# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 # CCDC Number: 440/211 data_mf369/FN98-74 #----------------------------------------------------------------------------- _audit_creation_date '1998-03-26' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #----------------------------------------------------------------------------- _publ_requested_journal ' NEW J. CHEM.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' P. BRAUNSTEIN' _publ_contact_author_address ; Universite Louis Pasteur Laboratoire de Chimie de Coordination UMR 7513 4, rue Blaise Pascal 67000 Starsbourg, cedex FRANCE ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 0033-388416030 ' _publ_contact_author_fax ' 0033-388416030 ' _publ_contact_author_email ' braunstein@chimie.u-strasbg.fr ' loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_title ; A new class of anionic phosphino-oxazoline ligands in palladium and ruthenium complexes; catalytic properties for the transfer hydrogenation of acetophenone ; _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 ; ENTER OTHER 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. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; _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 ; 'DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #----------------------------------------------------------------------------- _cell_length_a 17.293(2) _cell_length_b 9.7528(13) _cell_length_c 17.6784(6) _cell_angle_alpha 90 _cell_angle_beta 115.2840(9) _cell_angle_gamma 90 _cell_volume 2695.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 180.2 _cell_measurement_reflns_used 14366 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.0 #----------------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #----------------------------------------------------------------------------- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'chip' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 642.95 _chemical_formula_analytical ? _chemical_formula_sum 'C32 H30 N2 O2 P2 Pd ' _chemical_formula_moiety 'C32 H30 N2 O2 P2 Pd ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1312.00 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.837 _exptl_special_details ; ? ; #----------------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 180.2 _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_type 'Quantum CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method 'area detector' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 24477 _reflns_number_total 6934 _reflns_number_gt 6934 _reflns_threshold_expression I>0.00\s(I) _diffrn_reflns_av_R_equivalents 0.05719 _diffrn_reflns_av_sigmaI/netI 0.080 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 30.04 _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 0 128 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 120 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 8 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 8 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 8 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pd 0 4 -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) 0.43829(2) 0.58092(3) 0.18491(2) 0.01345(6) 1.000 . Uani d ? P(1) 0.35083(6) 0.70009(9) 0.06828(6) 0.0150(3) 1.000 . Uani d ? P(2) 0.37896(6) 0.36597(9) 0.15759(6) 0.0151(3) 1.000 . Uani d ? O(1) 0.5190(2) 0.9842(2) 0.17982(15) 0.0233(7) 1.000 . Uani d ? O(2) 0.5603(2) 0.3011(2) 0.38041(15) 0.0216(7) 1.000 . Uani d ? N(1) 0.5016(2) 0.7676(3) 0.2161(2) 0.0149(8) 1.000 . Uani d ? N(2) 0.5154(2) 0.4885(3) 0.2977(2) 0.0149(8) 1.000 . Uani d ? C(1) 0.3897(2) 0.8661(4) 0.0934(2) 0.0203(10) 1.000 . Uani d ? C(2) 0.4674(2) 0.8696(3) 0.1616(2) 0.0177(10) 1.000 . Uani d ? C(3) 0.5908(3) 0.8004(4) 0.2673(2) 0.0249(11) 1.000 . Uani d ? C(4) 0.5909(3) 0.9564(4) 0.2589(2) 0.0258(11) 1.000 . Uani d ? C(5) 0.3505(2) 0.6583(3) -0.0326(2) 0.0159(10) 1.000 . Uani d ? C(6) 0.3924(2) 0.5461(3) -0.0436(2) 0.0207(10) 1.000 . Uani d ? C(7) 0.3947(3) 0.5205(4) -0.1210(3) 0.0273(12) 1.000 . Uani d ? C(8) 0.3547(3) 0.6088(4) -0.1874(2) 0.0283(12) 1.000 . Uani d ? C(9) 0.3135(3) 0.7248(4) -0.1766(2) 0.0288(12) 1.000 . Uani d ? C(10) 0.3105(3) 0.7489(4) -0.0997(2) 0.0243(11) 1.000 . Uani d ? C(11) 0.2379(2) 0.6991(4) 0.0464(2) 0.0164(10) 1.000 . Uani d ? C(12) 0.1800(2) 0.6092(3) -0.0110(2) 0.0199(11) 1.000 . Uani d ? C(13) 0.0962(2) 0.6019(4) -0.0207(2) 0.0229(11) 1.000 . Uani d ? C(14) 0.0694(3) 0.6874(4) 0.0276(3) 0.0303(12) 1.000 . Uani d ? C(15) 0.1258(3) 0.7764(4) 0.0840(2) 0.0266(12) 1.000 . Uani d ? C(16) 0.2103(3) 0.7843(4) 0.0937(2) 0.0222(11) 1.000 . Uani d ? C(17) 0.4531(2) 0.2714(3) 0.2412(2) 0.0182(10) 1.000 . Uani d ? C(18) 0.5072(2) 0.3526(4) 0.3026(2) 0.0165(10) 1.000 . Uani d ? C(19) 0.5800(3) 0.5383(4) 0.3765(2) 0.0251(11) 1.000 . Uani d ? C(20) 0.5907(2) 0.4200(4) 0.4358(2) 0.0254(10) 1.000 . Uani d ? C(21) 0.3635(2) 0.2815(3) 0.0604(2) 0.0166(10) 1.000 . Uani d ? C(22) 0.4341(2) 0.2240(3) 0.0528(2) 0.0195(10) 1.000 . Uani d ? C(23) 0.4245(3) 0.1632(4) -0.0217(3) 0.0276(12) 1.000 . Uani d ? C(24) 0.3451(3) 0.1579(4) -0.0886(3) 0.0325(13) 1.000 . Uani d ? C(25) 0.2739(3) 0.2162(4) -0.0822(2) 0.0307(12) 1.000 . Uani d ? C(26) 0.2845(3) 0.2766(4) -0.0072(2) 0.0207(11) 1.000 . Uani d ? C(27) 0.2753(2) 0.3460(4) 0.1611(2) 0.0167(10) 1.000 . Uani d ? C(28) 0.2376(3) 0.4566(4) 0.1828(2) 0.0221(11) 1.000 . Uani d ? C(29) 0.1625(3) 0.4381(4) 0.1916(2) 0.0311(13) 1.000 . Uani d ? C(30) 0.1234(3) 0.3105(5) 0.1783(2) 0.0317(13) 1.000 . Uani d ? C(31) 0.1612(3) 0.2004(4) 0.1562(2) 0.0296(12) 1.000 . Uani d ? C(32) 0.2360(3) 0.2174(4) 0.1480(2) 0.0214(11) 1.000 . Uani d ? H(1) 0.3595 0.9477 0.0625 0.024 1.000 . Uiso c ? H(2) 0.6083 0.7726 0.3256 0.030 1.000 . Uiso c ? H(3) 0.6283 0.7569 0.2456 0.030 1.000 . Uiso c ? H(4) 0.6444 0.9880 0.2582 0.031 1.000 . Uiso c ? H(5) 0.5833 1.0010 0.3050 0.031 1.000 . Uiso c ? H(6) 0.4211 0.4827 0.0031 0.025 1.000 . Uiso c ? H(7) 0.4248 0.4397 -0.1277 0.033 1.000 . Uiso c ? H(8) 0.3552 0.5900 -0.2417 0.034 1.000 . Uiso c ? H(9) 0.2866 0.7897 -0.2228 0.035 1.000 . Uiso c ? H(10) 0.2803 0.8295 -0.0929 0.029 1.000 . Uiso c ? H(11) 0.1987 0.5504 -0.0451 0.024 1.000 . Uiso c ? H(12) 0.0559 0.5376 -0.0609 0.027 1.000 . Uiso c ? H(13) 0.0102 0.6831 0.0209 0.036 1.000 . Uiso c ? H(14) 0.1069 0.8351 0.1179 0.032 1.000 . Uiso c ? H(15) 0.2501 0.8495 0.1335 0.027 1.000 . Uiso c ? H(16) 0.4551 0.1710 0.2432 0.022 1.000 . Uiso c ? H(17) 0.6337 0.5576 0.3724 0.030 1.000 . Uiso c ? H(18) 0.5606 0.6212 0.3946 0.030 1.000 . Uiso c ? H(19) 0.5559 0.4343 0.4668 0.030 1.000 . Uiso c ? H(20) 0.6508 0.4088 0.4754 0.030 1.000 . Uiso c ? H(21) 0.4906 0.2266 0.1004 0.023 1.000 . Uiso c ? H(22) 0.4742 0.1241 -0.0268 0.033 1.000 . Uiso c ? H(23) 0.3383 0.1135 -0.1408 0.039 1.000 . Uiso c ? H(24) 0.2175 0.2142 -0.1299 0.037 1.000 . Uiso c ? H(25) 0.2348 0.3164 -0.0023 0.025 1.000 . Uiso c ? H(26) 0.2643 0.5475 0.1917 0.027 1.000 . Uiso c ? H(27) 0.1366 0.5159 0.2075 0.037 1.000 . Uiso c ? H(28) 0.0700 0.2978 0.1842 0.038 1.000 . Uiso c ? H(29) 0.1340 0.1099 0.1466 0.036 1.000 . Uiso c ? H(30) 0.2620 0.1391 0.1328 0.026 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) 0.01226(14) 0.01781(12) 0.01010(12) -0.00045(14) 0.00460(11) 0.00011(13) P(1) 0.0130(6) 0.0200(5) 0.0116(5) 0.0005(4) 0.0049(5) 0.0019(4) P(2) 0.0149(6) 0.0179(4) 0.0124(5) -0.0010(4) 0.0057(5) -0.0008(4) O(1) 0.025(2) 0.0202(13) 0.0182(15) -0.0058(12) 0.0023(13) -0.0002(11) O(2) 0.024(2) 0.0221(13) 0.0128(14) 0.0019(12) 0.0028(13) 0.0052(11) N(1) 0.013(2) 0.0187(15) 0.0098(15) -0.0046(13) 0.0021(14) -0.0023(12) N(2) 0.015(2) 0.0137(14) 0.011(2) -0.0018(13) 0.0006(15) 0.0025(12) C(1) 0.020(2) 0.022(2) 0.020(2) 0.001(2) 0.009(2) 0.004(2) C(2) 0.019(2) 0.018(2) 0.018(2) -0.002(2) 0.011(2) -0.004(2) C(3) 0.018(2) 0.033(2) 0.019(2) -0.007(2) 0.004(2) 0.001(2) C(4) 0.023(3) 0.033(2) 0.017(2) -0.005(2) 0.005(2) -0.002(2) C(5) 0.012(2) 0.024(2) 0.016(2) -0.0001(15) 0.009(2) 0.0033(15) C(6) 0.022(2) 0.024(2) 0.018(2) -0.002(2) 0.010(2) 0.004(2) C(7) 0.033(3) 0.031(2) 0.030(3) -0.001(2) 0.024(2) -0.005(2) C(8) 0.022(2) 0.052(3) 0.014(2) -0.007(2) 0.011(2) -0.004(2) C(9) 0.022(3) 0.049(3) 0.012(2) 0.001(2) 0.004(2) 0.011(2) C(10) 0.019(2) 0.036(2) 0.018(2) 0.007(2) 0.009(2) 0.005(2) C(11) 0.014(2) 0.026(2) 0.012(2) 0.000(2) 0.007(2) 0.004(2) C(12) 0.022(2) 0.024(2) 0.018(2) 0.002(2) 0.012(2) 0.003(2) C(13) 0.015(2) 0.029(2) 0.020(2) -0.006(2) 0.004(2) 0.002(2) C(14) 0.017(2) 0.046(3) 0.033(3) 0.004(2) 0.015(2) 0.015(2) C(15) 0.026(3) 0.036(2) 0.025(2) 0.010(2) 0.017(2) 0.005(2) C(16) 0.018(2) 0.032(2) 0.018(2) 0.002(2) 0.008(2) 0.002(2) C(17) 0.016(2) 0.013(2) 0.023(2) -0.0002(15) 0.007(2) 0.001(2) C(18) 0.014(2) 0.024(2) 0.013(2) 0.004(2) 0.008(2) 0.005(2) C(19) 0.028(3) 0.026(2) 0.012(2) -0.001(2) 0.000(2) 0.001(2) C(20) 0.024(2) 0.032(2) 0.014(2) 0.001(2) 0.002(2) 0.000(2) C(21) 0.022(2) 0.015(2) 0.017(2) -0.0022(15) 0.013(2) 0.0007(15) C(22) 0.022(2) 0.016(2) 0.024(2) -0.002(2) 0.014(2) 0.004(2) C(23) 0.040(3) 0.027(2) 0.030(3) 0.002(2) 0.029(2) 0.003(2) C(24) 0.052(3) 0.031(2) 0.025(3) -0.008(2) 0.026(3) -0.006(2) C(25) 0.033(3) 0.041(2) 0.014(2) -0.011(2) 0.007(2) -0.002(2) C(26) 0.025(2) 0.024(2) 0.017(2) 0.000(2) 0.013(2) -0.004(2) C(27) 0.018(2) 0.027(2) 0.007(2) 0.000(2) 0.006(2) 0.0031(15) C(28) 0.024(2) 0.030(2) 0.016(2) 0.001(2) 0.012(2) 0.001(2) C(29) 0.025(3) 0.051(3) 0.023(2) 0.011(2) 0.016(2) 0.008(2) C(30) 0.018(3) 0.060(3) 0.021(2) 0.000(2) 0.012(2) 0.009(2) C(31) 0.024(3) 0.041(2) 0.018(2) -0.014(2) 0.004(2) 0.003(2) C(32) 0.024(2) 0.026(2) 0.017(2) -0.007(2) 0.011(2) -0.001(2) #----------------------------------------------------------------------------- _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _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 6934 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0773 _refine_ls_wR_factor_all 0.0675 _refine_ls_wR_factor_ref 0.0675 _refine_ls_goodness_of_fit_all 1.365 _refine_ls_goodness_of_fit_ref 1.365 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0010 _refine_diff_density_min -1.36 _refine_diff_density_max 1.74 #----------------------------------------------------------------------------- _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) 2.2860(10) . . yes Pd(1) P(2) 2.2929(9) . . yes Pd(1) N(1) 2.074(3) . . yes Pd(1) N(2) 2.073(3) . . yes P(1) C(1) 1.737(4) . . yes P(1) C(5) 1.827(3) . . yes P(1) C(11) 1.822(4) . . yes P(2) C(17) 1.750(4) . . yes P(2) C(21) 1.819(3) . . yes P(2) C(27) 1.831(4) . . yes O(1) C(2) 1.380(4) . . yes O(1) C(4) 1.446(4) . . yes O(2) C(18) 1.382(4) . . yes O(2) C(20) 1.464(4) . . yes N(1) C(2) 1.335(4) . . yes N(1) C(3) 1.451(5) . . yes N(2) C(18) 1.339(4) . . yes N(2) C(19) 1.448(4) . . yes C(1) C(2) 1.370(5) . . yes C(1) H(1) 0.98 . . no C(3) C(4) 1.529(5) . . yes C(3) H(2) 0.98 . . no C(3) H(3) 0.98 . . no C(4) H(4) 0.98 . . no C(4) H(5) 0.98 . . no C(5) C(6) 1.371(4) . . yes C(5) C(10) 1.402(5) . . yes C(6) C(7) 1.408(5) . . yes C(6) H(6) 0.98 . . no C(7) C(8) 1.380(5) . . yes C(7) H(7) 0.98 . . no C(8) C(9) 1.392(5) . . yes C(8) H(8) 0.98 . . no C(9) C(10) 1.402(5) . . yes C(9) H(9) 0.98 . . no C(10) H(10) 0.98 . . no C(11) C(12) 1.390(5) . . yes C(11) C(16) 1.400(5) . . yes C(12) C(13) 1.388(5) . . yes C(12) H(11) 0.98 . . no C(13) C(14) 1.406(5) . . yes C(13) H(12) 0.98 . . no C(14) C(15) 1.367(6) . . yes C(14) H(13) 0.98 . . no C(15) C(16) 1.398(5) . . yes C(15) H(14) 0.98 . . no C(16) H(15) 0.98 . . no C(17) C(18) 1.347(5) . . yes C(17) H(16) 0.98 . . no C(19) C(20) 1.516(5) . . yes C(19) H(17) 0.98 . . no C(19) H(18) 0.98 . . no C(20) H(19) 0.98 . . no C(20) H(20) 0.98 . . no C(21) C(22) 1.401(5) . . yes C(21) C(26) 1.380(5) . . yes C(22) C(23) 1.389(5) . . yes C(22) H(21) 0.98 . . no C(23) C(24) 1.378(6) . . yes C(23) H(22) 0.98 . . no C(24) C(25) 1.405(6) . . yes C(24) H(23) 0.98 . . no C(25) C(26) 1.389(5) . . yes C(25) H(24) 0.98 . . no C(26) H(25) 0.98 . . no C(27) C(28) 1.396(5) . . yes C(27) C(32) 1.398(4) . . yes C(28) C(29) 1.385(5) . . yes C(28) H(26) 0.98 . . no C(29) C(30) 1.388(5) . . yes C(29) H(27) 0.98 . . no C(30) C(31) 1.396(5) . . yes C(30) H(28) 0.98 . . no C(31) C(32) 1.372(5) . . yes C(31) H(29) 0.98 . . no C(32) H(30) 0.98 . . 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) 102.16(4) . . . yes P(1) Pd(1) N(1) 82.20(8) . . . yes P(1) Pd(1) N(2) 174.17(8) . . . yes P(2) Pd(1) N(1) 175.18(9) . . . yes P(2) Pd(1) N(2) 81.42(8) . . . yes N(1) Pd(1) N(2) 94.40(11) . . . yes Pd(1) P(1) C(1) 102.03(13) . . . yes Pd(1) P(1) C(5) 119.46(12) . . . yes Pd(1) P(1) C(11) 115.15(11) . . . yes C(1) P(1) C(5) 107.3(2) . . . yes C(1) P(1) C(11) 108.8(2) . . . yes C(5) P(1) C(11) 103.6(2) . . . yes Pd(1) P(2) C(17) 101.74(12) . . . yes Pd(1) P(2) C(21) 119.00(11) . . . yes Pd(1) P(2) C(27) 116.52(12) . . . yes C(17) P(2) C(21) 108.6(2) . . . yes C(17) P(2) C(27) 106.9(2) . . . yes C(21) P(2) C(27) 103.5(2) . . . yes C(2) O(1) C(4) 106.1(3) . . . yes C(18) O(2) C(20) 105.9(3) . . . yes Pd(1) N(1) C(2) 116.2(2) . . . yes Pd(1) N(1) C(3) 131.2(2) . . . yes C(2) N(1) C(3) 108.2(3) . . . yes Pd(1) N(2) C(18) 116.8(3) . . . yes Pd(1) N(2) C(19) 134.0(2) . . . yes C(18) N(2) C(19) 109.2(3) . . . yes P(1) C(1) C(2) 112.1(3) . . . yes P(1) C(1) H(1) 124.0 . . . no C(2) C(1) H(1) 124.0 . . . no O(1) C(2) N(1) 113.1(3) . . . yes O(1) C(2) C(1) 121.3(3) . . . yes N(1) C(2) C(1) 125.6(3) . . . yes N(1) C(3) C(4) 101.8(3) . . . yes N(1) C(3) H(2) 111.4 . . . no N(1) C(3) H(3) 111.4 . . . no C(4) C(3) H(2) 111.4 . . . no C(4) C(3) H(3) 111.4 . . . no H(2) C(3) H(3) 109.5 . . . no O(1) C(4) C(3) 104.1(3) . . . yes O(1) C(4) H(4) 110.8 . . . no O(1) C(4) H(5) 110.8 . . . no C(3) C(4) H(4) 110.8 . . . no C(3) C(4) H(5) 110.8 . . . no H(4) C(4) H(5) 109.5 . . . no P(1) C(5) C(6) 122.3(3) . . . yes P(1) C(5) C(10) 118.7(3) . . . yes C(6) C(5) C(10) 118.8(3) . . . yes C(5) C(6) C(7) 121.0(3) . . . yes C(5) C(6) H(6) 119.5 . . . no C(7) C(6) H(6) 119.5 . . . no C(6) C(7) C(8) 120.3(3) . . . yes C(6) C(7) H(7) 119.9 . . . no C(8) C(7) H(7) 119.9 . . . no C(7) C(8) C(9) 119.3(3) . . . yes C(7) C(8) H(8) 120.3 . . . no C(9) C(8) H(8) 120.3 . . . no C(8) C(9) C(10) 120.1(4) . . . yes C(8) C(9) H(9) 119.9 . . . no C(10) C(9) H(9) 119.9 . . . no C(5) C(10) C(9) 120.4(3) . . . yes C(5) C(10) H(10) 119.8 . . . no C(9) C(10) H(10) 119.8 . . . no P(1) C(11) C(12) 122.0(3) . . . yes P(1) C(11) C(16) 118.5(3) . . . yes C(12) C(11) C(16) 119.2(3) . . . yes C(11) C(12) C(13) 120.7(3) . . . yes C(11) C(12) H(11) 119.7 . . . no C(13) C(12) H(11) 119.7 . . . no C(12) C(13) C(14) 119.6(3) . . . yes C(12) C(13) H(12) 120.2 . . . no C(14) C(13) H(12) 120.2 . . . no C(13) C(14) C(15) 120.1(4) . . . yes C(13) C(14) H(13) 120.0 . . . no C(15) C(14) H(13) 120.0 . . . no C(14) C(15) C(16) 120.5(3) . . . yes C(14) C(15) H(14) 119.8 . . . no C(16) C(15) H(14) 119.8 . . . no C(11) C(16) C(15) 119.9(4) . . . yes C(11) C(16) H(15) 120.0 . . . no C(15) C(16) H(15) 120.0 . . . no P(2) C(17) C(18) 112.1(3) . . . yes P(2) C(17) H(16) 123.9 . . . no C(18) C(17) H(16) 123.9 . . . no O(2) C(18) N(2) 112.4(3) . . . yes O(2) C(18) C(17) 121.7(3) . . . yes N(2) C(18) C(17) 125.9(4) . . . yes N(2) C(19) C(20) 103.1(3) . . . yes N(2) C(19) H(17) 111.1 . . . no N(2) C(19) H(18) 111.1 . . . no C(20) C(19) H(17) 111.1 . . . no C(20) C(19) H(18) 111.1 . . . no H(17) C(19) H(18) 109.5 . . . no O(2) C(20) C(19) 103.7(3) . . . yes O(2) C(20) H(19) 110.9 . . . no O(2) C(20) H(20) 110.9 . . . no C(19) C(20) H(19) 110.9 . . . no C(19) C(20) H(20) 110.9 . . . no H(19) C(20) H(20) 109.5 . . . no P(2) C(21) C(22) 119.3(3) . . . yes P(2) C(21) C(26) 121.7(3) . . . yes C(22) C(21) C(26) 119.0(3) . . . yes C(21) C(22) C(23) 120.3(4) . . . yes C(21) C(22) H(21) 119.8 . . . no C(23) C(22) H(21) 119.8 . . . no C(22) C(23) C(24) 120.2(4) . . . yes C(22) C(23) H(22) 119.9 . . . no C(24) C(23) H(22) 119.9 . . . no C(23) C(24) C(25) 120.1(4) . . . yes C(23) C(24) H(23) 120.0 . . . no C(25) C(24) H(23) 120.0 . . . no C(24) C(25) C(26) 119.1(4) . . . yes C(24) C(25) H(24) 120.5 . . . no C(26) C(25) H(24) 120.5 . . . no C(21) C(26) C(25) 121.3(4) . . . yes C(21) C(26) H(25) 119.3 . . . no C(25) C(26) H(25) 119.3 . . . no P(2) C(27) C(28) 120.4(3) . . . yes P(2) C(27) C(32) 120.2(3) . . . yes C(28) C(27) C(32) 119.2(3) . . . yes C(27) C(28) C(29) 120.0(4) . . . yes C(27) C(28) H(26) 120.0 . . . no C(29) C(28) H(26) 120.0 . . . no C(28) C(29) C(30) 120.7(4) . . . yes C(28) C(29) H(27) 119.7 . . . no C(30) C(29) H(27) 119.7 . . . no C(29) C(30) C(31) 119.0(4) . . . yes C(29) C(30) H(28) 120.5 . . . no C(31) C(30) H(28) 120.5 . . . no C(30) C(31) C(32) 120.8(4) . . . yes C(30) C(31) H(29) 119.6 . . . no C(32) C(31) H(29) 119.6 . . . no C(27) C(32) C(31) 120.2(3) . . . yes C(27) C(32) H(30) 119.9 . . . no C(31) C(32) H(30) 119.9 . . . 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 O(1) C(22) 3.138(4) . 1_565 no O(1) C(17) 3.373(4) . 1_565 no O(2) C(25) 3.466(5) . 4 no O(2) C(14) 3.467(5) . 2_545 no O(2) C(15) 3.542(5) . 2_545 no N(1) C(30) 3.433(5) . 2 no C(3) C(10) 3.545(6) . 4_565 no C(3) C(9) 3.553(6) . 4_565 no C(6) C(6) 3.485(8) . 3_665 no C(20) C(25) 3.573(6) . 4 no C(28) C(31) 3.544(5) . 2 no Pd(1) H(7) 2.9519 . 3_665 no O(1) H(16) 2.6176 . 1_565 no O(1) H(21) 2.6856 . 1_565 no O(1) H(22) 2.9522 . 3_665 no O(1) H(23) 2.9864 . 3_665 no O(2) H(13) 2.7699 . 2_545 no O(2) H(24) 2.8035 . 4 no O(2) H(14) 2.9245 . 2_545 no N(1) H(28) 2.5681 . 2 no N(2) H(8) 2.9114 . 3_665 no C(2) H(22) 2.9596 . 3_665 no C(4) H(23) 2.9161 . 3_665 no C(7) H(6) 2.9706 . 3_665 no C(8) H(21) 2.9303 . 3_665 no C(9) H(3) 2.9027 . 4_464 no C(12) H(2) 2.8540 . 4_464 no C(14) H(18) 2.9554 . 4_464 no C(18) H(14) 2.8758 . 2_545 no C(25) H(20) 2.9841 . 4_454 no C(26) H(20) 2.8466 . 4_454 no C(29) H(15) 2.9316 . 2_545 no C(31) H(26) 2.8548 . 2_545 no H(3) H(23) 2.5059 . 3_665 no H(3) H(9) 2.5912 . 4_565 no H(4) H(23) 2.4304 . 3_665 no H(5) H(11) 2.5963 . 4_565 no H(5) H(16) 2.6052 . 1_565 no H(5) H(12) 2.6366 . 4_565 no H(8) H(24) 2.4010 . 2_554 no H(10) H(17) 2.5857 . 4_464 no H(16) H(27) 2.5977 . 2_545 no H(20) H(25) 2.5702 . 4 no H(22) H(22) 2.6129 . 3_655 no #-----------------------------------------------------------------------------