Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data__2126[(CNC-Me)Pdpy](BF4)2 _database_code_CSD 191341 _journal_coden_Cambridge 186 loop_ _publ_author_name 'Odile Eisenstein' 'Martin Albrecht' 'Eric Clot' 'Robert H. Crabtree' 'J. W. Faller' 'Stephan Grundemann' 'Claire Megret' 'John Miecznikowski' _publ_contact_author_name 'Dr Odile Eisenstein' _publ_contact_author_address ; LSDSMS Universite Montpellier 2 UMR 5636, cc14 Montpellier Cedex 05 FRANCE ; _publ_contact_author_email 'ODILE.EISENSTEIN@UNIV-MONTP2.FR' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Outer sphere anion participation can modify the mechanism for conformer interconversion in Pd pincer complexes ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1994). J. Appl. Cryst., 26, 343. ; _audit_creation_date '2002-08-05' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; #============================================================================== _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'Denzo-SMN' _computing_data_reduction 'Denzo-SMN' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows v. 1.06 (MSC 1999)' _computing_publication_material 'teXsan for Windows v. 1.06 (MSC 1999)' #------------------------------------------------------------------------------ _cell_length_a 9.8872(5) _cell_length_b 9.9387(5) _cell_length_c 12.7418(6) _cell_angle_alpha 77.790(3) _cell_angle_beta 86.260(3) _cell_angle_gamma 85.324(3) _cell_volume 1218.21(10) _cell_formula_units_Z 2 _cell_measurement_temperature 183.2 _cell_measurement_reflns_used 15853 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 626.44 _chemical_formula_analytical ? _chemical_formula_sum 'C20 H22 B2 F8 N6 Pd ' _chemical_formula_moiety 'C20 H22 N6 Pd, 2(B F4)' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 624.00 _exptl_absorpt_coefficient_mu 0.845 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 0.947 _exptl_special_details ; multi-scan from symmetry-related measurements (Blessing 1995) SORTAV R.H Blessing, Acta Cryst., A51, 33-37 (1995), J. Appl. Cryst., 30, 421-426 (1997). ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 183.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 15462 _reflns_number_total 5578 _reflns_number_gt 3701 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.04690 _diffrn_reflns_av_sigmaI/netI 0.112 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.55 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 40 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 44 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; B 0 4 0.000 0.001 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; F 0 16 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 12 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Pd 0 2 -1.177 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pd(1) 0.18559(3) 0.74706(3) 0.29648(2) 0.03464(9) 1.000 . Uani d ? F(1) 0.5541(3) 0.0285(4) 0.2075(3) 0.0943(12) 1.000 . Uani d ? F(2) 0.5969(4) 0.0875(4) 0.3586(4) 0.130(2) 1.000 . Uani d ? F(3) 0.3806(3) 0.0570(4) 0.3233(3) 0.0978(13) 1.000 . Uani d ? F(4) 0.5323(3) -0.1205(3) 0.3608(3) 0.0798(10) 1.000 . Uani d ? F(5) -0.0623(6) 0.4267(4) 0.1315(4) 0.173(2) 1.000 . Uani d ? F(6) -0.1155(4) 0.6547(4) 0.1155(3) 0.111(2) 1.000 . Uani d ? F(7) -0.0437(5) 0.5274(4) 0.2694(5) 0.149(2) 1.000 . Uani d ? F(8) -0.2407(4) 0.4937(5) 0.2161(3) 0.119(2) 1.000 . Uani d ? N(1) 0.2969(3) 0.5785(3) 0.4937(3) 0.0405(10) 1.000 . Uani d ? N(2) 0.3171(3) 0.4506(3) 0.3782(3) 0.0432(10) 1.000 . Uani d ? N(3) -0.0509(3) 0.9339(3) 0.2284(3) 0.0408(10) 1.000 . Uani d ? N(4) 0.1151(4) 1.0220(3) 0.1296(3) 0.0412(10) 1.000 . Uani d ? N(5) 0.0692(3) 0.7796(3) 0.4301(3) 0.0367(9) 1.000 . Uani d ? N(6) 0.3035(3) 0.7177(3) 0.1668(3) 0.0385(10) 1.000 . Uani d ? C(1) 0.1247(4) 0.7607(4) 0.5267(3) 0.0402(12) 1.000 . Uani d ? C(2) 0.0514(5) 0.7925(4) 0.6150(3) 0.0470(13) 1.000 . Uani d ? C(3) -0.0804(5) 0.8502(5) 0.6042(4) 0.049(1) 1.000 . Uani d ? C(4) -0.1354(4) 0.8677(4) 0.5068(4) 0.0455(13) 1.000 . Uani d ? C(5) -0.0624(4) 0.8301(4) 0.4212(3) 0.0384(12) 1.000 . Uani d ? C(6) 0.2705(5) 0.7029(5) 0.5372(3) 0.0484(13) 1.000 . Uani d ? C(7) -0.1244(4) 0.8399(4) 0.3146(4) 0.0443(13) 1.000 . Uani d ? C(11) 0.2746(4) 0.5782(4) 0.3911(3) 0.0382(12) 1.000 . Uani d ? C(12) 0.3499(4) 0.4503(5) 0.5467(4) 0.0486(13) 1.000 . Uani d ? C(13) 0.3626(4) 0.3709(4) 0.4736(4) 0.050(1) 1.000 . Uani d ? C(14) 0.3137(5) 0.3981(5) 0.2805(4) 0.061(2) 1.000 . Uani d ? C(21) 0.0834(4) 0.9141(4) 0.2091(3) 0.0371(11) 1.000 . Uani d ? C(22) -0.1047(5) 1.0526(5) 0.1633(4) 0.051(1) 1.000 . Uani d ? C(23) -0.0012(5) 1.1069(5) 0.1015(4) 0.052(1) 1.000 . Uani d ? C(24) 0.2496(5) 1.0509(5) 0.0816(4) 0.054(1) 1.000 . Uani d ? C(31) 0.4393(5) 0.7282(4) 0.1663(4) 0.0481(13) 1.000 . Uani d ? C(32) 0.5243(6) 0.7097(6) 0.0809(5) 0.072(2) 1.000 . Uani d ? C(33) 0.4703(8) 0.6816(6) -0.0068(5) 0.083(2) 1.000 . Uani d ? C(34) 0.3339(8) 0.6685(5) -0.0074(4) 0.074(2) 1.000 . Uani d ? C(35) 0.2521(5) 0.6867(5) 0.0811(4) 0.052(1) 1.000 . Uani d ? B(1) 0.5154(6) 0.0166(6) 0.3145(5) 0.051(2) 1.000 . Uani d ? B(2) -0.1143(8) 0.5277(7) 0.1797(6) 0.075(2) 1.000 . Uani d ? H(1) 0.0911 0.7749 0.6829 0.057 1.000 . Uiso c ? H(2) -0.1312 0.8769 0.6633 0.059 1.000 . Uiso c ? H(3) -0.2259 0.9067 0.4979 0.055 1.000 . Uiso c ? H(4) 0.2900 0.6815 0.6111 0.058 1.000 . Uiso c ? H(5) 0.3283 0.7709 0.4995 0.058 1.000 . Uiso c ? H(6) -0.2167 0.8740 0.3193 0.053 1.000 . Uiso c ? H(7) -0.1197 0.7508 0.2981 0.053 1.000 . Uiso c ? H(8) 0.3726 0.4244 0.6198 0.058 1.000 . Uiso c ? H(9) 0.3964 0.2770 0.4852 0.060 1.000 . Uiso c ? H(10) 0.3832 0.4360 0.2306 0.073 1.000 . Uiso c ? H(11) 0.2278 0.4236 0.2502 0.073 1.000 . Uiso c ? H(12) 0.3279 0.3004 0.2969 0.073 1.000 . Uiso c ? H(13) -0.1969 1.0881 0.1628 0.061 1.000 . Uiso c ? H(14) -0.0059 1.1892 0.0476 0.062 1.000 . Uiso c ? H(15) 0.3162 0.9975 0.1262 0.065 1.000 . Uiso c ? H(16) 0.2583 1.0280 0.0127 0.065 1.000 . Uiso c ? H(17) 0.2624 1.1462 0.0746 0.065 1.000 . Uiso c ? H(18) 0.4766 0.7492 0.2274 0.058 1.000 . Uiso c ? H(19) 0.6194 0.7165 0.0827 0.086 1.000 . Uiso c ? H(20) 0.5275 0.6708 -0.0677 0.099 1.000 . Uiso c ? H(21) 0.2959 0.6473 -0.0680 0.088 1.000 . Uiso c ? H(22) 0.1573 0.6771 0.0811 0.063 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0349(2) 0.0321(2) 0.0337(2) 0.00099(12) 0.00061(12) -0.00179(12) F(1) 0.080(2) 0.124(3) 0.066(2) -0.021(2) -0.001(2) 0.013(2) F(2) 0.127(3) 0.130(3) 0.160(4) -0.036(3) -0.045(3) -0.069(3) F(3) 0.061(2) 0.098(3) 0.127(3) 0.038(2) -0.004(2) -0.024(2) F(4) 0.084(2) 0.059(2) 0.082(2) 0.018(2) -0.005(2) 0.009(2) F(5) 0.309(7) 0.076(3) 0.118(4) 0.024(3) 0.072(4) -0.026(2) F(6) 0.137(3) 0.069(2) 0.113(3) -0.015(2) 0.033(3) 0.007(2) F(7) 0.156(4) 0.073(3) 0.228(5) 0.003(3) -0.105(4) -0.030(3) F(8) 0.098(3) 0.168(4) 0.072(2) -0.034(3) 0.007(2) 0.023(2) N(1) 0.037(2) 0.040(2) 0.039(2) 0.001(2) -0.001(2) 0.001(2) N(2) 0.043(2) 0.032(2) 0.048(2) 0.002(2) 0.001(2) 0.003(2) N(3) 0.039(2) 0.038(2) 0.044(2) 0.003(2) -0.009(2) -0.004(2) N(4) 0.047(2) 0.040(2) 0.034(2) -0.000(2) -0.007(2) 0.001(2) N(5) 0.038(2) 0.035(2) 0.035(2) -0.003(2) 0.004(2) -0.005(1) N(6) 0.045(2) 0.034(2) 0.033(2) 0.001(2) 0.000(2) -0.001(1) C(1) 0.045(3) 0.037(2) 0.037(2) -0.007(2) 0.002(2) -0.003(2) C(2) 0.062(3) 0.042(3) 0.037(3) -0.011(2) 0.005(2) -0.008(2) C(3) 0.060(3) 0.048(3) 0.042(3) -0.013(2) 0.014(2) -0.015(2) C(4) 0.034(2) 0.042(3) 0.060(3) -0.007(2) 0.013(2) -0.011(2) C(5) 0.035(2) 0.033(2) 0.044(3) -0.002(2) 0.006(2) -0.004(2) C(6) 0.048(3) 0.052(3) 0.041(3) -0.003(2) -0.005(2) 0.000(2) C(7) 0.032(2) 0.047(3) 0.053(3) -0.001(2) 0.002(2) -0.010(2) C(11) 0.033(2) 0.033(2) 0.044(3) -0.001(2) 0.004(2) 0.001(2) C(12) 0.037(3) 0.045(3) 0.052(3) -0.003(2) -0.007(2) 0.017(2) C(13) 0.041(3) 0.034(2) 0.068(3) -0.003(2) -0.002(2) 0.006(2) C(14) 0.072(4) 0.042(3) 0.066(3) 0.000(3) 0.009(3) -0.011(2) C(21) 0.039(2) 0.034(2) 0.039(2) -0.000(2) -0.003(2) -0.009(2) C(22) 0.048(3) 0.057(3) 0.044(3) 0.010(2) -0.013(2) -0.005(2) C(23) 0.062(3) 0.045(3) 0.043(3) 0.007(2) -0.016(2) 0.002(2) C(24) 0.056(3) 0.051(3) 0.046(3) -0.006(2) -0.004(2) 0.009(2) C(31) 0.047(3) 0.044(3) 0.048(3) -0.001(2) 0.003(2) -0.001(2) C(32) 0.068(4) 0.064(4) 0.073(4) 0.001(3) 0.030(3) -0.005(3) C(33) 0.101(5) 0.075(4) 0.061(4) 0.011(4) 0.033(4) -0.008(3) C(34) 0.124(6) 0.053(3) 0.041(3) 0.014(3) -0.006(3) -0.009(2) C(35) 0.070(3) 0.044(3) 0.039(3) 0.009(2) -0.010(2) -0.004(2) B(1) 0.047(3) 0.044(3) 0.060(4) 0.010(3) -0.011(3) -0.007(3) B(2) 0.092(6) 0.063(5) 0.073(5) -0.009(4) 0.008(4) -0.021(4) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3701 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.041 _refine_ls_wR_factor_all 0.057 _refine_ls_wR_factor_ref 0.049 _refine_ls_goodness_of_fit_all 1.104 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.50 _refine_diff_density_max 0.92 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) N(5) 2.060(4) . . ? Pd(1) N(6) 2.017(4) . . ? Pd(1) C(11) 2.021(4) . . ? Pd(1) C(21) 2.027(4) . . ? F(1) B(1) 1.376(7) . . ? F(2) B(1) 1.334(7) . . ? F(3) B(1) 1.364(6) . . ? F(4) B(1) 1.367(6) . . ? F(5) B(2) 1.336(8) . . ? F(6) B(2) 1.350(8) . . ? F(7) B(2) 1.377(9) . . ? F(8) B(2) 1.348(9) . . ? N(1) C(6) 1.457(6) . . ? N(1) C(11) 1.341(5) . . ? N(1) C(12) 1.388(5) . . ? N(2) C(11) 1.343(5) . . ? N(2) C(13) 1.383(6) . . ? N(2) C(14) 1.450(6) . . ? N(3) C(7) 1.476(6) . . ? N(3) C(21) 1.341(5) . . ? N(3) C(22) 1.380(6) . . ? N(4) C(21) 1.352(5) . . ? N(4) C(23) 1.390(6) . . ? N(4) C(24) 1.452(6) . . ? N(5) C(1) 1.351(5) . . ? N(5) C(5) 1.359(5) . . ? N(6) C(31) 1.355(6) . . ? N(6) C(35) 1.337(6) . . ? C(1) C(2) 1.377(6) . . ? C(1) C(6) 1.511(6) . . ? C(2) C(3) 1.383(7) . . ? C(2) H(1) 0.95 . . no C(3) C(4) 1.359(6) . . ? C(3) H(2) 0.95 . . no C(4) C(5) 1.370(6) . . ? C(4) H(3) 0.95 . . no C(5) C(7) 1.507(6) . . ? C(6) H(4) 0.95 . . no C(6) H(5) 0.95 . . no C(7) H(6) 0.95 . . no C(7) H(7) 0.95 . . no C(12) C(13) 1.336(7) . . ? C(12) H(8) 0.95 . . no C(13) H(9) 0.95 . . no C(14) H(10) 0.95 . . no C(14) H(11) 0.95 . . no C(14) H(12) 0.95 . . no C(22) C(23) 1.328(7) . . ? C(22) H(13) 0.95 . . no C(23) H(14) 0.95 . . no C(24) H(15) 0.95 . . no C(24) H(16) 0.95 . . no C(24) H(17) 0.95 . . no C(31) C(32) 1.366(7) . . ? C(31) H(18) 0.95 . . no C(32) C(33) 1.359(9) . . ? C(32) H(19) 0.95 . . no C(33) C(34) 1.366(9) . . ? C(33) H(20) 0.95 . . no C(34) C(35) 1.379(8) . . ? C(34) H(21) 0.95 . . no C(35) H(22) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(5) Pd(1) N(6) 178.5(2) . . . ? N(5) Pd(1) C(11) 87.8(2) . . . ? N(5) Pd(1) C(21) 88.4(2) . . . ? N(6) Pd(1) C(11) 92.1(2) . . . ? N(6) Pd(1) C(21) 91.8(2) . . . ? C(11) Pd(1) C(21) 175.6(2) . . . ? C(6) N(1) C(11) 121.5(4) . . . ? C(6) N(1) C(12) 127.2(4) . . . ? C(11) N(1) C(12) 111.2(4) . . . ? C(11) N(2) C(13) 110.5(4) . . . ? C(11) N(2) C(14) 126.3(4) . . . ? C(13) N(2) C(14) 123.2(4) . . . ? C(7) N(3) C(21) 121.4(4) . . . ? C(7) N(3) C(22) 126.7(4) . . . ? C(21) N(3) C(22) 111.9(4) . . . ? C(21) N(4) C(23) 109.8(4) . . . ? C(21) N(4) C(24) 126.5(4) . . . ? C(23) N(4) C(24) 123.7(4) . . . ? Pd(1) N(5) C(1) 120.7(3) . . . ? Pd(1) N(5) C(5) 120.5(3) . . . ? C(1) N(5) C(5) 118.6(4) . . . ? Pd(1) N(6) C(31) 119.4(3) . . . ? Pd(1) N(6) C(35) 122.0(3) . . . ? C(31) N(6) C(35) 118.5(4) . . . ? N(5) C(1) C(2) 121.5(4) . . . ? N(5) C(1) C(6) 118.7(4) . . . ? C(2) C(1) C(6) 119.8(4) . . . ? C(1) C(2) C(3) 119.6(4) . . . ? C(1) C(2) H(1) 120.2 . . . no C(3) C(2) H(1) 120.2 . . . no C(2) C(3) C(4) 118.3(4) . . . ? C(2) C(3) H(2) 120.9 . . . no C(4) C(3) H(2) 120.8 . . . no C(3) C(4) C(5) 121.1(4) . . . ? C(3) C(4) H(3) 119.5 . . . no C(5) C(4) H(3) 119.5 . . . no N(5) C(5) C(4) 120.8(4) . . . ? N(5) C(5) C(7) 117.3(4) . . . ? C(4) C(5) C(7) 121.9(4) . . . ? N(1) C(6) C(1) 112.3(4) . . . ? N(1) C(6) H(4) 108.8 . . . no N(1) C(6) H(5) 108.8 . . . no C(1) C(6) H(4) 108.8 . . . no C(1) C(6) H(5) 108.8 . . . no H(4) C(6) H(5) 109.4 . . . no N(3) C(7) C(5) 110.6(4) . . . ? N(3) C(7) H(6) 109.2 . . . no N(3) C(7) H(7) 109.2 . . . no C(5) C(7) H(6) 109.2 . . . no C(5) C(7) H(7) 109.2 . . . no H(6) C(7) H(7) 109.5 . . . no Pd(1) C(11) N(1) 120.2(3) . . . ? Pd(1) C(11) N(2) 134.7(4) . . . ? N(1) C(11) N(2) 105.0(4) . . . ? N(1) C(12) C(13) 105.9(4) . . . ? N(1) C(12) H(8) 127.0 . . . no C(13) C(12) H(8) 127.0 . . . no N(2) C(13) C(12) 107.4(4) . . . ? N(2) C(13) H(9) 126.3 . . . no C(12) C(13) H(9) 126.3 . . . no N(2) C(14) H(10) 109.5 . . . no N(2) C(14) H(11) 109.5 . . . no N(2) C(14) H(12) 109.5 . . . no H(10) C(14) H(11) 109.5 . . . no H(10) C(14) H(12) 109.5 . . . no H(11) C(14) H(12) 109.5 . . . no Pd(1) C(21) N(3) 119.0(3) . . . ? Pd(1) C(21) N(4) 136.3(3) . . . ? N(3) C(21) N(4) 104.7(4) . . . ? N(3) C(22) C(23) 105.9(4) . . . ? N(3) C(22) H(13) 127.1 . . . no C(23) C(22) H(13) 127.1 . . . no N(4) C(23) C(22) 107.9(4) . . . ? N(4) C(23) H(14) 126.1 . . . no C(22) C(23) H(14) 126.1 . . . no N(4) C(24) H(15) 109.5 . . . no N(4) C(24) H(16) 109.5 . . . no N(4) C(24) H(17) 109.5 . . . no H(15) C(24) H(16) 109.5 . . . no H(15) C(24) H(17) 109.5 . . . no H(16) C(24) H(17) 109.5 . . . no N(6) C(31) C(32) 122.1(5) . . . ? N(6) C(31) H(18) 118.9 . . . no C(32) C(31) H(18) 118.9 . . . no C(31) C(32) C(33) 118.7(6) . . . ? C(31) C(32) H(19) 120.6 . . . no C(33) C(32) H(19) 120.7 . . . no C(32) C(33) C(34) 120.2(6) . . . ? C(32) C(33) H(20) 119.9 . . . no C(34) C(33) H(20) 119.9 . . . no C(33) C(34) C(35) 119.1(6) . . . ? C(33) C(34) H(21) 120.4 . . . no C(35) C(34) H(21) 120.5 . . . no N(6) C(35) C(34) 121.3(5) . . . ? N(6) C(35) H(22) 119.3 . . . no C(34) C(35) H(22) 119.3 . . . no F(1) B(1) F(2) 108.8(5) . . . ? F(1) B(1) F(3) 108.8(5) . . . ? F(1) B(1) F(4) 106.5(5) . . . ? F(2) B(1) F(3) 114.6(5) . . . ? F(2) B(1) F(4) 109.6(5) . . . ? F(3) B(1) F(4) 108.2(5) . . . ? F(5) B(2) F(6) 114.0(7) . . . ? F(5) B(2) F(7) 110.0(7) . . . ? F(5) B(2) F(8) 105.8(7) . . . ? F(6) B(2) F(7) 109.0(6) . . . ? F(6) B(2) F(8) 111.6(7) . . . ? F(7) B(2) F(8) 106.1(6) . . . ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pd(1) F(7) 3.355(4) . . no F(1) C(22) 3.403(6) . 1_645 no F(1) C(33) 3.428(7) . 2_665 no F(1) C(31) 3.430(6) . 1_545 no F(1) C(24) 3.471(6) . 1_545 no F(2) C(6) 3.108(6) . 2_666 no F(3) C(3) 3.174(6) . 2_566 no F(3) C(4) 3.291(6) . 2_566 no F(3) C(14) 3.336(6) . . no F(3) C(24) 3.431(6) . 1_545 no F(4) C(13) 3.061(5) . 2_656 no F(4) C(31) 3.368(6) . 1_545 no F(4) C(12) 3.379(6) . 2_656 no F(4) C(7) 3.412(5) . 1_645 no F(5) C(23) 3.283(7) . 1_545 no F(5) C(34) 3.493(10) . 2_565 no F(5) C(2) 3.496(6) . 2_566 no F(5) F(5) 3.544(9) . 2_565 no F(6) C(7) 3.428(6) . . no F(6) C(23) 3.443(6) . 2_575 no F(6) N(3) 3.504(6) . . no F(6) C(32) 3.600(8) . 1_455 no F(7) C(2) 3.214(6) . 2_566 no F(7) C(7) 3.303(6) . . no F(7) C(1) 3.542(7) . 2_566 no F(8) C(12) 3.287(7) . 2_566 no F(8) C(32) 3.334(8) . 1_455 no F(8) C(6) 3.342(6) . 2_566 no F(8) C(34) 3.591(8) . 2_565 no N(1) C(12) 3.494(6) . 2_666 no N(1) C(13) 3.509(6) . 2_666 no C(2) C(4) 3.546(6) . 2_576 no C(2) C(22) 3.577(7) . 2_576 no C(3) C(5) 3.526(6) . 2_576 no C(3) C(14) 3.539(7) . 2_566 no C(4) C(13) 3.358(6) . 2_566 no C(12) C(12) 3.274(9) . 2_666 no C(12) C(13) 3.441(7) . 2_666 no C(33) C(33) 3.578(13) . 2_665 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Pd(1) N(5) C(1) C(2) . . . . 174.7(3) no Pd(1) N(5) C(1) C(6) . . . . -5.4(5) no Pd(1) N(5) C(5) C(4) . . . . -172.0(3) no Pd(1) N(5) C(5) C(7) . . . . 9.2(5) no Pd(1) N(6) C(31) C(32) . . . . -179.9(4) no Pd(1) N(6) C(35) C(34) . . . . 179.3(4) no Pd(1) C(11) N(1) C(6) . . . . -6.1(5) no Pd(1) C(11) N(1) C(12) . . . . 175.8(3) no Pd(1) C(11) N(2) C(13) . . . . -175.4(3) no Pd(1) C(11) N(2) C(14) . . . . 2.7(7) no Pd(1) C(21) N(3) C(7) . . . . 2.5(6) no Pd(1) C(21) N(3) C(22) . . . . 179.3(3) no Pd(1) C(21) N(4) C(23) . . . . -179.5(4) no Pd(1) C(21) N(4) C(24) . . . . -1.6(8) no N(1) C(6) C(1) N(5) . . . . -50.1(5) no N(1) C(6) C(1) C(2) . . . . 129.7(4) no N(1) C(11) Pd(1) N(5) . . . . -35.5(3) no N(1) C(11) Pd(1) N(6) . . . . 143.0(3) no N(1) C(11) Pd(1) C(21) . . . . -64.9(25) no N(1) C(11) N(2) C(13) . . . . 1.5(5) no N(1) C(11) N(2) C(14) . . . . 179.7(4) no N(1) C(12) C(13) N(2) . . . . -0.2(5) no N(2) C(11) Pd(1) N(5) . . . . 141.1(4) no N(2) C(11) Pd(1) N(6) . . . . -40.4(4) no N(2) C(11) Pd(1) C(21) . . . . 111.7(23) no N(2) C(11) N(1) C(6) . . . . 176.5(4) no N(2) C(11) N(1) C(12) . . . . -1.6(5) no N(3) C(7) C(5) N(5) . . . . -61.5(5) no N(3) C(7) C(5) C(4) . . . . 119.8(4) no N(3) C(21) Pd(1) N(5) . . . . -40.3(4) no N(3) C(21) Pd(1) N(6) . . . . 141.2(4) no N(3) C(21) Pd(1) C(11) . . . . -10.9(26) no N(3) C(21) N(4) C(23) . . . . 0.1(5) no N(3) C(21) N(4) C(24) . . . . 178.0(4) no N(3) C(22) C(23) N(4) . . . . -0.4(6) no N(4) C(21) Pd(1) N(5) . . . . 139.3(5) no N(4) C(21) Pd(1) N(6) . . . . -39.2(5) no N(4) C(21) Pd(1) C(11) . . . . 168.7(21) no N(4) C(21) N(3) C(7) . . . . -177.2(4) no N(4) C(21) N(3) C(22) . . . . -0.4(5) no N(5) Pd(1) N(6) C(31) . . . . 18.6(52) no N(5) Pd(1) N(6) C(35) . . . . -162.0(49) no N(5) C(1) C(2) C(3) . . . . -2.6(7) no N(5) C(5) C(4) C(3) . . . . -2.8(7) no N(6) Pd(1) N(5) C(1) . . . . -42.7(52) no N(6) Pd(1) N(5) C(5) . . . . 132.6(50) no N(6) C(31) C(32) C(33) . . . . 0.8(8) no N(6) C(35) C(34) C(33) . . . . 0.5(8) no C(1) N(5) Pd(1) C(11) . . . . 41.1(3) no C(1) N(5) Pd(1) C(21) . . . . -141.0(3) no C(1) N(5) C(5) C(4) . . . . 3.3(6) no C(1) N(5) C(5) C(7) . . . . -175.5(4) no C(1) C(2) C(3) C(4) . . . . 3.0(7) no C(1) C(6) N(1) C(11) . . . . 57.9(5) no C(1) C(6) N(1) C(12) . . . . -124.3(4) no C(2) C(1) N(5) C(5) . . . . -0.6(6) no C(2) C(3) C(4) C(5) . . . . -0.4(7) no C(3) C(2) C(1) C(6) . . . . 177.6(4) no C(3) C(4) C(5) C(7) . . . . 175.9(4) no C(5) N(5) Pd(1) C(11) . . . . -143.7(3) no C(5) N(5) Pd(1) C(21) . . . . 34.2(3) no C(5) N(5) C(1) C(6) . . . . 179.3(4) no C(5) C(7) N(3) C(21) . . . . 55.9(5) no C(5) C(7) N(3) C(22) . . . . -120.5(5) no C(6) N(1) C(12) C(13) . . . . -176.8(4) no C(7) N(3) C(22) C(23) . . . . 177.2(4) no C(11) Pd(1) N(6) C(31) . . . . -65.1(3) no C(11) Pd(1) N(6) C(35) . . . . 114.3(4) no C(11) N(1) C(12) C(13) . . . . 1.2(5) no C(11) N(2) C(13) C(12) . . . . -0.8(5) no C(12) C(13) N(2) C(14) . . . . -179.1(4) no C(21) Pd(1) N(6) C(31) . . . . 117.0(3) no C(21) Pd(1) N(6) C(35) . . . . -63.7(4) no C(21) N(3) C(22) C(23) . . . . 0.5(6) no C(21) N(4) C(23) C(22) . . . . 0.2(6) no C(22) C(23) N(4) C(24) . . . . -177.8(5) no C(31) N(6) C(35) C(34) . . . . -1.4(7) no C(31) C(32) C(33) C(34) . . . . -1.7(9) no C(32) C(31) N(6) C(35) . . . . 0.7(7) no C(32) C(33) C(34) C(35) . . . . 1.1(9) no #------------------------------------------------------------------------------ #============================================================================== #============================================================================== # End of CIF #==============================================================================