# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address P.Braunstein ;Laboratoire de Chimie de Coordination, Institut de Chimie (UMR 7177 CNRS), Universit\'e de Strasbourg, 4 rue Blaise Pascal, CS 90032 F-67081 Strasbourg Cedex, France, ; R.Pattacini ;Laboratoire de Chimie de Coordination, Institut de Chimie (UMR 7177 CNRS), Universit\'e de Strasbourg, 4 rue Blaise Pascal, CS 90032 F-67081 Strasbourg Cedex, France, ; S.Zhang ;Laboratoire de Chimie de Coordination, Institut de Chimie (UMR 7177 CNRS), Universit\'e de Strasbourg, 4 rue Blaise Pascal, CS 90032 F-67081 Strasbourg Cedex, France, ; S.Jie ;Laboratoire de Chimie de Coordination, Institut de Chimie (UMR 7177 CNRS), Universit\'e de Strasbourg, 4 rue Blaise Pascal, CS 90032 F-67081 Strasbourg Cedex, France, ; _publ_contact_author_address ;Laboratoire de Chimie de Coordination, Institut de Chimie (UMR 7177 CNRS), Universit\'e Louis Pasteur, 4 rue Blaise Pascal, CS 90032 F-67081 Strasbourg Cedex, France, ; _publ_contact_author_email braunstein@unistra.fr _publ_contact_author_fax '+33 390241308' _publ_contact_author_phone '+33 390241322' _publ_contact_author_name 'Dr. Pierre Braunstein' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 831824' #TrackingRef 'Allcifs.cif' _ccdc_journal_manuscript_code DaltonTrans _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H32 Cl4 Co N2 O2 P2 Pd, C2 H3 N' _chemical_formula_sum 'C34 H35 Cl4 Co N3 O2 P2 Pd' _chemical_formula_weight 886.72 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' -x,-y,-z _cell_length_a 12.5554(4) _cell_length_b 12.9516(5) _cell_length_c 13.0189(5) _cell_angle_alpha 81.649(2) _cell_angle_beta 88.148(2) _cell_angle_gamma 63.361(2) _cell_volume 1870.96(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9506 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description preism _exptl_crystal_colour blue _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 894 _exptl_absorpt_coefficient_mu 1.330 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18204 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.50 _reflns_number_total 7750 _reflns_number_gt 5413 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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^)+(0.0481P)^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 7750 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.003 _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 Pd1 Pd 0.19983(2) 0.31413(2) 0.286010(19) 0.03108(9) Uani 1 1 d . . . Co1 Co -0.06006(4) 0.85459(4) 0.19549(4) 0.04100(14) Uani 1 1 d . . . P2 P 0.23196(7) 0.43977(7) 0.16475(7) 0.0310(2) Uani 1 1 d . . . P1 P 0.33002(7) 0.29222(7) 0.41219(7) 0.0345(2) Uani 1 1 d . . . Cl1 Cl 0.06049(7) 0.32115(8) 0.16618(7) 0.0431(2) Uani 1 1 d . . . Cl2 Cl -0.08290(9) 0.72478(9) 0.31808(8) 0.0582(3) Uani 1 1 d . . . Cl4 Cl 0.03318(11) 0.94520(11) 0.26270(9) 0.0743(3) Uani 1 1 d . . . Cl3 Cl -0.23107(9) 0.98860(9) 0.11289(9) 0.0663(3) Uani 1 1 d . . . N1 N 0.1758(2) 0.1891(2) 0.3917(2) 0.0347(6) Uani 1 1 d . . . O2 O 0.1707(2) 0.6453(2) -0.01992(19) 0.0462(6) Uani 1 1 d . . . N2 N 0.0488(2) 0.7709(2) 0.0817(2) 0.0404(7) Uani 1 1 d . . . O1 O 0.2436(2) 0.0417(2) 0.5218(2) 0.0588(7) Uani 1 1 d . . . C11 C 0.4767(3) 0.2815(3) 0.3868(3) 0.0374(8) Uani 1 1 d . . . C27 C 0.2974(3) 0.3552(3) 0.0601(2) 0.0334(7) Uani 1 1 d . . . C26 C 0.2752(3) 0.5948(3) 0.2589(3) 0.0482(9) Uani 1 1 d . . . H26 H 0.2064 0.6045 0.2941 0.058 Uiso 1 1 calc R . . C6 C 0.1525(3) 0.4863(3) 0.4811(3) 0.0431(9) Uani 1 1 d . . . H6 H 0.1146 0.4995 0.4169 0.052 Uiso 1 1 calc R . . C19 C 0.0993(3) 0.6667(3) 0.0613(3) 0.0362(8) Uani 1 1 d . . . C16 C 0.5119(3) 0.3598(3) 0.4190(3) 0.0497(10) Uani 1 1 d . . . H16 H 0.4592 0.4201 0.4532 0.060 Uiso 1 1 calc R . . C21 C 0.3204(3) 0.5126(3) 0.1918(3) 0.0363(8) Uani 1 1 d . . . C20 C 0.0893(3) 0.5647(3) 0.1191(3) 0.0357(8) Uani 1 1 d . . . H20A H 0.0478 0.5394 0.0747 0.043 Uiso 1 1 calc R . . H20B H 0.0408 0.5890 0.1787 0.043 Uiso 1 1 calc R . . C5 C 0.2633(3) 0.3919(3) 0.5039(3) 0.0371(8) Uani 1 1 d . . . C3 C 0.2542(3) 0.1284(3) 0.4639(3) 0.0426(9) Uani 1 1 d . . . C9 C 0.2636(4) 0.4484(4) 0.6709(3) 0.0559(11) Uani 1 1 d . . . H9 H 0.3012 0.4365 0.7350 0.067 Uiso 1 1 calc R . . C12 C 0.5567(3) 0.1928(3) 0.3355(3) 0.0477(9) Uani 1 1 d . . . H12 H 0.5343 0.1396 0.3142 0.057 Uiso 1 1 calc R . . C10 C 0.3191(3) 0.3726(3) 0.6006(3) 0.0481(9) Uani 1 1 d . . . H10 H 0.3932 0.3090 0.6174 0.058 Uiso 1 1 calc R . . C1 C 0.0892(3) 0.1406(3) 0.3929(3) 0.0509(10) Uani 1 1 d . . . H1A H 0.0880 0.1126 0.3280 0.061 Uiso 1 1 calc R . . H1B H 0.0095 0.1985 0.4053 0.061 Uiso 1 1 calc R . . C32 C 0.4074(3) 0.2590(3) 0.0801(3) 0.0495(9) Uani 1 1 d . . . H32 H 0.4510 0.2486 0.1403 0.059 Uiso 1 1 calc R . . C29 C 0.2791(4) 0.2871(4) -0.0967(3) 0.0538(10) Uani 1 1 d . . . H29 H 0.2351 0.2964 -0.1564 0.065 Uiso 1 1 calc R . . C28 C 0.2351(3) 0.3695(3) -0.0302(3) 0.0429(9) Uani 1 1 d . . . H28 H 0.1627 0.4354 -0.0465 0.051 Uiso 1 1 calc R . . C25 C 0.3310(4) 0.6629(3) 0.2743(3) 0.0587(11) Uani 1 1 d . . . H25 H 0.3003 0.7179 0.3196 0.070 Uiso 1 1 calc R . . C22 C 0.4233(3) 0.4971(4) 0.1410(3) 0.0536(10) Uani 1 1 d . . . H22 H 0.4551 0.4418 0.0962 0.064 Uiso 1 1 calc R . . C4 C 0.3580(3) 0.1482(3) 0.4830(3) 0.0517(10) Uani 1 1 d . . . H4A H 0.4295 0.0877 0.4589 0.062 Uiso 1 1 calc R . . H4B H 0.3691 0.1461 0.5568 0.062 Uiso 1 1 calc R . . C15 C 0.6251(4) 0.3476(4) 0.3998(4) 0.0672(12) Uani 1 1 d . . . H15 H 0.6489 0.3997 0.4214 0.081 Uiso 1 1 calc R . . C8 C 0.1530(4) 0.5419(4) 0.6475(3) 0.0576(11) Uani 1 1 d . . . H8 H 0.1159 0.5919 0.6960 0.069 Uiso 1 1 calc R . . C7 C 0.0976(3) 0.5610(3) 0.5529(3) 0.0552(10) Uani 1 1 d . . . H7 H 0.0232 0.6243 0.5369 0.066 Uiso 1 1 calc R . . C23 C 0.4792(4) 0.5652(4) 0.1576(4) 0.0684(13) Uani 1 1 d . . . H23 H 0.5496 0.5540 0.1246 0.082 Uiso 1 1 calc R . . C13 C 0.6700(3) 0.1826(4) 0.3156(3) 0.0594(11) Uani 1 1 d . . . H13 H 0.7228 0.1241 0.2797 0.071 Uiso 1 1 calc R . . C24 C 0.4322(4) 0.6479(4) 0.2215(4) 0.0679(13) Uani 1 1 d . . . H24 H 0.4690 0.6947 0.2296 0.081 Uiso 1 1 calc R . . C30 C 0.3876(4) 0.1916(4) -0.0748(3) 0.0613(11) Uani 1 1 d . . . H30 H 0.4166 0.1357 -0.1193 0.074 Uiso 1 1 calc R . . C17 C 0.0843(4) 0.8422(3) 0.0028(3) 0.0609(11) Uani 1 1 d . . . H17A H 0.1239 0.8793 0.0351 0.073 Uiso 1 1 calc R . . H17B H 0.0155 0.9019 -0.0382 0.073 Uiso 1 1 calc R . . C14 C 0.7029(4) 0.2592(4) 0.3492(3) 0.0667(12) Uani 1 1 d . . . H14 H 0.7795 0.2513 0.3376 0.080 Uiso 1 1 calc R . . C2 C 0.1363(4) 0.0409(4) 0.4825(3) 0.0712(13) Uani 1 1 d . . . H2A H 0.0781 0.0532 0.5360 0.085 Uiso 1 1 calc R . . H2B H 0.1554 -0.0329 0.4587 0.085 Uiso 1 1 calc R . . C48 C 0.3650(4) -0.0230(4) 0.2433(4) 0.0789(15) Uani 1 1 d . . . C18 C 0.1690(4) 0.7557(3) -0.0639(3) 0.0640(12) Uani 1 1 d . . . H18A H 0.1404 0.7775 -0.1358 0.077 Uiso 1 1 calc R . . H18B H 0.2480 0.7513 -0.0601 0.077 Uiso 1 1 calc R . . C31 C 0.4534(4) 0.1781(4) 0.0122(3) 0.0643(12) Uani 1 1 d . . . H31 H 0.5285 0.1150 0.0255 0.077 Uiso 1 1 calc R . . C33 C 0.2832(4) 0.0093(4) 0.1558(4) 0.0824(14) Uani 1 1 d . . . H33A H 0.2540 -0.0478 0.1567 0.124 Uiso 1 1 calc R . . H33B H 0.3236 0.0129 0.0925 0.124 Uiso 1 1 calc R . . H33C H 0.2175 0.0843 0.1600 0.124 Uiso 1 1 calc R . . N3 N 0.4286(4) -0.0490(5) 0.3111(4) 0.131(2) Uani 1 1 d . . . 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 Pd1 0.03448(15) 0.02767(15) 0.03158(16) -0.00342(11) -0.00163(11) -0.01446(11) Co1 0.0492(3) 0.0328(3) 0.0422(3) -0.0049(2) -0.0005(2) -0.0195(2) P2 0.0324(4) 0.0283(5) 0.0315(5) -0.0024(4) -0.0017(4) -0.0134(4) P1 0.0352(5) 0.0300(5) 0.0355(5) -0.0017(4) -0.0063(4) -0.0124(4) Cl1 0.0473(5) 0.0522(6) 0.0391(5) -0.0068(4) -0.0035(4) -0.0302(4) Cl2 0.0733(7) 0.0501(6) 0.0507(6) 0.0029(5) 0.0056(5) -0.0305(5) Cl4 0.0913(8) 0.0857(8) 0.0779(8) -0.0303(7) 0.0067(6) -0.0626(7) Cl3 0.0630(6) 0.0502(6) 0.0712(8) -0.0031(5) -0.0158(5) -0.0132(5) N1 0.0413(16) 0.0255(15) 0.0407(18) -0.0033(13) 0.0016(13) -0.0183(13) O2 0.0547(15) 0.0385(15) 0.0407(15) -0.0030(12) 0.0066(12) -0.0180(12) N2 0.0476(17) 0.0288(17) 0.0423(19) -0.0027(14) -0.0008(13) -0.0155(14) O1 0.088(2) 0.0448(16) 0.0493(17) 0.0116(13) -0.0095(14) -0.0395(15) C11 0.0358(18) 0.036(2) 0.034(2) 0.0010(16) -0.0079(15) -0.0115(16) C27 0.0357(18) 0.0337(19) 0.031(2) -0.0040(15) 0.0042(14) -0.0166(15) C26 0.053(2) 0.046(2) 0.052(3) -0.0077(19) -0.0031(18) -0.0269(19) C6 0.040(2) 0.047(2) 0.045(2) -0.0115(18) 0.0020(16) -0.0202(18) C19 0.0352(18) 0.032(2) 0.038(2) -0.0002(16) -0.0089(15) -0.0133(16) C16 0.046(2) 0.055(3) 0.052(3) -0.013(2) 0.0062(18) -0.0248(19) C21 0.0387(19) 0.035(2) 0.036(2) 0.0056(16) -0.0104(15) -0.0192(16) C20 0.0350(18) 0.0270(18) 0.044(2) -0.0020(15) -0.0028(15) -0.0137(15) C5 0.0413(19) 0.039(2) 0.034(2) -0.0003(16) 0.0003(15) -0.0218(17) C3 0.055(2) 0.033(2) 0.039(2) -0.0029(17) -0.0009(18) -0.0200(18) C9 0.071(3) 0.080(3) 0.032(2) -0.011(2) 0.0012(19) -0.046(3) C12 0.051(2) 0.042(2) 0.041(2) -0.0047(18) -0.0054(18) -0.0118(18) C10 0.049(2) 0.058(3) 0.041(2) -0.0033(19) -0.0054(18) -0.0276(19) C1 0.061(2) 0.044(2) 0.056(3) -0.004(2) 0.004(2) -0.032(2) C32 0.046(2) 0.050(2) 0.042(2) -0.0075(19) -0.0023(17) -0.0123(19) C29 0.067(3) 0.069(3) 0.039(2) -0.016(2) 0.0076(19) -0.041(2) C28 0.040(2) 0.046(2) 0.043(2) -0.0070(18) 0.0000(17) -0.0201(17) C25 0.065(3) 0.050(3) 0.068(3) -0.015(2) -0.012(2) -0.029(2) C22 0.057(2) 0.070(3) 0.049(3) -0.009(2) 0.0007(19) -0.042(2) C4 0.056(2) 0.035(2) 0.055(3) 0.0058(19) -0.0137(19) -0.0146(18) C15 0.063(3) 0.080(3) 0.078(3) -0.022(3) 0.014(2) -0.047(3) C8 0.065(3) 0.072(3) 0.051(3) -0.026(2) 0.023(2) -0.041(3) C7 0.040(2) 0.056(3) 0.069(3) -0.022(2) 0.010(2) -0.0177(19) C23 0.065(3) 0.099(4) 0.067(3) -0.008(3) 0.003(2) -0.061(3) C13 0.045(2) 0.062(3) 0.048(3) -0.001(2) 0.0080(18) -0.007(2) C24 0.078(3) 0.069(3) 0.078(3) -0.002(3) -0.020(3) -0.053(3) C30 0.072(3) 0.056(3) 0.057(3) -0.026(2) 0.023(2) -0.027(2) C17 0.082(3) 0.038(2) 0.056(3) 0.005(2) 0.012(2) -0.025(2) C14 0.047(2) 0.090(4) 0.064(3) -0.005(3) 0.008(2) -0.033(3) C2 0.101(4) 0.072(3) 0.063(3) 0.009(3) -0.002(3) -0.063(3) C48 0.057(3) 0.089(4) 0.079(4) -0.045(3) 0.014(3) -0.013(3) C18 0.090(3) 0.044(3) 0.055(3) 0.001(2) 0.018(2) -0.030(2) C31 0.061(3) 0.054(3) 0.063(3) -0.018(2) 0.012(2) -0.010(2) C33 0.074(3) 0.094(4) 0.073(4) -0.026(3) 0.006(3) -0.028(3) N3 0.091(3) 0.162(5) 0.103(4) -0.064(4) -0.022(3) -0.010(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 Pd1 N1 2.090(3) . ? Pd1 P1 2.2523(8) . ? Pd1 P2 2.2592(9) . ? Pd1 Cl1 2.3442(8) . ? Co1 N2 2.060(3) . ? Co1 Cl3 2.2459(11) . ? Co1 Cl2 2.2537(10) . ? Co1 Cl4 2.2604(10) . ? P2 C27 1.813(3) . ? P2 C21 1.819(3) . ? P2 C20 1.836(3) . ? P1 C5 1.791(3) . ? P1 C11 1.806(3) . ? P1 C4 1.841(3) . ? N1 C3 1.274(4) . ? N1 C1 1.478(4) . ? O2 C19 1.341(4) . ? O2 C18 1.452(4) . ? N2 C19 1.273(4) . ? N2 C17 1.474(4) . ? O1 C3 1.314(4) . ? O1 C2 1.461(4) . ? C11 C12 1.386(5) . ? C11 C16 1.392(5) . ? C27 C28 1.375(4) . ? C27 C32 1.383(5) . ? C26 C21 1.384(5) . ? C26 C25 1.387(5) . ? C6 C7 1.381(5) . ? C6 C5 1.384(5) . ? C19 C20 1.477(4) . ? C16 C15 1.376(5) . ? C21 C22 1.377(5) . ? C5 C10 1.395(5) . ? C3 C4 1.471(4) . ? C9 C10 1.377(5) . ? C9 C8 1.378(6) . ? C12 C13 1.387(5) . ? C1 C2 1.517(5) . ? C32 C31 1.380(5) . ? C29 C30 1.371(5) . ? C29 C28 1.379(5) . ? C25 C24 1.374(6) . ? C22 C23 1.392(5) . ? C15 C14 1.369(6) . ? C8 C7 1.369(5) . ? C23 C24 1.358(6) . ? C13 C14 1.360(6) . ? C30 C31 1.367(6) . ? C17 C18 1.515(5) . ? C48 N3 1.117(6) . ? C48 C33 1.442(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 P1 81.55(7) . . ? N1 Pd1 P2 176.10(7) . . ? P1 Pd1 P2 99.77(3) . . ? N1 Pd1 Cl1 92.17(7) . . ? P1 Pd1 Cl1 173.71(3) . . ? P2 Pd1 Cl1 86.49(3) . . ? N2 Co1 Cl3 105.86(8) . . ? N2 Co1 Cl2 110.55(8) . . ? Cl3 Co1 Cl2 114.01(4) . . ? N2 Co1 Cl4 105.27(8) . . ? Cl3 Co1 Cl4 109.57(5) . . ? Cl2 Co1 Cl4 111.11(4) . . ? C27 P2 C21 109.13(15) . . ? C27 P2 C20 109.70(15) . . ? C21 P2 C20 101.46(14) . . ? C27 P2 Pd1 103.71(10) . . ? C21 P2 Pd1 122.76(11) . . ? C20 P2 Pd1 109.83(11) . . ? C5 P1 C11 108.07(15) . . ? C5 P1 C4 105.13(17) . . ? C11 P1 C4 104.60(16) . . ? C5 P1 Pd1 112.70(11) . . ? C11 P1 Pd1 123.26(11) . . ? C4 P1 Pd1 100.99(11) . . ? C3 N1 C1 107.8(3) . . ? C3 N1 Pd1 119.7(2) . . ? C1 N1 Pd1 131.9(2) . . ? C19 O2 C18 106.6(3) . . ? C19 N2 C17 107.2(3) . . ? C19 N2 Co1 135.8(2) . . ? C17 N2 Co1 117.0(2) . . ? C3 O1 C2 106.2(3) . . ? C12 C11 C16 119.0(3) . . ? C12 C11 P1 119.7(3) . . ? C16 C11 P1 121.3(3) . . ? C28 C27 C32 118.4(3) . . ? C28 C27 P2 123.1(3) . . ? C32 C27 P2 117.5(3) . . ? C21 C26 C25 120.9(4) . . ? C7 C6 C5 120.6(3) . . ? N2 C19 O2 117.6(3) . . ? N2 C19 C20 126.6(3) . . ? O2 C19 C20 115.7(3) . . ? C15 C16 C11 119.7(4) . . ? C22 C21 C26 119.4(3) . . ? C22 C21 P2 122.6(3) . . ? C26 C21 P2 117.7(3) . . ? C19 C20 P2 114.9(2) . . ? C6 C5 C10 119.2(3) . . ? C6 C5 P1 119.9(3) . . ? C10 C5 P1 120.8(3) . . ? N1 C3 O1 118.3(3) . . ? N1 C3 C4 123.1(3) . . ? O1 C3 C4 118.6(3) . . ? C10 C9 C8 120.8(4) . . ? C11 C12 C13 120.6(3) . . ? C9 C10 C5 119.5(4) . . ? N1 C1 C2 102.9(3) . . ? C31 C32 C27 121.2(3) . . ? C30 C29 C28 120.0(4) . . ? C27 C28 C29 120.7(3) . . ? C24 C25 C26 118.9(4) . . ? C21 C22 C23 119.3(4) . . ? C3 C4 P1 107.9(2) . . ? C14 C15 C16 120.4(4) . . ? C7 C8 C9 120.1(4) . . ? C8 C7 C6 119.9(4) . . ? C24 C23 C22 120.8(4) . . ? C14 C13 C12 119.3(4) . . ? C23 C24 C25 120.7(3) . . ? C31 C30 C29 120.3(4) . . ? N2 C17 C18 104.3(3) . . ? C13 C14 C15 121.0(4) . . ? O1 C2 C1 104.8(3) . . ? N3 C48 C33 179.4(6) . . ? O2 C18 C17 104.2(3) . . ? C30 C31 C32 119.4(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.745 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.088 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 831825' #TrackingRef 'Allcifs.cif' _ccdc_journal_manuscript_code DaltonTrans _chemical_formula_moiety 'C32 H32 Cl2 N2 Ni O2 P2' _chemical_formula_sum 'C32 H32 Cl2 N2 Ni O2 P2' _chemical_formula_weight 668.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 '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' 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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_int_tables_number 61 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' '-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 8.2701(2) _cell_length_b 15.3634(7) _cell_length_c 24.168(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3070.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3456 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.943 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6317 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3502 _reflns_number_gt 2203 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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^)+(0.0790P)^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 3502 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0958 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1487 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.000 _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 1.0000 0.0000 0.0000 0.02097(19) Uani 1 2 d S . . P1 P 0.93271(10) 0.09400(6) 0.08254(4) 0.0251(2) Uani 1 1 d . . . Cl1 Cl 1.12531(9) 0.12707(5) -0.03918(4) 0.0280(2) Uani 1 1 d . . . N1 N 0.7795(3) 0.05029(18) -0.02219(12) 0.0235(6) Uani 1 1 d . . . O1 O 0.5785(3) 0.14715(15) -0.01775(11) 0.0319(6) Uani 1 1 d . . . C1 C 0.6628(4) 0.0189(2) -0.06331(17) 0.0338(9) Uani 1 1 d . . . H1A H 0.6186 -0.0372 -0.0526 0.041 Uiso 1 1 calc R . . H1B H 0.7125 0.0136 -0.0995 0.041 Uiso 1 1 calc R . . C2 C 0.5319(4) 0.0890(2) -0.06332(18) 0.0358(9) Uani 1 1 d . . . H2A H 0.5301 0.1201 -0.0983 0.043 Uiso 1 1 calc R . . H2B H 0.4260 0.0638 -0.0568 0.043 Uiso 1 1 calc R . . C3 C 0.7245(4) 0.1193(2) -0.00082(13) 0.0227(7) Uani 1 1 d . . . C4 C 0.8110(4) 0.1715(2) 0.04190(14) 0.0267(8) Uani 1 1 d . . . H4A H 0.7342 0.2014 0.0656 0.032 Uiso 1 1 calc R . . H4B H 0.8802 0.2145 0.0245 0.032 Uiso 1 1 calc R . . C5 C 1.0680(4) 0.1638(2) 0.12360(15) 0.0280(8) Uani 1 1 d . . . C6 C 1.0480(5) 0.1766(3) 0.17990(17) 0.0458(11) Uani 1 1 d . . . H6 H 0.9614 0.1509 0.1982 0.055 Uiso 1 1 calc R . . C7 C 1.1579(5) 0.2279(3) 0.20914(17) 0.0574(13) Uani 1 1 d . . . H7 H 1.1454 0.2354 0.2471 0.069 Uiso 1 1 calc R . . C8 C 1.2847(5) 0.2674(3) 0.18207(18) 0.0483(11) Uani 1 1 d . . . H8 H 1.3560 0.3027 0.2016 0.058 Uiso 1 1 calc R . . C9 C 1.3066(4) 0.2548(2) 0.12584(15) 0.0359(9) Uani 1 1 d . . . H9 H 1.3922 0.2814 0.1075 0.043 Uiso 1 1 calc R . . C10 C 1.1996(4) 0.2022(2) 0.09725(15) 0.0307(8) Uani 1 1 d . . . H10 H 1.2159 0.1923 0.0597 0.037 Uiso 1 1 calc R . . C11 C 0.7887(4) 0.0511(2) 0.13306(14) 0.0285(8) Uani 1 1 d . . . C12 C 0.8278(5) -0.0274(3) 0.15792(16) 0.0416(10) Uani 1 1 d . . . H12 H 0.9254 -0.0543 0.1495 0.050 Uiso 1 1 calc R . . C13 C 0.7221(6) -0.0663(3) 0.19534(18) 0.0555(12) Uani 1 1 d . . . H13 H 0.7494 -0.1189 0.2118 0.067 Uiso 1 1 calc R . . C14 C 0.5778(6) -0.0270(4) 0.20792(18) 0.0561(13) Uani 1 1 d . . . H14 H 0.5077 -0.0529 0.2331 0.067 Uiso 1 1 calc R . . C15 C 0.5369(5) 0.0500(4) 0.18356(19) 0.0541(13) Uani 1 1 d . . . H15 H 0.4385 0.0760 0.1919 0.065 Uiso 1 1 calc R . . C16 C 0.6418(4) 0.0899(3) 0.14614(17) 0.0432(10) Uani 1 1 d . . . H16 H 0.6133 0.1425 0.1299 0.052 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 0.0164(3) 0.0179(3) 0.0287(4) 0.0012(3) -0.0031(2) -0.0005(2) P1 0.0202(5) 0.0229(5) 0.0322(5) 0.0021(4) -0.0026(4) -0.0007(4) Cl1 0.0246(4) 0.0213(5) 0.0380(5) 0.0028(4) 0.0019(4) -0.0029(3) N1 0.0172(13) 0.0217(16) 0.0315(15) 0.0017(13) -0.0040(12) -0.0012(12) O1 0.0204(11) 0.0295(14) 0.0458(15) -0.0018(12) -0.0093(11) 0.0048(10) C1 0.0230(17) 0.031(2) 0.047(2) -0.0070(18) -0.0086(17) 0.0016(15) C2 0.0238(18) 0.037(2) 0.046(2) -0.007(2) -0.0138(17) 0.0021(16) C3 0.0182(15) 0.0189(18) 0.0311(18) 0.0041(16) 0.0001(14) -0.0007(14) C4 0.0254(17) 0.0201(19) 0.0347(19) -0.0003(16) 0.0000(15) 0.0032(14) C5 0.0251(17) 0.0259(19) 0.0330(19) 0.0006(17) -0.0044(16) 0.0005(15) C6 0.037(2) 0.062(3) 0.039(2) -0.013(2) 0.0028(19) -0.017(2) C7 0.053(2) 0.083(4) 0.035(2) -0.016(2) 0.003(2) -0.025(2) C8 0.041(2) 0.055(3) 0.049(3) -0.013(2) -0.005(2) -0.016(2) C9 0.0299(18) 0.035(2) 0.043(2) -0.0008(19) -0.0049(18) -0.0063(17) C10 0.0284(18) 0.029(2) 0.035(2) 0.0019(16) -0.0031(16) -0.0012(16) C11 0.0265(17) 0.031(2) 0.0284(18) 0.0005(16) -0.0034(15) -0.0070(16) C12 0.046(2) 0.042(2) 0.037(2) 0.005(2) 0.0004(18) -0.0074(19) C13 0.069(3) 0.054(3) 0.043(2) 0.015(2) 0.002(2) -0.017(3) C14 0.055(3) 0.076(4) 0.038(3) 0.003(3) 0.009(2) -0.025(3) C15 0.032(2) 0.085(4) 0.046(3) -0.013(3) 0.013(2) -0.016(2) C16 0.035(2) 0.050(3) 0.044(2) -0.002(2) 0.0056(19) -0.0026(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.052(2) 5_755 ? Ni1 N1 2.052(2) . ? Ni1 Cl1 2.4045(8) 5_755 ? Ni1 Cl1 2.4045(8) . ? Ni1 P1 2.5249(9) 5_755 ? Ni1 P1 2.5249(9) . ? P1 C11 1.828(3) . ? P1 C5 1.841(3) . ? P1 C4 1.843(3) . ? N1 C3 1.264(4) . ? N1 C1 1.467(4) . ? O1 C3 1.345(4) . ? O1 C2 1.469(4) . ? C1 C2 1.528(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.490(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.384(5) . ? C5 C10 1.392(5) . ? C6 C7 1.395(5) . ? C6 H6 0.9300 . ? C7 C8 1.378(6) . ? C7 H7 0.9300 . ? C8 C9 1.385(5) . ? C8 H8 0.9300 . ? C9 C10 1.383(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.385(5) . ? C11 C16 1.390(5) . ? C12 C13 1.392(5) . ? C12 H12 0.9300 . ? C13 C14 1.371(6) . ? C13 H13 0.9300 . ? C14 C15 1.363(7) . ? C14 H14 0.9300 . ? C15 C16 1.395(6) . ? C15 H15 0.9300 . ? C16 H16 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 N1 180.0(2) 5_755 . ? N1 Ni1 Cl1 88.53(8) 5_755 5_755 ? N1 Ni1 Cl1 91.47(8) . 5_755 ? N1 Ni1 Cl1 91.47(8) 5_755 . ? N1 Ni1 Cl1 88.53(8) . . ? Cl1 Ni1 Cl1 180.00(5) 5_755 . ? N1 Ni1 P1 78.18(8) 5_755 5_755 ? N1 Ni1 P1 101.82(8) . 5_755 ? Cl1 Ni1 P1 86.66(3) 5_755 5_755 ? Cl1 Ni1 P1 93.34(3) . 5_755 ? N1 Ni1 P1 101.82(8) 5_755 . ? N1 Ni1 P1 78.18(8) . . ? Cl1 Ni1 P1 93.34(3) 5_755 . ? Cl1 Ni1 P1 86.66(3) . . ? P1 Ni1 P1 180.00(6) 5_755 . ? C11 P1 C5 104.25(16) . . ? C11 P1 C4 103.48(16) . . ? C5 P1 C4 104.04(16) . . ? C11 P1 Ni1 117.71(12) . . ? C5 P1 Ni1 128.71(12) . . ? C4 P1 Ni1 93.96(11) . . ? C3 N1 C1 108.4(3) . . ? C3 N1 Ni1 121.9(2) . . ? C1 N1 Ni1 129.6(2) . . ? C3 O1 C2 105.7(2) . . ? N1 C1 C2 103.5(3) . . ? N1 C1 H1A 111.1 . . ? C2 C1 H1A 111.1 . . ? N1 C1 H1B 111.1 . . ? C2 C1 H1B 111.1 . . ? H1A C1 H1B 109.0 . . ? O1 C2 C1 104.0(3) . . ? O1 C2 H2A 110.9 . . ? C1 C2 H2A 110.9 . . ? O1 C2 H2B 110.9 . . ? C1 C2 H2B 110.9 . . ? H2A C2 H2B 109.0 . . ? N1 C3 O1 117.7(3) . . ? N1 C3 C4 124.2(3) . . ? O1 C3 C4 118.1(3) . . ? C3 C4 P1 106.5(2) . . ? C3 C4 H4A 110.4 . . ? P1 C4 H4A 110.4 . . ? C3 C4 H4B 110.4 . . ? P1 C4 H4B 110.4 . . ? H4A C4 H4B 108.6 . . ? C6 C5 C10 118.9(3) . . ? C6 C5 P1 122.6(3) . . ? C10 C5 P1 118.4(3) . . ? C5 C6 C7 120.0(4) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C8 C7 C6 120.3(4) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 120.2(4) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 119.3(4) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C5 121.3(3) . . ? C9 C10 H10 119.4 . . ? C5 C10 H10 119.4 . . ? C12 C11 C16 118.5(3) . . ? C12 C11 P1 116.8(3) . . ? C16 C11 P1 124.5(3) . . ? C11 C12 C13 120.6(4) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 120.1(4) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 120.1(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.5(4) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C11 C16 C15 120.2(4) . . ? C11 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.615 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.182 data_compound3 _database_code_depnum_ccdc_archive 'CCDC 831826' #TrackingRef 'Allcifs.cif' _ccdc_journal_manuscript_code DaltonTrans _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C32 H32 Cl2 N2 Ni O2 P2, 2(C H Cl3)' _chemical_formula_sum 'C34 H34 Cl8 N2 Ni O2 P2' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour green _diffrn_ambient_temperature 173(2) _chemical_formula_weight 906.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 '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' N N 0.0061 0.0033 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7779(6) _cell_length_b 11.0881(5) _cell_length_c 18.3495(11) _cell_angle_alpha 88.468(4) _cell_angle_beta 83.143(3) _cell_angle_gamma 78.299(4) _cell_volume 1934.14(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4531 _cell_measurement_theta_min 0.98 _cell_measurement_theta_max 26.34 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 1.172 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9816 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6657 _reflns_number_gt 5226 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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. Comments to alerts: RFACG01_ALERT_3_B The value of the R factor is > 0.15 R factor given 0.162 RFACR01_ALERT_3_B The value of the weighted R factor is > 0.35 Weighted R factor given 0.396 PLAT082_ALERT_2_B High R1 Value 0.16 PLAT084_ALERT_2_B High wR2 Value 0.40 PLAT234_ALERT_4_B Large Hirshfeld Difference C14 -- C15 0.26 Ang. PLAT341_ALERT_3_B Low Bond Precision on C-C Bonds 0.0286 Ang The crystals were of poor quality and visibly twinned. This resutled in poor refinement parameters, although the connectivity is well established. ; _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^)+(0.0407P)^2^+127.4968P] 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 6657 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1823 _refine_ls_R_factor_gt 0.1615 _refine_ls_wR_factor_ref 0.3959 _refine_ls_wR_factor_gt 0.3896 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.000 _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 0.7692(2) 0.56658(19) 0.16535(12) 0.0228(5) Uani 1 1 d . . . P1 P 0.8974(5) 0.5476(4) 0.2726(2) 0.0259(9) Uani 1 1 d . . . P2 P 0.5847(4) 0.7540(4) 0.1995(2) 0.0248(9) Uani 1 1 d . . . N1 N 0.9248(15) 0.6670(11) 0.1331(8) 0.029(3) Uani 1 1 d . . . N2 N 0.6807(15) 0.6064(13) 0.0666(7) 0.027(3) Uani 1 1 d . . . Cl1 Cl 0.5956(5) 0.4470(4) 0.2069(2) 0.0315(10) Uani 1 1 d . . . Cl2 Cl 0.9304(5) 0.3824(4) 0.1145(2) 0.0332(10) Uani 1 1 d . . . Cl3 Cl 0.3339(7) 0.3504(7) 0.3675(4) 0.0718(18) Uani 1 1 d . . . Cl4 Cl 0.5700(7) 0.3913(5) 0.4358(3) 0.0606(16) Uani 1 1 d . . . Cl5 Cl 0.5673(7) 0.1503(5) 0.3830(4) 0.0633(17) Uani 1 1 d . . . Cl6 Cl 0.2631(6) 0.1939(5) 0.2131(3) 0.0509(13) Uani 1 1 d . . . Cl7 Cl 0.1263(6) -0.0142(5) 0.2132(3) 0.0503(13) Uani 1 1 d . . . Cl8 Cl 0.2244(6) 0.0897(5) 0.0757(3) 0.0532(14) Uani 1 1 d . . . O1 O 1.1507(13) 0.6879(12) 0.1286(7) 0.038(3) Uani 1 1 d . . . O2 O 0.4932(14) 0.6729(11) 0.0065(7) 0.035(3) Uani 1 1 d . . . C1 C 1.0717(19) 0.5523(17) 0.2227(10) 0.033(4) Uani 1 1 d . . . H1A H 1.1303 0.5826 0.2541 0.040 Uiso 1 1 calc R . . H1B H 1.1190 0.4711 0.2050 0.040 Uiso 1 1 calc R . . C2 C 1.0404(17) 0.6400(15) 0.1592(9) 0.026(4) Uani 1 1 d . . . C3 C 0.9467(19) 0.7463(19) 0.0682(10) 0.034(4) Uani 1 1 d . . . H3A H 0.8798 0.8241 0.0727 0.041 Uiso 1 1 calc R . . H3B H 0.9366 0.7058 0.0235 0.041 Uiso 1 1 calc R . . C4 C 1.0968(19) 0.7662(17) 0.0680(11) 0.037(4) Uani 1 1 d . . . H4A H 1.1526 0.7408 0.0216 0.044 Uiso 1 1 calc R . . H4B H 1.0974 0.8520 0.0765 0.044 Uiso 1 1 calc R . . C5 C 0.9300(17) 0.4139(15) 0.3324(9) 0.026(4) Uani 1 1 d . . . C6 C 0.981(2) 0.4178(17) 0.3985(12) 0.043(5) Uani 1 1 d . . . H6 H 0.9944 0.4930 0.4142 0.052 Uiso 1 1 calc R . . C7 C 1.013(2) 0.3144(18) 0.4441(11) 0.041(5) Uani 1 1 d . . . H7 H 1.0523 0.3179 0.4873 0.049 Uiso 1 1 calc R . . C8 C 0.980(2) 0.205(2) 0.4198(11) 0.041(5) Uani 1 1 d . . . H8 H 0.9955 0.1351 0.4490 0.049 Uiso 1 1 calc R . . C9 C 0.927(2) 0.1991(18) 0.3539(11) 0.044(5) Uani 1 1 d . . . H9 H 0.9105 0.1247 0.3387 0.053 Uiso 1 1 calc R . . C10 C 0.8988(18) 0.3050(16) 0.3095(10) 0.030(4) Uani 1 1 d . . . H10 H 0.8600 0.3019 0.2659 0.037 Uiso 1 1 calc R . . C11 C 0.8618(18) 0.6778(14) 0.3355(9) 0.025(4) Uani 1 1 d . . . C12 C 0.945(2) 0.7660(17) 0.3373(11) 0.038(4) Uani 1 1 d . . . H12 H 1.0267 0.7594 0.3048 0.046 Uiso 1 1 calc R . . C13 C 0.910(3) 0.8600(18) 0.3848(12) 0.047(5) Uani 1 1 d . . . H13 H 0.9701 0.9139 0.3885 0.056 Uiso 1 1 calc R . . C14 C 0.782(3) 0.875(2) 0.4282(13) 0.066(8) Uani 1 1 d . . . H14 H 0.7533 0.9442 0.4582 0.079 Uiso 1 1 calc R . . C15 C 0.697(2) 0.792(2) 0.4281(12) 0.047(5) Uani 1 1 d . . . H15 H 0.6128 0.8008 0.4591 0.056 Uiso 1 1 calc R . . C16 C 0.737(2) 0.6965(18) 0.3823(10) 0.038(4) Uani 1 1 d . . . H16 H 0.6794 0.6398 0.3817 0.045 Uiso 1 1 calc R . . C17 C 0.4663(16) 0.7244(16) 0.1329(10) 0.031(4) Uani 1 1 d . . . H17A H 0.4041 0.6723 0.1553 0.037 Uiso 1 1 calc R . . H17B H 0.4091 0.8015 0.1186 0.037 Uiso 1 1 calc R . . C18 C 0.5512(18) 0.6646(15) 0.0696(10) 0.029(4) Uani 1 1 d . . . C19 C 0.723(2) 0.5461(17) -0.0063(9) 0.034(4) Uani 1 1 d . . . H19A H 0.7245 0.4584 -0.0030 0.040 Uiso 1 1 calc R . . H19B H 0.8147 0.5590 -0.0276 0.040 Uiso 1 1 calc R . . C20 C 0.603(2) 0.614(2) -0.0520(11) 0.040(5) Uani 1 1 d . . . H20A H 0.6357 0.6755 -0.0847 0.047 Uiso 1 1 calc R . . H20B H 0.5691 0.5565 -0.0805 0.047 Uiso 1 1 calc R . . C21 C 0.6290(16) 0.9004(14) 0.1709(9) 0.025(4) Uani 1 1 d . . . C22 C 0.7071(19) 0.9556(18) 0.2123(9) 0.034(4) Uani 1 1 d . . . H22 H 0.7358 0.9168 0.2551 0.041 Uiso 1 1 calc R . . C23 C 0.745(2) 1.067(2) 0.1927(11) 0.045(5) Uani 1 1 d . . . H23 H 0.7935 1.1032 0.2235 0.054 Uiso 1 1 calc R . . C24 C 0.711(2) 1.1236(17) 0.1290(11) 0.037(4) Uani 1 1 d . . . H24 H 0.7407 1.1964 0.1155 0.045 Uiso 1 1 calc R . . C25 C 0.635(3) 1.0762(19) 0.0852(12) 0.050(6) Uani 1 1 d . . . H25 H 0.6118 1.1160 0.0418 0.060 Uiso 1 1 calc R . . C26 C 0.5899(18) 0.9616(15) 0.1062(10) 0.029(4) Uani 1 1 d . . . H26 H 0.5352 0.9289 0.0769 0.035 Uiso 1 1 calc R . . C27 C 0.4613(17) 0.7920(15) 0.2829(10) 0.028(4) Uani 1 1 d . . . C28 C 0.409(2) 0.6935(19) 0.3218(11) 0.038(4) Uani 1 1 d . . . H28 H 0.4380 0.6130 0.3048 0.046 Uiso 1 1 calc R . . C29 C 0.3169(19) 0.718(2) 0.3829(12) 0.043(5) Uani 1 1 d . . . H29 H 0.2786 0.6546 0.4053 0.051 Uiso 1 1 calc R . . C30 C 0.279(2) 0.8292(19) 0.4123(11) 0.042(5) Uani 1 1 d . . . H30 H 0.2180 0.8413 0.4556 0.050 Uiso 1 1 calc R . . C31 C 0.3322(19) 0.934(2) 0.3765(12) 0.044(5) Uani 1 1 d . . . H31 H 0.3079 1.0131 0.3963 0.053 Uiso 1 1 calc R . . C32 C 0.420(2) 0.9083(17) 0.3122(10) 0.034(4) Uani 1 1 d . . . H32 H 0.4534 0.9726 0.2873 0.041 Uiso 1 1 calc R . . C33 C 0.514(2) 0.3105(18) 0.3675(11) 0.040(5) Uani 1 1 d . . . H33 H 0.5589 0.3312 0.3195 0.048 Uiso 1 1 calc R . . C34 C 0.148(2) 0.1242(17) 0.1678(12) 0.044(5) Uani 1 1 d . . . H34 H 0.0564 0.1804 0.1680 0.053 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 0.0198(10) 0.0189(10) 0.0302(12) 0.0007(8) -0.0046(8) -0.0039(8) P1 0.024(2) 0.020(2) 0.034(2) -0.0011(18) -0.0055(18) -0.0038(17) P2 0.021(2) 0.021(2) 0.033(2) -0.0016(17) -0.0053(18) -0.0038(17) N1 0.031(8) 0.008(6) 0.049(9) -0.012(6) 0.005(7) -0.008(6) N2 0.035(8) 0.028(8) 0.020(7) -0.005(6) -0.004(6) -0.015(6) Cl1 0.032(2) 0.026(2) 0.038(2) 0.0025(17) -0.0032(18) -0.0090(17) Cl2 0.033(2) 0.026(2) 0.037(2) -0.0028(18) -0.0039(18) 0.0023(17) Cl3 0.050(4) 0.075(4) 0.092(5) 0.005(4) -0.015(3) -0.010(3) Cl4 0.078(4) 0.043(3) 0.064(4) -0.013(3) -0.010(3) -0.015(3) Cl5 0.080(4) 0.032(3) 0.076(4) -0.003(3) 0.000(3) -0.013(3) Cl6 0.056(3) 0.042(3) 0.056(3) 0.002(2) -0.017(3) -0.009(2) Cl7 0.057(3) 0.038(3) 0.054(3) 0.004(2) -0.005(3) -0.006(2) Cl8 0.062(4) 0.052(3) 0.042(3) 0.000(2) -0.007(3) -0.002(3) O1 0.030(7) 0.041(8) 0.042(8) 0.001(6) -0.005(6) -0.004(6) O2 0.048(8) 0.023(6) 0.035(7) 0.003(5) -0.020(6) -0.003(6) C1 0.028(9) 0.027(9) 0.042(11) 0.006(8) -0.012(8) 0.003(7) C2 0.022(9) 0.026(9) 0.028(9) 0.003(7) 0.000(7) -0.003(7) C3 0.027(9) 0.049(11) 0.030(9) 0.006(8) 0.003(7) -0.019(8) C4 0.030(10) 0.029(10) 0.047(11) -0.003(8) 0.002(8) -0.001(8) C5 0.023(8) 0.018(8) 0.033(9) 0.000(7) -0.001(7) 0.005(6) C6 0.049(12) 0.022(9) 0.062(14) -0.010(9) -0.011(10) -0.009(9) C7 0.043(12) 0.041(11) 0.042(11) 0.010(9) -0.020(9) -0.008(9) C8 0.029(10) 0.052(12) 0.038(11) 0.013(9) -0.002(8) -0.005(9) C9 0.058(13) 0.024(10) 0.042(11) -0.007(8) 0.009(10) 0.003(9) C10 0.025(9) 0.030(9) 0.036(10) 0.010(8) -0.007(7) -0.006(7) C11 0.036(9) 0.014(7) 0.029(9) 0.007(6) -0.011(7) -0.015(7) C12 0.046(12) 0.035(10) 0.038(10) 0.008(8) -0.012(9) -0.016(9) C13 0.062(15) 0.029(10) 0.055(13) 0.005(9) -0.030(12) -0.010(10) C14 0.09(2) 0.057(15) 0.042(13) -0.009(11) -0.034(13) 0.033(14) C15 0.037(11) 0.057(14) 0.045(12) -0.021(10) -0.012(9) 0.003(10) C16 0.029(10) 0.040(11) 0.042(11) -0.009(9) -0.013(8) 0.005(8) C17 0.008(7) 0.033(9) 0.052(11) 0.006(8) -0.007(7) -0.001(7) C18 0.032(10) 0.020(8) 0.041(10) 0.007(7) -0.016(8) -0.014(7) C19 0.036(10) 0.034(10) 0.031(10) 0.005(8) -0.009(8) -0.005(8) C20 0.032(10) 0.052(12) 0.038(11) -0.001(9) -0.013(8) -0.010(9) C21 0.015(8) 0.019(8) 0.041(10) -0.005(7) 0.001(7) -0.010(6) C22 0.036(10) 0.053(12) 0.024(9) 0.005(8) -0.006(8) -0.029(9) C23 0.046(12) 0.063(14) 0.042(11) 0.009(10) -0.008(9) -0.047(11) C24 0.033(10) 0.028(10) 0.053(12) -0.005(8) 0.010(9) -0.016(8) C25 0.063(15) 0.037(12) 0.044(12) 0.014(9) 0.001(11) -0.002(10) C26 0.023(9) 0.026(9) 0.039(10) 0.001(7) -0.007(7) -0.005(7) C27 0.019(8) 0.028(9) 0.036(10) -0.002(7) -0.013(7) 0.003(7) C28 0.036(11) 0.042(11) 0.040(11) -0.008(9) -0.004(9) -0.014(9) C29 0.019(9) 0.049(12) 0.059(13) 0.012(10) 0.005(9) -0.012(8) C30 0.038(11) 0.044(12) 0.038(11) 0.000(9) 0.001(9) 0.000(9) C31 0.020(9) 0.045(12) 0.059(13) -0.021(10) 0.003(9) 0.009(8) C32 0.043(11) 0.030(10) 0.031(10) 0.004(8) -0.006(8) -0.009(8) C33 0.036(11) 0.039(11) 0.047(12) -0.009(9) 0.004(9) -0.017(9) C34 0.038(11) 0.024(10) 0.068(14) -0.003(9) -0.011(10) 0.000(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.083(14) . ? Ni1 N2 2.098(14) . ? Ni1 Cl1 2.402(5) . ? Ni1 P1 2.439(5) . ? Ni1 Cl2 2.444(5) . ? Ni1 P2 2.499(5) . ? P1 C5 1.819(17) . ? P1 C11 1.824(17) . ? P1 C1 1.845(19) . ? P2 C21 1.812(16) . ? P2 C27 1.834(18) . ? P2 C17 1.858(17) . ? N1 C2 1.26(2) . ? N1 C3 1.48(2) . ? N2 C18 1.29(2) . ? N2 C19 1.49(2) . ? Cl3 C33 1.72(2) . ? Cl4 C33 1.76(2) . ? Cl5 C33 1.77(2) . ? Cl6 C34 1.78(2) . ? Cl7 C34 1.76(2) . ? Cl8 C34 1.78(2) . ? O1 C2 1.35(2) . ? O1 C4 1.47(2) . ? O2 C18 1.34(2) . ? O2 C20 1.49(2) . ? C1 C2 1.52(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 C4 1.53(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.37(3) . ? C5 C10 1.39(2) . ? C6 C7 1.41(3) . ? C6 H6 0.9300 . ? C7 C8 1.41(3) . ? C7 H7 0.9300 . ? C8 C9 1.38(3) . ? C8 H8 0.9300 . ? C9 C10 1.41(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C16 1.38(3) . ? C11 C12 1.40(2) . ? C12 C13 1.34(3) . ? C12 H12 0.9300 . ? C13 C14 1.38(4) . ? C13 H13 0.9300 . ? C14 C15 1.37(4) . ? C14 H14 0.9300 . ? C15 C16 1.33(3) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.44(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C19 C20 1.58(2) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.38(2) . ? C21 C26 1.41(2) . ? C22 C23 1.38(3) . ? C22 H22 0.9300 . ? C23 C24 1.36(3) . ? C23 H23 0.9300 . ? C24 C25 1.34(3) . ? C24 H24 0.9300 . ? C25 C26 1.46(3) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C32 1.37(2) . ? C27 C28 1.44(3) . ? C28 C29 1.35(3) . ? C28 H28 0.9300 . ? C29 C30 1.32(3) . ? C29 H29 0.9300 . ? C30 C31 1.48(3) . ? C30 H30 0.9300 . ? C31 C32 1.37(3) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 H33 0.9800 . ? C34 H34 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 91.8(6) . . ? N1 Ni1 Cl1 177.5(5) . . ? N2 Ni1 Cl1 90.6(4) . . ? N1 Ni1 P1 78.0(5) . . ? N2 Ni1 P1 169.7(4) . . ? Cl1 Ni1 P1 99.56(17) . . ? N1 Ni1 Cl2 88.6(4) . . ? N2 Ni1 Cl2 92.6(4) . . ? Cl1 Ni1 Cl2 90.73(16) . . ? P1 Ni1 Cl2 88.95(16) . . ? N1 Ni1 P2 93.8(4) . . ? N2 Ni1 P2 78.4(4) . . ? Cl1 Ni1 P2 87.28(16) . . ? P1 Ni1 P2 100.26(16) . . ? Cl2 Ni1 P2 170.77(17) . . ? C5 P1 C11 103.8(7) . . ? C5 P1 C1 104.2(8) . . ? C11 P1 C1 104.5(8) . . ? C5 P1 Ni1 126.4(6) . . ? C11 P1 Ni1 117.8(5) . . ? C1 P1 Ni1 96.8(6) . . ? C21 P2 C27 103.7(8) . . ? C21 P2 C17 104.5(8) . . ? C27 P2 C17 101.7(8) . . ? C21 P2 Ni1 116.1(5) . . ? C27 P2 Ni1 131.2(6) . . ? C17 P2 Ni1 94.7(6) . . ? C2 N1 C3 106.5(14) . . ? C2 N1 Ni1 119.5(12) . . ? C3 N1 Ni1 131.6(12) . . ? C18 N2 C19 108.9(14) . . ? C18 N2 Ni1 118.4(12) . . ? C19 N2 Ni1 129.6(11) . . ? C2 O1 C4 104.9(13) . . ? C18 O2 C20 107.8(14) . . ? C2 C1 P1 104.5(11) . . ? C2 C1 H1A 110.9 . . ? P1 C1 H1A 110.9 . . ? C2 C1 H1B 110.9 . . ? P1 C1 H1B 110.9 . . ? H1A C1 H1B 108.9 . . ? N1 C2 O1 119.8(15) . . ? N1 C2 C1 125.4(15) . . ? O1 C2 C1 114.7(14) . . ? N1 C3 C4 104.6(15) . . ? N1 C3 H3A 110.8 . . ? C4 C3 H3A 110.8 . . ? N1 C3 H3B 110.8 . . ? C4 C3 H3B 110.8 . . ? H3A C3 H3B 108.9 . . ? O1 C4 C3 104.0(14) . . ? O1 C4 H4A 111.0 . . ? C3 C4 H4A 111.0 . . ? O1 C4 H4B 111.0 . . ? C3 C4 H4B 111.0 . . ? H4A C4 H4B 109.0 . . ? C6 C5 C10 119.7(16) . . ? C6 C5 P1 122.6(14) . . ? C10 C5 P1 117.6(13) . . ? C5 C6 C7 123.6(17) . . ? C5 C6 H6 118.2 . . ? C7 C6 H6 118.2 . . ? C8 C7 C6 115.5(18) . . ? C8 C7 H7 122.3 . . ? C6 C7 H7 122.3 . . ? C9 C8 C7 122.1(18) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C8 C9 C10 120.4(19) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C5 C10 C9 118.5(17) . . ? C5 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C16 C11 C12 116.5(17) . . ? C16 C11 P1 117.8(13) . . ? C12 C11 P1 125.5(15) . . ? C13 C12 C11 122(2) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 119(2) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C15 C14 C13 122(2) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C16 C15 C14 118(2) . . ? C16 C15 H15 121.0 . . ? C14 C15 H15 121.0 . . ? C15 C16 C11 123(2) . . ? C15 C16 H16 118.3 . . ? C11 C16 H16 118.3 . . ? C18 C17 P2 108.5(11) . . ? C18 C17 H17A 110.0 . . ? P2 C17 H17A 110.0 . . ? C18 C17 H17B 110.0 . . ? P2 C17 H17B 110.0 . . ? H17A C17 H17B 108.4 . . ? N2 C18 O2 116.2(16) . . ? N2 C18 C17 126.4(15) . . ? O2 C18 C17 117.3(15) . . ? N2 C19 C20 102.0(14) . . ? N2 C19 H19A 111.4 . . ? C20 C19 H19A 111.4 . . ? N2 C19 H19B 111.4 . . ? C20 C19 H19B 111.4 . . ? H19A C19 H19B 109.2 . . ? O2 C20 C19 102.2(14) . . ? O2 C20 H20A 111.3 . . ? C19 C20 H20A 111.3 . . ? O2 C20 H20B 111.3 . . ? C19 C20 H20B 111.3 . . ? H20A C20 H20B 109.2 . . ? C22 C21 C26 116.7(15) . . ? C22 C21 P2 120.0(14) . . ? C26 C21 P2 123.2(12) . . ? C21 C22 C23 122.4(17) . . ? C21 C22 H22 118.8 . . ? C23 C22 H22 118.8 . . ? C24 C23 C22 120.7(17) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C25 C24 C23 120.9(18) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 119.3(19) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C21 C26 C25 119.9(17) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C32 C27 C28 117.8(17) . . ? C32 C27 P2 124.0(14) . . ? C28 C27 P2 118.1(13) . . ? C29 C28 C27 119.6(18) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C30 C29 C28 122.9(19) . . ? C30 C29 H29 118.5 . . ? C28 C29 H29 118.5 . . ? C29 C30 C31 120.2(18) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C32 C31 C30 115.9(18) . . ? C32 C31 H31 122.0 . . ? C30 C31 H31 122.0 . . ? C27 C32 C31 123.3(18) . . ? C27 C32 H32 118.4 . . ? C31 C32 H32 118.4 . . ? Cl3 C33 Cl4 111.0(11) . . ? Cl3 C33 Cl5 110.8(11) . . ? Cl4 C33 Cl5 108.8(12) . . ? Cl3 C33 H33 108.7 . . ? Cl4 C33 H33 108.7 . . ? Cl5 C33 H33 108.7 . . ? Cl7 C34 Cl6 109.3(12) . . ? Cl7 C34 Cl8 108.8(10) . . ? Cl6 C34 Cl8 108.8(12) . . ? Cl7 C34 H34 109.9 . . ? Cl6 C34 H34 109.9 . . ? Cl8 C34 H34 109.9 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 2.130 _refine_diff_density_min -1.139 _refine_diff_density_rms 0.244 data_compound4 _database_code_depnum_ccdc_archive 'CCDC 831827' #TrackingRef 'Allcifs.cif' _ccdc_journal_manuscript_code DaltonTrans _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C32 H32 Cl2 N2 Ni O4 P2, 4(C H Cl3)' _chemical_formula_sum 'C36 H36 Cl14 N2 Ni O4 P2' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 173(2) _chemical_formula_weight 1177.6909 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 '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' Cl Cl 0.1484 0.1585 '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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2269(4) _cell_length_b 10.5261(4) _cell_length_c 13.0935(6) _cell_angle_alpha 66.761(2) _cell_angle_beta 69.761(2) _cell_angle_gamma 80.429(2) _cell_volume 1214.46(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4562 _cell_measurement_theta_min 0.98 _cell_measurement_theta_max 26.44 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 594 _exptl_absorpt_coefficient_mu 1.274 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7694 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0422 _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 -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5547 _reflns_number_gt 4311 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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^)+(0.0567P)^2^+1.5024P] 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 5547 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1279 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.5000 0.0000 1.0000 0.01898(13) Uani 1 2 d S . . N1 N 0.6916(2) -0.0995(2) 0.9889(2) 0.0214(5) Uani 1 1 d . . . O1 O 0.49748(19) 0.03758(19) 1.14538(16) 0.0230(4) Uani 1 1 d . . . O2 O 0.9061(2) -0.1581(2) 1.0064(2) 0.0310(5) Uani 1 1 d . . . Cl1 Cl 0.60633(7) 0.22438(7) 0.87316(6) 0.02623(16) Uani 1 1 d . . . Cl2 Cl 0.21627(16) -0.00907(17) 1.41615(13) 0.0865(4) Uani 1 1 d . . . Cl3 Cl 0.20012(17) -0.29431(14) 1.44872(11) 0.0914(5) Uani 1 1 d . . . Cl4 Cl 0.05415(12) -0.08207(15) 1.30821(12) 0.0736(3) Uani 1 1 d . . . Cl5 Cl -0.05131(10) -0.38986(11) 1.27471(10) 0.0554(3) Uani 1 1 d . . . Cl6 Cl 0.14521(14) -0.61973(17) 1.31491(13) 0.1033(6) Uani 1 1 d . . . Cl7 Cl 0.16249(11) -0.44035(10) 1.08123(9) 0.0525(2) Uani 1 1 d . . . P1 P 0.62176(7) 0.03817(7) 1.18047(6) 0.02101(16) Uani 1 1 d . . . C1 C 0.7883(3) -0.0783(3) 1.0199(2) 0.0218(5) Uani 1 1 d . . . C2 C 0.7393(3) -0.2123(3) 0.9435(3) 0.0268(6) Uani 1 1 d . . . H2A H 0.7489 -0.1796 0.8610 0.032 Uiso 1 1 calc R . . H2B H 0.6750 -0.2875 0.9857 0.032 Uiso 1 1 calc R . . C3 C 0.8811(3) -0.2583(3) 0.9644(3) 0.0350(7) Uani 1 1 d . . . H3A H 0.8781 -0.3512 1.0224 0.042 Uiso 1 1 calc R . . H3B H 0.9534 -0.2562 0.8925 0.042 Uiso 1 1 calc R . . C4 C 0.7850(3) 0.0292(3) 1.0673(3) 0.0256(6) Uani 1 1 d . . . H4A H 0.7993 0.1185 1.0038 0.031 Uiso 1 1 calc R . . H4B H 0.8614 0.0105 1.0996 0.031 Uiso 1 1 calc R . . C5 C 0.6326(3) 0.1959(3) 1.1987(2) 0.0258(6) Uani 1 1 d . . . C6 C 0.5368(3) 0.3028(3) 1.1673(3) 0.0312(6) Uani 1 1 d . . . H6 H 0.4667 0.2886 1.1432 0.037 Uiso 1 1 calc R . . C7 C 0.5461(4) 0.4301(3) 1.1717(3) 0.0394(8) Uani 1 1 d . . . H7 H 0.4822 0.5015 1.1509 0.047 Uiso 1 1 calc R . . C8 C 0.6509(4) 0.4506(3) 1.2073(3) 0.0418(8) Uani 1 1 d . . . H8 H 0.6572 0.5360 1.2104 0.050 Uiso 1 1 calc R . . C9 C 0.7466(4) 0.3446(4) 1.2385(3) 0.0419(8) Uani 1 1 d . . . H9 H 0.8163 0.3590 1.2629 0.050 Uiso 1 1 calc R . . C10 C 0.7387(3) 0.2177(3) 1.2335(3) 0.0330(7) Uani 1 1 d . . . H10 H 0.8039 0.1472 1.2531 0.040 Uiso 1 1 calc R . . C11 C 0.6231(3) -0.1070(3) 1.3118(2) 0.0241(6) Uani 1 1 d . . . C12 C 0.6095(3) -0.2368(3) 1.3115(3) 0.0316(7) Uani 1 1 d . . . H12 H 0.6003 -0.2444 1.2459 0.038 Uiso 1 1 calc R . . C13 C 0.6100(4) -0.3543(3) 1.4095(3) 0.0361(7) Uani 1 1 d . . . H13 H 0.6035 -0.4409 1.4087 0.043 Uiso 1 1 calc R . . C14 C 0.6201(3) -0.3436(3) 1.5078(3) 0.0356(7) Uani 1 1 d . . . H14 H 0.6218 -0.4229 1.5727 0.043 Uiso 1 1 calc R . . C15 C 0.6278(4) -0.2156(4) 1.5101(3) 0.0398(8) Uani 1 1 d . . . H15 H 0.6318 -0.2086 1.5776 0.048 Uiso 1 1 calc R . . C16 C 0.6297(3) -0.0970(3) 1.4126(3) 0.0330(7) Uani 1 1 d . . . H16 H 0.6353 -0.0108 1.4147 0.040 Uiso 1 1 calc R . . C17 C 0.2040(4) -0.1225(4) 1.3524(3) 0.0439(8) Uani 1 1 d . . . H17 H 0.2858 -0.1123 1.2833 0.053 Uiso 1 1 calc R . . C18 C 0.1213(4) -0.4478(4) 1.2253(3) 0.0439(8) Uani 1 1 d . . . H18 H 0.1842 -0.3890 1.2278 0.053 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 0.0175(2) 0.0199(2) 0.0217(3) -0.00938(19) -0.00674(19) -0.00010(18) N1 0.0185(10) 0.0227(11) 0.0234(11) -0.0097(9) -0.0055(9) -0.0001(9) O1 0.0221(9) 0.0260(10) 0.0232(10) -0.0108(8) -0.0074(8) -0.0012(8) O2 0.0213(10) 0.0321(11) 0.0471(13) -0.0215(10) -0.0141(9) 0.0052(8) Cl1 0.0257(3) 0.0224(3) 0.0287(4) -0.0078(3) -0.0065(3) -0.0039(3) Cl2 0.0899(9) 0.1120(11) 0.0816(9) -0.0694(9) -0.0048(7) -0.0261(8) Cl3 0.1014(10) 0.0652(8) 0.0581(7) 0.0046(6) -0.0018(7) 0.0062(7) Cl4 0.0528(6) 0.0943(9) 0.0839(9) -0.0417(7) -0.0254(6) 0.0034(6) Cl5 0.0470(5) 0.0587(6) 0.0607(6) -0.0290(5) -0.0087(5) -0.0014(4) Cl6 0.0608(7) 0.0999(11) 0.0794(9) 0.0320(8) -0.0204(7) 0.0105(7) Cl7 0.0564(6) 0.0562(6) 0.0471(5) -0.0235(4) -0.0105(4) -0.0078(4) P1 0.0215(3) 0.0202(3) 0.0236(4) -0.0090(3) -0.0081(3) -0.0017(3) C1 0.0158(12) 0.0243(13) 0.0233(13) -0.0081(11) -0.0042(10) -0.0006(10) C2 0.0246(14) 0.0273(14) 0.0340(16) -0.0174(12) -0.0099(12) 0.0031(11) C3 0.0256(15) 0.0336(16) 0.056(2) -0.0266(15) -0.0145(14) 0.0041(13) C4 0.0200(13) 0.0301(14) 0.0305(15) -0.0138(12) -0.0074(11) -0.0045(11) C5 0.0292(14) 0.0231(13) 0.0260(14) -0.0097(11) -0.0066(12) -0.0050(11) C6 0.0337(16) 0.0251(14) 0.0331(16) -0.0107(12) -0.0086(13) -0.0004(12) C7 0.050(2) 0.0240(15) 0.0355(18) -0.0112(13) -0.0046(15) 0.0024(14) C8 0.062(2) 0.0291(16) 0.0320(17) -0.0169(13) 0.0010(16) -0.0141(16) C9 0.051(2) 0.0428(19) 0.0386(19) -0.0191(15) -0.0091(16) -0.0188(16) C10 0.0338(16) 0.0318(16) 0.0359(17) -0.0136(13) -0.0102(13) -0.0057(13) C11 0.0232(13) 0.0252(13) 0.0253(14) -0.0098(11) -0.0088(11) -0.0003(11) C12 0.0438(18) 0.0277(15) 0.0237(15) -0.0090(12) -0.0087(13) -0.0075(13) C13 0.0489(19) 0.0243(14) 0.0297(16) -0.0065(12) -0.0072(14) -0.0065(14) C14 0.0417(18) 0.0319(16) 0.0259(16) -0.0041(12) -0.0090(14) -0.0021(14) C15 0.056(2) 0.0398(18) 0.0278(16) -0.0101(14) -0.0192(15) -0.0041(16) C16 0.0458(18) 0.0286(15) 0.0305(16) -0.0124(13) -0.0166(14) -0.0016(13) C17 0.044(2) 0.047(2) 0.0368(19) -0.0165(16) -0.0041(15) -0.0075(16) C18 0.0360(18) 0.054(2) 0.0383(19) -0.0074(16) -0.0116(15) -0.0149(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.049(2) . ? Ni1 N1 2.049(2) 2_657 ? Ni1 O1 2.0826(19) 2_657 ? Ni1 O1 2.0827(19) . ? Ni1 Cl1 2.4553(7) 2_657 ? Ni1 Cl1 2.4553(7) . ? N1 C1 1.271(3) . ? N1 C2 1.471(3) . ? O1 P1 1.495(2) . ? O2 C1 1.349(3) . ? O2 C3 1.457(4) . ? Cl2 C17 1.745(4) . ? Cl3 C17 1.747(4) . ? Cl4 C17 1.751(4) . ? Cl5 C18 1.752(4) . ? Cl6 C18 1.757(4) . ? Cl7 C18 1.757(4) . ? P1 C5 1.794(3) . ? P1 C11 1.797(3) . ? P1 C4 1.827(3) . ? C1 C4 1.481(4) . ? C2 C3 1.533(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.394(4) . ? C5 C10 1.395(4) . ? C6 C7 1.385(4) . ? C6 H6 0.9300 . ? C7 C8 1.383(5) . ? C7 H7 0.9300 . ? C8 C9 1.387(5) . ? C8 H8 0.9300 . ? C9 C10 1.379(4) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C16 1.389(4) . ? C11 C12 1.398(4) . ? C12 C13 1.388(4) . ? C12 H12 0.9300 . ? C13 C14 1.375(5) . ? C13 H13 0.9300 . ? C14 C15 1.375(5) . ? C14 H14 0.9300 . ? C15 C16 1.387(4) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 H17 0.9800 . ? C18 H18 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N1 180.0 . 2_657 ? N1 Ni1 O1 88.31(8) . 2_657 ? N1 Ni1 O1 91.69(8) 2_657 2_657 ? N1 Ni1 O1 91.69(8) . . ? N1 Ni1 O1 88.31(8) 2_657 . ? O1 Ni1 O1 180.0 2_657 . ? N1 Ni1 Cl1 88.27(6) . 2_657 ? N1 Ni1 Cl1 91.73(7) 2_657 2_657 ? O1 Ni1 Cl1 89.42(6) 2_657 2_657 ? O1 Ni1 Cl1 90.58(6) . 2_657 ? N1 Ni1 Cl1 91.73(7) . . ? N1 Ni1 Cl1 88.27(7) 2_657 . ? O1 Ni1 Cl1 90.58(6) 2_657 . ? O1 Ni1 Cl1 89.42(6) . . ? Cl1 Ni1 Cl1 179.999(1) 2_657 . ? C1 N1 C2 108.0(2) . . ? C1 N1 Ni1 127.62(19) . . ? C2 N1 Ni1 124.32(17) . . ? P1 O1 Ni1 126.15(11) . . ? C1 O2 C3 106.0(2) . . ? O1 P1 C5 112.73(12) . . ? O1 P1 C11 110.96(12) . . ? C5 P1 C11 109.93(13) . . ? O1 P1 C4 111.82(12) . . ? C5 P1 C4 103.49(13) . . ? C11 P1 C4 107.56(13) . . ? N1 C1 O2 117.7(2) . . ? N1 C1 C4 125.7(2) . . ? O2 C1 C4 116.6(2) . . ? N1 C2 C3 103.5(2) . . ? N1 C2 H2A 111.1 . . ? C3 C2 H2A 111.1 . . ? N1 C2 H2B 111.1 . . ? C3 C2 H2B 111.1 . . ? H2A C2 H2B 109.0 . . ? O2 C3 C2 104.3(2) . . ? O2 C3 H3A 110.9 . . ? C2 C3 H3A 110.9 . . ? O2 C3 H3B 110.9 . . ? C2 C3 H3B 110.9 . . ? H3A C3 H3B 108.9 . . ? C1 C4 P1 113.49(19) . . ? C1 C4 H4A 108.9 . . ? P1 C4 H4A 108.9 . . ? C1 C4 H4B 108.9 . . ? P1 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C10 119.9(3) . . ? C6 C5 P1 117.4(2) . . ? C10 C5 P1 122.4(2) . . ? C7 C6 C5 120.0(3) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C6 119.7(3) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 120.5(3) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 120.2(3) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C5 119.7(3) . . ? C9 C10 H10 120.2 . . ? C5 C10 H10 120.2 . . ? C16 C11 C12 119.3(3) . . ? C16 C11 P1 124.5(2) . . ? C12 C11 P1 116.0(2) . . ? C13 C12 C11 119.6(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C12 120.6(3) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 120.0(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 120.5(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 120.0(3) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? Cl2 C17 Cl3 111.4(2) . . ? Cl2 C17 Cl4 110.3(2) . . ? Cl3 C17 Cl4 109.4(2) . . ? Cl2 C17 H17 108.5 . . ? Cl3 C17 H17 108.5 . . ? Cl4 C17 H17 108.5 . . ? Cl5 C18 Cl7 110.6(2) . . ? Cl5 C18 Cl6 110.2(2) . . ? Cl7 C18 Cl6 108.5(2) . . ? Cl5 C18 H18 109.2 . . ? Cl7 C18 H18 109.2 . . ? Cl6 C18 H18 109.2 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.920 _refine_diff_density_min -1.214 _refine_diff_density_rms 0.088