 -156(7) . . . . ? C51 C56 C51' C57' -171(7) . . . . ? C55' C56 C51' C57' -177(6) . . . . ? C55 C56 C51' C57' 22(6) . . . . ? C53 C52 C51' C56 158(7) . . . . ? C53' C52 C51' C56 -2(8) . . . . ? C51 C52 C51' C56 -10(5) . . . . ? C53 C52 C51' C57' -21(5) . . . . ? C53' C52 C51' C57' 180(5) . . . . ? C51 C52 C51' C57' 171(7) . . . . ? C53 C52 C53' C54' -91(26) . . . . ? C51' C52 C53' C54' 0(8) . . . . ? C51 C52 C53' C54' 8(6) . . . . ? C52 C53' C54' C55' 0(11) . . . . ? C51 C56 C55' C54' -11(7) . . . . ? C51' C56 C55' C54' -5(10) . . . . ? C55 C56 C55' C54' 89(29) . . . . ? C53' C54' C55' C56 2(13) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.718 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.089