Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_sxc6 _database_code_CSD 158059 #--------------------------------------------------------------------------- _journal_coden_Cambridge 186 _audit_creation_date '1999-10-06' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; 2001-02-07 - passes checkcif tests with minor warnings ; #--------------------------------------------------------------------------- #-- _publ_requested_journal ' J. Chem. Soc., Dalton Trans. ' _publ_requested_category ' CM ' _publ_contact_author_name ' Dr Geoffrey Salem ' _publ_contact_author_address ; Dr Geoffrey Salem Chemistry Department, The Faculties Australian National University Canberra A. C. T. 0200 AUSTRALIA ; _publ_contact_letter ; ENTER TEXT OF LETTER ; loop_ _publ_author_name _publ_author_address ' Swarup Chatterjee ' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; 'George, Mark D' ; ? ; ' Geoffrey Salem ' ; Chemistry Department, The Faculties, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Anthony C. Willis ' ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_section_title ; sxc6 ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. de Meulenaer, J. & Tompa, H. (1965), Acta Cryst. 19, 1014. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #--------------------------------------------------------------------------- #-- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #--------------------------------------------------------------------------- #-- _cell_length_a 8.982(2) _cell_length_b 13.436(2) _cell_length_c 13.797(2) _cell_angle_alpha 90 _cell_angle_beta 102.87(1) _cell_angle_gamma 90 _cell_volume 1623.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16.5 _cell_measurement_theta_max 19.5 #--------------------------------------------------------------------------- #-- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' #--------------------------------------------------------------------------- #-- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 744.35 _chemical_formula_analytical ? _chemical_formula_sum 'C29 H33 Cl F6 N P3 Pd ' _chemical_formula_moiety 'C29 H33 Cl N P2 Pd 1+, F6 P 1-' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 752.00 _exptl_absorpt_coefficient_mu 0.845 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.927 _exptl_absorpt_correction_T_min 0.852 _exptl_special_details ; The scan width was (1.20+0.34tan\q)\% with an \w scan speed of 2\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Mass attenuation coefficients for absorption from International Tables for X-ray Crystallography, Vol IV (1974) Table 2.1C. ; #--------------------------------------------------------------------------- #-- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.58 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 5016 _reflns_number_total 3899 _reflns_number_gt 3259 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.03500 _diffrn_reflns_av_sigmaI/netI 0.050 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.54 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.02368 _diffrn_orient_matrix_UB_12 0.07279 _diffrn_orient_matrix_UB_13 -0.00198 _diffrn_orient_matrix_UB_21 -0.00690 _diffrn_orient_matrix_UB_22 -0.00247 _diffrn_orient_matrix_UB_23 0.07131 _diffrn_orient_matrix_UB_31 0.11151 _diffrn_orient_matrix_UB_32 0.01531 _diffrn_orient_matrix_UB_33 0.02095 #--------------------------------------------------------------------------- #-- 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 58 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 66 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 2 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 12 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 2 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 6 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pd 0 2 -1.177 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------- #-- 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) 0.49060(4) 0.5000 0.72641(3) 0.04052(9) 1.000 . Uani d ? Cl(1) 0.3839(2) 0.7258(2) 0.6098(1) 0.0671(6) 1.000 . Uani d ? P(1) 0.6507(1) 0.4970(2) 0.61360(9) 0.0494(4) 1.000 . Uani d ? P(2) 0.6270(2) 0.6317(1) 0.7918(1) 0.0445(4) 1.000 . Uani d ? P(3) 0.0774(3) 0.5845(2) 0.3294(2) 0.0798(7) 1.000 . Uani d ? F(1) -0.0120(6) 0.5143(5) 0.3899(3) 0.122(2) 1.000 . Uani d ? F(2) 0.1922(7) 0.6071(5) 0.4284(4) 0.162(3) 1.000 . Uani d ? F(3) -0.0168(8) 0.6754(4) 0.3499(4) 0.162(3) 1.000 . Uani d ? F(4) 0.1636(8) 0.6522(5) 0.2691(4) 0.152(3) 1.000 . Uani d ? F(5) -0.0350(7) 0.5565(6) 0.2358(3) 0.190(3) 1.000 . Uani d ? F(6) 0.1840(6) 0.4985(6) 0.3143(4) 0.159(2) 1.000 . Uani d ? N(1) 0.3456(5) 0.3761(4) 0.6713(3) 0.052(2) 1.000 . Uani d ? C(1) 0.780(1) 0.3927(7) 0.6192(7) 0.078(3) 1.000 . Uani d ? C(2) 0.5620(7) 0.5121(8) 0.4821(4) 0.071(2) 1.000 . Uani d ? C(3) 0.7771(8) 0.6038(6) 0.6392(6) 0.054(2) 1.000 . Uani d ? C(4) 0.8838(8) 0.6263(6) 0.5834(5) 0.074(3) 1.000 . Uani d ? C(5) 0.9727(9) 0.7103(7) 0.6051(7) 0.090(3) 1.000 . Uani d ? C(6) 0.9587(9) 0.7728(7) 0.6809(8) 0.104(4) 1.000 . Uani d ? C(7) 0.8542(8) 0.7508(6) 0.7376(6) 0.085(3) 1.000 . Uani d ? C(8) 0.7646(7) 0.6660(5) 0.7171(5) 0.055(2) 1.000 . Uani d ? C(9) 0.7450(8) 0.6072(5) 0.9142(4) 0.074(2) 1.000 . Uani d ? C(10) 0.5299(6) 0.7485(4) 0.8033(4) 0.043(2) 1.000 . Uani d ? C(11) 0.4216(6) 0.7874(4) 0.7233(4) 0.049(2) 1.000 . Uani d ? C(12) 0.3444(7) 0.8747(5) 0.7324(5) 0.063(2) 1.000 . Uani d ? C(13) 0.3736(8) 0.9239(5) 0.8213(5) 0.072(2) 1.000 . Uani d ? C(14) 0.4809(8) 0.8888(5) 0.9000(5) 0.075(2) 1.000 . Uani d ? C(15) 0.5573(7) 0.8026(5) 0.8921(5) 0.062(2) 1.000 . Uani d ? C(16) 0.3567(5) 0.4991(8) 0.8299(3) 0.047(1) 1.000 . Uani d ? C(17) 0.3346(8) 0.5740(5) 0.8961(5) 0.060(2) 1.000 . Uani d ? C(18) 0.2402(9) 0.5607(5) 0.9608(5) 0.072(3) 1.000 . Uani d ? C(19) 0.1549(7) 0.4728(5) 0.9582(5) 0.056(2) 1.000 . Uani d ? C(20) 0.0551(8) 0.4570(5) 1.0252(5) 0.073(2) 1.000 . Uani d ? C(21) -0.0304(8) 0.3753(8) 1.0195(6) 0.086(3) 1.000 . Uani d ? C(22) -0.0220(9) 0.3044(7) 0.9496(6) 0.088(3) 1.000 . Uani d ? C(23) 0.0760(8) 0.3127(6) 0.8871(5) 0.071(2) 1.000 . Uani d ? C(24) 0.1693(7) 0.3991(5) 0.8908(4) 0.054(2) 1.000 . Uani d ? C(25) 0.2748(6) 0.4117(4) 0.8282(4) 0.044(2) 1.000 . Uani d ? C(26) 0.3083(7) 0.3302(5) 0.7620(4) 0.057(2) 1.000 . Uani d ? C(27) 0.433(1) 0.2639(6) 0.8169(6) 0.091(3) 1.000 . Uani d ? C(28) 0.401(1) 0.3014(6) 0.6107(6) 0.077(3) 1.000 . Uani d ? C(29) 0.2059(7) 0.4201(6) 0.6076(4) 0.072(2) 1.000 . Uani d ? H(1) 0.8457 0.3895 0.6835 0.093 1.000 . Uiso c ? H(2) 0.8394 0.4010 0.5708 0.093 1.000 . Uiso c ? H(3) 0.7230 0.3327 0.6064 0.093 1.000 . Uiso c ? H(4) 0.5094 0.5739 0.4723 0.085 1.000 . Uiso c ? H(5) 0.6386 0.5110 0.4445 0.085 1.000 . Uiso c ? H(6) 0.4919 0.4593 0.4611 0.085 1.000 . Uiso c ? H(7) 0.8953 0.5839 0.5304 0.089 1.000 . Uiso c ? H(8) 1.0454 0.7252 0.5666 0.108 1.000 . Uiso c ? H(9) 1.0203 0.8308 0.6944 0.124 1.000 . Uiso c ? H(10) 0.8438 0.7936 0.7906 0.102 1.000 . Uiso c ? H(11) 0.8142 0.5547 0.9100 0.089 1.000 . Uiso c ? H(12) 0.8008 0.6655 0.9386 0.089 1.000 . Uiso c ? H(13) 0.6820 0.5885 0.9580 0.089 1.000 . Uiso c ? H(14) 0.2716 0.9002 0.6772 0.075 1.000 . Uiso c ? H(15) 0.3188 0.9829 0.8284 0.086 1.000 . Uiso c ? H(16) 0.5026 0.9248 0.9608 0.090 1.000 . Uiso c ? H(17) 0.6305 0.7788 0.9480 0.074 1.000 . Uiso c ? H(18) 0.3864 0.6357 0.8962 0.072 1.000 . Uiso c ? H(19) 0.2326 0.6112 1.0076 0.086 1.000 . Uiso c ? H(20) 0.0500 0.5057 1.0743 0.087 1.000 . Uiso c ? H(21) -0.0967 0.3663 1.0637 0.103 1.000 . Uiso c ? H(22) -0.0863 0.2476 0.9444 0.106 1.000 . Uiso c ? H(23) 0.0820 0.2609 0.8412 0.085 1.000 . Uiso c ? H(24) 0.2185 0.2912 0.7415 0.068 1.000 . Uiso c ? H(25) 0.4026 0.2356 0.8727 0.109 1.000 . Uiso c ? H(26) 0.5233 0.3017 0.8390 0.109 1.000 . Uiso c ? H(27) 0.4513 0.2123 0.7740 0.109 1.000 . Uiso c ? H(28) 0.4907 0.2710 0.6488 0.093 1.000 . Uiso c ? H(29) 0.4242 0.3326 0.5540 0.093 1.000 . Uiso c ? H(30) 0.3247 0.2523 0.5899 0.093 1.000 . Uiso c ? H(31) 0.2310 0.4504 0.5511 0.086 1.000 . Uiso c ? H(32) 0.1322 0.3693 0.5866 0.086 1.000 . Uiso c ? H(33) 0.1653 0.4689 0.6444 0.086 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) 0.0411(2) 0.0365(2) 0.0444(2) -0.0031(3) 0.0105(1) -0.0032(3) Cl(1) 0.071(1) 0.077(1) 0.0474(9) 0.013(1) 0.0006(9) 0.0030(9) P(1) 0.0451(7) 0.0480(8) 0.0580(8) 0.004(1) 0.0177(6) -0.002(1) P(2) 0.0390(8) 0.0377(8) 0.0533(9) 0.0012(7) 0.0027(7) -0.0032(7) P(3) 0.094(2) 0.067(1) 0.071(1) 0.013(1) 0.004(1) -0.008(1) F(1) 0.158(4) 0.097(4) 0.122(3) -0.005(5) 0.057(3) -0.009(4) F(2) 0.162(5) 0.152(6) 0.132(4) 0.029(5) -0.050(4) -0.027(4) F(3) 0.192(7) 0.130(5) 0.174(5) 0.095(5) 0.064(5) 0.024(5) F(4) 0.192(7) 0.112(5) 0.177(5) 0.004(5) 0.092(5) 0.027(4) F(5) 0.157(5) 0.31(1) 0.085(3) -0.090(6) 0.001(3) -0.045(4) F(6) 0.168(5) 0.089(3) 0.243(6) 0.002(6) 0.093(5) -0.046(7) N(1) 0.050(3) 0.057(3) 0.051(3) -0.010(3) 0.017(2) -0.008(3) C(1) 0.070(6) 0.056(5) 0.109(7) 0.020(5) 0.025(5) -0.002(5) C(2) 0.076(4) 0.087(5) 0.054(3) -0.011(5) 0.024(3) -0.011(5) C(3) 0.037(4) 0.047(5) 0.079(5) 0.008(3) 0.015(4) 0.005(4) C(4) 0.053(4) 0.078(5) 0.101(5) 0.004(4) 0.036(4) 0.003(4) C(5) 0.060(5) 0.075(6) 0.150(8) -0.006(4) 0.053(5) 0.012(6) C(6) 0.057(5) 0.084(7) 0.17(1) -0.023(5) 0.032(6) 0.010(7) C(7) 0.050(4) 0.068(5) 0.139(7) -0.015(4) 0.025(5) -0.015(5) C(8) 0.042(3) 0.047(4) 0.076(4) -0.005(3) 0.016(3) 0.002(3) C(9) 0.072(5) 0.068(5) 0.066(4) 0.016(4) -0.020(4) -0.001(4) C(10) 0.037(3) 0.039(3) 0.050(3) -0.002(3) 0.003(3) -0.001(3) C(11) 0.037(3) 0.047(3) 0.062(4) -0.001(3) 0.011(3) 0.002(3) C(12) 0.045(3) 0.059(4) 0.084(5) 0.003(3) 0.014(3) 0.012(4) C(13) 0.075(5) 0.043(4) 0.107(6) 0.001(4) 0.039(4) -0.016(4) C(14) 0.074(5) 0.056(4) 0.091(5) 0.000(4) 0.011(4) -0.024(4) C(15) 0.062(4) 0.054(4) 0.063(4) 0.009(3) 0.000(3) -0.012(3) C(16) 0.054(3) 0.045(3) 0.045(2) 0.002(5) 0.016(2) -0.002(5) C(17) 0.074(4) 0.042(3) 0.071(4) 0.001(3) 0.031(4) 0.003(3) C(18) 0.091(6) 0.059(5) 0.073(5) 0.017(4) 0.033(4) -0.004(4) C(19) 0.052(3) 0.061(5) 0.060(4) 0.016(3) 0.020(3) 0.023(3) C(20) 0.065(4) 0.088(6) 0.072(4) 0.033(4) 0.031(4) 0.026(4) C(21) 0.073(5) 0.118(8) 0.076(5) 0.012(6) 0.039(4) 0.038(5) C(22) 0.073(5) 0.098(7) 0.100(6) -0.013(5) 0.033(5) 0.037(5) C(23) 0.073(5) 0.079(5) 0.063(4) -0.016(4) 0.017(4) 0.021(4) C(24) 0.045(3) 0.063(4) 0.052(3) 0.012(3) 0.006(3) 0.019(3) C(25) 0.042(3) 0.043(3) 0.046(3) -0.002(3) 0.007(3) 0.008(3) C(26) 0.063(4) 0.049(4) 0.061(4) -0.014(3) 0.018(3) 0.002(3) C(27) 0.137(8) 0.053(5) 0.089(6) 0.007(5) 0.038(6) 0.003(4) C(28) 0.096(6) 0.056(5) 0.084(6) -0.023(5) 0.029(5) -0.025(4) C(29) 0.060(4) 0.090(5) 0.059(4) -0.019(4) 0.001(3) -0.001(4) #--------------------------------------------------------------------------- #-- _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) + 0.00010|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; The absolute structure was determined by comparing the agreement factors given below with those obtained from refinement of a model with all coordinates transformed by (-x,-y,-z) -- R = 0.0324, Rw = 0.0277 and S = 1.61. This indicates that the original model corresponds to the absolute configuration. Even more definitive is the fact that it is consistent with the known chirality of the synthetic precursors. ; _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3259 _refine_ls_number_parameters 369 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_all 0.0282 _refine_ls_wR_factor_ref 0.0260 _refine_ls_goodness_of_fit_all 1.418 _refine_ls_goodness_of_fit_ref 1.515 _refine_ls_shift/su_max 0.0070 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.32 _refine_diff_density_max 0.50 #--------------------------------------------------------------------------- #-- _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) P(1) 2.343(1) . . yes Pd(1) P(2) 2.226(2) . . yes Pd(1) N(1) 2.146(5) . . yes Pd(1) C(16) 2.061(4) . . yes Cl(1) C(11) 1.737(6) . . yes P(1) C(1) 1.811(9) . . yes P(1) C(2) 1.823(5) . . yes P(1) C(3) 1.816(8) . . yes P(2) C(8) 1.835(6) . . yes P(2) C(9) 1.813(6) . . yes P(2) C(10) 1.819(6) . . yes P(3) F(1) 1.590(6) . . yes P(3) F(2) 1.546(5) . . yes P(3) F(3) 1.547(5) . . yes P(3) F(4) 1.551(6) . . yes P(3) F(5) 1.499(5) . . yes P(3) F(6) 1.545(7) . . yes N(1) C(26) 1.498(7) . . yes N(1) C(28) 1.463(9) . . yes N(1) C(29) 1.485(7) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(1) H(3) 0.95 . . no C(2) H(4) 0.95 . . no C(2) H(5) 0.95 . . no C(2) H(6) 0.95 . . no C(3) C(4) 1.390(9) . . yes C(3) C(8) 1.385(9) . . yes C(4) C(5) 1.38(1) . . yes C(4) H(7) 0.95 . . no C(5) C(6) 1.37(1) . . yes C(5) H(8) 0.95 . . no C(6) C(7) 1.38(1) . . yes C(6) H(9) 0.95 . . no C(7) C(8) 1.388(9) . . yes C(7) H(10) 0.95 . . no C(9) H(11) 0.95 . . no C(9) H(12) 0.95 . . no C(9) H(13) 0.95 . . no C(10) C(11) 1.400(7) . . yes C(10) C(15) 1.399(7) . . yes C(11) C(12) 1.383(8) . . yes C(12) C(13) 1.367(8) . . yes C(12) H(14) 0.95 . . no C(13) C(14) 1.366(9) . . yes C(13) H(15) 0.95 . . no C(14) C(15) 1.363(9) . . yes C(14) H(16) 0.95 . . no C(15) H(17) 0.95 . . no C(16) C(17) 1.403(9) . . yes C(16) C(25) 1.38(1) . . yes C(17) C(18) 1.373(8) . . yes C(17) H(18) 0.95 . . no C(18) C(19) 1.404(9) . . yes C(18) H(19) 0.95 . . no C(19) C(20) 1.439(8) . . yes C(19) C(24) 1.384(8) . . yes C(20) C(21) 1.33(1) . . yes C(20) H(20) 0.95 . . no C(21) C(22) 1.37(1) . . yes C(21) H(21) 0.95 . . no C(22) C(23) 1.367(9) . . yes C(22) H(22) 0.95 . . no C(23) C(24) 1.426(9) . . yes C(23) H(23) 0.95 . . no C(24) C(25) 1.428(7) . . yes C(25) C(26) 1.500(8) . . yes C(26) C(27) 1.50(1) . . yes C(26) H(24) 0.95 . . no C(27) H(25) 0.95 . . no C(27) H(26) 0.95 . . no C(27) H(27) 0.95 . . no C(28) H(28) 0.95 . . no C(28) H(29) 0.95 . . no C(28) H(30) 0.95 . . no C(29) H(31) 0.95 . . no C(29) H(32) 0.95 . . no C(29) H(33) 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 P(1) Pd(1) P(2) 85.36(7) . . . yes P(1) Pd(1) N(1) 99.5(1) . . . yes P(1) Pd(1) C(16) 177.5(2) . . . yes P(2) Pd(1) N(1) 175.1(1) . . . yes P(2) Pd(1) C(16) 94.4(2) . . . yes N(1) Pd(1) C(16) 80.8(3) . . . yes Pd(1) P(1) C(1) 117.9(3) . . . yes Pd(1) P(1) C(2) 117.5(2) . . . yes Pd(1) P(1) C(3) 107.9(3) . . . yes C(1) P(1) C(2) 105.3(4) . . . yes C(1) P(1) C(3) 103.6(3) . . . yes C(2) P(1) C(3) 102.8(4) . . . yes Pd(1) P(2) C(8) 110.5(2) . . . yes Pd(1) P(2) C(9) 112.8(2) . . . yes Pd(1) P(2) C(10) 119.3(2) . . . yes C(8) P(2) C(9) 104.0(3) . . . yes C(8) P(2) C(10) 103.2(3) . . . yes C(9) P(2) C(10) 105.5(3) . . . yes F(1) P(3) F(2) 88.2(3) . . . yes F(1) P(3) F(3) 90.7(3) . . . yes F(1) P(3) F(4) 179.2(4) . . . yes F(1) P(3) F(5) 88.9(3) . . . yes F(1) P(3) F(6) 91.6(4) . . . yes F(2) P(3) F(3) 88.2(3) . . . yes F(2) P(3) F(4) 92.5(4) . . . yes F(2) P(3) F(5) 176.6(4) . . . yes F(2) P(3) F(6) 87.4(3) . . . yes F(3) P(3) F(4) 89.6(4) . . . yes F(3) P(3) F(5) 93.7(4) . . . yes F(3) P(3) F(6) 175.0(4) . . . yes F(4) P(3) F(5) 90.3(3) . . . yes F(4) P(3) F(6) 88.1(3) . . . yes F(5) P(3) F(6) 90.8(4) . . . yes Pd(1) N(1) C(26) 104.7(3) . . . yes Pd(1) N(1) C(28) 118.5(4) . . . yes Pd(1) N(1) C(29) 105.4(4) . . . yes C(26) N(1) C(28) 111.3(6) . . . yes C(26) N(1) C(29) 110.0(5) . . . yes C(28) N(1) C(29) 106.6(5) . . . yes P(1) C(1) H(1) 109.5 . . . no P(1) C(1) H(2) 109.5 . . . no P(1) C(1) H(3) 109.5 . . . no H(1) C(1) H(2) 109.5 . . . no H(1) C(1) H(3) 109.5 . . . no H(2) C(1) H(3) 109.5 . . . no P(1) C(2) H(4) 109.5 . . . no P(1) C(2) H(5) 109.5 . . . no P(1) C(2) H(6) 109.5 . . . no H(4) C(2) H(5) 109.5 . . . no H(4) C(2) H(6) 109.5 . . . no H(5) C(2) H(6) 109.5 . . . no P(1) C(3) C(4) 122.9(7) . . . yes P(1) C(3) C(8) 118.2(6) . . . yes C(4) C(3) C(8) 119.0(7) . . . yes C(3) C(4) C(5) 119.7(8) . . . yes C(3) C(4) H(7) 120.1 . . . no C(5) C(4) H(7) 120.1 . . . no C(4) C(5) C(6) 121.5(7) . . . yes C(4) C(5) H(8) 119.3 . . . no C(6) C(5) H(8) 119.3 . . . no C(5) C(6) C(7) 119.4(8) . . . yes C(5) C(6) H(9) 120.3 . . . no C(7) C(6) H(9) 120.3 . . . no C(6) C(7) C(8) 119.8(8) . . . yes C(6) C(7) H(10) 120.1 . . . no C(8) C(7) H(10) 120.1 . . . no P(2) C(8) C(3) 117.8(5) . . . yes P(2) C(8) C(7) 121.6(5) . . . yes C(3) C(8) C(7) 120.6(6) . . . yes P(2) C(9) H(11) 109.5 . . . no P(2) C(9) H(12) 109.5 . . . no P(2) C(9) H(13) 109.5 . . . no H(11) C(9) H(12) 109.5 . . . no H(11) C(9) H(13) 109.5 . . . no H(12) C(9) H(13) 109.5 . . . no P(2) C(10) C(11) 121.0(4) . . . yes P(2) C(10) C(15) 122.1(4) . . . yes C(11) C(10) C(15) 116.9(5) . . . yes Cl(1) C(11) C(10) 119.7(5) . . . yes Cl(1) C(11) C(12) 119.0(5) . . . yes C(10) C(11) C(12) 121.3(6) . . . yes C(11) C(12) C(13) 119.5(6) . . . yes C(11) C(12) H(14) 120.3 . . . no C(13) C(12) H(14) 120.3 . . . no C(12) C(13) C(14) 120.5(6) . . . yes C(12) C(13) H(15) 119.8 . . . no C(14) C(13) H(15) 119.8 . . . no C(13) C(14) C(15) 120.6(6) . . . yes C(13) C(14) H(16) 119.7 . . . no C(15) C(14) H(16) 119.7 . . . no C(10) C(15) C(14) 121.2(6) . . . yes C(10) C(15) H(17) 119.4 . . . no C(14) C(15) H(17) 119.4 . . . no Pd(1) C(16) C(17) 129.5(6) . . . yes Pd(1) C(16) C(25) 112.5(5) . . . yes C(17) C(16) C(25) 117.9(5) . . . yes C(16) C(17) C(18) 121.8(6) . . . yes C(16) C(17) H(18) 119.1 . . . no C(18) C(17) H(18) 119.1 . . . no C(17) C(18) C(19) 120.4(7) . . . yes C(17) C(18) H(19) 119.8 . . . no C(19) C(18) H(19) 119.8 . . . no C(18) C(19) C(20) 121.5(6) . . . yes C(18) C(19) C(24) 119.1(6) . . . yes C(20) C(19) C(24) 119.4(6) . . . yes C(19) C(20) C(21) 121.1(7) . . . yes C(19) C(20) H(20) 119.4 . . . no C(21) C(20) H(20) 119.4 . . . no C(20) C(21) C(22) 119.5(6) . . . yes C(20) C(21) H(21) 120.2 . . . no C(22) C(21) H(21) 120.2 . . . no C(21) C(22) C(23) 122.1(8) . . . yes C(21) C(22) H(22) 118.9 . . . no C(23) C(22) H(22) 118.9 . . . no C(22) C(23) C(24) 119.9(7) . . . yes C(22) C(23) H(23) 120.0 . . . no C(24) C(23) H(23) 120.0 . . . no C(19) C(24) C(23) 117.7(6) . . . yes C(19) C(24) C(25) 119.7(6) . . . yes C(23) C(24) C(25) 122.6(6) . . . yes C(16) C(25) C(24) 120.8(6) . . . yes C(16) C(25) C(26) 116.9(5) . . . yes C(24) C(25) C(26) 122.2(6) . . . yes N(1) C(26) C(25) 108.7(5) . . . yes N(1) C(26) C(27) 112.8(6) . . . yes N(1) C(26) H(24) 108.1 . . . no C(25) C(26) C(27) 110.8(5) . . . yes C(25) C(26) H(24) 108.1 . . . no C(27) C(26) H(24) 108.1 . . . no C(26) C(27) H(25) 109.5 . . . no C(26) C(27) H(26) 109.5 . . . no C(26) C(27) H(27) 109.5 . . . no H(25) C(27) H(26) 109.5 . . . no H(25) C(27) H(27) 109.5 . . . no H(26) C(27) H(27) 109.5 . . . no N(1) C(28) H(28) 109.5 . . . no N(1) C(28) H(29) 109.5 . . . no N(1) C(28) H(30) 109.5 . . . no H(28) C(28) H(29) 109.5 . . . no H(28) C(28) H(30) 109.5 . . . no H(29) C(28) H(30) 109.5 . . . no N(1) C(29) H(31) 109.5 . . . no N(1) C(29) H(32) 109.5 . . . no N(1) C(29) H(33) 109.5 . . . no H(31) C(29) H(32) 109.5 . . . no H(31) C(29) H(33) 109.5 . . . no H(32) C(29) H(33) 109.5 . . . no #--------------------------------------------------------------------------- #-- 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 Cl(1) F(2) 3.139(6) . . no F(1) C(4) 3.374(8) . 1_455 no F(1) C(29) 3.441(8) . . no F(1) C(6) 3.45(1) . 2_646 no F(2) C(2) 3.481(9) . . no F(2) C(29) 3.508(9) . . no F(3) C(26) 3.429(9) . 2_556 no F(3) C(5) 3.57(1) . 1_455 no F(3) C(1) 3.58(1) . 2_656 no F(3) C(4) 3.591(9) . 1_455 no F(4) C(23) 3.44(1) . 2_556 no F(4) C(1) 3.57(1) . 2_656 no F(5) C(20) 3.455(8) . 1_554 no F(5) C(13) 3.461(9) . 2_546 no F(6) C(6) 3.30(1) . 2_646 no F(6) C(7) 3.40(1) . 2_646 no C(9) C(20) 3.503(9) . 1_655 no C(14) C(19) 3.598(9) . 2_657 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) P(1) C(3) C(4) . . . . -177.8(6) no Pd(1) P(1) C(3) C(8) . . . . 1.3(6) no Pd(1) P(2) C(8) C(3) . . . . -5.9(6) no Pd(1) P(2) C(8) C(7) . . . . 174.5(5) no Pd(1) P(2) C(10) C(11) . . . . -48.2(5) no Pd(1) P(2) C(10) C(15) . . . . 130.7(5) no Pd(1) N(1) C(26) C(25) . . . . 42.4(5) no Pd(1) N(1) C(26) C(27) . . . . -80.8(6) no Pd(1) C(16) C(17) C(18) . . . . -180.0(5) no Pd(1) C(16) C(25) C(24) . . . . -176.7(4) no Pd(1) C(16) C(25) C(26) . . . . 6.4(7) no Cl(1) C(11) C(10) P(2) . . . . -2.3(7) no Cl(1) C(11) C(10) C(15) . . . . 178.7(5) no Cl(1) C(11) C(12) C(13) . . . . -179.8(5) no P(1) Pd(1) P(2) C(8) . . . . 4.9(2) no P(1) Pd(1) P(2) C(9) . . . . -111.0(3) no P(1) Pd(1) P(2) C(10) . . . . 124.3(2) no P(1) Pd(1) N(1) C(26) . . . . 145.9(4) no P(1) Pd(1) N(1) C(28) . . . . 21.2(5) no P(1) Pd(1) N(1) C(29) . . . . -98.0(3) no P(1) Pd(1) C(16) C(17) . . . . 101(6) no P(1) Pd(1) C(16) C(25) . . . . -81(6) no P(1) C(3) C(4) C(5) . . . . 178.0(6) no P(1) C(3) C(8) P(2) . . . . 2.8(8) no P(1) C(3) C(8) C(7) . . . . -177.6(6) no P(2) Pd(1) P(1) C(1) . . . . 113.1(3) no P(2) Pd(1) P(1) C(2) . . . . -119.2(4) no P(2) Pd(1) P(1) C(3) . . . . -3.7(3) no P(2) Pd(1) N(1) C(26) . . . . -45(2) no P(2) Pd(1) N(1) C(28) . . . . -169(1) no P(2) Pd(1) N(1) C(29) . . . . 71(2) no P(2) Pd(1) C(16) C(17) . . . . 16.3(6) no P(2) Pd(1) C(16) C(25) . . . . -166.4(4) no P(2) C(8) C(3) C(4) . . . . -178.0(5) no P(2) C(8) C(7) C(6) . . . . 178.6(6) no P(2) C(10) C(11) C(12) . . . . 178.2(4) no P(2) C(10) C(15) C(14) . . . . -178.5(5) no N(1) Pd(1) P(1) C(1) . . . . -67.8(4) no N(1) Pd(1) P(1) C(2) . . . . 59.9(4) no N(1) Pd(1) P(1) C(3) . . . . 175.4(3) no N(1) Pd(1) P(2) C(8) . . . . -165(2) no N(1) Pd(1) P(2) C(9) . . . . 79(2) no N(1) Pd(1) P(2) C(10) . . . . -45(2) no N(1) Pd(1) C(16) C(17) . . . . -162.6(6) no N(1) Pd(1) C(16) C(25) . . . . 14.7(4) no N(1) C(26) C(25) C(16) . . . . -34.4(7) no N(1) C(26) C(25) C(24) . . . . 148.8(5) no C(1) P(1) Pd(1) C(16) . . . . 28(6) no C(1) P(1) C(3) C(4) . . . . 56.5(7) no C(1) P(1) C(3) C(8) . . . . -124.4(7) no C(2) P(1) Pd(1) C(16) . . . . 155(6) no C(2) P(1) C(3) C(4) . . . . -52.9(7) no C(2) P(1) C(3) C(8) . . . . 126.2(6) no C(3) P(1) Pd(1) C(16) . . . . -89(6) no C(3) C(4) C(5) C(6) . . . . 0(1) no C(3) C(8) P(2) C(9) . . . . 115.4(6) no C(3) C(8) P(2) C(10) . . . . -134.6(5) no C(3) C(8) C(7) C(6) . . . . -1(1) no C(4) C(3) C(8) C(7) . . . . 2(1) no C(4) C(5) C(6) C(7) . . . . 1(2) no C(5) C(4) C(3) C(8) . . . . -1(1) no C(5) C(6) C(7) C(8) . . . . 0(1) no C(7) C(8) P(2) C(9) . . . . -64.2(6) no C(7) C(8) P(2) C(10) . . . . 45.8(6) no C(8) P(2) Pd(1) C(16) . . . . -177.5(3) no C(8) P(2) C(10) C(11) . . . . 74.8(5) no C(8) P(2) C(10) C(15) . . . . -106.3(6) no C(9) P(2) Pd(1) C(16) . . . . 66.6(3) no C(9) P(2) C(10) C(11) . . . . -176.4(5) no C(9) P(2) C(10) C(15) . . . . 2.6(6) no C(10) P(2) Pd(1) C(16) . . . . -58.1(3) no C(10) C(11) C(12) C(13) . . . . -0.3(9) no C(10) C(15) C(14) C(13) . . . . 1(1) no C(11) C(10) C(15) C(14) . . . . 0(1) no C(11) C(12) C(13) C(14) . . . . 2(1) no C(12) C(11) C(10) C(15) . . . . -0.7(9) no C(12) C(13) C(14) C(15) . . . . -2(1) no C(16) Pd(1) N(1) C(26) . . . . -31.6(4) no C(16) Pd(1) N(1) C(28) . . . . -156.4(6) no C(16) Pd(1) N(1) C(29) . . . . 84.5(4) no C(16) C(17) C(18) C(19) . . . . -4(1) no C(16) C(25) C(24) C(19) . . . . -3.8(8) no C(16) C(25) C(24) C(23) . . . . 176.2(6) no C(16) C(25) C(26) C(27) . . . . 90.1(7) no C(17) C(16) C(25) C(24) . . . . 1.0(9) no C(17) C(16) C(25) C(26) . . . . -175.9(5) no C(17) C(18) C(19) C(20) . . . . -179.9(6) no C(17) C(18) C(19) C(24) . . . . 1(1) no C(18) C(17) C(16) C(25) . . . . 3(1) no C(18) C(19) C(20) C(21) . . . . 177.1(7) no C(18) C(19) C(24) C(23) . . . . -177.3(6) no C(18) C(19) C(24) C(25) . . . . 2.7(9) no C(19) C(20) C(21) C(22) . . . . 1(1) no C(19) C(24) C(23) C(22) . . . . -1(1) no C(19) C(24) C(25) C(26) . . . . 173.0(5) no C(20) C(19) C(24) C(23) . . . . 3.7(9) no C(20) C(19) C(24) C(25) . . . . -176.3(5) no C(20) C(21) C(22) C(23) . . . . 2(1) no C(21) C(20) C(19) C(24) . . . . -4(1) no C(21) C(22) C(23) C(24) . . . . -3(1) no C(22) C(23) C(24) C(25) . . . . 179.4(6) no C(23) C(24) C(25) C(26) . . . . -7.1(9) no C(24) C(25) C(26) C(27) . . . . -86.8(7) no C(25) C(26) N(1) C(28) . . . . 171.6(5) no C(25) C(26) N(1) C(29) . . . . -70.4(6) no C(27) C(26) N(1) C(28) . . . . 48.4(7) no C(27) C(26) N(1) C(29) . . . . 166.3(6) no #--------------------------------------------------------------------------- #-- #===END