Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Douglas W. Stephan' 'Katie T. K. Chan' 'Pingrong Wei' _publ_contact_author_name 'Prof Douglas W. Stephan' _publ_contact_author_address ; Department of Chemistry & Biochemistry University of Windsor 401 Sunset Windsor Ontario N9B3P4 CANADA ; _publ_contact_author_email STEPHAN@UWINDSOR.CA _publ_section_title ; Metallated Triphenylphosphinimine Complexes ; data_(o-C6H4PPh2NSiMe3)BCl2 _database_code_CSD 211243 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C21 H23 B Cl2 N P Si' _chemical_formula_weight 430.17 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' _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 9.264(6) _cell_length_b 14.245(8) _cell_length_c 17.380(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.035(11) _cell_angle_gamma 90.00 _cell_volume 2293(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.411 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.729405 _exptl_absorpt_correction_T_max 1.000000 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 9762 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0821 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 23.34 _reflns_number_total 3289 _reflns_number_gt 1835 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0337P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3289 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0975 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 B1 B -0.0207(5) 0.0380(3) 0.1701(2) 0.0438(12) Uani 1 1 d . . . Cl1 Cl -0.15394(11) -0.06075(7) 0.14836(5) 0.0635(3) Uani 1 1 d . . . Cl2 Cl -0.09266(12) 0.14640(7) 0.12207(6) 0.0685(3) Uani 1 1 d . . . P1 P 0.14931(10) 0.01045(6) 0.28859(5) 0.0377(3) Uani 1 1 d . . . N1 N -0.0048(3) 0.05180(17) 0.25966(13) 0.0387(7) Uani 1 1 d . . . Si1 Si -0.13269(13) 0.11275(8) 0.31758(6) 0.0607(4) Uani 1 1 d . . . C1 C 0.1356(4) 0.0091(2) 0.13945(18) 0.0369(9) Uani 1 1 d . . . C2 C 0.2351(4) -0.0084(2) 0.19786(17) 0.0363(9) Uani 1 1 d . . . C3 C 0.3758(4) -0.0391(2) 0.1834(2) 0.0476(10) Uani 1 1 d . . . H3A H 0.4393 -0.0505 0.2238 0.057 Uiso 1 1 calc R . . C4 C 0.4189(4) -0.0521(3) 0.1078(2) 0.0515(10) Uani 1 1 d . . . H4A H 0.5125 -0.0717 0.0969 0.062 Uiso 1 1 calc R . . C5 C 0.3220(5) -0.0359(2) 0.0488(2) 0.0529(11) Uani 1 1 d . . . H5A H 0.3508 -0.0455 -0.0018 0.063 Uiso 1 1 calc R . . C6 C 0.1827(4) -0.0056(3) 0.06363(18) 0.0501(10) Uani 1 1 d . . . H6A H 0.1196 0.0051 0.0229 0.060 Uiso 1 1 calc R . . C7 C 0.1324(4) -0.0997(2) 0.33897(17) 0.0397(9) Uani 1 1 d . . . C8 C -0.0012(5) -0.1435(3) 0.3434(2) 0.0564(11) Uani 1 1 d . . . H8A H -0.0822 -0.1142 0.3227 0.068 Uiso 1 1 calc R . . C9 C -0.0154(6) -0.2313(3) 0.3785(2) 0.0779(14) Uani 1 1 d . . . H9A H -0.1054 -0.2601 0.3810 0.093 Uiso 1 1 calc R . . C10 C 0.1031(7) -0.2750(3) 0.4093(2) 0.0779(15) Uani 1 1 d . . . H10A H 0.0931 -0.3325 0.4340 0.093 Uiso 1 1 calc R . . C11 C 0.2354(6) -0.2343(3) 0.4036(2) 0.0689(13) Uani 1 1 d . . . H11A H 0.3158 -0.2652 0.4232 0.083 Uiso 1 1 calc R . . C12 C 0.2518(4) -0.1466(3) 0.3689(2) 0.0569(11) Uani 1 1 d . . . H12A H 0.3429 -0.1195 0.3657 0.068 Uiso 1 1 calc R . . C13 C 0.2524(4) 0.0913(2) 0.34597(18) 0.0398(10) Uani 1 1 d . . . C14 C 0.2842(5) 0.0770(3) 0.4236(2) 0.0710(13) Uani 1 1 d . . . H14A H 0.2565 0.0217 0.4479 0.085 Uiso 1 1 calc R . . C15 C 0.3576(5) 0.1458(4) 0.4639(2) 0.0885(16) Uani 1 1 d . . . H15A H 0.3792 0.1362 0.5156 0.106 Uiso 1 1 calc R . . C16 C 0.3986(5) 0.2274(3) 0.4293(3) 0.0755(14) Uani 1 1 d . . . H16A H 0.4456 0.2736 0.4577 0.091 Uiso 1 1 calc R . . C17 C 0.3709(4) 0.2414(3) 0.3530(3) 0.0637(12) Uani 1 1 d . . . H17A H 0.4012 0.2963 0.3289 0.076 Uiso 1 1 calc R . . C18 C 0.2977(4) 0.1738(3) 0.3120(2) 0.0509(11) Uani 1 1 d . . . H18A H 0.2782 0.1839 0.2602 0.061 Uiso 1 1 calc R . . C19 C -0.1068(5) 0.0804(4) 0.4203(2) 0.1071(19) Uani 1 1 d . . . H19A H -0.0118 0.0985 0.4366 0.161 Uiso 1 1 calc R . . H19B H -0.1180 0.0138 0.4262 0.161 Uiso 1 1 calc R . . H19C H -0.1774 0.1122 0.4513 0.161 Uiso 1 1 calc R . . C20 C -0.3177(5) 0.0762(4) 0.2908(3) 0.1087(18) Uani 1 1 d . . . H20A H -0.3355 0.0920 0.2379 0.163 Uiso 1 1 calc R . . H20B H -0.3862 0.1080 0.3230 0.163 Uiso 1 1 calc R . . H20C H -0.3273 0.0096 0.2975 0.163 Uiso 1 1 calc R . . C21 C -0.1075(5) 0.2393(3) 0.3080(3) 0.117(2) Uani 1 1 d . . . H21A H -0.1224 0.2573 0.2553 0.175 Uiso 1 1 calc R . . H21B H -0.0112 0.2557 0.3234 0.175 Uiso 1 1 calc R . . H21C H -0.1757 0.2714 0.3402 0.175 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 B1 0.047(3) 0.042(3) 0.042(2) 0.004(2) -0.002(2) -0.002(2) Cl1 0.0455(8) 0.0796(8) 0.0655(6) -0.0069(6) -0.0064(5) -0.0175(6) Cl2 0.0579(8) 0.0791(8) 0.0684(7) 0.0253(6) -0.0027(6) 0.0149(6) P1 0.0333(7) 0.0450(6) 0.0348(5) -0.0010(5) -0.0021(4) -0.0015(5) N1 0.034(2) 0.0413(18) 0.0407(16) -0.0026(14) 0.0002(14) 0.0036(14) Si1 0.0458(9) 0.0722(9) 0.0641(7) -0.0160(6) 0.0052(6) 0.0098(6) C1 0.034(2) 0.041(2) 0.036(2) -0.0026(17) -0.0027(17) -0.0040(18) C2 0.032(2) 0.042(2) 0.0351(19) -0.0011(17) 0.0000(17) -0.0022(19) C3 0.042(3) 0.057(3) 0.044(2) 0.0004(18) -0.009(2) -0.0001(19) C4 0.034(3) 0.065(3) 0.055(3) 0.002(2) 0.010(2) 0.004(2) C5 0.051(3) 0.069(3) 0.038(2) 0.001(2) 0.008(2) -0.006(2) C6 0.046(3) 0.068(3) 0.037(2) -0.002(2) -0.0067(19) -0.009(2) C7 0.039(3) 0.043(2) 0.037(2) 0.0006(18) -0.0005(18) -0.001(2) C8 0.056(3) 0.055(3) 0.058(3) 0.007(2) -0.003(2) -0.001(2) C9 0.086(4) 0.058(3) 0.090(3) 0.011(3) 0.005(3) -0.016(3) C10 0.108(5) 0.053(3) 0.073(3) 0.014(2) 0.012(3) 0.004(3) C11 0.084(4) 0.061(3) 0.062(3) 0.011(2) 0.001(3) 0.023(3) C12 0.045(3) 0.069(3) 0.057(3) 0.008(2) 0.000(2) 0.005(2) C13 0.035(3) 0.048(3) 0.037(2) -0.0028(18) 0.0023(17) -0.0003(18) C14 0.094(4) 0.080(3) 0.039(2) 0.002(2) -0.005(2) -0.030(3) C15 0.117(5) 0.103(4) 0.045(3) -0.013(3) -0.021(3) -0.028(3) C16 0.076(4) 0.071(4) 0.079(4) -0.030(3) -0.018(3) -0.012(3) C17 0.073(3) 0.046(3) 0.072(3) -0.002(2) -0.016(3) -0.011(2) C18 0.061(3) 0.047(3) 0.044(2) -0.001(2) -0.013(2) 0.000(2) C19 0.109(5) 0.153(5) 0.060(3) -0.010(3) 0.024(3) 0.040(4) C20 0.044(4) 0.165(5) 0.117(4) -0.047(4) 0.017(3) 0.006(3) C21 0.116(5) 0.077(4) 0.156(5) -0.026(4) 0.021(4) 0.027(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 B1 N1 1.576(4) . ? B1 C1 1.597(5) . ? B1 Cl2 1.877(4) . ? B1 Cl1 1.909(4) . ? P1 N1 1.624(3) . ? P1 C2 1.787(3) . ? P1 C13 1.798(3) . ? P1 C7 1.803(4) . ? N1 Si1 1.781(3) . ? Si1 C21 1.825(5) . ? Si1 C20 1.850(4) . ? Si1 C19 1.860(4) . ? C1 C2 1.393(4) . ? C1 C6 1.404(4) . ? C2 C3 1.397(4) . ? C3 C4 1.387(4) . ? C4 C5 1.382(5) . ? C5 C6 1.385(5) . ? C7 C8 1.389(5) . ? C7 C12 1.393(5) . ? C8 C9 1.397(5) . ? C9 C10 1.371(6) . ? C10 C11 1.359(6) . ? C11 C12 1.395(5) . ? C13 C18 1.381(4) . ? C13 C14 1.395(4) . ? C14 C15 1.384(5) . ? C15 C16 1.363(6) . ? C16 C17 1.365(5) . ? C17 C18 1.377(5) . ? 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 B1 C1 106.1(3) . . ? N1 B1 Cl2 111.7(3) . . ? C1 B1 Cl2 112.7(3) . . ? N1 B1 Cl1 110.3(2) . . ? C1 B1 Cl1 109.3(3) . . ? Cl2 B1 Cl1 106.8(2) . . ? N1 P1 C2 99.96(15) . . ? N1 P1 C13 113.95(15) . . ? C2 P1 C13 110.46(16) . . ? N1 P1 C7 112.92(16) . . ? C2 P1 C7 109.66(15) . . ? C13 P1 C7 109.52(16) . . ? B1 N1 P1 110.0(2) . . ? B1 N1 Si1 123.9(2) . . ? P1 N1 Si1 125.94(15) . . ? N1 Si1 C21 110.16(18) . . ? N1 Si1 C20 109.68(17) . . ? C21 Si1 C20 111.9(2) . . ? N1 Si1 C19 109.68(17) . . ? C21 Si1 C19 108.4(2) . . ? C20 Si1 C19 106.9(2) . . ? C2 C1 C6 116.8(3) . . ? C2 C1 B1 113.8(3) . . ? C6 C1 B1 129.3(3) . . ? C1 C2 C3 122.8(3) . . ? C1 C2 P1 108.8(3) . . ? C3 C2 P1 128.4(3) . . ? C4 C3 C2 118.8(3) . . ? C5 C4 C3 119.5(4) . . ? C4 C5 C6 121.3(3) . . ? C5 C6 C1 120.7(3) . . ? C8 C7 C12 118.1(3) . . ? C8 C7 P1 119.7(3) . . ? C12 C7 P1 122.0(3) . . ? C7 C8 C9 120.7(4) . . ? C10 C9 C8 120.1(5) . . ? C11 C10 C9 120.0(5) . . ? C10 C11 C12 120.8(4) . . ? C7 C12 C11 120.3(4) . . ? C18 C13 C14 118.3(3) . . ? C18 C13 P1 118.0(3) . . ? C14 C13 P1 123.7(3) . . ? C15 C14 C13 119.3(4) . . ? C16 C15 C14 121.2(4) . . ? C15 C16 C17 120.1(4) . . ? C16 C17 C18 119.5(4) . . ? C17 C18 C13 121.6(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 23.34 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.254 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.049 #===end data_(o-C6H4PPh2NSiMe3)AlMe2//(o-C6H4PPh2NSiMe3)Al(Me)Cl _database_code_CSD 211244 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C45 H54 Al2 C21 N2 P2 Si2' _chemical_formula_weight 831.44 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' Al Al 0.0645 0.0514 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 20.492(12) _cell_length_b 9.113(5) _cell_length_c 26.214(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4895(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.259 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.143729 _exptl_absorpt_correction_T_max 0.256552 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 19914 _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_sigmaI/netI 0.0950 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 23.18 _reflns_number_total 5764 _reflns_number_gt 3468 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1134P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.23(16) _refine_ls_number_reflns 5764 _refine_ls_number_parameters 487 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1590 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 0.818 _refine_ls_restrained_S_all 0.818 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 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 Al1 Al 0.34857(13) 0.1452(3) 0.43732(12) 0.0773(8) Uani 1 1 d . . . Al2 Al -0.01945(11) 0.6177(2) 0.13952(10) 0.0586(6) Uani 1 1 d . . . N1 N 0.2776(3) 0.2577(5) 0.4082(2) 0.0494(14) Uani 1 1 d . . . N2 N 0.0543(2) 0.7018(5) 0.1764(2) 0.0477(15) Uani 1 1 d . . . P1 P 0.29141(8) 0.43078(18) 0.40825(7) 0.0415(4) Uani 1 1 d . . . P2 P 0.04643(8) 0.87446(17) 0.18603(7) 0.0414(4) Uani 1 1 d . . . Si1 Si 0.20157(12) 0.1776(3) 0.38859(10) 0.0733(7) Uani 1 1 d . . . Si2 Si 0.12392(10) 0.5950(2) 0.19197(10) 0.0643(6) Uani 1 1 d . . . Cl1 Cl -0.0809(2) 0.4985(4) 0.1886(2) 0.1683(15) Uani 1 1 d . . . C1 C 0.3991(3) 0.0409(7) 0.3793(3) 0.055(2) Uani 1 1 d . . . H1A H 0.4151 0.1127 0.3556 0.082 Uiso 1 1 calc R . . H1B H 0.3704 -0.0256 0.3618 0.082 Uiso 1 1 calc R . . H1C H 0.4351 -0.0127 0.3934 0.082 Uiso 1 1 calc R . . C2 C 0.3134(4) 0.0058(8) 0.4896(4) 0.081(3) Uani 1 1 d . . . H2A H 0.2906 0.0598 0.5155 0.121 Uiso 1 1 calc R . . H2B H 0.3489 -0.0474 0.5049 0.121 Uiso 1 1 calc R . . H2C H 0.2840 -0.0619 0.4736 0.121 Uiso 1 1 calc R . . C3 C 0.3943(4) 0.3295(8) 0.4618(3) 0.061(2) Uani 1 1 d . . . C4 C 0.4541(4) 0.3522(11) 0.4900(3) 0.075(2) Uani 1 1 d . . . H4A H 0.4786 0.2711 0.4997 0.090 Uiso 1 1 calc R . . C5 C 0.4753(4) 0.4871(12) 0.5025(3) 0.074(3) Uani 1 1 d . . . H5A H 0.5143 0.4964 0.5203 0.089 Uiso 1 1 calc R . . C6 C 0.4411(4) 0.6124(11) 0.4898(3) 0.075(2) Uani 1 1 d . . . H6A H 0.4563 0.7038 0.5001 0.090 Uiso 1 1 calc R . . C7 C 0.3832(4) 0.6020(9) 0.4612(3) 0.063(2) Uani 1 1 d . . . H7A H 0.3599 0.6850 0.4516 0.075 Uiso 1 1 calc R . . C8 C 0.3621(3) 0.4597(8) 0.4478(3) 0.0449(18) Uani 1 1 d . . . C9 C 0.3096(3) 0.4987(8) 0.3441(3) 0.0466(18) Uani 1 1 d . . . C10 C 0.3158(4) 0.6461(9) 0.3343(3) 0.065(2) Uani 1 1 d . . . H10A H 0.3079 0.7151 0.3597 0.078 Uiso 1 1 calc R . . C11 C 0.3348(4) 0.6909(12) 0.2843(5) 0.089(3) Uani 1 1 d . . . H11A H 0.3400 0.7903 0.2775 0.107 Uiso 1 1 calc R . . C12 C 0.3449(5) 0.5965(17) 0.2481(4) 0.092(4) Uani 1 1 d . . . H12A H 0.3562 0.6296 0.2157 0.110 Uiso 1 1 calc R . . C13 C 0.3391(4) 0.4481(15) 0.2569(4) 0.096(3) Uani 1 1 d . . . H13A H 0.3465 0.3813 0.2307 0.116 Uiso 1 1 calc R . . C14 C 0.3219(4) 0.3986(10) 0.3060(3) 0.071(2) Uani 1 1 d . . . H14A H 0.3189 0.2986 0.3127 0.085 Uiso 1 1 calc R . . C15 C 0.2243(3) 0.5362(7) 0.4352(3) 0.0475(18) Uani 1 1 d . . . C16 C 0.2135(5) 0.5178(10) 0.4874(4) 0.086(3) Uani 1 1 d . . . H16A H 0.2406 0.4555 0.5059 0.104 Uiso 1 1 calc R . . C17 C 0.1630(5) 0.5912(14) 0.5123(4) 0.108(4) Uani 1 1 d . . . H17A H 0.1571 0.5813 0.5474 0.129 Uiso 1 1 calc R . . C18 C 0.1234(5) 0.6754(12) 0.4849(5) 0.101(3) Uani 1 1 d . . . H18A H 0.0889 0.7218 0.5014 0.121 Uiso 1 1 calc R . . C19 C 0.1310(5) 0.6974(11) 0.4334(5) 0.100(3) Uani 1 1 d . . . H19A H 0.1024 0.7583 0.4157 0.119 Uiso 1 1 calc R . . C20 C 0.1830(4) 0.6259(9) 0.4073(4) 0.079(3) Uani 1 1 d . . . H20A H 0.1892 0.6392 0.3725 0.095 Uiso 1 1 calc R . . C21 C 0.1473(4) 0.1529(12) 0.4464(5) 0.109(4) Uani 1 1 d . . . H21A H 0.1373 0.2472 0.4608 0.164 Uiso 1 1 calc R . . H21B H 0.1694 0.0940 0.4713 0.164 Uiso 1 1 calc R . . H21C H 0.1075 0.1052 0.4364 0.164 Uiso 1 1 calc R . . C22 C 0.2234(5) 0.0001(9) 0.3565(5) 0.111(4) Uani 1 1 d . . . H22A H 0.2509 0.0197 0.3276 0.167 Uiso 1 1 calc R . . H22B H 0.1843 -0.0483 0.3453 0.167 Uiso 1 1 calc R . . H22C H 0.2462 -0.0618 0.3802 0.167 Uiso 1 1 calc R . . C23 C 0.1586(5) 0.2923(11) 0.3400(5) 0.118(4) Uani 1 1 d . . . H23A H 0.1461 0.3841 0.3550 0.177 Uiso 1 1 calc R . . H23B H 0.1204 0.2416 0.3282 0.177 Uiso 1 1 calc R . . H23C H 0.1873 0.3102 0.3117 0.177 Uiso 1 1 calc R . . C24 C 0.0056(4) 0.5014(8) 0.0784(3) 0.061(2) Uani 1 1 d . . . H24A H 0.0338 0.5590 0.0570 0.092 Uiso 1 1 calc R . . H24B H -0.0329 0.4749 0.0597 0.092 Uiso 1 1 calc R . . H24C H 0.0281 0.4141 0.0889 0.092 Uiso 1 1 calc R . . C26 C -0.0575(3) 0.8180(7) 0.1257(3) 0.0480(18) Uani 1 1 d . . . C27 C -0.1136(4) 0.8633(10) 0.0979(3) 0.062(2) Uani 1 1 d . . . H27A H -0.1387 0.7915 0.0821 0.074 Uiso 1 1 calc R . . C28 C -0.1327(4) 1.0050(10) 0.0932(3) 0.065(2) Uani 1 1 d . . . H28A H -0.1705 1.0279 0.0752 0.078 Uiso 1 1 calc R . . C29 C -0.0964(4) 1.1136(9) 0.1147(3) 0.063(2) Uani 1 1 d . . . H29A H -0.1094 1.2108 0.1110 0.075 Uiso 1 1 calc R . . C30 C -0.0393(4) 1.0805(7) 0.1426(3) 0.057(2) Uani 1 1 d . . . H30A H -0.0145 1.1548 0.1573 0.069 Uiso 1 1 calc R . . C31 C -0.0207(3) 0.9326(7) 0.1476(3) 0.0393(15) Uani 1 1 d . . . C32 C 0.0276(3) 0.9145(7) 0.2521(3) 0.0454(18) Uani 1 1 d . . . C33 C 0.0260(4) 1.0626(10) 0.2689(3) 0.072(2) Uani 1 1 d . . . H33A H 0.0378 1.1391 0.2473 0.086 Uiso 1 1 calc R . . C34 C 0.0061(4) 1.0892(12) 0.3194(4) 0.087(3) Uani 1 1 d . . . H34A H 0.0025 1.1859 0.3304 0.104 Uiso 1 1 calc R . . C35 C -0.0084(5) 0.9785(14) 0.3534(4) 0.088(3) Uani 1 1 d . . . H35A H -0.0185 0.9986 0.3873 0.106 Uiso 1 1 calc R . . C36 C -0.0073(4) 0.8364(13) 0.3351(4) 0.081(3) Uani 1 1 d . . . H36A H -0.0181 0.7599 0.3570 0.097 Uiso 1 1 calc R . . C37 C 0.0091(4) 0.8045(8) 0.2852(3) 0.062(2) Uani 1 1 d . . . H37A H 0.0078 0.7079 0.2738 0.075 Uiso 1 1 calc R . . C38 C 0.1174(3) 0.9830(7) 0.1701(3) 0.0432(17) Uani 1 1 d . . . C39 C 0.1649(3) 1.0153(7) 0.2056(3) 0.0533(19) Uani 1 1 d . . . H39A H 0.1585 0.9888 0.2395 0.064 Uiso 1 1 calc R . . C40 C 0.2239(4) 1.0885(9) 0.1915(5) 0.090(3) Uani 1 1 d . . . H40A H 0.2564 1.1067 0.2154 0.108 Uiso 1 1 calc R . . C41 C 0.2311(4) 1.1317(10) 0.1410(4) 0.086(3) Uani 1 1 d . . . H41A H 0.2684 1.1822 0.1310 0.103 Uiso 1 1 calc R . . C42 C 0.1847(5) 1.1012(11) 0.1064(4) 0.093(3) Uani 1 1 d . . . H42A H 0.1912 1.1301 0.0728 0.112 Uiso 1 1 calc R . . C43 C 0.1264(4) 1.0267(9) 0.1192(3) 0.068(2) Uani 1 1 d . . . H43A H 0.0949 1.0071 0.0946 0.082 Uiso 1 1 calc R . . C44 C 0.0960(5) 0.4015(8) 0.1955(6) 0.118(4) Uani 1 1 d . . . H44A H 0.0624 0.3929 0.2209 0.176 Uiso 1 1 calc R . . H44B H 0.1321 0.3396 0.2045 0.176 Uiso 1 1 calc R . . H44C H 0.0789 0.3721 0.1630 0.176 Uiso 1 1 calc R . . C45 C 0.1892(5) 0.6194(13) 0.1424(5) 0.124(4) Uani 1 1 d . . . H45A H 0.1718 0.5961 0.1093 0.186 Uiso 1 1 calc R . . H45B H 0.2251 0.5552 0.1498 0.186 Uiso 1 1 calc R . . H45C H 0.2040 0.7193 0.1426 0.186 Uiso 1 1 calc R . . C46 C 0.1589(4) 0.6405(10) 0.2552(4) 0.090(3) Uani 1 1 d . . . H46A H 0.1261 0.6283 0.2810 0.136 Uiso 1 1 calc R . . H46B H 0.1738 0.7404 0.2551 0.136 Uiso 1 1 calc R . . H46C H 0.1949 0.5764 0.2622 0.136 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 Al1 0.0845(18) 0.0636(15) 0.084(2) 0.0007(15) -0.0077(16) 0.0108(14) Al2 0.0525(13) 0.0546(13) 0.0686(16) -0.0126(12) -0.0107(13) -0.0086(11) N1 0.055(3) 0.048(3) 0.045(4) -0.005(3) -0.005(3) -0.008(3) N2 0.042(3) 0.049(3) 0.053(4) -0.001(3) -0.009(3) -0.014(3) P1 0.0402(10) 0.0460(10) 0.0383(10) -0.0023(9) -0.0019(9) 0.0005(8) P2 0.0381(9) 0.0456(9) 0.0406(11) -0.0018(9) -0.0043(9) -0.0023(8) Si1 0.0755(16) 0.0707(14) 0.0736(17) 0.0006(12) -0.0097(14) -0.0153(13) Si2 0.0581(13) 0.0575(12) 0.0771(17) -0.0048(12) -0.0104(13) 0.0129(10) Cl1 0.163(3) 0.149(3) 0.192(4) 0.001(3) 0.030(3) -0.037(2) C1 0.042(4) 0.031(3) 0.091(6) -0.023(4) 0.013(4) 0.023(3) C2 0.095(7) 0.065(5) 0.082(7) 0.031(5) -0.019(6) 0.000(5) C3 0.060(5) 0.074(5) 0.047(5) 0.004(4) 0.004(4) 0.016(4) C4 0.060(6) 0.109(8) 0.056(6) 0.014(5) -0.001(5) 0.016(5) C5 0.051(6) 0.127(8) 0.044(5) 0.004(5) -0.013(4) -0.003(6) C6 0.061(6) 0.106(7) 0.058(6) -0.016(5) -0.008(5) -0.030(5) C7 0.055(5) 0.072(5) 0.061(5) -0.012(4) 0.011(4) -0.002(4) C8 0.039(4) 0.062(5) 0.034(4) -0.005(3) 0.004(3) 0.001(3) C9 0.034(4) 0.059(5) 0.047(5) -0.003(4) -0.004(4) 0.004(3) C10 0.057(5) 0.074(6) 0.063(6) 0.015(4) -0.002(4) -0.002(4) C11 0.055(6) 0.118(8) 0.095(9) 0.064(7) -0.011(6) -0.020(5) C12 0.070(7) 0.173(12) 0.033(6) 0.018(7) 0.012(5) -0.017(7) C13 0.064(6) 0.169(11) 0.057(7) -0.024(7) 0.018(5) -0.006(7) C14 0.056(5) 0.103(6) 0.054(6) -0.008(5) 0.005(4) -0.003(5) C15 0.038(4) 0.055(4) 0.049(5) 0.003(4) -0.007(4) 0.001(3) C16 0.080(7) 0.107(7) 0.072(7) -0.015(5) -0.004(6) 0.015(5) C17 0.093(8) 0.153(10) 0.077(8) -0.012(7) 0.025(7) 0.040(7) C18 0.084(7) 0.122(8) 0.096(9) -0.010(7) 0.034(7) 0.030(7) C19 0.065(6) 0.111(8) 0.123(10) 0.016(7) 0.014(7) 0.029(5) C20 0.054(5) 0.109(7) 0.074(6) 0.021(6) 0.010(5) 0.012(5) C21 0.072(6) 0.140(9) 0.116(9) -0.013(7) 0.016(7) -0.038(6) C22 0.114(8) 0.064(6) 0.155(11) -0.018(6) -0.053(8) -0.025(5) C23 0.100(8) 0.104(8) 0.150(11) 0.010(7) -0.050(8) -0.033(6) C24 0.066(5) 0.056(4) 0.061(6) -0.021(4) 0.005(4) -0.012(4) C26 0.047(4) 0.063(4) 0.034(4) -0.001(3) 0.004(4) -0.002(4) C27 0.048(5) 0.086(6) 0.051(5) -0.003(4) -0.013(4) -0.009(4) C28 0.046(5) 0.090(6) 0.058(6) 0.008(5) -0.012(4) 0.012(5) C29 0.057(5) 0.075(5) 0.056(5) 0.003(4) -0.006(4) 0.023(4) C30 0.055(5) 0.064(5) 0.052(5) -0.004(4) -0.003(4) -0.003(4) C31 0.036(4) 0.046(4) 0.036(4) -0.001(3) 0.009(3) 0.004(3) C32 0.037(4) 0.048(4) 0.051(5) -0.008(4) -0.004(4) 0.004(3) C33 0.053(5) 0.104(7) 0.059(6) -0.011(5) 0.003(4) -0.014(5) C34 0.062(6) 0.122(8) 0.077(8) -0.060(6) 0.007(5) 0.004(5) C35 0.066(6) 0.158(11) 0.040(6) -0.003(7) 0.000(5) -0.016(7) C36 0.057(6) 0.136(9) 0.050(6) 0.017(6) 0.007(5) -0.021(6) C37 0.058(5) 0.068(5) 0.062(6) 0.007(4) 0.006(4) -0.007(4) C38 0.039(4) 0.047(4) 0.044(5) -0.006(3) -0.002(4) -0.006(3) C39 0.052(5) 0.064(5) 0.044(5) 0.001(3) 0.001(4) 0.000(4) C40 0.043(5) 0.113(7) 0.113(9) -0.008(7) 0.006(6) -0.032(5) C41 0.056(5) 0.119(7) 0.083(7) 0.004(6) 0.009(6) -0.035(5) C42 0.087(7) 0.131(8) 0.061(7) 0.005(6) 0.037(6) -0.034(6) C43 0.059(5) 0.095(6) 0.051(6) 0.000(4) 0.000(4) -0.017(5) C44 0.109(8) 0.068(5) 0.176(12) 0.005(7) -0.029(9) 0.020(5) C45 0.091(7) 0.174(10) 0.106(9) -0.010(8) 0.014(7) 0.054(7) C46 0.082(6) 0.104(7) 0.085(7) 0.012(6) -0.040(6) 0.014(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 Al1 N1 1.936(6) . ? Al1 C2 2.004(9) . ? Al1 C3 2.027(9) . ? Al1 C1 2.072(7) . ? Al2 N2 1.951(5) . ? Al2 C24 1.989(7) . ? Al2 C26 2.017(7) . ? Al2 Cl1 2.103(5) . ? N1 P1 1.602(5) . ? N1 Si1 1.796(6) . ? N2 P2 1.602(5) . ? N2 Si2 1.774(6) . ? P1 C8 1.802(7) . ? P1 C15 1.820(7) . ? P1 C9 1.831(8) . ? P2 C31 1.786(7) . ? P2 C38 1.808(7) . ? P2 C32 1.812(7) . ? Si1 C23 1.869(10) . ? Si1 C22 1.877(9) . ? Si1 C21 1.893(10) . ? Si2 C46 1.852(9) . ? Si2 C44 1.856(8) . ? Si2 C45 1.878(11) . ? C3 C8 1.406(10) . ? C3 C4 1.445(11) . ? C4 C5 1.345(11) . ? C5 C6 1.381(12) . ? C6 C7 1.405(11) . ? C7 C8 1.411(10) . ? C9 C10 1.373(10) . ? C9 C14 1.375(10) . ? C10 C11 1.425(13) . ? C11 C12 1.298(14) . ? C12 C13 1.377(15) . ? C13 C14 1.409(13) . ? C15 C20 1.383(10) . ? C15 C16 1.397(12) . ? C16 C17 1.396(12) . ? C17 C18 1.327(14) . ? C18 C19 1.375(15) . ? C19 C20 1.424(12) . ? C26 C31 1.410(9) . ? C26 C27 1.422(10) . ? C27 C28 1.355(10) . ? C28 C29 1.361(10) . ? C29 C30 1.413(10) . ? C30 C31 1.406(9) . ? C32 C37 1.378(10) . ? C32 C33 1.420(10) . ? C33 C34 1.407(12) . ? C34 C35 1.379(13) . ? C35 C36 1.381(13) . ? C36 C37 1.382(12) . ? C38 C39 1.379(9) . ? C38 C43 1.405(10) . ? C39 C40 1.428(10) . ? C40 C41 1.390(14) . ? C41 C42 1.342(13) . ? C42 C43 1.415(11) . ? 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 Al1 C2 109.7(3) . . ? N1 Al1 C3 91.9(3) . . ? C2 Al1 C3 118.4(4) . . ? N1 Al1 C1 109.1(3) . . ? C2 Al1 C1 113.0(4) . . ? C3 Al1 C1 112.4(3) . . ? N2 Al2 C24 114.1(3) . . ? N2 Al2 C26 91.9(3) . . ? C24 Al2 C26 115.9(3) . . ? N2 Al2 Cl1 111.4(2) . . ? C24 Al2 Cl1 111.9(3) . . ? C26 Al2 Cl1 110.2(2) . . ? P1 N1 Si1 123.6(3) . . ? P1 N1 Al1 112.8(3) . . ? Si1 N1 Al1 123.3(3) . . ? P2 N2 Si2 125.7(3) . . ? P2 N2 Al2 112.7(3) . . ? Si2 N2 Al2 121.4(3) . . ? N1 P1 C8 106.7(3) . . ? N1 P1 C15 112.8(3) . . ? C8 P1 C15 107.9(3) . . ? N1 P1 C9 111.5(3) . . ? C8 P1 C9 108.4(3) . . ? C15 P1 C9 109.3(3) . . ? N2 P2 C31 106.3(3) . . ? N2 P2 C38 114.8(3) . . ? C31 P2 C38 109.1(3) . . ? N2 P2 C32 111.7(3) . . ? C31 P2 C32 108.4(3) . . ? C38 P2 C32 106.3(3) . . ? N1 Si1 C23 112.1(4) . . ? N1 Si1 C22 105.8(4) . . ? C23 Si1 C22 106.8(5) . . ? N1 Si1 C21 109.2(4) . . ? C23 Si1 C21 109.6(5) . . ? C22 Si1 C21 113.4(5) . . ? N2 Si2 C46 113.2(4) . . ? N2 Si2 C44 106.5(3) . . ? C46 Si2 C44 106.7(5) . . ? N2 Si2 C45 110.4(4) . . ? C46 Si2 C45 108.5(5) . . ? C44 Si2 C45 111.5(6) . . ? C8 C3 C4 114.2(7) . . ? C8 C3 Al1 113.6(5) . . ? C4 C3 Al1 132.3(6) . . ? C5 C4 C3 122.0(8) . . ? C4 C5 C6 122.3(8) . . ? C5 C6 C7 120.0(8) . . ? C6 C7 C8 117.0(8) . . ? C3 C8 C7 124.5(7) . . ? C3 C8 P1 113.8(5) . . ? C7 C8 P1 121.6(6) . . ? C10 C9 C14 119.7(8) . . ? C10 C9 P1 121.4(6) . . ? C14 C9 P1 118.7(6) . . ? C9 C10 C11 118.5(9) . . ? C12 C11 C10 121.7(10) . . ? C11 C12 C13 120.9(10) . . ? C12 C13 C14 119.3(10) . . ? C9 C14 C13 119.8(9) . . ? C20 C15 C16 119.4(8) . . ? C20 C15 P1 124.7(7) . . ? C16 C15 P1 115.8(6) . . ? C15 C16 C17 121.3(9) . . ? C18 C17 C16 118.5(10) . . ? C17 C18 C19 123.2(9) . . ? C18 C19 C20 119.3(10) . . ? C15 C20 C19 118.4(9) . . ? C31 C26 C27 115.1(6) . . ? C31 C26 Al2 113.0(5) . . ? C27 C26 Al2 131.8(6) . . ? C28 C27 C26 123.9(7) . . ? C27 C28 C29 119.9(7) . . ? C28 C29 C30 120.8(7) . . ? C31 C30 C29 118.5(7) . . ? C30 C31 C26 121.8(6) . . ? C30 C31 P2 123.0(5) . . ? C26 C31 P2 114.9(5) . . ? C37 C32 C33 119.3(7) . . ? C37 C32 P2 120.9(6) . . ? C33 C32 P2 119.5(6) . . ? C34 C33 C32 117.6(9) . . ? C35 C34 C33 123.0(9) . . ? C34 C35 C36 117.2(9) . . ? C37 C36 C35 122.0(9) . . ? C32 C37 C36 120.6(8) . . ? C39 C38 C43 119.2(7) . . ? C39 C38 P2 122.0(6) . . ? C43 C38 P2 118.6(6) . . ? C38 C39 C40 121.5(8) . . ? C41 C40 C39 118.0(9) . . ? C42 C41 C40 120.6(8) . . ? C41 C42 C43 122.5(9) . . ? C38 C43 C42 118.1(8) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.18 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.609 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.054 #===end data_(o-C6H4PPh2NSiMe3)2Ga(o-C6H4PPh2NH) _database_code_CSD 211245 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C60 H61 Ga N3 P3 Si2' _chemical_formula_weight 1042.93 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 10.210(5) _cell_length_b 14.196(7) _cell_length_c 22.407(12) _cell_angle_alpha 78.956(10) _cell_angle_beta 79.552(9) _cell_angle_gamma 73.884(11) _cell_volume 3034(3) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.526407 _exptl_absorpt_correction_T_max 1.000000 _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 13176 _diffrn_reflns_av_R_equivalents 0.0761 _diffrn_reflns_av_sigmaI/netI 0.2111 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 23.30 _reflns_number_total 8673 _reflns_number_gt 3608 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8673 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1758 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.1827 _refine_ls_wR_factor_gt 0.1511 _refine_ls_goodness_of_fit_ref 0.830 _refine_ls_restrained_S_all 0.830 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.005 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 Ga1 Ga 0.64490(7) 0.85722(7) 0.73494(4) 0.0461(3) Uani 1 1 d . . . P1 P 0.73455(19) 1.00947(17) 0.62842(9) 0.0552(6) Uani 1 1 d . . . P2 P 0.80052(19) 0.62676(16) 0.82345(10) 0.0521(6) Uani 1 1 d . . . P3 P 0.34455(17) 0.99426(16) 0.83009(9) 0.0476(6) Uani 1 1 d . . . Si1 Si 0.5589(2) 0.56066(18) 0.80318(11) 0.0618(7) Uani 1 1 d . . . Si2 Si 0.4385(2) 1.18603(19) 0.79215(12) 0.0647(7) Uani 1 1 d . . . N1 N 0.6472(5) 0.9957(5) 0.6941(3) 0.0556(17) Uani 1 1 d . . . H1A H 0.6020 1.0460 0.7118 0.067 Uiso 1 1 calc R . . N2 N 0.6641(5) 0.6349(4) 0.7994(3) 0.0559(18) Uani 1 1 d . . . N3 N 0.4393(5) 1.0657(5) 0.8013(3) 0.0568(18) Uani 1 1 d . . . C1 C 0.6366(8) 1.0808(6) 0.5689(4) 0.059(2) Uani 1 1 d . . . C2 C 0.6882(10) 1.1329(9) 0.5182(5) 0.109(4) Uani 1 1 d . . . H2B H 0.7787 1.1371 0.5142 0.131 Uiso 1 1 calc R . . C3 C 0.6100(14) 1.1807(10) 0.4716(5) 0.140(5) Uani 1 1 d . . . H3B H 0.6486 1.2151 0.4363 0.168 Uiso 1 1 calc R . . C4 C 0.4734(13) 1.1771(10) 0.4780(6) 0.127(5) Uani 1 1 d . . . H4A H 0.4188 1.2104 0.4476 0.153 Uiso 1 1 calc R . . C5 C 0.4220(11) 1.1249(10) 0.5285(6) 0.118(4) Uani 1 1 d . . . H5A H 0.3314 1.1207 0.5329 0.141 Uiso 1 1 calc R . . C6 C 0.5017(9) 1.0772(7) 0.5738(4) 0.083(3) Uani 1 1 d . . . H6A H 0.4636 1.0417 0.6088 0.099 Uiso 1 1 calc R . . C7 C 0.8684(9) 1.0702(8) 0.6252(4) 0.065(2) Uani 1 1 d . . . C8 C 0.8353(10) 1.1693(10) 0.6293(4) 0.093(3) Uani 1 1 d . . . H8A H 0.7442 1.2050 0.6285 0.111 Uiso 1 1 calc R . . C9 C 0.9292(13) 1.2184(10) 0.6347(5) 0.117(4) Uani 1 1 d . . . H9A H 0.9008 1.2854 0.6383 0.140 Uiso 1 1 calc R . . C10 C 1.0630(16) 1.1700(12) 0.6349(5) 0.117(5) Uani 1 1 d . . . H10A H 1.1269 1.2039 0.6380 0.141 Uiso 1 1 calc R . . C11 C 1.1053(10) 1.0699(12) 0.6304(5) 0.121(5) Uani 1 1 d . . . H11A H 1.1971 1.0354 0.6308 0.145 Uiso 1 1 calc R . . C12 C 1.0051(10) 1.0216(8) 0.6253(4) 0.092(3) Uani 1 1 d . . . H12A H 1.0325 0.9545 0.6219 0.110 Uiso 1 1 calc R . . C13 C 0.8015(7) 0.8842(6) 0.6125(4) 0.053(2) Uani 1 1 d . . . C14 C 0.8867(8) 0.8616(9) 0.5569(4) 0.078(3) Uani 1 1 d . . . H14A H 0.9127 0.9118 0.5279 0.093 Uiso 1 1 calc R . . C15 C 0.9319(10) 0.7615(10) 0.5461(5) 0.095(4) Uani 1 1 d . . . H15A H 0.9873 0.7453 0.5099 0.114 Uiso 1 1 calc R . . C16 C 0.8928(10) 0.6902(8) 0.5894(5) 0.084(3) Uani 1 1 d . . . H16A H 0.9242 0.6243 0.5831 0.101 Uiso 1 1 calc R . . C17 C 0.8079(8) 0.7129(7) 0.6426(4) 0.061(2) Uani 1 1 d . . . H17A H 0.7804 0.6619 0.6703 0.073 Uiso 1 1 calc R . . C18 C 0.7605(7) 0.8109(7) 0.6570(3) 0.048(2) Uani 1 1 d . . . C19 C 0.7556(6) 0.8373(7) 0.8049(3) 0.051(2) Uani 1 1 d . . . C20 C 0.7809(7) 0.9200(6) 0.8190(3) 0.049(2) Uani 1 1 d . . . H20A H 0.7428 0.9813 0.7973 0.058 Uiso 1 1 calc R . . C21 C 0.8597(7) 0.9172(7) 0.8636(4) 0.060(2) Uani 1 1 d . . . H21A H 0.8727 0.9755 0.8718 0.073 Uiso 1 1 calc R . . C22 C 0.9193(8) 0.8265(7) 0.8958(4) 0.069(3) Uani 1 1 d . . . H22A H 0.9710 0.8231 0.9266 0.083 Uiso 1 1 calc R . . C23 C 0.9009(7) 0.7419(7) 0.8815(4) 0.068(2) Uani 1 1 d . . . H23A H 0.9444 0.6812 0.9022 0.081 Uiso 1 1 calc R . . C24 C 0.8202(7) 0.7422(6) 0.8374(3) 0.047(2) Uani 1 1 d . . . C25 C 0.8237(8) 0.5441(6) 0.8962(4) 0.052(2) Uani 1 1 d . . . C26 C 0.7240(9) 0.5681(7) 0.9460(5) 0.077(3) Uani 1 1 d . . . H26A H 0.6513 0.6242 0.9412 0.092 Uiso 1 1 calc R . . C27 C 0.7321(9) 0.5092(8) 1.0026(5) 0.092(3) Uani 1 1 d . . . H27A H 0.6645 0.5256 1.0354 0.111 Uiso 1 1 calc R . . C28 C 0.8418(10) 0.4247(7) 1.0108(5) 0.084(3) Uani 1 1 d . . . H28A H 0.8475 0.3844 1.0487 0.101 Uiso 1 1 calc R . . C29 C 0.9399(9) 0.4032(7) 0.9617(5) 0.074(3) Uani 1 1 d . . . H29A H 1.0129 0.3473 0.9665 0.089 Uiso 1 1 calc R . . C30 C 0.9336(8) 0.4620(6) 0.9052(4) 0.068(2) Uani 1 1 d . . . H30A H 1.0034 0.4465 0.8730 0.081 Uiso 1 1 calc R . . C31 C 0.9510(7) 0.5743(6) 0.7703(4) 0.055(2) Uani 1 1 d . . . C32 C 1.0672(9) 0.6105(7) 0.7563(5) 0.084(3) Uani 1 1 d . . . H32A H 1.0743 0.6609 0.7757 0.101 Uiso 1 1 calc R . . C33 C 1.1738(10) 0.5701(10) 0.7126(6) 0.114(4) Uani 1 1 d . . . H33A H 1.2496 0.5970 0.7013 0.136 Uiso 1 1 calc R . . C34 C 1.1696(10) 0.4948(9) 0.6870(5) 0.104(4) Uani 1 1 d . . . H34A H 1.2434 0.4679 0.6591 0.125 Uiso 1 1 calc R . . C35 C 1.0559(11) 0.4557(8) 0.7014(5) 0.102(4) Uani 1 1 d . . . H35A H 1.0518 0.4037 0.6827 0.122 Uiso 1 1 calc R . . C36 C 0.9488(9) 0.4947(7) 0.7439(5) 0.083(3) Uani 1 1 d . . . H36A H 0.8738 0.4669 0.7549 0.099 Uiso 1 1 calc R . . C37 C 0.5574(8) 0.5309(7) 0.7245(4) 0.091(3) Uani 1 1 d . . . H37A H 0.5316 0.5914 0.6969 0.137 Uiso 1 1 calc R . . H37B H 0.4924 0.4921 0.7273 0.137 Uiso 1 1 calc R . . H37C H 0.6475 0.4939 0.7095 0.137 Uiso 1 1 calc R . . C38 C 0.6094(8) 0.4389(6) 0.8543(4) 0.087(3) Uani 1 1 d . . . H38A H 0.6116 0.4507 0.8948 0.130 Uiso 1 1 calc R . . H38B H 0.6988 0.4025 0.8382 0.130 Uiso 1 1 calc R . . H38C H 0.5435 0.4013 0.8560 0.130 Uiso 1 1 calc R . . C39 C 0.3792(7) 0.6186(6) 0.8358(4) 0.068(2) Uani 1 1 d . . . H39A H 0.3466 0.6818 0.8118 0.101 Uiso 1 1 calc R . . H39B H 0.3777 0.6273 0.8774 0.101 Uiso 1 1 calc R . . H39C H 0.3208 0.5763 0.8351 0.101 Uiso 1 1 calc R . . C40 C 0.4433(6) 0.8625(5) 0.7412(3) 0.0381(18) Uani 1 1 d . . . C41 C 0.4145(7) 0.8107(6) 0.7007(3) 0.055(2) Uani 1 1 d . . . H41A H 0.4869 0.7791 0.6739 0.066 Uiso 1 1 calc R . . C42 C 0.2818(8) 0.8035(6) 0.6981(4) 0.064(2) Uani 1 1 d . . . H42A H 0.2673 0.7679 0.6701 0.076 Uiso 1 1 calc R . . C43 C 0.1734(8) 0.8494(6) 0.7370(4) 0.061(2) Uani 1 1 d . . . H43A H 0.0849 0.8438 0.7366 0.073 Uiso 1 1 calc R . . C44 C 0.1971(7) 0.9033(6) 0.7764(3) 0.054(2) Uani 1 1 d . . . H44A H 0.1231 0.9332 0.8031 0.064 Uiso 1 1 calc R . . C45 C 0.3269(7) 0.9160(5) 0.7785(3) 0.0431(19) Uani 1 1 d . . . C46 C 0.1675(7) 1.0627(6) 0.8556(4) 0.048(2) Uani 1 1 d . . . C47 C 0.0920(7) 1.1279(6) 0.8113(4) 0.064(2) Uani 1 1 d . . . H47A H 0.1286 1.1303 0.7700 0.077 Uiso 1 1 calc R . . C48 C -0.0361(8) 1.1889(7) 0.8280(5) 0.075(3) Uani 1 1 d . . . H48A H -0.0864 1.2306 0.7982 0.090 Uiso 1 1 calc R . . C49 C -0.0881(8) 1.1871(7) 0.8890(5) 0.078(3) Uani 1 1 d . . . H49A H -0.1729 1.2294 0.9003 0.094 Uiso 1 1 calc R . . C50 C -0.0180(8) 1.1247(7) 0.9335(4) 0.075(3) Uani 1 1 d . . . H50A H -0.0559 1.1234 0.9745 0.090 Uiso 1 1 calc R . . C51 C 0.1157(7) 1.0603(6) 0.9165(4) 0.061(2) Uani 1 1 d . . . H51A H 0.1654 1.0182 0.9463 0.074 Uiso 1 1 calc R . . C52 C 0.3991(7) 0.9107(6) 0.8973(3) 0.0441(19) Uani 1 1 d . . . C53 C 0.4958(7) 0.9294(7) 0.9280(4) 0.064(2) Uani 1 1 d . . . H53A H 0.5342 0.9829 0.9126 0.077 Uiso 1 1 calc R . . C54 C 0.5340(10) 0.8668(9) 0.9819(5) 0.087(3) Uani 1 1 d . . . H54A H 0.5984 0.8790 1.0020 0.105 Uiso 1 1 calc R . . C55 C 0.4779(10) 0.7877(8) 1.0054(4) 0.082(3) Uani 1 1 d . . . H55A H 0.5041 0.7473 1.0414 0.099 Uiso 1 1 calc R . . C56 C 0.3821(9) 0.7675(7) 0.9760(4) 0.077(3) Uani 1 1 d . . . H56A H 0.3438 0.7139 0.9913 0.092 Uiso 1 1 calc R . . C57 C 0.3459(8) 0.8310(6) 0.9224(4) 0.060(2) Uani 1 1 d . . . H57A H 0.2816 0.8183 0.9024 0.072 Uiso 1 1 calc R . . C58 C 0.4033(10) 1.2461(8) 0.7111(4) 0.118(4) Uani 1 1 d . . . H58A H 0.4671 1.2085 0.6819 0.178 Uiso 1 1 calc R . . H58B H 0.4139 1.3126 0.7039 0.178 Uiso 1 1 calc R . . H58C H 0.3110 1.2474 0.7065 0.178 Uiso 1 1 calc R . . C59 C 0.3111(8) 1.2610(7) 0.8487(4) 0.089(3) Uani 1 1 d . . . H59A H 0.3280 1.2314 0.8898 0.133 Uiso 1 1 calc R . . H59B H 0.2192 1.2619 0.8438 0.133 Uiso 1 1 calc R . . H59C H 0.3214 1.3276 0.8412 0.133 Uiso 1 1 calc R . . C60 C 0.6148(8) 1.1961(7) 0.7979(5) 0.114(4) Uani 1 1 d . . . H60A H 0.6382 1.1665 0.8381 0.171 Uiso 1 1 calc R . . H60B H 0.6160 1.2648 0.7910 0.171 Uiso 1 1 calc R . . H60C H 0.6804 1.1623 0.7676 0.171 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 Ga1 0.0328(4) 0.0577(6) 0.0454(6) -0.0038(5) -0.0050(4) -0.0100(4) P1 0.0426(12) 0.0737(17) 0.0460(14) 0.0034(13) -0.0064(10) -0.0172(11) P2 0.0422(12) 0.0499(15) 0.0657(15) -0.0032(12) -0.0182(10) -0.0105(10) P3 0.0319(10) 0.0553(15) 0.0540(14) -0.0113(12) -0.0039(9) -0.0077(10) Si1 0.0465(13) 0.0621(17) 0.0814(18) -0.0127(15) -0.0178(12) -0.0142(12) Si2 0.0448(13) 0.0605(18) 0.0891(19) -0.0186(15) -0.0072(12) -0.0098(12) N1 0.046(3) 0.062(5) 0.049(4) -0.009(4) 0.000(3) 0.000(3) N2 0.035(3) 0.060(4) 0.080(5) -0.015(4) -0.022(3) -0.011(3) N3 0.037(3) 0.053(5) 0.080(5) -0.014(4) -0.002(3) -0.013(3) C1 0.053(5) 0.078(7) 0.039(5) 0.013(5) -0.011(4) -0.018(5) C2 0.083(7) 0.158(11) 0.060(7) 0.042(7) -0.019(6) -0.022(7) C3 0.136(11) 0.190(14) 0.071(9) 0.056(9) -0.018(8) -0.053(10) C4 0.102(9) 0.183(14) 0.076(9) 0.018(9) -0.048(7) -0.004(9) C5 0.085(8) 0.179(13) 0.080(9) 0.008(9) -0.036(7) -0.021(8) C6 0.066(6) 0.116(8) 0.063(6) 0.011(6) -0.025(5) -0.023(6) C7 0.061(6) 0.085(8) 0.051(6) 0.005(6) -0.008(4) -0.029(6) C8 0.059(6) 0.115(10) 0.120(9) -0.021(8) -0.007(6) -0.048(7) C9 0.093(8) 0.138(12) 0.128(10) -0.034(9) -0.005(8) -0.040(9) C10 0.165(14) 0.136(13) 0.088(8) 0.013(9) -0.021(8) -0.115(12) C11 0.072(7) 0.180(14) 0.125(10) 0.056(10) -0.051(7) -0.086(9) C12 0.076(7) 0.097(8) 0.099(8) 0.028(6) -0.036(6) -0.029(6) C13 0.040(4) 0.066(6) 0.049(6) -0.010(5) -0.006(4) -0.005(4) C14 0.056(5) 0.135(10) 0.034(5) 0.004(6) 0.001(4) -0.027(6) C15 0.083(7) 0.108(10) 0.076(8) -0.047(8) 0.006(6) 0.016(7) C16 0.100(7) 0.074(8) 0.066(8) -0.015(7) -0.003(6) -0.002(6) C17 0.063(5) 0.064(7) 0.053(6) -0.008(5) -0.011(4) -0.009(5) C18 0.037(4) 0.059(6) 0.050(5) -0.006(5) -0.013(4) -0.014(4) C19 0.030(4) 0.080(7) 0.048(5) -0.013(5) -0.001(3) -0.022(4) C20 0.044(4) 0.039(5) 0.068(6) -0.004(4) -0.012(4) -0.018(4) C21 0.048(5) 0.062(6) 0.084(7) -0.020(6) -0.018(5) -0.024(5) C22 0.067(6) 0.073(7) 0.082(7) -0.011(6) -0.035(5) -0.028(5) C23 0.062(5) 0.061(6) 0.088(7) 0.002(5) -0.042(5) -0.016(5) C24 0.036(4) 0.047(5) 0.064(6) -0.009(5) -0.013(4) -0.013(4) C25 0.054(5) 0.046(6) 0.057(6) 0.012(5) -0.019(4) -0.017(4) C26 0.063(6) 0.070(7) 0.082(7) 0.013(6) -0.018(5) -0.002(5) C27 0.073(7) 0.110(9) 0.077(8) 0.014(7) 0.002(5) -0.022(6) C28 0.078(7) 0.083(8) 0.079(8) 0.026(6) -0.031(6) -0.015(6) C29 0.061(6) 0.061(7) 0.092(8) 0.012(6) -0.022(6) -0.006(5) C30 0.057(5) 0.062(6) 0.075(7) 0.012(6) -0.021(5) -0.008(5) C31 0.035(4) 0.052(6) 0.075(6) 0.000(5) -0.020(4) -0.002(4) C32 0.064(6) 0.072(7) 0.118(9) -0.018(7) -0.014(6) -0.017(6) C33 0.066(7) 0.095(10) 0.170(12) -0.029(9) 0.023(7) -0.022(7) C34 0.058(7) 0.096(10) 0.129(10) -0.020(8) 0.006(6) 0.020(7) C35 0.066(7) 0.098(9) 0.144(10) -0.062(8) -0.006(7) 0.002(7) C36 0.056(6) 0.081(8) 0.119(9) -0.041(7) -0.017(6) -0.007(5) C37 0.064(6) 0.100(8) 0.119(8) -0.045(7) -0.008(5) -0.018(5) C38 0.073(6) 0.065(7) 0.129(9) -0.003(6) -0.036(6) -0.021(5) C39 0.047(5) 0.083(7) 0.069(6) -0.002(5) -0.005(4) -0.018(4) C40 0.046(4) 0.038(5) 0.027(4) 0.006(4) -0.005(3) -0.012(4) C41 0.054(5) 0.067(6) 0.038(5) -0.002(5) 0.000(4) -0.015(4) C42 0.066(6) 0.085(7) 0.056(6) -0.011(5) -0.021(5) -0.037(5) C43 0.043(5) 0.079(7) 0.070(6) -0.015(5) -0.013(5) -0.023(5) C44 0.035(4) 0.064(6) 0.057(5) 0.000(5) -0.009(4) -0.009(4) C45 0.039(4) 0.044(5) 0.038(5) 0.012(4) -0.006(3) -0.010(4) C46 0.034(4) 0.056(6) 0.050(5) -0.011(5) 0.004(4) -0.009(4) C47 0.047(5) 0.073(7) 0.062(6) 0.002(5) -0.004(4) -0.007(5) C48 0.040(5) 0.087(7) 0.087(8) -0.004(6) -0.011(5) 0.000(5) C49 0.044(5) 0.078(7) 0.101(9) -0.010(7) -0.007(5) 0.000(5) C50 0.056(5) 0.084(7) 0.079(7) -0.032(6) 0.015(5) -0.012(5) C51 0.049(5) 0.064(6) 0.068(6) -0.013(5) -0.004(4) -0.008(4) C52 0.042(4) 0.037(5) 0.052(5) -0.004(4) -0.008(4) -0.008(4) C53 0.054(5) 0.075(7) 0.066(6) -0.011(6) -0.006(4) -0.022(5) C54 0.094(7) 0.106(9) 0.070(8) -0.006(7) -0.025(6) -0.034(7) C55 0.096(7) 0.081(8) 0.061(7) -0.006(6) -0.015(6) -0.009(6) C56 0.086(7) 0.072(7) 0.070(7) 0.002(6) -0.010(6) -0.024(6) C57 0.059(5) 0.054(6) 0.062(6) -0.004(5) -0.015(4) -0.003(5) C58 0.127(9) 0.093(8) 0.100(9) 0.016(7) -0.013(7) 0.008(7) C59 0.062(5) 0.085(7) 0.121(8) -0.060(7) -0.005(5) 0.005(5) C60 0.067(6) 0.104(9) 0.190(12) -0.051(8) -0.008(7) -0.039(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N1 2.007(6) . ? Ga1 C40 2.019(6) . ? Ga1 C19 2.028(7) . ? Ga1 C18 2.033(8) . ? P1 N1 1.585(6) . ? P1 C1 1.791(8) . ? P1 C7 1.792(9) . ? P1 C13 1.798(8) . ? P2 N2 1.550(5) . ? P2 C24 1.797(7) . ? P2 C31 1.836(8) . ? P2 C25 1.828(8) . ? P3 N3 1.564(6) . ? P3 C52 1.799(8) . ? P3 C45 1.812(7) . ? P3 C46 1.844(7) . ? Si1 N2 1.683(6) . ? Si1 C39 1.866(7) . ? Si1 C38 1.877(8) . ? Si1 C37 1.893(9) . ? Si2 N3 1.680(6) . ? Si2 C60 1.874(8) . ? Si2 C59 1.892(8) . ? Si2 C58 1.906(10) . ? C1 C2 1.338(11) . ? C1 C6 1.375(10) . ? C2 C3 1.385(13) . ? C3 C4 1.390(14) . ? C4 C5 1.336(14) . ? C5 C6 1.373(12) . ? C7 C8 1.370(12) . ? C7 C12 1.375(11) . ? C8 C9 1.365(13) . ? C9 C10 1.348(15) . ? C10 C11 1.384(15) . ? C11 C12 1.411(12) . ? C13 C18 1.396(10) . ? C13 C14 1.420(10) . ? C14 C15 1.420(13) . ? C15 C16 1.354(13) . ? C16 C17 1.376(11) . ? C17 C18 1.420(10) . ? C19 C20 1.372(9) . ? C19 C24 1.446(10) . ? C20 C21 1.380(9) . ? C21 C22 1.384(10) . ? C22 C23 1.369(10) . ? C23 C24 1.394(9) . ? C25 C30 1.388(10) . ? C25 C26 1.393(10) . ? C26 C27 1.380(11) . ? C27 C28 1.404(12) . ? C28 C29 1.366(11) . ? C29 C30 1.377(11) . ? C31 C32 1.382(10) . ? C31 C36 1.380(10) . ? C32 C33 1.398(13) . ? C33 C34 1.322(13) . ? C34 C35 1.382(13) . ? C35 C36 1.377(11) . ? C40 C41 1.389(9) . ? C40 C45 1.439(9) . ? C41 C42 1.398(9) . ? C42 C43 1.371(10) . ? C43 C44 1.364(10) . ? C44 C45 1.396(9) . ? C46 C51 1.368(10) . ? C46 C47 1.403(10) . ? C47 C48 1.385(10) . ? C48 C49 1.372(11) . ? C49 C50 1.363(11) . ? C50 C51 1.448(10) . ? C52 C57 1.371(10) . ? C52 C53 1.407(9) . ? C53 C54 1.402(11) . ? C54 C55 1.375(12) . ? C55 C56 1.391(11) . ? C56 C57 1.398(11) . ? 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 Ga1 C40 101.0(2) . . ? N1 Ga1 C19 102.6(3) . . ? C40 Ga1 C19 127.3(3) . . ? N1 Ga1 C18 86.8(3) . . ? C40 Ga1 C18 114.2(3) . . ? C19 Ga1 C18 113.5(3) . . ? N1 P1 C1 114.6(3) . . ? N1 P1 C7 114.1(4) . . ? C1 P1 C7 104.5(4) . . ? N1 P1 C13 102.8(4) . . ? C1 P1 C13 108.8(4) . . ? C7 P1 C13 112.1(4) . . ? N2 P2 C24 114.3(3) . . ? N2 P2 C31 111.6(3) . . ? C24 P2 C31 107.7(4) . . ? N2 P2 C25 114.2(3) . . ? C24 P2 C25 104.3(4) . . ? C31 P2 C25 104.0(4) . . ? N3 P3 C52 114.4(3) . . ? N3 P3 C45 114.4(3) . . ? C52 P3 C45 105.3(3) . . ? N3 P3 C46 111.9(3) . . ? C52 P3 C46 104.6(3) . . ? C45 P3 C46 105.3(3) . . ? N2 Si1 C39 111.5(3) . . ? N2 Si1 C38 113.4(3) . . ? C39 Si1 C38 105.0(4) . . ? N2 Si1 C37 110.9(4) . . ? C39 Si1 C37 109.0(4) . . ? C38 Si1 C37 106.8(4) . . ? N3 Si2 C60 109.1(4) . . ? N3 Si2 C59 115.5(4) . . ? C60 Si2 C59 108.1(4) . . ? N3 Si2 C58 109.1(4) . . ? C60 Si2 C58 105.9(5) . . ? C59 Si2 C58 108.8(4) . . ? P1 N1 Ga1 118.1(3) . . ? P2 N2 Si1 136.6(4) . . ? P3 N3 Si2 140.5(4) . . ? C2 C1 C6 117.7(8) . . ? C2 C1 P1 124.2(7) . . ? C6 C1 P1 117.9(7) . . ? C1 C2 C3 121.6(10) . . ? C2 C3 C4 119.6(10) . . ? C5 C4 C3 118.8(10) . . ? C4 C5 C6 120.7(10) . . ? C5 C6 C1 121.6(9) . . ? C8 C7 C12 115.8(9) . . ? C8 C7 P1 119.8(7) . . ? C12 C7 P1 124.0(9) . . ? C9 C8 C7 123.4(10) . . ? C8 C9 C10 120.3(12) . . ? C9 C10 C11 119.9(12) . . ? C10 C11 C12 118.1(11) . . ? C7 C12 C11 122.5(11) . . ? C18 C13 C14 121.9(8) . . ? C18 C13 P1 116.0(6) . . ? C14 C13 P1 122.0(8) . . ? C15 C14 C13 119.3(9) . . ? C16 C15 C14 118.9(9) . . ? C15 C16 C17 121.5(10) . . ? C16 C17 C18 122.8(9) . . ? C13 C18 C17 115.6(7) . . ? C13 C18 Ga1 116.1(6) . . ? C17 C18 Ga1 128.3(7) . . ? C20 C19 C24 117.4(6) . . ? C20 C19 Ga1 117.3(6) . . ? C24 C19 Ga1 125.1(6) . . ? C19 C20 C21 123.7(7) . . ? C22 C21 C20 119.2(8) . . ? C21 C22 C23 119.0(7) . . ? C22 C23 C24 123.3(8) . . ? C23 C24 C19 117.4(7) . . ? C23 C24 P2 119.5(6) . . ? C19 C24 P2 123.1(6) . . ? C30 C25 C26 118.5(8) . . ? C30 C25 P2 125.0(7) . . ? C26 C25 P2 116.5(6) . . ? C27 C26 C25 120.5(8) . . ? C26 C27 C28 120.4(9) . . ? C29 C28 C27 118.3(9) . . ? C30 C29 C28 121.8(8) . . ? C29 C30 C25 120.4(8) . . ? C32 C31 C36 118.6(8) . . ? C32 C31 P2 122.7(7) . . ? C36 C31 P2 118.7(6) . . ? C31 C32 C33 119.0(9) . . ? C34 C33 C32 121.7(11) . . ? C33 C34 C35 120.3(10) . . ? C34 C35 C36 119.2(10) . . ? C35 C36 C31 121.1(9) . . ? C41 C40 C45 116.3(6) . . ? C41 C40 Ga1 113.9(5) . . ? C45 C40 Ga1 129.7(5) . . ? C40 C41 C42 123.2(7) . . ? C43 C42 C41 119.4(7) . . ? C44 C43 C42 119.1(7) . . ? C43 C44 C45 123.3(7) . . ? C44 C45 C40 118.3(7) . . ? C44 C45 P3 119.4(6) . . ? C40 C45 P3 122.2(5) . . ? C51 C46 C47 119.8(7) . . ? C51 C46 P3 121.7(6) . . ? C47 C46 P3 118.0(6) . . ? C48 C47 C46 121.0(8) . . ? C49 C48 C47 119.3(9) . . ? C50 C49 C48 121.4(9) . . ? C49 C50 C51 119.7(8) . . ? C46 C51 C50 118.8(8) . . ? C57 C52 C53 117.4(7) . . ? C57 C52 P3 123.1(6) . . ? C53 C52 P3 119.5(6) . . ? C54 C53 C52 119.6(8) . . ? C55 C54 C53 121.0(9) . . ? C54 C55 C56 120.6(9) . . ? C57 C56 C55 117.2(9) . . ? C52 C57 C56 124.2(8) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.646 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.080 #===end data_(o-C6H4PPh2NPh)AlCl2 _database_code_CSD 211246 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C24 H19 Al Cl2 N P' _chemical_formula_weight 450.25 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' Al Al 0.0645 0.0514 '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' _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 9.746(5) _cell_length_b 17.166(9) _cell_length_c 14.235(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.233(11) _cell_angle_gamma 90.00 _cell_volume 2344(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 926 _exptl_absorpt_coefficient_mu 0.393 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.233828 _exptl_absorpt_correction_T_max 0.350982 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 9772 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 23.17 _reflns_number_total 3311 _reflns_number_gt 1728 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1835P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3311 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1418 _refine_ls_R_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.2768 _refine_ls_wR_factor_gt 0.2454 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.072 _refine_ls_shift/su_mean 0.008 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 Al1A Al 0.5485(5) 0.5883(3) 0.6497(3) 0.0453(12) Uani 0.50 1 d P . . Al1 Al 0.6232(5) 0.5868(3) 0.6868(3) 0.0390(12) Uani 0.50 1 d P . . Cl1 Cl 0.6652(3) 0.6411(2) 0.5627(2) 0.1336(12) Uani 1 1 d . . . Cl2 Cl 0.5966(3) 0.46711(14) 0.6723(2) 0.1095(10) Uani 1 1 d . . . P1 P 0.4264(5) 0.6767(3) 0.7969(4) 0.0309(12) Uani 0.50 1 d P . . P1A P 0.4888(4) 0.6794(3) 0.8245(3) 0.0299(12) Uani 0.50 1 d P . . N1 N 0.4563(9) 0.6310(5) 0.7226(7) 0.030(2) Uani 0.50 1 d P . . N1A N 0.5654(11) 0.6417(5) 0.7708(7) 0.043(2) Uani 0.50 1 d P . . C1 C 0.7709(17) 0.6183(7) 0.8101(7) 0.103(4) Uani 1 1 d . . . C2 C 0.8995(15) 0.6159(5) 0.8491(11) 0.116(5) Uani 1 1 d . . . H2A H 0.9608 0.5868 0.8200 0.139 Uiso 1 1 calc R . . C3 C 0.9525(8) 0.6561(6) 0.9355(9) 0.103(3) Uani 1 1 d . . . H3A H 1.0456 0.6514 0.9642 0.123 Uiso 1 1 calc R . . C4 C 0.8655(10) 0.7004(5) 0.9739(6) 0.089(3) Uani 1 1 d . . . H4A H 0.8971 0.7295 1.0286 0.107 Uiso 1 1 calc R . . C5 C 0.7265(9) 0.7025(4) 0.9307(7) 0.082(3) Uani 1 1 d . . . H5A H 0.6624 0.7320 0.9566 0.098 Uiso 1 1 calc R . . C6 C 0.6851(9) 0.6599(6) 0.8483(8) 0.081(3) Uani 1 1 d . . . C7 C 0.3924(6) 0.6359(3) 0.9110(4) 0.0405(15) Uani 1 1 d . . . C8 C 0.3933(8) 0.6743(4) 0.9945(5) 0.0630(19) Uani 1 1 d . . . H8A H 0.4216 0.7260 1.0005 0.076 Uiso 1 1 calc R . . C9 C 0.3525(9) 0.6365(5) 1.0707(5) 0.079(2) Uani 1 1 d . . . H9A H 0.3531 0.6627 1.1279 0.095 Uiso 1 1 calc R . . C10 C 0.3106(8) 0.5595(6) 1.0617(6) 0.082(2) Uani 1 1 d . . . H10A H 0.2836 0.5339 1.1130 0.098 Uiso 1 1 calc R . . C11 C 0.3087(8) 0.5210(4) 0.9784(6) 0.067(2) Uani 1 1 d . . . H11A H 0.2783 0.4696 0.9721 0.081 Uiso 1 1 calc R . . C12 C 0.3522(6) 0.5585(3) 0.9024(4) 0.0475(16) Uani 1 1 d . . . H12A H 0.3544 0.5317 0.8459 0.057 Uiso 1 1 calc R . . C13 C 0.4295(6) 0.7819(3) 0.8053(4) 0.0392(15) Uani 1 1 d . . . C14 C 0.5201(7) 0.8260(4) 0.7614(5) 0.0570(18) Uani 1 1 d . . . H14A H 0.5954 0.8022 0.7410 0.068 Uiso 1 1 calc R . . C15 C 0.4981(8) 0.9056(4) 0.7480(6) 0.072(2) Uani 1 1 d . . . H15A H 0.5588 0.9350 0.7188 0.086 Uiso 1 1 calc R . . C16 C 0.3867(8) 0.9408(4) 0.7780(5) 0.065(2) Uani 1 1 d . . . H16A H 0.3718 0.9940 0.7689 0.078 Uiso 1 1 calc R . . C17 C 0.2988(7) 0.8979(4) 0.8206(5) 0.061(2) Uani 1 1 d . . . H17A H 0.2244 0.9222 0.8415 0.074 Uiso 1 1 calc R . . C18 C 0.3174(7) 0.8186(4) 0.8336(4) 0.0508(16) Uani 1 1 d . . . H18A H 0.2544 0.7898 0.8614 0.061 Uiso 1 1 calc R . . C19 C 0.3124(11) 0.6323(6) 0.6741(9) 0.096(4) Uani 1 1 d . . . C20 C 0.3185(14) 0.5942(7) 0.5922(15) 0.115(5) Uani 1 1 d . . . C21 C 0.2073(19) 0.5827(5) 0.5344(8) 0.108(4) Uani 1 1 d . . . H21A H 0.2145 0.5565 0.4783 0.129 Uiso 1 1 calc R . . C22 C 0.0778(10) 0.6048(5) 0.5457(6) 0.073(2) Uani 1 1 d . . . H22A H 0.0005 0.5936 0.4991 0.087 Uiso 1 1 calc R . . C23 C 0.0637(7) 0.6429(4) 0.6254(6) 0.065(2) Uani 1 1 d . . . H23A H -0.0239 0.6590 0.6351 0.078 Uiso 1 1 calc R . . C24 C 0.1820(10) 0.6584(4) 0.6939(5) 0.067(2) Uani 1 1 d . . . H24A H 0.1758 0.6847 0.7501 0.081 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 Al1A 0.044(3) 0.053(3) 0.042(3) -0.010(2) 0.015(2) 0.003(2) Al1 0.025(2) 0.054(2) 0.036(3) -0.008(2) 0.003(2) 0.007(2) Cl1 0.104(2) 0.186(3) 0.114(2) 0.022(2) 0.0280(18) -0.0068(19) Cl2 0.120(2) 0.0872(16) 0.120(2) -0.0167(14) 0.0206(17) 0.0092(14) P1 0.031(3) 0.0302(19) 0.032(3) 0.0003(18) 0.008(2) 0.002(2) P1A 0.021(3) 0.0329(19) 0.033(3) -0.0043(18) -0.002(2) 0.000(2) N1 0.019(5) 0.031(5) 0.040(6) -0.014(4) 0.007(5) -0.002(4) N1A 0.047(7) 0.029(5) 0.053(7) -0.004(5) 0.012(6) 0.000(5) C1 0.155(12) 0.097(8) 0.069(7) -0.021(5) 0.054(8) -0.070(8) C2 0.128(10) 0.054(5) 0.200(14) -0.018(7) 0.122(10) -0.004(6) C3 0.024(4) 0.100(7) 0.172(11) 0.024(7) -0.016(6) 0.012(4) C4 0.088(7) 0.090(6) 0.075(6) -0.040(5) -0.025(5) 0.000(5) C5 0.056(5) 0.067(5) 0.130(8) 0.008(5) 0.037(6) 0.027(4) C6 0.060(6) 0.084(6) 0.079(6) 0.050(5) -0.044(5) -0.040(5) C7 0.044(4) 0.044(4) 0.036(4) 0.004(3) 0.012(3) 0.001(3) C8 0.087(5) 0.056(4) 0.050(4) -0.005(4) 0.025(4) -0.014(4) C9 0.099(7) 0.096(7) 0.044(5) 0.001(4) 0.016(4) 0.006(5) C10 0.080(6) 0.100(7) 0.072(6) 0.038(5) 0.029(5) 0.006(5) C11 0.066(5) 0.057(4) 0.076(6) 0.017(4) 0.006(4) -0.001(4) C12 0.052(4) 0.044(4) 0.045(4) 0.006(3) 0.005(3) -0.004(3) C13 0.049(4) 0.028(3) 0.043(4) 0.000(3) 0.012(3) 0.003(3) C14 0.054(4) 0.049(4) 0.073(5) 0.004(3) 0.024(4) 0.005(3) C15 0.084(6) 0.040(4) 0.092(6) 0.020(4) 0.018(5) -0.007(4) C16 0.079(6) 0.034(4) 0.076(5) 0.004(4) -0.006(4) 0.006(4) C17 0.058(5) 0.056(5) 0.066(5) -0.015(4) 0.000(4) 0.020(4) C18 0.052(4) 0.047(4) 0.057(4) -0.010(3) 0.019(3) -0.002(3) C19 0.053(6) 0.073(6) 0.130(9) 0.078(6) -0.070(6) -0.047(5) C20 0.072(8) 0.087(8) 0.199(17) 0.068(10) 0.062(9) 0.026(7) C21 0.203(13) 0.056(5) 0.094(8) 0.003(5) 0.108(10) 0.017(8) C22 0.095(7) 0.068(5) 0.042(5) -0.003(4) -0.021(5) -0.024(5) C23 0.033(4) 0.059(4) 0.106(7) 0.030(5) 0.022(4) 0.011(3) C24 0.110(8) 0.046(4) 0.038(4) -0.002(3) -0.006(5) -0.029(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 Al1A Al1 0.820(4) . ? Al1A N1 1.659(9) . ? Al1A N1A 1.933(11) . ? Al1A Cl1 2.037(5) . ? Al1A Cl2 2.145(5) . ? Al1A C20 2.248(16) . ? Al1A C19 2.503(16) . ? Al1 N1A 1.696(10) . ? Al1 N1 1.944(9) . ? Al1 Cl2 2.076(5) . ? Al1 Cl1 2.101(5) . ? Al1 C1 2.133(13) . ? P1 P1A 0.665(4) . ? P1 N1 1.389(9) . ? P1 N1A 1.585(11) . ? P1 C13 1.808(7) . ? P1 C7 1.852(7) . ? P1 C19 2.044(12) . ? P1A N1A 1.328(10) . ? P1A N1 1.653(10) . ? P1A C7 1.835(8) . ? P1A C13 1.857(7) . ? P1A C6 1.912(11) . ? N1 N1A 1.173(12) . ? N1 C19 1.448(13) . ? N1A C6 1.490(14) . ? C1 C2 1.278(16) . ? C1 C6 1.290(14) . ? C2 C3 1.424(16) . ? C3 C4 1.328(13) . ? C4 C5 1.385(12) . ? C5 C6 1.380(13) . ? C7 C8 1.358(8) . ? C7 C12 1.384(8) . ? C8 C9 1.382(10) . ? C9 C10 1.383(11) . ? C10 C11 1.354(11) . ? C11 C12 1.388(9) . ? C13 C18 1.382(8) . ? C13 C14 1.393(8) . ? C14 C15 1.391(9) . ? C15 C16 1.375(10) . ? C16 C17 1.353(10) . ? C17 C18 1.382(9) . ? C19 C20 1.348(17) . ? C19 C24 1.422(15) . ? C20 C21 1.254(17) . ? C21 C22 1.355(15) . ? C22 C23 1.339(11) . ? C23 C24 1.398(11) . ? 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 Al1 Al1A N1 97.5(6) . . ? Al1 Al1A N1A 61.1(5) . . ? N1 Al1A N1A 37.1(4) . . ? Al1 Al1A Cl1 83.0(5) . . ? N1 Al1A Cl1 127.4(4) . . ? N1A Al1A Cl1 111.3(4) . . ? Al1 Al1A Cl2 74.1(5) . . ? N1 Al1A Cl2 117.6(4) . . ? N1A Al1A Cl2 110.1(4) . . ? Cl1 Al1A Cl2 113.1(2) . . ? Al1 Al1A C20 161.7(7) . . ? N1 Al1A C20 65.9(6) . . ? N1A Al1A C20 103.0(6) . . ? Cl1 Al1A C20 112.8(4) . . ? Cl2 Al1A C20 106.0(4) . . ? Al1 Al1A C19 130.8(6) . . ? N1 Al1A C19 33.6(4) . . ? N1A Al1A C19 70.6(4) . . ? Cl1 Al1A C19 125.2(3) . . ? Cl2 Al1A C19 117.0(3) . . ? C20 Al1A C19 32.4(4) . . ? Al1A Al1 N1A 93.9(6) . . ? Al1A Al1 N1 57.8(5) . . ? N1A Al1 N1 36.8(4) . . ? Al1A Al1 Cl2 83.5(5) . . ? N1A Al1 Cl2 124.7(4) . . ? N1 Al1 Cl2 108.5(3) . . ? Al1A Al1 Cl1 74.2(5) . . ? N1A Al1 Cl1 119.0(4) . . ? N1 Al1 Cl1 110.1(3) . . ? Cl2 Al1 Cl1 113.3(2) . . ? Al1A Al1 C1 156.0(7) . . ? N1A Al1 C1 62.5(6) . . ? N1 Al1 C1 99.2(6) . . ? Cl2 Al1 C1 112.8(4) . . ? Cl1 Al1 C1 112.0(3) . . ? Al1A Cl1 Al1 22.79(12) . . ? Al1 Cl2 Al1A 22.34(11) . . ? P1A P1 N1 101.3(9) . . ? P1A P1 N1A 55.5(8) . . ? N1 P1 N1A 45.9(5) . . ? P1A P1 C13 83.7(8) . . ? N1 P1 C13 127.7(5) . . ? N1A P1 C13 112.9(5) . . ? P1A P1 C7 78.1(8) . . ? N1 P1 C7 123.2(5) . . ? N1A P1 C7 110.8(5) . . ? C13 P1 C7 108.9(4) . . ? P1A P1 C19 146.3(10) . . ? N1 P1 C19 45.1(6) . . ? N1A P1 C19 90.9(6) . . ? C13 P1 C19 115.4(4) . . ? C7 P1 C19 117.0(4) . . ? P1 P1A N1A 100.1(10) . . ? P1 P1A N1 55.5(8) . . ? N1A P1A N1 44.7(5) . . ? P1 P1A C7 81.1(8) . . ? N1A P1A C7 126.6(5) . . ? N1 P1A C7 110.1(4) . . ? P1 P1A C13 75.5(8) . . ? N1A P1A C13 124.7(5) . . ? N1 P1A C13 109.9(4) . . ? C7 P1A C13 107.5(4) . . ? P1 P1A C6 151.0(10) . . ? N1A P1A C6 51.0(7) . . ? N1 P1A C6 95.6(6) . . ? C7 P1A C6 115.2(4) . . ? C13 P1A C6 117.9(4) . . ? N1A N1 P1 75.9(7) . . ? N1A N1 C19 167.5(11) . . ? P1 N1 C19 92.1(9) . . ? N1A N1 P1A 52.8(6) . . ? P1 N1 P1A 23.2(2) . . ? C19 N1 P1A 115.4(9) . . ? N1A N1 Al1A 84.2(7) . . ? P1 N1 Al1A 159.4(7) . . ? C19 N1 Al1A 107.2(9) . . ? P1A N1 Al1A 136.9(6) . . ? N1A N1 Al1 60.0(6) . . ? P1 N1 Al1 136.0(7) . . ? C19 N1 Al1 131.7(9) . . ? P1A N1 Al1 112.8(5) . . ? Al1A N1 Al1 24.7(2) . . ? N1 N1A P1A 82.5(8) . . ? N1 N1A C6 167.3(11) . . ? P1A N1A C6 85.3(8) . . ? N1 N1A P1 58.2(6) . . ? P1A N1A P1 24.4(3) . . ? C6 N1A P1 109.7(9) . . ? N1 N1A Al1 83.2(7) . . ? P1A N1A Al1 165.5(9) . . ? C6 N1A Al1 108.9(8) . . ? P1 N1A Al1 141.3(8) . . ? N1 N1A Al1A 58.6(6) . . ? P1A N1A Al1A 141.0(8) . . ? C6 N1A Al1A 133.7(8) . . ? P1 N1A Al1A 116.6(7) . . ? Al1 N1A Al1A 25.0(2) . . ? C2 C1 C6 119.5(10) . . ? C2 C1 Al1 144.7(11) . . ? C6 C1 Al1 95.4(10) . . ? C1 C2 C3 122.5(9) . . ? C4 C3 C2 118.2(8) . . ? C3 C4 C5 118.6(8) . . ? C6 C5 C4 118.6(8) . . ? C1 C6 C5 122.6(8) . . ? C1 C6 N1A 93.0(11) . . ? C5 C6 N1A 144.3(11) . . ? C1 C6 P1A 136.4(10) . . ? C5 C6 P1A 100.9(9) . . ? N1A C6 P1A 43.8(5) . . ? C8 C7 C12 120.0(5) . . ? C8 C7 P1A 117.7(5) . . ? C12 C7 P1A 120.1(5) . . ? C8 C7 P1 127.6(5) . . ? C12 C7 P1 112.2(5) . . ? P1A C7 P1 20.78(13) . . ? C7 C8 C9 120.1(7) . . ? C8 C9 C10 119.8(7) . . ? C11 C10 C9 120.3(7) . . ? C10 C11 C12 119.9(7) . . ? C7 C12 C11 119.8(6) . . ? C18 C13 C14 118.7(5) . . ? C18 C13 P1 118.0(5) . . ? C14 C13 P1 121.2(5) . . ? C18 C13 P1A 129.1(5) . . ? C14 C13 P1A 112.1(4) . . ? P1 C13 P1A 20.86(13) . . ? C15 C14 C13 120.1(6) . . ? C16 C15 C14 120.0(7) . . ? C17 C16 C15 119.8(6) . . ? C16 C17 C18 121.2(6) . . ? C17 C18 C13 120.2(6) . . ? C20 C19 C24 120.2(8) . . ? C20 C19 N1 102.5(15) . . ? C24 C19 N1 137.2(13) . . ? C20 C19 P1 145.1(13) . . ? C24 C19 P1 94.7(10) . . ? N1 C19 P1 42.8(5) . . ? C20 C19 Al1A 63.3(10) . . ? C24 C19 Al1A 176.5(9) . . ? N1 C19 Al1A 39.3(6) . . ? P1 C19 Al1A 81.8(3) . . ? C21 C20 C19 118.6(11) . . ? C21 C20 Al1A 157.1(14) . . ? C19 C20 Al1A 84.3(12) . . ? C20 C21 C22 126.3(11) . . ? C23 C22 C21 118.4(8) . . ? C22 C23 C24 119.3(7) . . ? C23 C24 C19 117.2(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.17 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.385 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.089 #===end data_(o-C6H4PPh2NPh)GaCl2 _database_code_CSD 211247 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C24 H19 Cl2 Ga N P' _chemical_formula_weight 492.99 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' Ga Ga 0.2307 1.6083 '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 9.696(5) _cell_length_b 17.260(9) _cell_length_c 14.120(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.220(10) _cell_angle_gamma 90.00 _cell_volume 2325(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 1.492 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.104485 _exptl_absorpt_correction_T_max 0.351043 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 9644 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 23.25 _reflns_number_total 3306 _reflns_number_gt 2324 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0251P)^2^+5.8989P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3306 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1223 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.008 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 Ga1A Ga 0.53257(13) 0.59115(7) 0.64365(8) 0.0308(3) Uani 0.50 1 d P . . Ga1 Ga 0.6201(2) 0.59019(9) 0.68773(12) 0.0598(4) Uani 0.50 1 d P . . Cl1 Cl 0.66555(18) 0.64709(12) 0.55699(11) 0.0777(6) Uani 1 1 d . . . Cl2 Cl 0.60137(18) 0.46745(9) 0.66442(12) 0.0678(5) Uani 1 1 d . . . P1 P 0.4160(4) 0.6778(3) 0.7960(3) 0.0275(10) Uani 0.50 1 d P . . P1A P 0.4766(5) 0.6800(3) 0.8225(4) 0.0443(12) Uani 0.50 1 d P . . N1 N 0.4603(13) 0.6331(6) 0.7265(8) 0.069(3) Uani 0.50 1 d P . . N1A N 0.5683(8) 0.6442(4) 0.7727(5) 0.0253(18) Uani 0.50 1 d P . . C1 C 0.7928(16) 0.6132(6) 0.8155(6) 0.108(4) Uani 1 1 d . . . C2 C 0.9195(13) 0.6155(5) 0.8679(9) 0.114(4) Uani 1 1 d . . . H2A H 0.9879 0.5842 0.8492 0.137 Uiso 1 1 calc R . . C3 C 0.9557(8) 0.6584(5) 0.9442(7) 0.098(3) Uani 1 1 d . . . H3A H 1.0486 0.6592 0.9755 0.118 Uiso 1 1 calc R . . C4 C 0.8610(9) 0.7009(5) 0.9773(5) 0.091(3) Uani 1 1 d . . . H4A H 0.8859 0.7295 1.0336 0.109 Uiso 1 1 calc R . . C5 C 0.7240(8) 0.7023(5) 0.9272(7) 0.094(3) Uani 1 1 d . . . H5A H 0.6562 0.7327 0.9483 0.113 Uiso 1 1 calc R . . C6 C 0.6902(9) 0.6562(5) 0.8428(7) 0.087(3) Uani 1 1 d . . . C7 C 0.3884(6) 0.6376(3) 0.9124(3) 0.0413(13) Uani 1 1 d . . . C8 C 0.3914(7) 0.6767(4) 0.9979(4) 0.0631(18) Uani 1 1 d . . . H8A H 0.4179 0.7286 1.0028 0.076 Uiso 1 1 calc R . . C9 C 0.3556(8) 0.6394(5) 1.0750(4) 0.086(2) Uani 1 1 d . . . H9A H 0.3584 0.6662 1.1325 0.104 Uiso 1 1 calc R . . C10 C 0.3158(9) 0.5640(6) 1.0695(5) 0.090(3) Uani 1 1 d . . . H10A H 0.2910 0.5394 1.1226 0.107 Uiso 1 1 calc R . . C11 C 0.3125(7) 0.5247(4) 0.9861(6) 0.072(2) Uani 1 1 d . . . H11A H 0.2863 0.4728 0.9825 0.087 Uiso 1 1 calc R . . C12 C 0.3476(6) 0.5606(3) 0.9068(4) 0.0515(15) Uani 1 1 d . . . H12A H 0.3440 0.5333 0.8496 0.062 Uiso 1 1 calc R . . C13 C 0.4213(6) 0.7822(3) 0.8043(4) 0.0433(13) Uani 1 1 d . . . C14 C 0.5167(7) 0.8262(4) 0.7640(4) 0.0611(17) Uani 1 1 d . . . H14A H 0.5937 0.8026 0.7452 0.073 Uiso 1 1 calc R . . C15 C 0.4963(8) 0.9044(4) 0.7522(5) 0.0714(19) Uani 1 1 d . . . H15A H 0.5590 0.9339 0.7246 0.086 Uiso 1 1 calc R . . C16 C 0.3841(8) 0.9392(4) 0.7809(5) 0.069(2) Uani 1 1 d . . . H16A H 0.3717 0.9924 0.7727 0.083 Uiso 1 1 calc R . . C17 C 0.2891(7) 0.8971(4) 0.8215(4) 0.0622(18) Uani 1 1 d . . . H17A H 0.2126 0.9214 0.8402 0.075 Uiso 1 1 calc R . . C18 C 0.3087(6) 0.8184(3) 0.8343(4) 0.0545(15) Uani 1 1 d . . . H18A H 0.2463 0.7895 0.8631 0.065 Uiso 1 1 calc R . . C19 C 0.2969(9) 0.6397(5) 0.6876(7) 0.085(3) Uani 1 1 d . . . C20 C 0.3240(9) 0.6025(6) 0.6112(11) 0.106(4) Uani 1 1 d . . . C21 C 0.2151(12) 0.5853(4) 0.5376(6) 0.090(3) Uani 1 1 d . . . H21A H 0.2334 0.5616 0.4820 0.108 Uiso 1 1 calc R . . C22 C 0.0749(8) 0.6036(4) 0.5460(4) 0.069(2) Uani 1 1 d . . . H22A H -0.0002 0.5900 0.4983 0.083 Uiso 1 1 calc R . . C23 C 0.0548(6) 0.6422(4) 0.6274(5) 0.0617(17) Uani 1 1 d . . . H23A H -0.0349 0.6567 0.6350 0.074 Uiso 1 1 calc R . . C24 C 0.1658(9) 0.6590(4) 0.6962(4) 0.072(2) Uani 1 1 d . . . H24A H 0.1510 0.6847 0.7513 0.086 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 Ga1A 0.0211(6) 0.0440(8) 0.0265(6) -0.0036(5) 0.0020(5) 0.0009(6) Ga1 0.0785(12) 0.0523(10) 0.0587(9) -0.0028(8) 0.0395(9) 0.0041(9) Cl1 0.0533(10) 0.1251(16) 0.0595(10) 0.0255(10) 0.0231(8) -0.0061(10) Cl2 0.0760(12) 0.0528(10) 0.0755(11) -0.0180(8) 0.0159(9) 0.0098(8) P1 0.024(2) 0.0278(18) 0.032(2) 0.0001(16) 0.0067(16) 0.0048(19) P1A 0.052(3) 0.040(2) 0.045(3) 0.002(2) 0.017(2) 0.006(3) N1 0.070(9) 0.056(7) 0.089(8) -0.002(6) 0.034(7) 0.003(6) N1A 0.027(5) 0.026(5) 0.022(4) -0.010(3) 0.001(4) -0.001(4) C1 0.164(11) 0.109(8) 0.054(5) -0.014(5) 0.024(6) -0.075(8) C2 0.133(9) 0.066(6) 0.170(10) -0.041(6) 0.099(8) -0.021(6) C3 0.042(5) 0.082(6) 0.160(8) -0.019(6) -0.013(5) 0.007(4) C4 0.086(6) 0.095(6) 0.077(5) -0.038(4) -0.023(4) 0.007(5) C5 0.059(5) 0.074(6) 0.157(8) 0.026(6) 0.041(5) 0.036(4) C6 0.065(5) 0.079(6) 0.097(6) 0.049(5) -0.037(5) -0.037(4) C7 0.045(3) 0.039(3) 0.041(3) 0.002(3) 0.012(2) -0.001(3) C8 0.083(5) 0.064(4) 0.046(4) -0.007(3) 0.020(3) -0.004(4) C9 0.114(7) 0.109(7) 0.037(4) 0.001(4) 0.016(4) 0.012(5) C10 0.104(7) 0.109(7) 0.063(5) 0.042(5) 0.036(4) 0.017(5) C11 0.070(5) 0.055(4) 0.094(5) 0.024(4) 0.020(4) -0.009(3) C12 0.058(4) 0.047(4) 0.047(3) 0.006(3) 0.005(3) -0.005(3) C13 0.048(4) 0.032(3) 0.053(3) 0.000(3) 0.018(3) -0.001(3) C14 0.064(4) 0.051(4) 0.075(4) 0.011(3) 0.029(3) 0.008(3) C15 0.090(6) 0.044(4) 0.083(5) 0.020(4) 0.022(4) -0.006(4) C16 0.093(6) 0.033(4) 0.073(4) 0.003(3) -0.010(4) 0.009(4) C17 0.064(4) 0.048(4) 0.072(4) -0.009(3) 0.004(3) 0.025(3) C18 0.053(4) 0.048(4) 0.066(4) -0.013(3) 0.022(3) -0.004(3) C19 0.055(6) 0.067(6) 0.114(7) 0.056(5) -0.034(5) -0.030(4) C20 0.057(6) 0.096(8) 0.175(11) 0.081(8) 0.046(7) 0.017(5) C21 0.161(9) 0.060(5) 0.069(5) 0.015(4) 0.074(6) 0.029(6) C22 0.083(5) 0.066(5) 0.047(4) 0.012(3) -0.019(4) -0.024(4) C23 0.043(4) 0.064(4) 0.082(5) 0.017(4) 0.021(3) 0.014(3) C24 0.118(7) 0.050(4) 0.040(3) -0.004(3) -0.003(4) -0.022(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 Ga1A Ga1 0.9596(18) . ? Ga1A N1 1.636(11) . ? Ga1A C20 2.003(9) . ? Ga1A N1A 2.014(7) . ? Ga1A Cl1 2.157(2) . ? Ga1A Cl2 2.241(2) . ? Ga1 N1A 1.666(7) . ? Ga1 N1 1.885(11) . ? Ga1 Cl2 2.147(2) . ? Ga1 Cl1 2.203(2) . ? Ga1 C1 2.268(11) . ? Ga1 C6 2.455(11) . ? P1 P1A 0.640(4) . ? P1 N1 1.375(12) . ? P1 N1A 1.673(9) . ? P1 C13 1.806(7) . ? P1 C7 1.847(7) . ? P1 C19 1.866(9) . ? P1A N1A 1.374(9) . ? P1A N1 1.563(13) . ? P1A C7 1.807(8) . ? P1A C13 1.847(7) . ? P1A C6 2.080(11) . ? N1 N1A 1.147(12) . ? N1 C19 1.586(15) . ? N1A C6 1.416(10) . ? C1 C2 1.317(14) . ? C1 C6 1.352(13) . ? C2 C3 1.303(12) . ? C3 C4 1.323(11) . ? C4 C5 1.391(10) . ? C5 C6 1.422(12) . ? C7 C8 1.378(7) . ? C7 C12 1.385(7) . ? C8 C9 1.363(9) . ? C9 C10 1.357(10) . ? C10 C11 1.354(10) . ? C11 C12 1.376(8) . ? C13 C18 1.388(8) . ? C13 C14 1.393(8) . ? C14 C15 1.371(9) . ? C15 C16 1.365(9) . ? C16 C17 1.377(9) . ? C17 C18 1.380(8) . ? C19 C20 1.321(13) . ? C19 C24 1.341(11) . ? C20 C21 1.375(13) . ? C21 C22 1.421(11) . ? C22 C23 1.371(9) . ? C23 C24 1.347(9) . ? 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 Ga1 Ga1A N1 89.2(5) . . ? Ga1 Ga1A C20 153.1(5) . . ? N1 Ga1A C20 65.0(6) . . ? Ga1 Ga1A N1A 55.3(2) . . ? N1 Ga1A N1A 34.7(4) . . ? C20 Ga1A N1A 99.6(5) . . ? Ga1 Ga1A Cl1 80.02(13) . . ? N1 Ga1A Cl1 125.6(4) . . ? C20 Ga1A Cl1 120.5(3) . . ? N1A Ga1A Cl1 106.6(2) . . ? Ga1 Ga1A Cl2 71.95(13) . . ? N1 Ga1A Cl2 118.9(4) . . ? C20 Ga1A Cl2 112.8(3) . . ? N1A Ga1A Cl2 108.4(2) . . ? Cl1 Ga1A Cl2 107.86(9) . . ? Ga1A Ga1 N1A 96.5(3) . . ? Ga1A Ga1 N1 60.2(4) . . ? N1A Ga1 N1 37.1(4) . . ? Ga1A Ga1 Cl2 82.90(14) . . ? N1A Ga1 Cl2 129.4(3) . . ? N1 Ga1 Cl2 112.4(3) . . ? Ga1A Ga1 Cl1 74.59(13) . . ? N1A Ga1 Cl1 119.0(3) . . ? N1 Ga1 Cl1 111.4(4) . . ? Cl2 Ga1 Cl1 109.60(10) . . ? Ga1A Ga1 C1 163.0(4) . . ? N1A Ga1 C1 66.6(4) . . ? N1 Ga1 C1 103.2(5) . . ? Cl2 Ga1 C1 109.0(3) . . ? Cl1 Ga1 C1 111.1(2) . . ? Ga1A Ga1 C6 130.1(3) . . ? N1A Ga1 C6 33.8(4) . . ? N1 Ga1 C6 70.7(5) . . ? Cl2 Ga1 C6 126.67(19) . . ? Cl1 Ga1 C6 118.41(19) . . ? C1 Ga1 C6 33.0(3) . . ? Ga1A Cl1 Ga1 25.40(5) . . ? Ga1 Cl2 Ga1A 25.15(5) . . ? P1A P1 N1 94.6(11) . . ? P1A P1 N1A 52.0(9) . . ? N1 P1 N1A 42.9(5) . . ? P1A P1 C13 83.6(9) . . ? N1 P1 C13 126.7(6) . . ? N1A P1 C13 110.0(4) . . ? P1A P1 C7 76.4(9) . . ? N1 P1 C7 122.5(6) . . ? N1A P1 C7 108.5(4) . . ? C13 P1 C7 108.9(3) . . ? P1A P1 C19 150.7(11) . . ? N1 P1 C19 56.2(7) . . ? N1A P1 C19 99.0(5) . . ? C13 P1 C19 114.3(4) . . ? C7 P1 C19 115.6(4) . . ? P1 P1A N1A 106.5(10) . . ? P1 P1A N1 61.3(10) . . ? N1A P1A N1 45.4(5) . . ? P1 P1A C7 83.5(9) . . ? N1A P1A C7 127.4(5) . . ? N1 P1A C7 114.3(5) . . ? P1 P1A C13 76.3(9) . . ? N1A P1A C13 123.8(5) . . ? N1 P1A C13 113.1(5) . . ? C7 P1A C13 108.8(4) . . ? P1 P1A C6 149.0(11) . . ? N1A P1A C6 42.5(5) . . ? N1 P1A C6 87.8(6) . . ? C7 P1A C6 114.0(4) . . ? C13 P1A C6 117.7(4) . . ? N1A N1 P1 82.6(8) . . ? N1A N1 P1A 58.6(7) . . ? P1 N1 P1A 24.1(3) . . ? N1A N1 C19 160.1(11) . . ? P1 N1 C19 77.8(7) . . ? P1A N1 C19 101.8(8) . . ? N1A N1 Ga1A 91.0(8) . . ? P1 N1 Ga1A 170.5(9) . . ? P1A N1 Ga1A 149.3(9) . . ? C19 N1 Ga1A 108.2(8) . . ? N1A N1 Ga1 61.1(6) . . ? P1 N1 Ga1 143.6(9) . . ? P1A N1 Ga1 119.6(8) . . ? C19 N1 Ga1 138.5(9) . . ? Ga1A N1 Ga1 30.6(2) . . ? N1 N1A P1A 76.0(7) . . ? N1 N1A C6 170.5(10) . . ? P1A N1A C6 96.4(7) . . ? N1 N1A Ga1 81.9(7) . . ? P1A N1A Ga1 157.7(6) . . ? C6 N1A Ga1 105.4(7) . . ? N1 N1A P1 54.6(7) . . ? P1A N1A P1 21.5(3) . . ? C6 N1A P1 117.9(7) . . ? Ga1 N1A P1 136.5(5) . . ? N1 N1A Ga1A 54.3(6) . . ? P1A N1A Ga1A 130.1(5) . . ? C6 N1A Ga1A 133.4(7) . . ? Ga1 N1A Ga1A 28.26(13) . . ? P1 N1A Ga1A 108.6(4) . . ? C2 C1 C6 118.9(8) . . ? C2 C1 Ga1 159.3(10) . . ? C6 C1 Ga1 81.2(8) . . ? C3 C2 C1 124.7(9) . . ? C2 C3 C4 120.3(8) . . ? C3 C4 C5 119.4(7) . . ? C4 C5 C6 118.3(7) . . ? C1 C6 N1A 106.6(11) . . ? C1 C6 C5 118.3(7) . . ? N1A C6 C5 135.0(10) . . ? C1 C6 P1A 146.6(9) . . ? N1A C6 P1A 41.0(4) . . ? C5 C6 P1A 94.6(8) . . ? C1 C6 Ga1 65.9(7) . . ? N1A C6 Ga1 40.9(5) . . ? C5 C6 Ga1 173.4(6) . . ? P1A C6 Ga1 81.8(3) . . ? C8 C7 C12 118.8(5) . . ? C8 C7 P1A 118.5(5) . . ? C12 C7 P1A 121.0(4) . . ? C8 C7 P1 127.7(5) . . ? C12 C7 P1 113.2(4) . . ? P1A C7 P1 20.14(14) . . ? C9 C8 C7 120.0(6) . . ? C8 C9 C10 121.2(7) . . ? C11 C10 C9 119.6(7) . . ? C10 C11 C12 120.8(7) . . ? C11 C12 C7 119.7(6) . . ? C18 C13 C14 119.7(5) . . ? C18 C13 P1 117.0(4) . . ? C14 C13 P1 122.0(5) . . ? C18 C13 P1A 127.7(5) . . ? C14 C13 P1A 112.3(5) . . ? P1 C13 P1A 20.14(14) . . ? C15 C14 C13 119.6(6) . . ? C16 C15 C14 120.2(6) . . ? C15 C16 C17 121.3(6) . . ? C18 C17 C16 119.2(6) . . ? C17 C18 C13 120.0(6) . . ? C20 C19 C24 121.6(8) . . ? C20 C19 N1 85.3(10) . . ? C24 C19 N1 153.0(10) . . ? C20 C19 P1 131.1(10) . . ? C24 C19 P1 107.3(8) . . ? N1 C19 P1 46.1(5) . . ? C19 C20 C21 119.0(8) . . ? C19 C20 Ga1A 101.5(10) . . ? C21 C20 Ga1A 139.5(11) . . ? C20 C21 C22 120.4(7) . . ? C23 C22 C21 117.3(6) . . ? C24 C23 C22 119.7(7) . . ? C19 C24 C23 122.0(7) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.300 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.058 #===end data__{(C6H4PPh2NPh)PdCl]2 _database_code_CSD 211248 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C48 H38 Cl2 N2 P2 Pd2' _chemical_formula_weight 988.44 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.509(8) _cell_length_b 14.847(9) _cell_length_c 22.963(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.363(12) _cell_angle_gamma 90.00 _cell_volume 4208(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.173671 _exptl_absorpt_correction_T_max 0.256602 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 8873 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 23.23 _reflns_number_total 3008 _reflns_number_gt 2377 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0156P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3008 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0193 _refine_ls_wR_factor_ref 0.0373 _refine_ls_wR_factor_gt 0.0367 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 Pd1 Pd 0.120444(16) 0.471588(12) 0.275016(8) 0.03894(7) Uani 1 1 d . . . Cl1 Cl 0.03895(5) 0.40739(4) 0.18513(3) 0.05037(18) Uani 1 1 d . . . P1 P 0.23392(6) 0.62417(4) 0.34751(3) 0.04454(18) Uani 1 1 d . . . N1 N 0.19167(16) 0.52267(13) 0.35475(8) 0.0455(5) Uani 1 1 d . . . C1 C 0.2741(2) 0.61907(16) 0.27650(11) 0.0410(6) Uani 1 1 d . . . C2 C 0.3416(2) 0.68189(17) 0.25557(12) 0.0514(7) Uani 1 1 d . . . H2A H 0.3713 0.7289 0.2797 0.062 Uiso 1 1 calc R . . C3 C 0.3642(2) 0.6740(2) 0.19875(14) 0.0598(8) Uani 1 1 d . . . H3A H 0.4096 0.7152 0.1845 0.072 Uiso 1 1 calc R . . C4 C 0.3184(2) 0.6040(2) 0.16334(13) 0.0603(8) Uani 1 1 d . . . H4A H 0.3336 0.5983 0.1252 0.072 Uiso 1 1 calc R . . C5 C 0.2501(2) 0.54209(18) 0.18386(12) 0.0504(7) Uani 1 1 d . . . H5A H 0.2197 0.4961 0.1590 0.061 Uiso 1 1 calc R . . C6 C 0.22618(19) 0.54759(15) 0.24100(11) 0.0390(6) Uani 1 1 d . . . C7 C 0.1295(2) 0.70938(17) 0.34469(11) 0.0487(7) Uani 1 1 d . . . C8 C 0.1505(3) 0.80095(19) 0.33783(15) 0.0761(10) Uani 1 1 d . . . H8A H 0.2211 0.8207 0.3379 0.091 Uiso 1 1 calc R . . C9 C 0.0660(3) 0.8618(2) 0.33102(17) 0.0925(12) Uani 1 1 d . . . H9A H 0.0804 0.9227 0.3270 0.111 Uiso 1 1 calc R . . C10 C -0.0395(3) 0.8337(2) 0.33008(14) 0.0778(10) Uani 1 1 d . . . H10A H -0.0957 0.8754 0.3253 0.093 Uiso 1 1 calc R . . C11 C -0.0610(2) 0.7435(2) 0.33632(12) 0.0639(8) Uani 1 1 d . . . H11A H -0.1319 0.7241 0.3356 0.077 Uiso 1 1 calc R . . C12 C 0.0232(2) 0.68157(18) 0.34366(11) 0.0517(7) Uani 1 1 d . . . H12A H 0.0083 0.6208 0.3479 0.062 Uiso 1 1 calc R . . C13 C 0.3468(2) 0.64902(18) 0.40491(11) 0.0490(7) Uani 1 1 d . . . C14 C 0.4332(2) 0.59003(19) 0.41122(12) 0.0557(8) Uani 1 1 d . . . H14A H 0.4353 0.5457 0.3828 0.067 Uiso 1 1 calc R . . C15 C 0.5170(2) 0.5950(2) 0.45861(13) 0.0620(8) Uani 1 1 d . . . H15A H 0.5746 0.5547 0.4618 0.074 Uiso 1 1 calc R . . C16 C 0.5143(3) 0.6597(3) 0.50061(14) 0.0836(11) Uani 1 1 d . . . H16A H 0.5695 0.6632 0.5330 0.100 Uiso 1 1 calc R . . C17 C 0.4306(3) 0.7190(3) 0.49484(17) 0.1176(16) Uani 1 1 d . . . H17A H 0.4299 0.7636 0.5232 0.141 Uiso 1 1 calc R . . C18 C 0.3458(3) 0.7147(2) 0.44751(15) 0.0935(12) Uani 1 1 d . . . H18A H 0.2889 0.7557 0.4445 0.112 Uiso 1 1 calc R . . C19 C 0.17920(19) 0.48211(19) 0.40885(11) 0.0471(7) Uani 1 1 d . . . C20 C 0.1874(2) 0.3886(2) 0.41312(13) 0.0614(8) Uani 1 1 d . . . H20A H 0.2029 0.3553 0.3812 0.074 Uiso 1 1 calc R . . C21 C 0.1728(3) 0.3453(3) 0.46415(19) 0.0899(12) Uani 1 1 d . . . H21A H 0.1771 0.2828 0.4661 0.108 Uiso 1 1 calc R . . C22 C 0.1519(3) 0.3930(4) 0.51256(18) 0.0997(14) Uani 1 1 d . . . H22A H 0.1424 0.3629 0.5469 0.120 Uiso 1 1 calc R . . C23 C 0.1453(3) 0.4848(3) 0.50985(14) 0.0900(11) Uani 1 1 d . . . H23A H 0.1321 0.5174 0.5425 0.108 Uiso 1 1 calc R . . C24 C 0.1583(2) 0.5297(2) 0.45781(12) 0.0664(8) Uani 1 1 d . . . H24A H 0.1529 0.5922 0.4560 0.080 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 Pd1 0.03992(12) 0.03297(10) 0.04195(12) -0.00340(11) 0.00077(8) -0.00160(11) Cl1 0.0470(4) 0.0468(4) 0.0531(4) -0.0157(3) -0.0043(3) 0.0070(3) P1 0.0427(5) 0.0447(4) 0.0460(5) -0.0105(3) 0.0067(3) -0.0085(3) N1 0.0518(14) 0.0465(12) 0.0369(13) -0.0037(11) 0.0033(10) -0.0122(12) C1 0.0362(16) 0.0401(15) 0.0464(17) -0.0009(12) 0.0058(12) -0.0025(13) C2 0.0423(18) 0.0534(17) 0.057(2) 0.0002(15) 0.0026(14) -0.0051(14) C3 0.0384(19) 0.072(2) 0.070(2) 0.0202(18) 0.0109(16) -0.0012(16) C4 0.047(2) 0.088(2) 0.0489(19) 0.0051(17) 0.0157(15) 0.0070(18) C5 0.0436(18) 0.0558(18) 0.0521(18) -0.0071(14) 0.0082(13) 0.0041(15) C6 0.0355(15) 0.0404(15) 0.0412(16) 0.0014(12) 0.0064(12) 0.0043(12) C7 0.0439(19) 0.0479(17) 0.0545(18) -0.0119(13) 0.0085(14) -0.0080(14) C8 0.050(2) 0.0523(19) 0.130(3) -0.0155(19) 0.0259(19) -0.0078(17) C9 0.065(3) 0.0479(19) 0.168(4) -0.010(2) 0.029(2) -0.0049(19) C10 0.060(2) 0.061(2) 0.114(3) -0.0156(19) 0.016(2) 0.0048(18) C11 0.043(2) 0.069(2) 0.079(2) -0.0155(17) 0.0111(16) -0.0110(17) C12 0.048(2) 0.0489(16) 0.0576(19) -0.0124(14) 0.0078(14) -0.0098(15) C13 0.0445(19) 0.0567(17) 0.0465(18) -0.0135(14) 0.0100(13) -0.0108(15) C14 0.061(2) 0.0562(18) 0.050(2) -0.0084(14) 0.0094(16) -0.0062(16) C15 0.049(2) 0.080(2) 0.056(2) 0.0068(18) 0.0055(16) -0.0016(17) C16 0.055(3) 0.132(3) 0.060(2) -0.025(2) -0.0037(18) -0.015(2) C17 0.067(3) 0.159(4) 0.116(3) -0.093(3) -0.016(2) 0.009(3) C18 0.057(2) 0.113(3) 0.103(3) -0.065(2) -0.009(2) 0.009(2) C19 0.0375(16) 0.0620(19) 0.0390(17) 0.0025(15) -0.0023(12) -0.0068(15) C20 0.048(2) 0.069(2) 0.062(2) 0.0197(16) -0.0052(15) -0.0008(16) C21 0.077(3) 0.094(3) 0.089(3) 0.044(3) -0.013(2) -0.003(2) C22 0.079(3) 0.146(4) 0.069(3) 0.051(3) -0.006(2) -0.019(3) C23 0.074(3) 0.147(4) 0.048(2) 0.004(2) 0.0082(16) -0.015(3) C24 0.066(2) 0.086(2) 0.047(2) 0.0029(19) 0.0081(15) -0.0088(19) _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 C6 1.992(2) . ? Pd1 N1 2.047(2) . ? Pd1 Cl1 2.3502(12) . ? Pd1 Cl1 2.5130(13) 2 ? Pd1 Pd1 3.0453(17) 2 ? Cl1 Pd1 2.5130(13) 2 ? P1 N1 1.614(2) . ? P1 C1 1.784(3) . ? P1 C13 1.806(3) . ? P1 C7 1.812(3) . ? N1 C19 1.412(3) . ? C1 C2 1.395(3) . ? C1 C6 1.411(3) . ? C2 C3 1.384(4) . ? C3 C4 1.385(4) . ? C4 C5 1.388(4) . ? C5 C6 1.395(3) . ? C7 C12 1.388(3) . ? C7 C8 1.399(4) . ? C8 C9 1.380(4) . ? C9 C10 1.381(4) . ? C10 C11 1.378(4) . ? C11 C12 1.388(4) . ? C13 C14 1.381(4) . ? C13 C18 1.383(4) . ? C14 C15 1.385(4) . ? C15 C16 1.366(4) . ? C16 C17 1.358(5) . ? C17 C18 1.391(4) . ? C19 C24 1.388(4) . ? C19 C20 1.395(4) . ? C20 C21 1.375(4) . ? C21 C22 1.379(5) . ? C22 C23 1.366(5) . ? C23 C24 1.401(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Pd1 N1 85.45(10) . . ? C6 Pd1 Cl1 96.09(8) . . ? N1 Pd1 Cl1 177.79(6) . . ? C6 Pd1 Cl1 166.98(7) . 2 ? N1 Pd1 Cl1 94.04(7) . 2 ? Cl1 Pd1 Cl1 84.81(4) . 2 ? C6 Pd1 Pd1 122.10(7) . 2 ? N1 Pd1 Pd1 126.68(6) . 2 ? Cl1 Pd1 Pd1 53.66(2) . 2 ? Cl1 Pd1 Pd1 48.88(3) 2 2 ? Pd1 Cl1 Pd1 77.46(4) . 2 ? N1 P1 C1 101.54(10) . . ? N1 P1 C13 110.22(12) . . ? C1 P1 C13 111.88(13) . . ? N1 P1 C7 114.15(12) . . ? C1 P1 C7 107.79(12) . . ? C13 P1 C7 110.91(13) . . ? C19 N1 P1 125.01(17) . . ? C19 N1 Pd1 122.32(16) . . ? P1 N1 Pd1 110.84(11) . . ? C2 C1 C6 121.9(2) . . ? C2 C1 P1 124.25(19) . . ? C6 C1 P1 113.80(19) . . ? C3 C2 C1 119.7(3) . . ? C2 C3 C4 119.3(3) . . ? C3 C4 C5 121.1(3) . . ? C4 C5 C6 121.2(3) . . ? C5 C6 C1 116.8(2) . . ? C5 C6 Pd1 126.39(19) . . ? C1 C6 Pd1 116.50(18) . . ? C12 C7 C8 119.0(3) . . ? C12 C7 P1 118.4(2) . . ? C8 C7 P1 122.3(2) . . ? C9 C8 C7 119.6(3) . . ? C8 C9 C10 121.1(3) . . ? C11 C10 C9 119.6(3) . . ? C10 C11 C12 120.0(3) . . ? C11 C12 C7 120.7(3) . . ? C14 C13 C18 118.0(3) . . ? C14 C13 P1 116.9(2) . . ? C18 C13 P1 124.4(2) . . ? C13 C14 C15 121.9(3) . . ? C16 C15 C14 119.3(3) . . ? C17 C16 C15 119.7(3) . . ? C16 C17 C18 121.6(3) . . ? C13 C18 C17 119.5(3) . . ? C24 C19 C20 118.1(3) . . ? C24 C19 N1 123.9(3) . . ? C20 C19 N1 118.0(2) . . ? C21 C20 C19 120.5(3) . . ? C20 C21 C22 121.0(4) . . ? C23 C22 C21 119.6(3) . . ? C22 C23 C24 119.9(3) . . ? C19 C24 C23 120.8(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.23 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.214 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.044 #===end data_{(C6H4PPh2NPh)2PdCH2Cl2 _database_code_CSD 211249 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C49 H40 Cl2 N2 P2 Pd' _chemical_formula_weight 896.07 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.543(9) _cell_length_b 10.026(6) _cell_length_c 29.194(17) _cell_angle_alpha 90.00 _cell_angle_beta 95.731(11) _cell_angle_gamma 90.00 _cell_volume 4235(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 0.677 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.180604 _exptl_absorpt_correction_T_max 0.256563 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 17288 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 23.23 _reflns_number_total 6030 _reflns_number_gt 4242 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0345P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6030 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0691 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _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 0.728459(16) -0.11541(3) 0.895264(9) 0.03662(10) Uani 1 1 d . . . Cl1 Cl 0.23068(12) 0.38187(18) 0.86666(6) 0.1240(5) Uani 1 1 d . . . Cl2 Cl 0.22264(9) 0.09410(17) 0.85279(5) 0.1060(5) Uani 1 1 d . . . N1 N 0.66693(17) 0.0385(3) 0.85119(10) 0.0418(7) Uani 1 1 d . . . N2 N 0.86521(17) -0.0261(3) 0.90264(10) 0.0396(7) Uani 1 1 d . . . P1 P 0.56128(6) 0.04530(10) 0.86181(3) 0.0382(2) Uani 1 1 d . . . P2 P 0.93212(6) -0.15372(9) 0.90281(3) 0.0394(2) Uani 1 1 d . . . C1 C 0.6049(2) -0.2068(4) 0.88623(11) 0.0367(9) Uani 1 1 d . . . C2 C 0.5291(2) -0.1234(4) 0.87172(11) 0.0402(8) Uani 1 1 d . . . C3 C 0.4395(2) -0.1740(4) 0.86240(12) 0.0502(10) Uani 1 1 d . . . H3A H 0.3909 -0.1166 0.8531 0.060 Uiso 1 1 calc R . . C4 C 0.4229(3) -0.3078(4) 0.86694(13) 0.0575(11) Uani 1 1 d . . . H4A H 0.3632 -0.3415 0.8614 0.069 Uiso 1 1 calc R . . C5 C 0.4961(2) -0.3917(4) 0.87992(12) 0.0549(10) Uani 1 1 d . . . H5A H 0.4854 -0.4828 0.8822 0.066 Uiso 1 1 calc R . . C6 C 0.5857(2) -0.3431(4) 0.88962(12) 0.0444(9) Uani 1 1 d . . . H6A H 0.6335 -0.4022 0.8985 0.053 Uiso 1 1 calc R . . C7 C 0.7042(2) 0.0948(4) 0.81249(12) 0.0393(9) Uani 1 1 d . . . C8 C 0.6831(2) 0.2236(4) 0.79626(14) 0.0554(11) Uani 1 1 d . . . H8A H 0.6457 0.2781 0.8123 0.066 Uiso 1 1 calc R . . C9 C 0.7169(3) 0.2714(5) 0.75677(16) 0.0710(13) Uani 1 1 d . . . H9A H 0.6997 0.3558 0.7459 0.085 Uiso 1 1 calc R . . C10 C 0.7754(3) 0.1960(6) 0.73354(15) 0.0760(15) Uani 1 1 d . . . H10A H 0.7979 0.2284 0.7070 0.091 Uiso 1 1 calc R . . C11 C 0.8004(3) 0.0713(5) 0.75014(14) 0.0635(13) Uani 1 1 d . . . H11A H 0.8413 0.0201 0.7351 0.076 Uiso 1 1 calc R . . C12 C 0.7652(2) 0.0211(4) 0.78914(13) 0.0470(10) Uani 1 1 d . . . H12A H 0.7828 -0.0635 0.7997 0.056 Uiso 1 1 calc R . . C13 C 0.5471(2) 0.1412(4) 0.91300(12) 0.0418(9) Uani 1 1 d . . . C14 C 0.6005(3) 0.2516(4) 0.92377(14) 0.0554(11) Uani 1 1 d . . . H14A H 0.6443 0.2773 0.9043 0.066 Uiso 1 1 calc R . . C15 C 0.5906(3) 0.3256(5) 0.96308(17) 0.0743(13) Uani 1 1 d . . . H15A H 0.6276 0.4001 0.9699 0.089 Uiso 1 1 calc R . . C16 C 0.5256(4) 0.2882(6) 0.99213(16) 0.0804(15) Uani 1 1 d . . . H16A H 0.5183 0.3380 1.0184 0.096 Uiso 1 1 calc R . . C17 C 0.4726(4) 0.1789(6) 0.98223(17) 0.0828(15) Uani 1 1 d . . . H17A H 0.4296 0.1530 1.0021 0.099 Uiso 1 1 calc R . . C18 C 0.4817(3) 0.1054(5) 0.94280(14) 0.0648(11) Uani 1 1 d . . . H18A H 0.4440 0.0316 0.9361 0.078 Uiso 1 1 calc R . . C19 C 0.4838(2) 0.1140(4) 0.81536(11) 0.0391(8) Uani 1 1 d . . . C20 C 0.4748(2) 0.0466(4) 0.77399(13) 0.0541(10) Uani 1 1 d . . . H20A H 0.5038 -0.0354 0.7716 0.065 Uiso 1 1 calc R . . C21 C 0.4231(3) 0.0996(5) 0.73594(13) 0.0656(12) Uani 1 1 d . . . H21A H 0.4169 0.0532 0.7082 0.079 Uiso 1 1 calc R . . C22 C 0.3810(3) 0.2217(5) 0.73943(16) 0.0639(13) Uani 1 1 d . . . H22A H 0.3473 0.2589 0.7138 0.077 Uiso 1 1 calc R . . C23 C 0.3886(3) 0.2882(5) 0.78038(15) 0.0621(12) Uani 1 1 d . . . H23A H 0.3593 0.3700 0.7827 0.074 Uiso 1 1 calc R . . C24 C 0.4399(2) 0.2346(4) 0.81853(13) 0.0499(10) Uani 1 1 d . . . H24A H 0.4445 0.2803 0.8464 0.060 Uiso 1 1 calc R . . C25 C 0.7847(2) -0.2521(3) 0.93964(11) 0.0356(8) Uani 1 1 d . . . C26 C 0.8821(2) -0.2622(3) 0.94208(11) 0.0371(8) Uani 1 1 d . . . C27 C 0.9333(3) -0.3357(4) 0.97662(13) 0.0513(10) Uani 1 1 d . . . H27A H 0.9974 -0.3389 0.9777 0.062 Uiso 1 1 calc R . . C28 C 0.8881(3) -0.4038(4) 1.00912(13) 0.0592(11) Uani 1 1 d . . . H28A H 0.9217 -0.4515 1.0324 0.071 Uiso 1 1 calc R . . C29 C 0.7928(3) -0.4003(4) 1.00664(12) 0.0543(10) Uani 1 1 d . . . H29A H 0.7621 -0.4482 1.0277 0.065 Uiso 1 1 calc R . . C30 C 0.7429(2) -0.3256(4) 0.97280(12) 0.0451(9) Uani 1 1 d . . . H30A H 0.6788 -0.3241 0.9720 0.054 Uiso 1 1 calc R . . C31 C 0.9333(2) -0.2342(4) 0.84700(12) 0.0430(9) Uani 1 1 d . . . C32 C 0.8677(3) -0.3285(4) 0.83251(15) 0.0608(11) Uani 1 1 d . . . H32A H 0.8259 -0.3576 0.8524 0.073 Uiso 1 1 calc R . . C33 C 0.8640(3) -0.3805(5) 0.78773(17) 0.0805(14) Uani 1 1 d . . . H33A H 0.8197 -0.4442 0.7781 0.097 Uiso 1 1 calc R . . C34 C 0.9242(3) -0.3385(6) 0.75858(17) 0.0878(17) Uani 1 1 d . . . H34A H 0.9215 -0.3744 0.7291 0.105 Uiso 1 1 calc R . . C35 C 0.9898(3) -0.2428(6) 0.77186(16) 0.0796(15) Uani 1 1 d . . . H35A H 1.0304 -0.2133 0.7513 0.096 Uiso 1 1 calc R . . C36 C 0.9947(3) -0.1917(4) 0.81588(14) 0.0592(11) Uani 1 1 d . . . H36A H 1.0393 -0.1280 0.8251 0.071 Uiso 1 1 calc R . . C37 C 1.0522(2) -0.1281(4) 0.92412(11) 0.0413(9) Uani 1 1 d . . . C38 C 1.0765(2) -0.0216(4) 0.95380(12) 0.0474(10) Uani 1 1 d . . . H38A H 1.0324 0.0415 0.9598 0.057 Uiso 1 1 calc R . . C39 C 1.1663(3) -0.0102(4) 0.97419(13) 0.0576(11) Uani 1 1 d . . . H39A H 1.1822 0.0607 0.9939 0.069 Uiso 1 1 calc R . . C40 C 1.2319(3) -0.1026(5) 0.96559(14) 0.0652(12) Uani 1 1 d . . . H40A H 1.2922 -0.0937 0.9793 0.078 Uiso 1 1 calc R . . C41 C 1.2087(3) -0.2090(5) 0.93663(15) 0.0671(13) Uani 1 1 d . . . H41A H 1.2532 -0.2722 0.9312 0.080 Uiso 1 1 calc R . . C42 C 1.1193(2) -0.2217(4) 0.91566(13) 0.0556(11) Uani 1 1 d . . . H42A H 1.1041 -0.2929 0.8959 0.067 Uiso 1 1 calc R . . C43 C 0.8884(2) 0.1069(4) 0.89417(11) 0.0384(9) Uani 1 1 d . . . C44 C 0.9510(3) 0.1459(4) 0.86397(14) 0.0562(11) Uani 1 1 d . . . H44A H 0.9781 0.0817 0.8466 0.067 Uiso 1 1 calc R . . C45 C 0.9738(3) 0.2790(5) 0.85923(16) 0.0699(13) Uani 1 1 d . . . H45A H 1.0162 0.3028 0.8388 0.084 Uiso 1 1 calc R . . C46 C 0.9355(3) 0.3748(5) 0.88373(18) 0.0771(14) Uani 1 1 d . . . H46A H 0.9526 0.4636 0.8809 0.092 Uiso 1 1 calc R . . C47 C 0.8703(3) 0.3393(4) 0.91315(17) 0.0709(13) Uani 1 1 d . . . H47A H 0.8422 0.4046 0.9296 0.085 Uiso 1 1 calc R . . C48 C 0.8471(3) 0.2062(4) 0.91807(14) 0.0528(10) Uani 1 1 d . . . H48A H 0.8030 0.1832 0.9377 0.063 Uiso 1 1 calc R . . C49 C 0.2201(4) 0.2265(5) 0.89216(17) 0.1062(18) Uani 1 1 d . . . H49A H 0.1623 0.2234 0.9061 0.127 Uiso 1 1 calc R . . H49B H 0.2700 0.2152 0.9165 0.127 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 Pd1 0.03150(14) 0.03819(16) 0.03939(17) 0.00185(17) -0.00036(10) 0.00398(14) Cl1 0.1485(13) 0.1144(12) 0.1164(12) 0.0273(12) 0.0495(10) -0.0039(11) Cl2 0.0927(9) 0.1250(13) 0.1006(10) 0.0090(10) 0.0110(7) -0.0009(9) N1 0.0321(15) 0.0461(18) 0.0469(19) 0.0112(16) 0.0022(13) 0.0067(13) N2 0.0336(15) 0.0357(18) 0.0491(19) -0.0032(16) 0.0020(13) 0.0040(13) P1 0.0326(5) 0.0417(5) 0.0398(6) 0.0047(5) 0.0014(4) 0.0054(4) P2 0.0328(5) 0.0407(6) 0.0439(6) -0.0028(5) -0.0007(4) 0.0051(4) C1 0.0387(19) 0.043(2) 0.028(2) -0.0010(19) 0.0019(15) -0.0001(17) C2 0.0352(18) 0.048(2) 0.037(2) 0.001(2) 0.0048(15) 0.0056(18) C3 0.038(2) 0.061(3) 0.051(2) 0.003(2) 0.0013(17) 0.0016(19) C4 0.039(2) 0.065(3) 0.067(3) 0.003(3) -0.0041(19) -0.016(2) C5 0.064(2) 0.049(2) 0.051(2) 0.003(2) -0.0005(19) -0.011(2) C6 0.049(2) 0.044(2) 0.039(2) 0.002(2) -0.0034(17) 0.0020(17) C7 0.0307(17) 0.045(2) 0.041(2) 0.003(2) -0.0040(16) -0.0036(17) C8 0.047(2) 0.057(3) 0.062(3) 0.010(3) 0.008(2) -0.001(2) C9 0.052(3) 0.078(3) 0.081(4) 0.034(3) 0.000(2) -0.010(2) C10 0.049(3) 0.125(5) 0.053(3) 0.029(3) 0.000(2) -0.016(3) C11 0.047(2) 0.099(4) 0.045(3) -0.006(3) 0.007(2) -0.001(2) C12 0.038(2) 0.059(3) 0.043(2) -0.002(2) -0.0030(18) 0.0004(19) C13 0.042(2) 0.042(2) 0.040(2) 0.003(2) -0.0015(17) 0.0078(18) C14 0.057(2) 0.057(3) 0.051(3) -0.002(2) 0.0012(19) 0.005(2) C15 0.088(3) 0.064(3) 0.068(3) -0.012(3) -0.008(3) 0.004(3) C16 0.109(4) 0.084(4) 0.048(3) -0.017(3) 0.003(3) 0.027(3) C17 0.105(4) 0.086(4) 0.063(3) -0.003(3) 0.036(3) 0.017(3) C18 0.074(3) 0.062(3) 0.062(3) -0.004(3) 0.020(2) 0.003(2) C19 0.0307(17) 0.050(2) 0.037(2) 0.008(2) 0.0032(14) 0.0013(18) C20 0.054(2) 0.061(3) 0.046(3) 0.004(2) -0.0007(19) 0.010(2) C21 0.074(3) 0.079(4) 0.042(2) 0.002(3) -0.004(2) -0.003(3) C22 0.050(2) 0.085(4) 0.054(3) 0.030(3) -0.008(2) -0.004(2) C23 0.057(2) 0.067(3) 0.062(3) 0.019(3) 0.003(2) 0.017(2) C24 0.050(2) 0.054(3) 0.045(2) 0.003(2) 0.0005(18) 0.010(2) C25 0.0365(19) 0.035(2) 0.034(2) -0.0037(18) -0.0027(15) 0.0018(16) C26 0.040(2) 0.032(2) 0.039(2) -0.0034(19) -0.0019(16) 0.0040(16) C27 0.047(2) 0.047(2) 0.057(3) 0.003(2) -0.007(2) 0.0097(18) C28 0.070(3) 0.055(3) 0.049(3) 0.013(2) -0.011(2) 0.014(2) C29 0.065(3) 0.052(3) 0.045(2) 0.010(2) 0.0013(19) -0.001(2) C30 0.046(2) 0.048(2) 0.040(2) 0.000(2) 0.0005(18) 0.0023(18) C31 0.0365(19) 0.045(2) 0.046(2) -0.006(2) -0.0043(18) 0.0120(18) C32 0.052(2) 0.063(3) 0.065(3) -0.013(3) -0.003(2) 0.006(2) C33 0.065(3) 0.098(4) 0.075(3) -0.037(3) -0.015(3) 0.000(3) C34 0.075(3) 0.126(5) 0.061(3) -0.038(3) 0.002(3) 0.017(3) C35 0.065(3) 0.119(4) 0.055(3) -0.013(3) 0.009(2) 0.014(3) C36 0.050(2) 0.073(3) 0.055(3) -0.012(3) 0.005(2) 0.006(2) C37 0.0395(19) 0.047(2) 0.038(2) -0.001(2) 0.0035(16) 0.0044(19) C38 0.043(2) 0.056(3) 0.043(2) -0.002(2) 0.0028(18) 0.0044(18) C39 0.056(3) 0.070(3) 0.045(2) -0.006(2) -0.003(2) -0.011(2) C40 0.039(2) 0.093(4) 0.061(3) 0.007(3) -0.0099(19) -0.006(3) C41 0.038(2) 0.084(3) 0.078(3) 0.002(3) 0.001(2) 0.016(2) C42 0.045(2) 0.060(3) 0.060(3) -0.011(2) -0.0029(19) 0.012(2) C43 0.0355(18) 0.042(2) 0.036(2) 0.002(2) -0.0044(16) 0.0031(18) C44 0.062(3) 0.050(3) 0.057(3) 0.001(2) 0.007(2) -0.001(2) C45 0.077(3) 0.063(3) 0.070(3) 0.015(3) 0.009(2) -0.009(3) C46 0.090(3) 0.041(3) 0.095(4) 0.014(3) -0.012(3) -0.009(3) C47 0.084(3) 0.043(3) 0.084(4) -0.010(3) -0.003(3) 0.013(2) C48 0.056(2) 0.046(3) 0.057(3) 0.001(2) 0.0077(19) 0.007(2) C49 0.133(5) 0.107(4) 0.079(4) 0.011(4) 0.012(3) -0.003(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 Pd1 C25 2.004(3) . ? Pd1 C1 2.011(3) . ? Pd1 N1 2.146(3) . ? Pd1 N2 2.172(3) . ? Pd1 P2 2.9729(19) . ? Cl1 C49 1.740(6) . ? Cl2 C49 1.759(6) . ? N1 C7 1.419(4) . ? N1 P1 1.599(3) . ? N2 C43 1.404(5) . ? N2 P2 1.607(3) . ? P1 C2 1.786(4) . ? P1 C13 1.806(4) . ? P1 C19 1.810(3) . ? P2 C26 1.787(4) . ? P2 C37 1.813(3) . ? P2 C31 1.820(4) . ? C1 C6 1.400(5) . ? C1 C2 1.415(4) . ? C2 C3 1.399(5) . ? C3 C4 1.372(5) . ? C4 C5 1.380(5) . ? C5 C6 1.393(5) . ? C7 C12 1.385(5) . ? C7 C8 1.399(5) . ? C8 C9 1.383(5) . ? C9 C10 1.367(6) . ? C10 C11 1.376(6) . ? C11 C12 1.389(5) . ? C13 C14 1.371(5) . ? C13 C18 1.398(5) . ? C14 C15 1.386(6) . ? C15 C16 1.384(7) . ? C16 C17 1.355(7) . ? C17 C18 1.384(6) . ? C19 C24 1.375(5) . ? C19 C20 1.379(5) . ? C20 C21 1.384(5) . ? C21 C22 1.377(6) . ? C22 C23 1.364(6) . ? C23 C24 1.385(5) . ? C25 C30 1.402(5) . ? C25 C26 1.416(4) . ? C26 C27 1.401(5) . ? C27 C28 1.387(5) . ? C28 C29 1.381(5) . ? C29 C30 1.386(5) . ? C31 C32 1.379(5) . ? C31 C36 1.402(5) . ? C32 C33 1.403(5) . ? C33 C34 1.348(6) . ? C34 C35 1.381(7) . ? C35 C36 1.379(5) . ? C37 C42 1.394(5) . ? C37 C38 1.398(5) . ? C38 C39 1.385(5) . ? C39 C40 1.371(6) . ? C40 C41 1.382(6) . ? C41 C42 1.386(5) . ? C43 C44 1.385(5) . ? C43 C48 1.387(5) . ? C44 C45 1.385(6) . ? C45 C46 1.351(6) . ? C46 C47 1.388(6) . ? C47 C48 1.387(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 C25 Pd1 C1 94.27(14) . . ? C25 Pd1 N1 176.57(12) . . ? C1 Pd1 N1 86.30(12) . . ? C25 Pd1 N2 84.70(12) . . ? C1 Pd1 N2 176.58(12) . . ? N1 Pd1 N2 94.92(11) . . ? C25 Pd1 P2 61.61(10) . . ? C1 Pd1 P2 145.22(10) . . ? N1 Pd1 P2 119.33(7) . . ? N2 Pd1 P2 31.83(8) . . ? C7 N1 P1 126.1(2) . . ? C7 N1 Pd1 126.4(2) . . ? P1 N1 Pd1 105.41(15) . . ? C43 N2 P2 126.9(2) . . ? C43 N2 Pd1 127.4(2) . . ? P2 N2 Pd1 102.71(15) . . ? N1 P1 C2 105.28(15) . . ? N1 P1 C13 111.99(16) . . ? C2 P1 C13 108.45(17) . . ? N1 P1 C19 114.16(15) . . ? C2 P1 C19 109.13(16) . . ? C13 P1 C19 107.68(16) . . ? N2 P2 C26 101.64(15) . . ? N2 P2 C37 116.78(16) . . ? C26 P2 C37 107.80(15) . . ? N2 P2 C31 114.22(15) . . ? C26 P2 C31 110.19(18) . . ? C37 P2 C31 105.97(16) . . ? N2 P2 Pd1 45.46(10) . . ? C26 P2 Pd1 70.13(10) . . ? C37 P2 Pd1 157.78(12) . . ? C31 P2 Pd1 95.12(11) . . ? C6 C1 C2 116.2(3) . . ? C6 C1 Pd1 128.2(3) . . ? C2 C1 Pd1 115.4(3) . . ? C3 C2 C1 121.8(3) . . ? C3 C2 P1 124.5(3) . . ? C1 C2 P1 113.5(2) . . ? C4 C3 C2 120.3(4) . . ? C3 C4 C5 118.9(4) . . ? C4 C5 C6 121.5(4) . . ? C5 C6 C1 121.1(3) . . ? C12 C7 C8 117.1(4) . . ? C12 C7 N1 119.6(3) . . ? C8 C7 N1 123.3(3) . . ? C9 C8 C7 121.2(4) . . ? C10 C9 C8 120.8(4) . . ? C9 C10 C11 118.9(4) . . ? C10 C11 C12 120.8(4) . . ? C7 C12 C11 121.1(4) . . ? C14 C13 C18 118.0(4) . . ? C14 C13 P1 120.7(3) . . ? C18 C13 P1 121.3(3) . . ? C13 C14 C15 121.3(4) . . ? C16 C15 C14 119.8(5) . . ? C17 C16 C15 119.9(5) . . ? C16 C17 C18 120.5(5) . . ? C17 C18 C13 120.6(4) . . ? C24 C19 C20 119.1(3) . . ? C24 C19 P1 122.9(3) . . ? C20 C19 P1 117.9(3) . . ? C19 C20 C21 120.7(4) . . ? C22 C21 C20 119.5(4) . . ? C23 C22 C21 120.1(4) . . ? C22 C23 C24 120.3(4) . . ? C19 C24 C23 120.2(4) . . ? C30 C25 C26 115.4(3) . . ? C30 C25 Pd1 128.9(2) . . ? C26 C25 Pd1 115.0(2) . . ? C27 C26 C25 122.0(3) . . ? C27 C26 P2 124.1(3) . . ? C25 C26 P2 113.2(2) . . ? C28 C27 C26 119.8(3) . . ? C29 C28 C27 119.5(3) . . ? C28 C29 C30 120.2(4) . . ? C29 C30 C25 122.9(3) . . ? C32 C31 C36 118.4(4) . . ? C32 C31 P2 120.7(3) . . ? C36 C31 P2 120.6(3) . . ? C31 C32 C33 120.1(4) . . ? C34 C33 C32 120.3(5) . . ? C33 C34 C35 120.9(5) . . ? C36 C35 C34 119.3(5) . . ? C35 C36 C31 121.0(4) . . ? C42 C37 C38 119.1(3) . . ? C42 C37 P2 120.8(3) . . ? C38 C37 P2 119.7(3) . . ? C39 C38 C37 119.9(3) . . ? C40 C39 C38 120.7(4) . . ? C39 C40 C41 120.1(4) . . ? C40 C41 C42 120.2(4) . . ? C41 C42 C37 120.1(4) . . ? C44 C43 C48 117.6(4) . . ? C44 C43 N2 124.4(3) . . ? C48 C43 N2 118.0(3) . . ? C43 C44 C45 120.9(4) . . ? C46 C45 C44 121.1(4) . . ? C45 C46 C47 119.2(4) . . ? C48 C47 C46 120.0(4) . . ? C43 C48 C47 121.1(4) . . ? Cl1 C49 Cl2 112.8(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.23 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.455 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.051 #===end data_{(C6H4PPh2NPh)2Ni1.5C6H6 _database_code_CSD 211250 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C57 H47 N2 Ni P2' _chemical_formula_weight 880.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.703(7) _cell_length_b 13.353(8) _cell_length_c 17.039(10) _cell_angle_alpha 108.071(12) _cell_angle_beta 92.150(14) _cell_angle_gamma 108.907(11) _cell_volume 2366(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 922 _exptl_absorpt_coefficient_mu 0.517 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.168226 _exptl_absorpt_correction_T_max 0.256687 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 10265 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.2328 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 23.27 _reflns_number_total 6701 _reflns_number_gt 2797 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0008P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6701 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1619 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0474 _refine_ls_goodness_of_fit_ref 0.809 _refine_ls_restrained_S_all 0.809 _refine_ls_shift/su_max 0.005 _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 0.30652(6) 0.58232(5) 0.32978(4) 0.0379(2) Uani 1 1 d . . . P1 P 0.18659(12) 0.73765(10) 0.43475(8) 0.0351(4) Uani 1 1 d . . . P2 P 0.29333(13) 0.38753(11) 0.17488(9) 0.0465(4) Uani 1 1 d . . . N1 N 0.1859(3) 0.6594(3) 0.3408(2) 0.0365(11) Uani 1 1 d . . . N2 N 0.2188(3) 0.4673(3) 0.2177(2) 0.0417(11) Uani 1 1 d . . . C1 C 0.3616(4) 0.6499(4) 0.4474(3) 0.0302(13) Uani 1 1 d . . . C2 C 0.4356(4) 0.6205(3) 0.4954(3) 0.0355(14) Uani 1 1 d . . . H2A H 0.4735 0.5710 0.4680 0.043 Uiso 1 1 calc R . . C3 C 0.4555(4) 0.6609(4) 0.5815(3) 0.0439(14) Uani 1 1 d . . . H3A H 0.5051 0.6379 0.6106 0.053 Uiso 1 1 calc R . . C4 C 0.4023(5) 0.7349(4) 0.6245(3) 0.0478(15) Uani 1 1 d . . . H4A H 0.4186 0.7643 0.6825 0.057 Uiso 1 1 calc R . . C5 C 0.3243(4) 0.7662(4) 0.5815(3) 0.0423(15) Uani 1 1 d . . . H5A H 0.2882 0.8167 0.6097 0.051 Uiso 1 1 calc R . . C6 C 0.3020(4) 0.7187(4) 0.4938(3) 0.0300(13) Uani 1 1 d . . . C7 C 0.0481(4) 0.6973(4) 0.4795(3) 0.0346(13) Uani 1 1 d . . . C8 C -0.0387(4) 0.5887(4) 0.4422(3) 0.0434(14) Uani 1 1 d . . . H8A H -0.0267 0.5395 0.3938 0.052 Uiso 1 1 calc R . . C9 C -0.1431(4) 0.5549(4) 0.4781(3) 0.0571(16) Uani 1 1 d . . . H9A H -0.2015 0.4834 0.4528 0.068 Uiso 1 1 calc R . . C10 C -0.1609(5) 0.6266(5) 0.5510(3) 0.0608(17) Uani 1 1 d . . . H10A H -0.2304 0.6029 0.5748 0.073 Uiso 1 1 calc R . . C11 C -0.0746(5) 0.7341(4) 0.5885(3) 0.0519(16) Uani 1 1 d . . . H11A H -0.0861 0.7828 0.6375 0.062 Uiso 1 1 calc R . . C12 C 0.0279(4) 0.7678(4) 0.5527(3) 0.0448(15) Uani 1 1 d . . . H12A H 0.0853 0.8399 0.5780 0.054 Uiso 1 1 calc R . . C13 C 0.2171(5) 0.8834(4) 0.4442(3) 0.0330(13) Uani 1 1 d . . . C14 C 0.3365(5) 0.9522(4) 0.4513(3) 0.0614(17) Uani 1 1 d . . . H14A H 0.3997 0.9248 0.4536 0.074 Uiso 1 1 calc R . . C15 C 0.3621(5) 1.0633(5) 0.4550(3) 0.075(2) Uani 1 1 d . . . H15A H 0.4430 1.1103 0.4615 0.090 Uiso 1 1 calc R . . C16 C 0.2702(6) 1.1043(4) 0.4492(3) 0.0615(18) Uani 1 1 d . . . H16A H 0.2882 1.1779 0.4504 0.074 Uiso 1 1 calc R . . C17 C 0.1515(5) 1.0356(4) 0.4418(3) 0.0649(17) Uani 1 1 d . . . H17A H 0.0882 1.0626 0.4385 0.078 Uiso 1 1 calc R . . C18 C 0.1260(5) 0.9248(4) 0.4391(3) 0.0543(16) Uani 1 1 d . . . H18A H 0.0452 0.8784 0.4338 0.065 Uiso 1 1 calc R . . C19 C 0.1356(5) 0.6794(4) 0.2728(3) 0.0448(15) Uani 1 1 d . . . C20 C 0.0175(6) 0.6727(4) 0.2589(3) 0.0611(17) Uani 1 1 d . . . H20A H -0.0328 0.6556 0.2974 0.073 Uiso 1 1 calc R . . C21 C -0.0332(6) 0.6895(5) 0.1910(4) 0.091(2) Uani 1 1 d . . . H21A H -0.1145 0.6842 0.1841 0.109 Uiso 1 1 calc R . . C22 C 0.0424(8) 0.7143(5) 0.1344(4) 0.095(3) Uani 1 1 d . . . H22A H 0.0120 0.7258 0.0880 0.113 Uiso 1 1 calc R . . C23 C 0.1632(7) 0.7224(5) 0.1457(4) 0.084(2) Uani 1 1 d . . . H23A H 0.2134 0.7385 0.1069 0.101 Uiso 1 1 calc R . . C24 C 0.2094(5) 0.7061(4) 0.2160(4) 0.0607(17) Uani 1 1 d . . . H24A H 0.2911 0.7135 0.2243 0.073 Uiso 1 1 calc R . . C25 C 0.4427(5) 0.4584(4) 0.2348(3) 0.0450(15) Uani 1 1 d . . . C26 C 0.5424(5) 0.4287(4) 0.2079(3) 0.0560(17) Uani 1 1 d . . . H26A H 0.5323 0.3662 0.1609 0.067 Uiso 1 1 calc R . . C27 C 0.6557(5) 0.4955(5) 0.2534(4) 0.0628(18) Uani 1 1 d . . . H27A H 0.7233 0.4759 0.2387 0.075 Uiso 1 1 calc R . . C28 C 0.6711(5) 0.5909(4) 0.3207(3) 0.0567(16) Uani 1 1 d . . . H28A H 0.7489 0.6386 0.3486 0.068 Uiso 1 1 calc R . . C29 C 0.5693(5) 0.6147(4) 0.3460(3) 0.0467(15) Uani 1 1 d . . . H29A H 0.5811 0.6783 0.3924 0.056 Uiso 1 1 calc R . . C30 C 0.4504(4) 0.5495(4) 0.3064(3) 0.0311(13) Uani 1 1 d . . . C31 C 0.2275(5) 0.2425(4) 0.1730(3) 0.0505(16) Uani 1 1 d . . . C32 C 0.2837(5) 0.2058(5) 0.2258(3) 0.075(2) Uani 1 1 d . . . H32A H 0.3567 0.2548 0.2602 0.090 Uiso 1 1 calc R . . C33 C 0.2329(7) 0.0968(6) 0.2284(4) 0.102(3) Uani 1 1 d . . . H33A H 0.2711 0.0734 0.2645 0.123 Uiso 1 1 calc R . . C34 C 0.1266(8) 0.0255(6) 0.1772(5) 0.109(3) Uani 1 1 d . . . H34A H 0.0912 -0.0474 0.1777 0.131 Uiso 1 1 calc R . . C35 C 0.0718(7) 0.0626(6) 0.1246(4) 0.114(3) Uani 1 1 d . . . H35A H -0.0008 0.0134 0.0896 0.137 Uiso 1 1 calc R . . C36 C 0.1206(6) 0.1693(5) 0.1222(3) 0.085(2) Uani 1 1 d . . . H36A H 0.0814 0.1920 0.0862 0.102 Uiso 1 1 calc R . . C37 C 0.3070(4) 0.3766(5) 0.0667(3) 0.0482(15) Uani 1 1 d . . . C38 C 0.3185(5) 0.2814(5) 0.0079(4) 0.077(2) Uani 1 1 d . . . H38A H 0.3096 0.2179 0.0224 0.092 Uiso 1 1 calc R . . C39 C 0.3428(5) 0.2800(5) -0.0715(4) 0.087(2) Uani 1 1 d . . . H39A H 0.3521 0.2171 -0.1095 0.105 Uiso 1 1 calc R . . C40 C 0.3528(5) 0.3745(6) -0.0930(4) 0.079(2) Uani 1 1 d . . . H40A H 0.3679 0.3748 -0.1462 0.095 Uiso 1 1 calc R . . C41 C 0.3406(4) 0.4671(5) -0.0361(4) 0.0702(18) Uani 1 1 d . . . H41A H 0.3467 0.5294 -0.0515 0.084 Uiso 1 1 calc R . . C42 C 0.3188(4) 0.4703(4) 0.0449(3) 0.0610(17) Uani 1 1 d . . . H42A H 0.3126 0.5346 0.0833 0.073 Uiso 1 1 calc R . . C43 C 0.0892(5) 0.4199(4) 0.1964(3) 0.0509(16) Uani 1 1 d . . . C44 C 0.0177(5) 0.3798(4) 0.2515(3) 0.0628(18) Uani 1 1 d . . . H44A H 0.0550 0.3853 0.3026 0.075 Uiso 1 1 calc R . . C45 C -0.1091(6) 0.3317(4) 0.2306(4) 0.084(2) Uani 1 1 d . . . H45A H -0.1562 0.3041 0.2672 0.100 Uiso 1 1 calc R . . C46 C -0.1648(7) 0.3251(6) 0.1543(5) 0.108(3) Uani 1 1 d . . . H46A H -0.2494 0.2931 0.1401 0.129 Uiso 1 1 calc R . . C47 C -0.0969(6) 0.3649(5) 0.1015(4) 0.093(2) Uani 1 1 d . . . H47A H -0.1349 0.3591 0.0505 0.111 Uiso 1 1 calc R . . C48 C 0.0286(6) 0.4141(4) 0.1217(3) 0.0733(19) Uani 1 1 d . . . H48A H 0.0736 0.4440 0.0853 0.088 Uiso 1 1 calc R . . C49 C 0.3946(18) 0.1124(9) -0.2964(8) 0.142(5) Uani 1 1 d . . . H49A H 0.4519 0.1576 -0.3191 0.170 Uiso 1 1 calc R . . C50 C 0.2763(19) 0.1028(9) -0.3063(6) 0.134(4) Uani 1 1 d . . . H50A H 0.2525 0.1406 -0.3376 0.161 Uiso 1 1 calc R . . C51 C 0.1905(12) 0.0401(13) -0.2724(9) 0.145(4) Uani 1 1 d . . . H51A H 0.1101 0.0373 -0.2783 0.174 Uiso 1 1 calc R . . C52 C 0.2255(16) -0.0184(11) -0.2297(8) 0.144(6) Uani 1 1 d . . . H52A H 0.1670 -0.0644 -0.2082 0.172 Uiso 1 1 calc R . . C53 C 0.343(2) -0.0116(10) -0.2176(7) 0.150(6) Uani 1 1 d . . . H53A H 0.3657 -0.0503 -0.1867 0.179 Uiso 1 1 calc R . . C54 C 0.4287(11) 0.0541(13) -0.2521(9) 0.136(4) Uani 1 1 d . . . H54A H 0.5097 0.0588 -0.2451 0.164 Uiso 1 1 calc R . . C55 C 0.5894(15) 0.0680(18) -0.0252(11) 0.188(7) Uani 1 1 d . . . H55A H 0.6496 0.1152 -0.0448 0.226 Uiso 1 1 calc R . . C56 C 0.513(2) 0.1068(10) 0.0189(12) 0.169(7) Uani 1 1 d . . . H56A H 0.5253 0.1832 0.0341 0.203 Uiso 1 1 calc R . . C57 C 0.4201(17) 0.043(2) 0.0420(9) 0.186(7) Uani 1 1 d . . . H57A H 0.3630 0.0702 0.0687 0.223 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 0.0365(5) 0.0361(4) 0.0358(5) 0.0058(3) 0.0023(4) 0.0124(4) P1 0.0318(10) 0.0298(9) 0.0398(10) 0.0084(7) 0.0041(7) 0.0093(7) P2 0.0497(11) 0.0425(10) 0.0423(10) 0.0048(8) 0.0021(8) 0.0195(8) N1 0.044(3) 0.032(3) 0.026(3) 0.001(2) -0.005(2) 0.014(2) N2 0.036(3) 0.039(3) 0.038(3) -0.006(2) 0.006(2) 0.017(2) C1 0.021(3) 0.028(3) 0.042(4) 0.016(3) 0.002(3) 0.006(3) C2 0.041(4) 0.029(3) 0.026(3) 0.003(3) 0.005(3) 0.004(3) C3 0.042(4) 0.044(4) 0.045(4) 0.016(3) -0.003(3) 0.013(3) C4 0.051(4) 0.049(4) 0.035(4) 0.006(3) -0.003(3) 0.016(3) C5 0.031(4) 0.041(4) 0.055(4) 0.014(3) 0.007(3) 0.015(3) C6 0.033(4) 0.029(3) 0.030(4) 0.009(3) 0.000(3) 0.016(3) C7 0.036(4) 0.031(3) 0.037(4) 0.011(3) 0.009(3) 0.012(3) C8 0.041(4) 0.040(4) 0.051(4) 0.013(3) 0.000(3) 0.018(3) C9 0.036(4) 0.057(4) 0.066(5) 0.027(4) 0.012(3) -0.006(3) C10 0.058(5) 0.081(5) 0.066(5) 0.048(4) 0.033(4) 0.030(4) C11 0.061(5) 0.036(4) 0.067(4) 0.019(3) 0.026(4) 0.023(3) C12 0.044(4) 0.035(3) 0.053(4) 0.017(3) 0.015(3) 0.009(3) C13 0.032(4) 0.035(3) 0.034(3) 0.009(2) 0.004(3) 0.017(3) C14 0.035(4) 0.055(4) 0.096(5) 0.035(4) 0.006(3) 0.009(3) C15 0.044(5) 0.059(5) 0.120(5) 0.053(4) -0.008(4) -0.001(4) C16 0.072(5) 0.032(4) 0.070(4) 0.017(3) 0.002(4) 0.007(4) C17 0.074(5) 0.045(4) 0.089(5) 0.028(4) 0.027(4) 0.032(4) C18 0.045(4) 0.040(4) 0.075(4) 0.026(3) 0.017(3) 0.006(3) C19 0.041(4) 0.038(3) 0.049(4) 0.009(3) -0.001(4) 0.012(3) C20 0.062(5) 0.079(4) 0.049(4) 0.029(3) 0.008(3) 0.027(4) C21 0.082(6) 0.117(6) 0.067(6) 0.022(5) -0.014(5) 0.040(5) C22 0.153(9) 0.056(5) 0.052(5) 0.003(4) -0.044(6) 0.030(6) C23 0.110(7) 0.079(5) 0.056(5) 0.029(4) 0.008(5) 0.018(5) C24 0.072(5) 0.063(4) 0.051(4) 0.028(3) 0.004(4) 0.020(3) C25 0.038(4) 0.049(4) 0.045(4) 0.018(3) -0.001(3) 0.011(3) C26 0.059(5) 0.066(4) 0.052(4) 0.018(3) 0.007(4) 0.036(4) C27 0.058(5) 0.077(5) 0.074(5) 0.031(4) 0.029(4) 0.042(4) C28 0.044(4) 0.068(5) 0.057(5) 0.024(4) 0.006(3) 0.018(3) C29 0.035(4) 0.047(4) 0.048(4) 0.006(3) 0.007(3) 0.011(3) C30 0.033(4) 0.021(3) 0.040(4) 0.008(3) 0.001(3) 0.012(3) C31 0.060(5) 0.040(4) 0.050(4) 0.011(3) 0.010(3) 0.018(3) C32 0.110(6) 0.057(5) 0.047(4) 0.010(3) -0.001(4) 0.022(4) C33 0.179(9) 0.062(5) 0.091(6) 0.044(5) 0.039(5) 0.056(5) C34 0.140(9) 0.045(5) 0.132(8) 0.023(5) 0.052(6) 0.022(5) C35 0.122(8) 0.054(6) 0.136(7) 0.011(5) 0.001(5) 0.014(5) C36 0.087(6) 0.035(4) 0.102(5) 0.006(4) -0.020(4) 0.003(4) C37 0.064(4) 0.043(4) 0.032(4) 0.006(3) 0.008(3) 0.019(3) C38 0.117(6) 0.060(5) 0.053(5) 0.010(4) 0.016(4) 0.041(4) C39 0.128(6) 0.088(6) 0.051(5) 0.009(4) 0.009(4) 0.058(5) C40 0.073(5) 0.119(7) 0.042(5) 0.018(5) 0.007(3) 0.040(5) C41 0.071(5) 0.087(5) 0.061(5) 0.037(4) 0.012(4) 0.027(4) C42 0.077(5) 0.051(4) 0.054(5) 0.014(3) 0.014(3) 0.023(3) C43 0.045(4) 0.040(4) 0.040(4) -0.016(3) -0.007(3) 0.009(3) C44 0.065(5) 0.038(4) 0.059(5) 0.003(3) 0.009(4) -0.003(3) C45 0.061(6) 0.060(4) 0.098(6) 0.003(4) 0.033(4) 0.002(4) C46 0.046(6) 0.107(6) 0.099(7) -0.038(5) -0.007(5) 0.007(4) C47 0.051(6) 0.135(7) 0.065(6) -0.007(4) -0.019(4) 0.041(5) C48 0.060(5) 0.097(5) 0.048(5) 0.008(4) -0.009(4) 0.026(4) C49 0.172(15) 0.092(8) 0.122(9) 0.021(7) 0.033(10) 0.009(10) C50 0.173(12) 0.098(8) 0.089(7) 0.024(5) -0.004(9) 0.004(10) C51 0.166(13) 0.098(10) 0.104(9) -0.010(6) -0.001(9) 0.007(10) C52 0.179(16) 0.085(9) 0.110(10) 0.004(7) 0.045(11) 0.000(10) C53 0.274(19) 0.063(8) 0.099(8) 0.014(6) 0.051(13) 0.053(12) C54 0.154(12) 0.095(9) 0.126(10) -0.010(6) 0.006(9) 0.047(10) C55 0.179(15) 0.118(11) 0.272(16) 0.103(11) 0.030(12) 0.023(10) C56 0.150(13) 0.124(12) 0.208(14) -0.025(11) -0.012(10) 0.097(12) C57 0.138(14) 0.25(2) 0.199(11) 0.097(14) 0.077(10) 0.086(12) _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 C30 1.898(5) . ? Ni1 C1 1.910(5) . ? Ni1 N1 1.982(4) . ? Ni1 N2 2.018(3) . ? P1 N1 1.616(3) . ? P1 C6 1.783(4) . ? P1 C7 1.812(4) . ? P1 C13 1.815(5) . ? P2 N2 1.612(4) . ? P2 C25 1.786(5) . ? P2 C37 1.821(5) . ? P2 C31 1.827(5) . ? N1 C19 1.414(5) . ? N2 C43 1.423(5) . ? C1 C2 1.394(5) . ? C1 C6 1.400(6) . ? C2 C3 1.377(5) . ? C3 C4 1.373(6) . ? C4 C5 1.389(6) . ? C5 C6 1.407(5) . ? C7 C12 1.391(5) . ? C7 C8 1.401(5) . ? C8 C9 1.394(5) . ? C9 C10 1.382(6) . ? C10 C11 1.390(5) . ? C11 C12 1.375(5) . ? C13 C18 1.362(6) . ? C13 C14 1.377(5) . ? C14 C15 1.395(6) . ? C15 C16 1.369(6) . ? C16 C17 1.370(6) . ? C17 C18 1.396(6) . ? C19 C20 1.363(6) . ? C19 C24 1.374(6) . ? C20 C21 1.391(6) . ? C21 C22 1.377(7) . ? C22 C23 1.384(7) . ? C23 C24 1.400(6) . ? C25 C26 1.398(6) . ? C25 C30 1.407(5) . ? C26 C27 1.372(6) . ? C27 C28 1.378(6) . ? C28 C29 1.379(6) . ? C29 C30 1.390(5) . ? C31 C36 1.367(6) . ? C31 C32 1.385(6) . ? C32 C33 1.400(6) . ? C33 C34 1.361(8) . ? C34 C35 1.377(8) . ? C35 C36 1.367(6) . ? C37 C42 1.379(6) . ? C37 C38 1.403(6) . ? C38 C39 1.387(6) . ? C39 C40 1.392(7) . ? C40 C41 1.367(6) . ? C41 C42 1.404(6) . ? C43 C44 1.396(6) . ? C43 C48 1.401(6) . ? C44 C45 1.393(6) . ? C45 C46 1.398(7) . ? C46 C47 1.342(7) . ? C47 C48 1.379(6) . ? C49 C50 1.347(11) . ? C49 C54 1.371(11) . ? C50 C51 1.356(10) . ? C51 C52 1.359(12) . ? C52 C53 1.351(12) . ? C53 C54 1.384(10) . ? C55 C56 1.322(13) . ? C55 C57 1.381(14) 2_655 ? C56 C57 1.306(12) . ? C57 C55 1.381(14) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C30 Ni1 C1 93.8(2) . . ? C30 Ni1 N1 160.33(16) . . ? C1 Ni1 N1 89.98(19) . . ? C30 Ni1 N2 89.23(19) . . ? C1 Ni1 N2 160.86(16) . . ? N1 Ni1 N2 93.47(16) . . ? N1 P1 C6 102.4(2) . . ? N1 P1 C7 116.7(2) . . ? C6 P1 C7 106.7(2) . . ? N1 P1 C13 112.6(2) . . ? C6 P1 C13 113.5(2) . . ? C7 P1 C13 105.1(2) . . ? N2 P2 C25 103.6(2) . . ? N2 P2 C37 113.3(2) . . ? C25 P2 C37 108.0(2) . . ? N2 P2 C31 114.6(2) . . ? C25 P2 C31 112.1(3) . . ? C37 P2 C31 105.3(3) . . ? C19 N1 P1 118.9(4) . . ? C19 N1 Ni1 122.4(3) . . ? P1 N1 Ni1 114.9(2) . . ? C43 N2 P2 116.4(3) . . ? C43 N2 Ni1 123.5(3) . . ? P2 N2 Ni1 112.9(2) . . ? C2 C1 C6 114.3(4) . . ? C2 C1 Ni1 127.0(4) . . ? C6 C1 Ni1 117.1(4) . . ? C3 C2 C1 123.3(5) . . ? C4 C3 C2 120.3(5) . . ? C3 C4 C5 120.1(5) . . ? C4 C5 C6 117.7(5) . . ? C1 C6 C5 123.9(4) . . ? C1 C6 P1 115.5(4) . . ? C5 C6 P1 120.5(4) . . ? C12 C7 C8 118.5(4) . . ? C12 C7 P1 122.3(4) . . ? C8 C7 P1 119.0(4) . . ? C9 C8 C7 119.6(4) . . ? C10 C9 C8 120.7(5) . . ? C9 C10 C11 119.9(5) . . ? C12 C11 C10 119.4(5) . . ? C11 C12 C7 121.8(4) . . ? C18 C13 C14 119.1(5) . . ? C18 C13 P1 122.3(4) . . ? C14 C13 P1 118.5(4) . . ? C13 C14 C15 119.6(5) . . ? C16 C15 C14 121.1(6) . . ? C15 C16 C17 119.2(5) . . ? C16 C17 C18 119.7(6) . . ? C13 C18 C17 121.3(5) . . ? C20 C19 C24 117.1(5) . . ? C20 C19 N1 124.4(6) . . ? C24 C19 N1 118.5(6) . . ? C19 C20 C21 124.6(6) . . ? C22 C21 C20 116.9(7) . . ? C21 C22 C23 120.8(7) . . ? C22 C23 C24 119.6(7) . . ? C19 C24 C23 120.9(6) . . ? C26 C25 C30 124.6(5) . . ? C26 C25 P2 121.6(5) . . ? C30 C25 P2 113.7(4) . . ? C27 C26 C25 117.3(5) . . ? C26 C27 C28 121.2(5) . . ? C27 C28 C29 119.0(5) . . ? C28 C29 C30 124.1(5) . . ? C29 C30 C25 113.6(4) . . ? C29 C30 Ni1 127.2(4) . . ? C25 C30 Ni1 118.6(4) . . ? C36 C31 C32 118.6(5) . . ? C36 C31 P2 121.4(5) . . ? C32 C31 P2 120.0(5) . . ? C31 C32 C33 121.5(6) . . ? C34 C33 C32 118.7(7) . . ? C33 C34 C35 119.4(8) . . ? C36 C35 C34 122.0(8) . . ? C35 C36 C31 119.8(6) . . ? C42 C37 C38 119.4(5) . . ? C42 C37 P2 117.9(5) . . ? C38 C37 P2 122.4(5) . . ? C39 C38 C37 121.4(6) . . ? C38 C39 C40 118.7(6) . . ? C41 C40 C39 120.1(6) . . ? C40 C41 C42 121.7(6) . . ? C37 C42 C41 118.8(5) . . ? C44 C43 C48 117.6(5) . . ? C44 C43 N2 120.2(5) . . ? C48 C43 N2 122.2(6) . . ? C45 C44 C43 120.6(5) . . ? C44 C45 C46 119.5(6) . . ? C47 C46 C45 120.3(8) . . ? C46 C47 C48 120.9(7) . . ? C47 C48 C43 121.0(6) . . ? C50 C49 C54 118.5(13) . . ? C49 C50 C51 122.7(13) . . ? C50 C51 C52 118.1(14) . . ? C53 C52 C51 121.7(17) . . ? C52 C53 C54 118.9(16) . . ? C49 C54 C53 120.2(13) . . ? C56 C55 C57 119.8(11) . 2_655 ? C57 C56 C55 122.9(12) . . ? C56 C57 C55 117.0(13) . 2_655 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.236 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.050 #===end data_[(Ph3P)3NiBr].0.5[Ni(o-C6H4PPh2N3,5-C6H3Me2)2].0.5C6H6 _database_code_CSD 211251 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C83 H71 Br N Ni1.50 P4' _chemical_formula_weight 1374.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 15.719(10) _cell_length_b 13.700(8) _cell_length_c 35.49(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.364(12) _cell_angle_gamma 90.00 _cell_volume 7643(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2852 _exptl_absorpt_coefficient_mu 1.021 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.176673 _exptl_absorpt_correction_T_max 0.256595 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 31772 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.1212 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 23.22 _reflns_number_total 10835 _reflns_number_gt 5538 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0661P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10835 _refine_ls_number_parameters 801 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1126 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 0.818 _refine_ls_restrained_S_all 0.818 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.5000 0.43292(6) 0.2500 0.0423(3) Uani 1 2 d S . . Ni2 Ni 0.22219(4) 0.24783(4) -0.040270(17) 0.03997(19) Uani 1 1 d . . . Br1 Br 0.13221(4) 0.22549(4) 0.014920(16) 0.0597(2) Uani 1 1 d . . . P1 P 0.33043(10) 0.37448(9) 0.22221(4) 0.0466(4) Uani 1 1 d . . . P2 P 0.33099(9) 0.14177(9) -0.02645(4) 0.0435(4) Uani 1 1 d . . . P3 P 0.14842(9) 0.19079(10) -0.09202(4) 0.0466(4) Uani 1 1 d . . . P4 P 0.25442(9) 0.41281(9) -0.04063(4) 0.0440(4) Uani 1 1 d . . . N1 N 0.4255(3) 0.3333(3) 0.22390(11) 0.0442(11) Uani 1 1 d . . . C1 C 0.3502(4) 0.5017(3) 0.21451(15) 0.0472(14) Uani 1 1 d . . . C2 C 0.2907(4) 0.5646(4) 0.19693(16) 0.0664(17) Uani 1 1 d . . . H2A H 0.2355 0.5435 0.1920 0.080 Uiso 1 1 calc R . . C3 C 0.3155(5) 0.6572(5) 0.18732(18) 0.078(2) Uani 1 1 d . . . H3A H 0.2772 0.7006 0.1763 0.094 Uiso 1 1 calc R . . C4 C 0.3987(5) 0.6847(4) 0.19446(17) 0.070(2) Uani 1 1 d . . . H4A H 0.4161 0.7467 0.1870 0.084 Uiso 1 1 calc R . . C5 C 0.4577(4) 0.6243(4) 0.21214(15) 0.0573(16) Uani 1 1 d . . . H5A H 0.5130 0.6460 0.2165 0.069 Uiso 1 1 calc R . . C6 C 0.4326(4) 0.5283(4) 0.22371(14) 0.0481(15) Uani 1 1 d . . . C7 C 0.2647(4) 0.3606(4) 0.26388(16) 0.0553(15) Uani 1 1 d . . . C8 C 0.2600(4) 0.4350(5) 0.28966(18) 0.084(2) Uani 1 1 d . . . H8A H 0.2907 0.4921 0.2857 0.100 Uiso 1 1 calc R . . C9 C 0.2095(6) 0.4259(7) 0.3218(2) 0.117(3) Uani 1 1 d . . . H9A H 0.2061 0.4777 0.3387 0.141 Uiso 1 1 calc R . . C10 C 0.1663(5) 0.3441(8) 0.3287(2) 0.098(3) Uani 1 1 d . . . H10A H 0.1335 0.3389 0.3503 0.118 Uiso 1 1 calc R . . C11 C 0.1703(5) 0.2697(6) 0.3045(3) 0.109(3) Uani 1 1 d . . . H11A H 0.1405 0.2125 0.3096 0.130 Uiso 1 1 calc R . . C12 C 0.2192(5) 0.2768(5) 0.2713(2) 0.093(2) Uani 1 1 d . . . H12A H 0.2206 0.2248 0.2545 0.112 Uiso 1 1 calc R . . C13 C 0.2640(4) 0.3285(4) 0.18439(15) 0.0506(15) Uani 1 1 d . . . C14 C 0.1759(5) 0.3374(5) 0.18582(19) 0.082(2) Uani 1 1 d . . . H14A H 0.1506 0.3622 0.2074 0.098 Uiso 1 1 calc R . . C15 C 0.1251(5) 0.3100(5) 0.1554(2) 0.097(2) Uani 1 1 d . . . H15A H 0.0664 0.3180 0.1566 0.117 Uiso 1 1 calc R . . C16 C 0.1618(5) 0.2706(5) 0.1232(2) 0.082(2) Uani 1 1 d . . . H16A H 0.1281 0.2492 0.1033 0.098 Uiso 1 1 calc R . . C17 C 0.2493(5) 0.2641(4) 0.12164(18) 0.0749(19) Uani 1 1 d . . . H17A H 0.2743 0.2400 0.0999 0.090 Uiso 1 1 calc R . . C18 C 0.3013(4) 0.2927(4) 0.15170(17) 0.0631(17) Uani 1 1 d . . . H18A H 0.3602 0.2879 0.1499 0.076 Uiso 1 1 calc R . . C19 C 0.4515(3) 0.2370(4) 0.21317(13) 0.0430(13) Uani 1 1 d . . . C20 C 0.4042(4) 0.1550(4) 0.22147(15) 0.0593(16) Uani 1 1 d . . . H20A H 0.3536 0.1619 0.2346 0.071 Uiso 1 1 calc R . . C21 C 0.4307(5) 0.0619(4) 0.21063(19) 0.078(2) Uani 1 1 d . . . C22 C 0.5069(6) 0.0549(5) 0.1910(2) 0.090(2) Uani 1 1 d . . . H22A H 0.5258 -0.0067 0.1839 0.108 Uiso 1 1 calc R . . C23 C 0.5559(4) 0.1350(5) 0.18152(16) 0.0644(17) Uani 1 1 d . . . C24 C 0.5266(4) 0.2249(4) 0.19358(13) 0.0494(15) Uani 1 1 d . . . H24A H 0.5590 0.2800 0.1883 0.059 Uiso 1 1 calc R . . C25 C 0.3791(5) -0.0291(4) 0.2222(2) 0.132(3) Uani 1 1 d . . . H25A H 0.4059 -0.0866 0.2124 0.198 Uiso 1 1 calc R . . H25B H 0.3223 -0.0242 0.2122 0.198 Uiso 1 1 calc R . . H25C H 0.3769 -0.0331 0.2492 0.198 Uiso 1 1 calc R . . C26 C 0.6375(5) 0.1215(5) 0.16018(18) 0.105(3) Uani 1 1 d . . . H26A H 0.6451 0.0536 0.1544 0.158 Uiso 1 1 calc R . . H26B H 0.6844 0.1440 0.1753 0.158 Uiso 1 1 calc R . . H26C H 0.6350 0.1583 0.1372 0.158 Uiso 1 1 calc R . . C27 C 0.3038(4) 0.0103(3) -0.02267(14) 0.0443(14) Uani 1 1 d . . . C28 C 0.2305(4) -0.0149(4) -0.00361(17) 0.0652(18) Uani 1 1 d . . . H28A H 0.1954 0.0336 0.0060 0.078 Uiso 1 1 calc R . . C29 C 0.2092(4) -0.1130(5) 0.00120(18) 0.081(2) Uani 1 1 d . . . H29A H 0.1602 -0.1299 0.0142 0.097 Uiso 1 1 calc R . . C30 C 0.2613(5) -0.1854(4) -0.01340(19) 0.076(2) Uani 1 1 d . . . H30A H 0.2473 -0.2508 -0.0102 0.091 Uiso 1 1 calc R . . C31 C 0.3338(4) -0.1602(4) -0.03270(18) 0.0686(18) Uani 1 1 d . . . H31A H 0.3684 -0.2085 -0.0428 0.082 Uiso 1 1 calc R . . C32 C 0.3551(4) -0.0620(4) -0.03711(15) 0.0562(16) Uani 1 1 d . . . H32A H 0.4044 -0.0452 -0.0499 0.067 Uiso 1 1 calc R . . C33 C 0.3803(3) 0.1689(4) 0.01941(14) 0.0451(14) Uani 1 1 d . . . C34 C 0.4118(4) 0.2647(4) 0.02544(16) 0.0559(15) Uani 1 1 d . . . H34A H 0.4061 0.3115 0.0066 0.067 Uiso 1 1 calc R . . C35 C 0.4509(4) 0.2890(4) 0.05901(18) 0.0627(17) Uani 1 1 d . . . H35A H 0.4699 0.3524 0.0630 0.075 Uiso 1 1 calc R . . C36 C 0.4621(4) 0.2196(5) 0.08687(17) 0.0696(18) Uani 1 1 d . . . H36A H 0.4900 0.2357 0.1092 0.084 Uiso 1 1 calc R . . C37 C 0.4315(4) 0.1259(5) 0.08127(18) 0.0722(19) Uani 1 1 d . . . H37A H 0.4383 0.0793 0.1001 0.087 Uiso 1 1 calc R . . C38 C 0.3906(4) 0.1008(4) 0.04774(16) 0.0566(16) Uani 1 1 d . . . H38A H 0.3701 0.0377 0.0444 0.068 Uiso 1 1 calc R . . C39 C 0.4241(4) 0.1421(3) -0.05768(14) 0.0434(14) Uani 1 1 d . . . C40 C 0.4098(4) 0.1438(4) -0.09651(16) 0.0547(15) Uani 1 1 d . . . H40A H 0.3546 0.1388 -0.1059 0.066 Uiso 1 1 calc R . . C41 C 0.4774(5) 0.1530(4) -0.12124(16) 0.0630(17) Uani 1 1 d . . . H41A H 0.4667 0.1552 -0.1470 0.076 Uiso 1 1 calc R . . C42 C 0.5600(5) 0.1591(4) -0.10832(19) 0.0669(18) Uani 1 1 d . . . H42A H 0.6047 0.1651 -0.1252 0.080 Uiso 1 1 calc R . . C43 C 0.5756(4) 0.1560(4) -0.07031(18) 0.0635(17) Uani 1 1 d . . . H43A H 0.6312 0.1590 -0.0613 0.076 Uiso 1 1 calc R . . C44 C 0.5085(4) 0.1484(4) -0.04530(16) 0.0546(15) Uani 1 1 d . . . H44A H 0.5200 0.1476 -0.0196 0.066 Uiso 1 1 calc R . . C45 C 0.1965(3) 0.1987(4) -0.13917(14) 0.0463(14) Uani 1 1 d . . . C46 C 0.2531(4) 0.2737(4) -0.14562(16) 0.0610(16) Uani 1 1 d . . . H46A H 0.2655 0.3172 -0.1262 0.073 Uiso 1 1 calc R . . C47 C 0.2923(4) 0.2863(5) -0.1804(2) 0.079(2) Uani 1 1 d . . . H47A H 0.3298 0.3378 -0.1841 0.095 Uiso 1 1 calc R . . C48 C 0.2749(5) 0.2219(6) -0.2090(2) 0.094(2) Uani 1 1 d . . . H48A H 0.3018 0.2284 -0.2322 0.113 Uiso 1 1 calc R . . C49 C 0.2175(6) 0.1476(6) -0.20334(19) 0.098(2) Uani 1 1 d . . . H49A H 0.2051 0.1046 -0.2229 0.118 Uiso 1 1 calc R . . C50 C 0.1781(4) 0.1360(5) -0.16882(17) 0.076(2) Uani 1 1 d . . . H50A H 0.1389 0.0859 -0.1655 0.091 Uiso 1 1 calc R . . C51 C 0.0424(4) 0.2480(4) -0.10011(17) 0.0574(15) Uani 1 1 d . . . C52 C -0.0090(4) 0.2734(4) -0.06934(18) 0.0720(18) Uani 1 1 d . . . H52A H 0.0116 0.2628 -0.0451 0.086 Uiso 1 1 calc R . . C53 C -0.0886(5) 0.3133(5) -0.0739(2) 0.089(2) Uani 1 1 d . . . H53A H -0.1218 0.3273 -0.0530 0.107 Uiso 1 1 calc R . . C54 C -0.1186(5) 0.3322(6) -0.1095(3) 0.103(3) Uani 1 1 d . . . H54A H -0.1721 0.3602 -0.1128 0.123 Uiso 1 1 calc R . . C55 C -0.0704(5) 0.3101(6) -0.1397(2) 0.105(3) Uani 1 1 d . . . H55A H -0.0915 0.3222 -0.1638 0.125 Uiso 1 1 calc R . . C56 C 0.0101(4) 0.2697(5) -0.13553(19) 0.079(2) Uani 1 1 d . . . H56A H 0.0427 0.2571 -0.1568 0.095 Uiso 1 1 calc R . . C57 C 0.1198(4) 0.0599(4) -0.08826(15) 0.0506(15) Uani 1 1 d . . . C58 C 0.0451(4) 0.0314(5) -0.07180(19) 0.084(2) Uani 1 1 d . . . H58A H 0.0067 0.0780 -0.0634 0.101 Uiso 1 1 calc R . . C59 C 0.0267(6) -0.0685(7) -0.0676(2) 0.116(3) Uani 1 1 d . . . H59A H -0.0232 -0.0876 -0.0557 0.139 Uiso 1 1 calc R . . C60 C 0.0818(7) -0.1377(6) -0.0809(2) 0.103(3) Uani 1 1 d . . . H60A H 0.0681 -0.2035 -0.0793 0.124 Uiso 1 1 calc R . . C61 C 0.1565(5) -0.1096(5) -0.0965(2) 0.088(2) Uani 1 1 d . . . H61A H 0.1946 -0.1566 -0.1050 0.106 Uiso 1 1 calc R . . C62 C 0.1763(4) -0.0127(4) -0.09999(16) 0.0662(18) Uani 1 1 d . . . H62A H 0.2282 0.0052 -0.1103 0.079 Uiso 1 1 calc R . . C63 C 0.1575(3) 0.4838(3) -0.05039(16) 0.0458(14) Uani 1 1 d . . . C64 C 0.1170(4) 0.5432(4) -0.02459(17) 0.0734(19) Uani 1 1 d . . . H64A H 0.1406 0.5515 -0.0007 0.088 Uiso 1 1 calc R . . C65 C 0.0415(5) 0.5909(5) -0.0339(2) 0.094(2) Uani 1 1 d . . . H65A H 0.0157 0.6302 -0.0159 0.112 Uiso 1 1 calc R . . C66 C 0.0052(4) 0.5818(5) -0.0676(2) 0.077(2) Uani 1 1 d . . . H66A H -0.0453 0.6145 -0.0731 0.093 Uiso 1 1 calc R . . C67 C 0.0428(4) 0.5237(4) -0.09445(19) 0.0700(18) Uani 1 1 d . . . H67A H 0.0180 0.5170 -0.1182 0.084 Uiso 1 1 calc R . . C68 C 0.1175(4) 0.4754(4) -0.08595(18) 0.0635(17) Uani 1 1 d . . . H68A H 0.1423 0.4360 -0.1042 0.076 Uiso 1 1 calc R . . C69 C 0.2934(4) 0.4706(3) 0.00309(15) 0.0455(14) Uani 1 1 d . . . C70 C 0.3592(4) 0.5392(4) 0.00383(18) 0.0723(19) Uani 1 1 d . . . H70A H 0.3862 0.5568 -0.0184 0.087 Uiso 1 1 calc R . . C71 C 0.3845(5) 0.5814(5) 0.0379(2) 0.093(2) Uani 1 1 d . . . H71A H 0.4293 0.6258 0.0382 0.112 Uiso 1 1 calc R . . C72 C 0.3447(5) 0.5587(5) 0.0704(2) 0.081(2) Uani 1 1 d . . . H72A H 0.3605 0.5891 0.0928 0.097 Uiso 1 1 calc R . . C73 C 0.2802(5) 0.4901(5) 0.07018(18) 0.0717(19) Uani 1 1 d . . . H73A H 0.2534 0.4738 0.0926 0.086 Uiso 1 1 calc R . . C74 C 0.2553(4) 0.4453(4) 0.03703(17) 0.0627(17) Uani 1 1 d . . . H74A H 0.2128 0.3981 0.0374 0.075 Uiso 1 1 calc R . . C75 C 0.3290(3) 0.4618(4) -0.07592(14) 0.0432(14) Uani 1 1 d . . . C76 C 0.3220(4) 0.5565(4) -0.09076(16) 0.0615(17) Uani 1 1 d . . . H76A H 0.2789 0.5973 -0.0822 0.074 Uiso 1 1 calc R . . C77 C 0.3779(4) 0.5906(4) -0.11790(18) 0.0738(19) Uani 1 1 d . . . H77A H 0.3721 0.6536 -0.1274 0.089 Uiso 1 1 calc R . . C78 C 0.4427(4) 0.5301(5) -0.13090(17) 0.0701(19) Uani 1 1 d . . . H78A H 0.4805 0.5520 -0.1491 0.084 Uiso 1 1 calc R . . C79 C 0.4498(4) 0.4382(5) -0.11650(17) 0.0691(18) Uani 1 1 d . . . H79A H 0.4922 0.3968 -0.1253 0.083 Uiso 1 1 calc R . . C80 C 0.3941(4) 0.4053(4) -0.08881(16) 0.0549(16) Uani 1 1 d . . . H80A H 0.4015 0.3431 -0.0788 0.066 Uiso 1 1 calc R . . C81 C 0.0420(8) 0.3037(11) -0.2450(4) 0.238(6) Uiso 1 1 d . . . H81A H 0.0728 0.2460 -0.2429 0.285 Uiso 1 1 calc R . . C82 C 0.0785(10) 0.3924(12) -0.2382(4) 0.232(6) Uiso 1 1 d . . . H82A H 0.1353 0.3945 -0.2307 0.279 Uiso 1 1 calc R . . C83 C 0.0338(10) 0.4804(11) -0.2421(5) 0.272(8) Uiso 1 1 d . . . H83A H 0.0564 0.5381 -0.2326 0.327 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 0.0503(7) 0.0333(5) 0.0432(6) 0.000 0.0032(5) 0.000 Ni2 0.0428(4) 0.0366(4) 0.0405(4) 0.0007(3) 0.0006(3) 0.0028(3) Br1 0.0684(5) 0.0563(4) 0.0547(4) 0.0021(3) 0.0207(3) 0.0014(3) P1 0.0516(11) 0.0431(8) 0.0452(9) -0.0004(7) -0.0017(8) 0.0037(7) P2 0.0451(10) 0.0423(8) 0.0430(9) 0.0011(7) -0.0024(7) 0.0064(7) P3 0.0459(10) 0.0509(9) 0.0430(9) -0.0041(7) 0.0009(8) 0.0004(7) P4 0.0519(10) 0.0357(8) 0.0446(9) 0.0021(7) 0.0030(8) 0.0024(6) N1 0.048(3) 0.037(2) 0.047(3) -0.007(2) -0.005(2) 0.001(2) C1 0.049(4) 0.043(3) 0.050(4) -0.001(3) 0.003(3) 0.009(3) C2 0.068(5) 0.066(4) 0.065(4) 0.003(3) -0.006(4) 0.012(4) C3 0.099(7) 0.054(4) 0.081(5) 0.013(4) -0.009(5) 0.021(4) C4 0.109(7) 0.043(4) 0.059(4) 0.007(3) 0.012(5) 0.009(4) C5 0.070(5) 0.047(4) 0.055(4) 0.007(3) 0.016(3) 0.010(3) C6 0.056(4) 0.046(3) 0.042(3) 0.004(3) 0.010(3) 0.014(3) C7 0.054(4) 0.055(4) 0.056(4) -0.001(3) -0.002(3) 0.004(3) C8 0.098(6) 0.091(5) 0.062(5) -0.015(4) 0.010(4) -0.011(4) C9 0.153(9) 0.145(8) 0.054(5) -0.026(5) 0.028(6) 0.000(7) C10 0.101(7) 0.136(8) 0.059(5) 0.018(6) 0.022(5) 0.018(6) C11 0.117(7) 0.091(6) 0.119(7) 0.020(5) 0.049(6) -0.004(5) C12 0.101(6) 0.084(5) 0.096(6) -0.003(4) 0.042(5) -0.007(4) C13 0.051(5) 0.053(3) 0.048(4) 0.000(3) -0.006(3) 0.001(3) C14 0.058(6) 0.112(6) 0.076(5) -0.027(4) -0.010(4) 0.003(4) C15 0.058(5) 0.128(6) 0.106(6) -0.024(5) -0.016(5) 0.010(4) C16 0.081(6) 0.089(5) 0.074(5) -0.005(4) -0.026(5) 0.005(4) C17 0.093(6) 0.082(5) 0.049(4) 0.002(4) -0.006(4) 0.008(4) C18 0.061(5) 0.075(4) 0.054(4) 0.003(3) -0.009(4) 0.000(3) C19 0.053(4) 0.042(3) 0.034(3) -0.004(3) -0.002(3) 0.002(3) C20 0.073(5) 0.044(4) 0.061(4) -0.007(3) 0.006(3) -0.002(3) C21 0.101(6) 0.053(4) 0.081(5) -0.018(4) 0.001(5) 0.000(4) C22 0.123(7) 0.058(5) 0.088(5) -0.036(4) -0.011(5) 0.033(5) C23 0.084(5) 0.061(4) 0.049(4) -0.012(3) 0.001(4) 0.011(4) C24 0.064(4) 0.046(4) 0.038(3) 0.002(3) 0.000(3) 0.004(3) C25 0.159(8) 0.049(4) 0.187(9) -0.015(5) 0.019(7) -0.035(5) C26 0.112(7) 0.117(6) 0.086(5) -0.023(4) 0.021(5) 0.044(5) C27 0.047(4) 0.038(3) 0.048(3) 0.006(3) -0.003(3) 0.003(3) C28 0.071(5) 0.045(4) 0.079(5) 0.006(3) 0.006(4) 0.003(3) C29 0.079(5) 0.068(5) 0.094(5) 0.012(4) 0.021(4) -0.005(4) C30 0.084(6) 0.045(4) 0.098(5) 0.007(4) -0.009(5) -0.007(4) C31 0.066(5) 0.046(4) 0.094(5) -0.008(3) -0.006(4) 0.009(3) C32 0.056(4) 0.048(4) 0.066(4) 0.002(3) 0.001(3) 0.000(3) C33 0.048(4) 0.049(3) 0.039(3) -0.005(3) -0.001(3) 0.014(3) C34 0.061(4) 0.047(4) 0.060(4) -0.002(3) -0.008(3) 0.011(3) C35 0.062(5) 0.060(4) 0.066(4) -0.021(4) -0.011(4) 0.008(3) C36 0.064(5) 0.099(5) 0.045(4) -0.009(4) -0.011(3) 0.007(4) C37 0.083(5) 0.086(5) 0.048(4) 0.014(4) -0.002(4) 0.012(4) C38 0.068(5) 0.054(4) 0.048(4) 0.006(3) -0.004(3) 0.006(3) C39 0.057(4) 0.033(3) 0.040(4) 0.004(2) 0.000(3) 0.007(3) C40 0.059(4) 0.056(4) 0.049(4) -0.003(3) -0.004(4) 0.005(3) C41 0.081(5) 0.066(4) 0.042(4) -0.005(3) 0.008(4) 0.007(4) C42 0.061(5) 0.069(4) 0.071(5) 0.009(4) 0.028(4) 0.011(3) C43 0.052(4) 0.078(4) 0.061(4) 0.007(3) 0.009(4) 0.003(3) C44 0.057(5) 0.058(4) 0.048(4) 0.006(3) -0.001(4) 0.010(3) C45 0.053(4) 0.045(3) 0.041(3) 0.003(3) 0.004(3) 0.001(3) C46 0.062(4) 0.068(4) 0.054(4) 0.003(3) 0.006(3) 0.003(3) C47 0.078(5) 0.088(5) 0.071(5) 0.024(4) 0.015(4) 0.000(4) C48 0.111(7) 0.122(7) 0.050(5) 0.012(5) 0.023(5) 0.006(5) C49 0.134(8) 0.116(7) 0.046(5) -0.017(4) 0.007(5) 0.008(6) C50 0.103(6) 0.080(5) 0.046(4) -0.016(4) 0.010(4) -0.008(4) C51 0.061(4) 0.058(4) 0.053(4) -0.009(3) -0.002(3) 0.002(3) C52 0.066(5) 0.087(5) 0.063(4) -0.010(4) 0.002(4) 0.007(4) C53 0.060(6) 0.111(6) 0.096(6) -0.025(5) 0.006(5) 0.027(4) C54 0.067(6) 0.137(7) 0.104(7) -0.034(6) -0.029(6) 0.042(5) C55 0.091(7) 0.147(7) 0.075(5) -0.022(5) -0.033(5) 0.051(5) C56 0.073(5) 0.100(5) 0.064(5) -0.009(4) -0.011(4) 0.027(4) C57 0.047(4) 0.048(3) 0.056(4) 0.000(3) -0.003(3) -0.012(3) C58 0.071(5) 0.074(5) 0.108(6) 0.020(4) 0.019(5) -0.011(4) C59 0.090(7) 0.115(7) 0.143(8) 0.033(6) 0.015(6) -0.045(6) C60 0.124(8) 0.060(5) 0.126(7) 0.011(5) -0.016(6) -0.019(5) C61 0.106(7) 0.058(5) 0.100(6) -0.006(4) -0.007(5) -0.007(4) C62 0.070(5) 0.053(4) 0.076(5) -0.004(3) -0.003(4) -0.008(3) C63 0.056(4) 0.037(3) 0.045(4) 0.007(3) 0.006(3) -0.004(3) C64 0.085(6) 0.078(4) 0.057(4) -0.015(4) -0.004(4) 0.031(4) C65 0.096(7) 0.096(5) 0.090(6) -0.015(5) -0.005(5) 0.053(5) C66 0.064(5) 0.065(4) 0.103(6) 0.016(4) 0.000(5) 0.026(4) C67 0.061(5) 0.071(4) 0.078(5) 0.021(4) -0.018(4) 0.009(4) C68 0.073(5) 0.057(4) 0.061(5) -0.002(3) 0.008(4) 0.002(3) C69 0.055(4) 0.036(3) 0.045(4) -0.001(3) -0.006(3) 0.005(3) C70 0.086(6) 0.065(4) 0.066(5) -0.002(4) 0.001(4) -0.007(4) C71 0.097(6) 0.094(5) 0.087(6) -0.027(5) -0.011(5) -0.031(4) C72 0.091(6) 0.085(5) 0.067(5) -0.025(4) -0.023(5) 0.006(4) C73 0.094(6) 0.067(4) 0.054(4) -0.006(4) 0.004(4) 0.009(4) C74 0.083(5) 0.055(4) 0.050(4) -0.010(3) -0.001(4) -0.002(3) C75 0.047(4) 0.036(3) 0.047(3) 0.001(3) -0.002(3) 0.000(3) C76 0.059(4) 0.058(4) 0.068(4) 0.008(3) 0.011(4) -0.001(3) C77 0.082(5) 0.063(4) 0.076(5) 0.024(4) 0.010(4) -0.012(4) C78 0.066(5) 0.088(5) 0.056(4) 0.008(4) 0.010(4) -0.018(4) C79 0.062(5) 0.076(5) 0.070(4) -0.012(4) 0.021(4) -0.001(4) C80 0.058(4) 0.044(3) 0.063(4) 0.000(3) 0.002(3) -0.006(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 C6 1.920(5) 2_655 ? Ni1 C6 1.920(5) . ? Ni1 N1 2.020(4) . ? Ni1 N1 2.020(4) 2_655 ? Ni2 P2 2.2948(18) . ? Ni2 P3 2.3023(19) . ? Ni2 P4 2.3164(19) . ? Ni2 Br1 2.4426(13) . ? P1 N1 1.598(4) . ? P1 C1 1.792(5) . ? P1 C13 1.809(6) . ? P1 C7 1.819(6) . ? P2 C33 1.836(5) . ? P2 C39 1.842(5) . ? P2 C27 1.856(5) . ? P3 C45 1.844(5) . ? P3 C57 1.854(5) . ? P3 C51 1.863(6) . ? P4 C63 1.838(6) . ? P4 C69 1.843(5) . ? P4 C75 1.848(5) . ? N1 C19 1.433(6) . ? C1 C6 1.382(7) . ? C1 C2 1.414(7) . ? C2 C3 1.371(8) . ? C3 C4 1.384(8) . ? C4 C5 1.389(8) . ? C5 C6 1.434(7) . ? C7 C8 1.371(7) . ? C7 C12 1.380(8) . ? C8 C9 1.400(9) . ? C9 C10 1.334(10) . ? C10 C11 1.332(9) . ? C11 C12 1.415(9) . ? C13 C14 1.391(8) . ? C13 C18 1.392(7) . ? C14 C15 1.390(8) . ? C15 C16 1.391(9) . ? C16 C17 1.380(9) . ? C17 C18 1.397(8) . ? C19 C20 1.380(7) . ? C19 C24 1.384(7) . ? C20 C21 1.396(7) . ? C21 C22 1.394(9) . ? C21 C25 1.545(8) . ? C22 C23 1.383(8) . ? C23 C24 1.385(7) . ? C23 C26 1.505(8) . ? C27 C32 1.378(7) . ? C27 C28 1.383(7) . ? C28 C29 1.397(7) . ? C29 C30 1.389(8) . ? C30 C31 1.377(8) . ? C31 C32 1.395(7) . ? C33 C38 1.381(7) . ? C33 C34 1.419(7) . ? C34 C35 1.378(7) . ? C35 C36 1.382(8) . ? C36 C37 1.385(8) . ? C37 C38 1.392(8) . ? C39 C40 1.395(7) . ? C39 C44 1.398(7) . ? C40 C41 1.389(7) . ? C41 C42 1.376(8) . ? C42 C43 1.370(8) . ? C43 C44 1.386(7) . ? C45 C46 1.379(7) . ? C45 C50 1.388(7) . ? C46 C47 1.392(7) . ? C47 C48 1.372(9) . ? C48 C49 1.376(9) . ? C49 C50 1.386(8) . ? C51 C56 1.385(8) . ? C51 C52 1.406(7) . ? C52 C53 1.375(8) . ? C53 C54 1.368(9) . ? C54 C55 1.352(9) . ? C55 C56 1.388(8) . ? C57 C58 1.371(7) . ? C57 C62 1.399(7) . ? C58 C59 1.406(9) . ? C59 C60 1.370(10) . ? C60 C61 1.357(9) . ? C61 C62 1.369(8) . ? C63 C64 1.383(7) . ? C63 C68 1.411(7) . ? C64 C65 1.392(9) . ? C65 C66 1.330(8) . ? C66 C67 1.378(8) . ? C67 C68 1.380(8) . ? C69 C74 1.393(7) . ? C69 C70 1.399(7) . ? C70 C71 1.395(8) . ? C71 C72 1.352(8) . ? C72 C73 1.381(8) . ? C73 C74 1.381(8) . ? C75 C80 1.364(7) . ? C75 C76 1.404(7) . ? C76 C77 1.389(7) . ? C77 C78 1.395(8) . ? C78 C79 1.363(8) . ? C79 C80 1.395(7) . ? C81 C82 1.365(15) . ? C81 C81 1.36(3) 2_554 ? C82 C83 1.402(16) . ? C83 C83 1.20(3) 2_554 ? 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 C6 Ni1 C6 94.3(4) 2_655 . ? C6 Ni1 N1 177.73(19) 2_655 . ? C6 Ni1 N1 85.4(2) . . ? C6 Ni1 N1 85.4(2) 2_655 2_655 ? C6 Ni1 N1 177.73(19) . 2_655 ? N1 Ni1 N1 95.0(2) . 2_655 ? P2 Ni2 P3 109.06(6) . . ? P2 Ni2 P4 117.15(7) . . ? P3 Ni2 P4 115.84(6) . . ? P2 Ni2 Br1 100.59(5) . . ? P3 Ni2 Br1 107.80(6) . . ? P4 Ni2 Br1 104.74(4) . . ? N1 P1 C1 100.8(2) . . ? N1 P1 C13 116.1(2) . . ? C1 P1 C13 109.0(3) . . ? N1 P1 C7 117.9(2) . . ? C1 P1 C7 109.0(2) . . ? C13 P1 C7 103.8(3) . . ? C33 P2 C39 101.6(3) . . ? C33 P2 C27 103.2(2) . . ? C39 P2 C27 103.3(2) . . ? C33 P2 Ni2 111.78(16) . . ? C39 P2 Ni2 117.66(17) . . ? C27 P2 Ni2 117.29(19) . . ? C45 P3 C57 102.9(2) . . ? C45 P3 C51 101.9(3) . . ? C57 P3 C51 101.6(3) . . ? C45 P3 Ni2 119.77(19) . . ? C57 P3 Ni2 113.10(18) . . ? C51 P3 Ni2 115.21(18) . . ? C63 P4 C69 101.6(2) . . ? C63 P4 C75 102.0(2) . . ? C69 P4 C75 101.9(2) . . ? C63 P4 Ni2 109.67(17) . . ? C69 P4 Ni2 119.08(17) . . ? C75 P4 Ni2 119.88(16) . . ? C19 N1 P1 125.7(3) . . ? C19 N1 Ni1 125.3(3) . . ? P1 N1 Ni1 108.5(2) . . ? C6 C1 C2 124.0(5) . . ? C6 C1 P1 112.5(4) . . ? C2 C1 P1 123.0(5) . . ? C3 C2 C1 119.0(6) . . ? C2 C3 C4 118.4(6) . . ? C3 C4 C5 123.2(6) . . ? C4 C5 C6 119.5(6) . . ? C1 C6 C5 115.7(5) . . ? C1 C6 Ni1 116.7(4) . . ? C5 C6 Ni1 127.7(5) . . ? C8 C7 C12 117.4(6) . . ? C8 C7 P1 119.9(5) . . ? C12 C7 P1 122.7(5) . . ? C7 C8 C9 120.8(7) . . ? C10 C9 C8 120.9(8) . . ? C11 C10 C9 120.1(7) . . ? C10 C11 C12 120.7(7) . . ? C7 C12 C11 120.1(7) . . ? C14 C13 C18 119.1(6) . . ? C14 C13 P1 120.8(5) . . ? C18 C13 P1 119.8(5) . . ? C15 C14 C13 121.0(6) . . ? C14 C15 C16 120.2(7) . . ? C17 C16 C15 118.5(7) . . ? C16 C17 C18 122.0(6) . . ? C13 C18 C17 119.1(6) . . ? C20 C19 C24 118.2(5) . . ? C20 C19 N1 122.5(5) . . ? C24 C19 N1 119.3(4) . . ? C19 C20 C21 121.6(6) . . ? C22 C21 C20 117.3(6) . . ? C22 C21 C25 122.2(6) . . ? C20 C21 C25 120.4(6) . . ? C23 C22 C21 123.3(6) . . ? C22 C23 C24 116.4(6) . . ? C22 C23 C26 120.2(6) . . ? C24 C23 C26 123.4(6) . . ? C19 C24 C23 123.2(5) . . ? C32 C27 C28 119.5(5) . . ? C32 C27 P2 122.4(4) . . ? C28 C27 P2 118.0(4) . . ? C27 C28 C29 120.1(5) . . ? C30 C29 C28 120.0(6) . . ? C31 C30 C29 119.9(6) . . ? C30 C31 C32 119.9(5) . . ? C27 C32 C31 120.7(5) . . ? C38 C33 C34 118.4(5) . . ? C38 C33 P2 123.8(4) . . ? C34 C33 P2 117.8(4) . . ? C35 C34 C33 120.5(5) . . ? C34 C35 C36 120.5(6) . . ? C35 C36 C37 119.5(6) . . ? C36 C37 C38 120.7(6) . . ? C33 C38 C37 120.5(5) . . ? C40 C39 C44 117.2(5) . . ? C40 C39 P2 118.0(5) . . ? C44 C39 P2 124.6(4) . . ? C41 C40 C39 120.4(6) . . ? C42 C41 C40 121.3(6) . . ? C43 C42 C41 119.3(6) . . ? C42 C43 C44 120.0(6) . . ? C43 C44 C39 121.8(5) . . ? C46 C45 C50 117.9(5) . . ? C46 C45 P3 117.6(4) . . ? C50 C45 P3 124.5(4) . . ? C45 C46 C47 121.9(6) . . ? C48 C47 C46 119.3(6) . . ? C47 C48 C49 119.7(6) . . ? C48 C49 C50 120.7(7) . . ? C49 C50 C45 120.5(6) . . ? C56 C51 C52 116.3(6) . . ? C56 C51 P3 123.5(5) . . ? C52 C51 P3 120.1(5) . . ? C53 C52 C51 122.2(6) . . ? C54 C53 C52 119.6(7) . . ? C55 C54 C53 119.8(7) . . ? C54 C55 C56 121.4(7) . . ? C51 C56 C55 120.7(6) . . ? C58 C57 C62 118.1(5) . . ? C58 C57 P3 121.0(5) . . ? C62 C57 P3 120.8(4) . . ? C57 C58 C59 120.0(7) . . ? C60 C59 C58 120.3(7) . . ? C61 C60 C59 119.7(7) . . ? C60 C61 C62 120.6(7) . . ? C61 C62 C57 121.2(6) . . ? C64 C63 C68 115.8(5) . . ? C64 C63 P4 124.8(5) . . ? C68 C63 P4 119.3(4) . . ? C63 C64 C65 121.0(6) . . ? C66 C65 C64 122.0(7) . . ? C65 C66 C67 119.5(6) . . ? C66 C67 C68 119.7(6) . . ? C67 C68 C63 122.0(6) . . ? C74 C69 C70 118.3(5) . . ? C74 C69 P4 118.6(4) . . ? C70 C69 P4 123.1(5) . . ? C71 C70 C69 120.1(6) . . ? C72 C71 C70 120.8(6) . . ? C71 C72 C73 119.8(6) . . ? C74 C73 C72 120.7(6) . . ? C73 C74 C69 120.3(6) . . ? C80 C75 C76 117.2(5) . . ? C80 C75 P4 120.1(4) . . ? C76 C75 P4 122.8(4) . . ? C77 C76 C75 121.5(5) . . ? C76 C77 C78 119.7(5) . . ? C79 C78 C77 118.9(5) . . ? C78 C79 C80 120.8(6) . . ? C75 C80 C79 121.9(5) . . ? C82 C81 C81 116.8(10) . 2_554 ? C81 C82 C83 122.5(17) . . ? C83 C83 C82 119.3(11) 2_554 . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 23.22 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.697 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.069 #===end