# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1913 data_wtwong529-wywong018 #--------------------------------------------------------------------- _audit_creation_date 'Mon Mar 23 10:59:52 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #---------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR92' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #---------------------------------------------------------------------- _cell_length_a 9.889(1) _cell_length_b 17.607(2) _cell_length_c 10.282(1) _cell_angle_alpha 90 _cell_angle_beta 107.90(1) _cell_angle_gamma 90 _cell_volume 1703.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _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' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.190 _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_meas ? _chemical_formula_weight 860.32 _chemical_formula_analytical ? _chemical_formula_sum 'C38 H30 Cl2 N2 P2 Pd2 ' _chemical_formula_moiety 'C38 H30 Cl2 N2 P2 Pd2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 856.00 _exptl_absorpt_coefficient_mu 1.338 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'MARResearch Image Plate scanner' _diffrn_measurement_method 'omega scans with profile analysis' _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 16020 _reflns_number_total 2685 _reflns_number_observed 1755 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1 _diffrn_reflns_theta_max 25.55 _diffrn_reflns_reduction_process ? _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 76 0.003 0.002 'International Tables' H 0 60 0.000 0.000 'International Tables' P 0 4 0.102 0.094 'International Tables' Pd 0 4 -0.999 1.007 'International Tables' Cl 0 4 0.148 0.159 'International Tables' N 0 4 0.006 0.003 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Pd(1) 1.11479(5) 0.05715(4) 0.58579(6) 0.0451(2) Uij ? ? Cl(1) 1.3533(2) 0.0767(1) 0.6089(2) 0.0728(8) Uij ? ? P(1) 1.1193(2) 0.1460(1) 0.7397(2) 0.0469(7) Uij ? ? N(1) 0.9109(5) 0.0326(3) 0.5549(6) 0.041(2) Uij ? ? C(1) 0.8172(7) 0.0679(5) 0.5859(7) 0.053(3) Uij ? ? C(2) 0.8203(7) 0.1392(5) 0.6629(8) 0.048(3) Uij ? ? C(3) 0.6871(7) 0.1690(5) 0.6610(8) 0.062(3) Uij ? ? C(4) 0.6787(8) 0.2358(6) 0.7263(10) 0.075(4) Uij ? ? C(5) 0.8009(9) 0.2733(5) 0.7981(9) 0.073(3) Uij ? ? C(6) 0.9318(7) 0.2447(5) 0.8019(9) 0.064(3) Uij ? ? C(7) 0.9431(7) 0.1789(4) 0.7345(7) 0.045(3) Uij ? ? C(8) 1.2100(7) 0.2332(5) 0.7201(9) 0.049(3) Uij ? ? C(9) 1.1779(8) 0.2631(5) 0.5892(10) 0.070(3) Uij ? ? C(10) 1.2300(10) 0.3324(6) 0.5642(10) 0.080(4) Uij ? ? C(11) 1.3201(10) 0.3706(5) 0.669(1) 0.070(4) Uij ? ? C(12) 1.3563(9) 0.3422(6) 0.797(1) 0.076(4) Uij ? ? C(13) 1.3013(8) 0.2735(6) 0.8243(8) 0.068(3) Uij ? ? C(14) 1.2005(8) 0.1098(4) 0.9124(7) 0.051(3) Uij ? ? C(15) 1.3440(9) 0.0949(5) 0.9565(9) 0.071(3) Uij ? ? C(16) 1.4041(9) 0.0617(6) 1.085(1) 0.087(4) Uij ? ? C(17) 1.3216(10) 0.0413(5) 1.1634(9) 0.075(3) Uij ? ? C(18) 1.1789(10) 0.0551(6) 1.1186(10) 0.084(4) Uij ? ? C(19) 1.1177(8) 0.0907(5) 0.9939(9) 0.068(3) Uij ? ? H(1) 0.6026 0.1424 0.6141 0.0750 Uij ? ? H(2) 0.5887 0.2562 0.7221 0.0903 Uij ? ? H(3) 0.7952 0.3192 0.8449 0.0872 Uij ? ? H(4) 1.0155 0.2708 0.8522 0.0770 Uij ? ? H(5) 1.1180 0.2351 0.5146 0.0837 Uij ? ? H(6) 1.2029 0.3528 0.4744 0.0962 Uij ? ? H(7) 1.3582 0.4178 0.6529 0.0846 Uij ? ? H(8) 1.4205 0.3695 0.8694 0.0909 Uij ? ? H(9) 1.3269 0.2546 0.9152 0.0811 Uij ? ? H(10) 1.4015 0.1067 0.9003 0.0855 Uij ? ? H(11) 1.5037 0.0534 1.1183 0.1038 Uij ? ? H(12) 1.3632 0.0175 1.2493 0.0900 Uij ? ? H(13) 1.1213 0.0403 1.1729 0.1011 Uij ? ? H(14) 1.0190 0.1019 0.9646 0.0812 Uij ? ? H(15) 0.7261 0.0448 0.5544 0.0637 Uij ? ? 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) 0.0367(3) 0.0504(4) 0.0474(4) -0.0035(3) 0.0119(2) -0.0009(4) Cl(1) 0.040(1) 0.082(2) 0.098(2) -0.013(1) 0.024(1) -0.022(1) P(1) 0.041(1) 0.052(2) 0.046(1) -0.0010(9) 0.0092(10) -0.003(1) N(1) 0.036(3) 0.036(4) 0.046(4) -0.004(3) 0.007(3) -0.003(3) C(1) 0.040(4) 0.071(7) 0.044(5) -0.008(4) 0.008(4) 0.007(5) C(2) 0.055(5) 0.056(6) 0.036(5) 0.006(4) 0.018(4) 0.007(4) C(3) 0.045(5) 0.080(8) 0.067(6) 0.006(4) 0.024(4) 0.000(6) C(4) 0.062(6) 0.083(8) 0.085(8) 0.022(5) 0.029(5) -0.002(6) C(5) 0.079(6) 0.061(7) 0.085(8) 0.003(5) 0.035(6) -0.011(6) C(6) 0.053(5) 0.063(7) 0.080(7) -0.004(4) 0.026(4) -0.012(6) C(7) 0.045(4) 0.046(6) 0.044(5) -0.001(4) 0.014(4) 0.001(4) C(8) 0.043(4) 0.050(6) 0.054(6) -0.004(4) 0.016(4) -0.007(5) C(9) 0.080(6) 0.056(7) 0.065(7) -0.021(5) 0.009(5) -0.002(6) C(10) 0.096(7) 0.077(8) 0.065(8) -0.014(6) 0.022(6) 0.006(6) C(11) 0.074(6) 0.059(7) 0.090(9) -0.010(5) 0.042(6) -0.009(7) C(12) 0.074(6) 0.061(7) 0.096(9) -0.031(5) 0.032(6) -0.038(6) C(13) 0.070(5) 0.073(7) 0.054(6) -0.010(5) 0.011(5) -0.030(6) C(14) 0.053(5) 0.052(6) 0.044(6) 0.004(4) 0.008(4) -0.002(4) C(15) 0.068(6) 0.098(8) 0.047(6) 0.021(5) 0.018(5) 0.013(5) C(16) 0.067(6) 0.106(9) 0.081(8) 0.025(6) 0.014(5) 0.010(7) C(17) 0.082(7) 0.076(8) 0.068(7) 0.021(5) 0.024(5) 0.035(6) C(18) 0.085(6) 0.099(8) 0.075(7) 0.000(6) 0.034(5) 0.023(7) C(19) 0.051(5) 0.090(8) 0.062(7) -0.008(4) 0.017(5) 0.010(6) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _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 1755 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0468 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0362 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.699 _refine_ls_shift/esd_max 0.0130 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.72 _refine_diff_density_max 0.58 #------------------------------------------------------------------------------ _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) Cl(1) 2.322(2) ? ? yes Pd(1) P(1) 2.217(2) ? ? yes Pd(1) N(1) 1.990(5) ? ? yes Pd(1) N(1) 2.105(6) ? ? yes P(1) C(7) 1.821(7) ? ? yes P(1) C(8) 1.819(8) ? ? yes P(1) C(14) 1.824(8) ? ? yes N(1) C(1) 1.236(8) ? ? yes C(1) C(2) 1.48(1) ? ? yes C(2) C(3) 1.412(9) ? ? yes C(2) C(7) 1.398(9) ? ? yes C(3) C(4) 1.37(1) ? ? yes C(4) C(5) 1.38(1) ? ? yes C(5) C(6) 1.378(10) ? ? yes C(6) C(7) 1.372(10) ? ? yes C(8) C(9) 1.39(1) ? ? yes C(8) C(13) 1.368(10) ? ? yes C(9) C(10) 1.38(1) ? ? yes C(10) C(11) 1.35(1) ? ? yes C(11) C(12) 1.35(1) ? ? yes C(12) C(13) 1.39(1) ? ? yes C(14) C(15) 1.376(9) ? ? yes C(14) C(19) 1.381(10) ? ? yes C(15) C(16) 1.40(1) ? ? yes C(16) C(17) 1.36(1) ? ? yes C(17) C(18) 1.36(1) ? ? yes C(18) C(19) 1.39(1) ? ? yes #------------------------------------------------------------------------------ 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 Cl(1) Pd(1) P(1) 91.46(7) ? ? ? yes Cl(1) Pd(1) N(1) 174.8(2) ? ? ? yes Cl(1) Pd(1) N(1) 94.9(2) ? ? ? yes P(1) Pd(1) N(1) 93.7(2) ? ? ? yes P(1) Pd(1) N(1) 173.1(1) ? ? ? yes N(1) Pd(1) N(1) 79.9(2) ? ? ? yes Pd(1) P(1) C(7) 113.2(3) ? ? ? yes Pd(1) P(1) C(8) 114.7(3) ? ? ? yes Pd(1) P(1) C(14) 110.7(3) ? ? ? yes C(7) P(1) C(8) 103.2(3) ? ? ? yes C(7) P(1) C(14) 105.7(3) ? ? ? yes C(8) P(1) C(14) 108.6(4) ? ? ? yes Pd(1) N(1) Pd(1) 100.1(2) ? ? ? yes Pd(1) N(1) C(1) 130.8(5) ? ? ? yes Pd(1) N(1) C(1) 127.8(5) ? ? ? yes N(1) C(1) C(2) 132.1(6) ? ? ? yes C(1) C(2) C(3) 116.2(7) ? ? ? yes C(1) C(2) C(7) 125.3(6) ? ? ? yes C(3) C(2) C(7) 118.5(7) ? ? ? yes C(2) C(3) C(4) 120.5(7) ? ? ? yes C(3) C(4) C(5) 120.0(7) ? ? ? yes C(4) C(5) C(6) 120.1(8) ? ? ? yes C(5) C(6) C(7) 121.1(7) ? ? ? yes P(1) C(7) C(2) 121.7(6) ? ? ? yes P(1) C(7) C(6) 118.6(6) ? ? ? yes C(2) C(7) C(6) 119.7(6) ? ? ? yes P(1) C(8) C(9) 117.0(6) ? ? ? yes P(1) C(8) C(13) 125.4(7) ? ? ? yes C(9) C(8) C(13) 117.5(8) ? ? ? yes C(8) C(9) C(10) 122.0(8) ? ? ? yes C(9) C(10) C(11) 118.9(9) ? ? ? yes C(10) C(11) C(12) 120.5(9) ? ? ? yes C(11) C(12) C(13) 121.2(8) ? ? ? yes C(8) C(13) C(12) 119.8(9) ? ? ? yes P(1) C(14) C(15) 119.2(6) ? ? ? yes P(1) C(14) C(19) 120.7(6) ? ? ? yes C(15) C(14) C(19) 119.9(7) ? ? ? yes C(14) C(15) C(16) 119.0(7) ? ? ? yes C(15) C(16) C(17) 120.8(7) ? ? ? yes C(16) C(17) C(18) 120.0(8) ? ? ? yes C(17) C(18) C(19) 120.3(8) ? ? ? yes C(14) C(19) C(18) 119.9(7) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_XF138 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H55 Cl4 N2 O P3 Pd2' _chemical_formula_weight 1327.62 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.574(1) _cell_length_b 13.636(1) _cell_length_c 20.058(1) _cell_angle_alpha 80.03(1) _cell_angle_beta 75.67(1) _cell_angle_gamma 81.04(1) _cell_volume 3258.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 159 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.833 _exptl_absorpt_correction_T_max 1.144 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; Rigaku RU-200 rotating-anode generator powered at 50kV/90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS IIc' _diffrn_measurement_method ; Data was collected to 0.82\%A and 85% completeness by taking 28 oscillation photos in the range of 0 - 162\%, \D\f = 6\%, 8 min. per frame. Crystal to detector distance is 78.146mm, background level -50. ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9163 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0839 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.52 _reflns_number_total 9163 _reflns_number_gt 7937 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BioteX 1.0 (MSC, 1995)' _computing_cell_refinement 'BioteX 1.0 (MSC, 1995)' _computing_data_reduction 'BioteX 1.0 (MSC, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PC (Siemens, 1990)' _computing_publication_material ? _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^)+(0.1019P)^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 SHELXL _refine_ls_extinction_coef 0.0056(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9163 _refine_ls_number_parameters 718 _refine_ls_number_restraints 1113 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1741 _refine_ls_wR_factor_gt 0.1642 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.003 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.09081(3) 0.96946(3) 0.30784(2) 0.05283(12) Uani 1 1 d . . . Pd2 Pd 0.31728(3) 0.67448(3) 0.27680(2) 0.05316(12) Uani 1 1 d . . . Cl1 Cl 0.27294(12) 0.90581(12) 0.31426(8) 0.0704(4) Uani 1 1 d . . . Cl2 Cl 0.09246(14) 1.08000(12) 0.38072(9) 0.0810(5) Uani 1 1 d . . . Cl3 Cl 0.44011(13) 0.66935(12) 0.34555(8) 0.0736(4) Uani 1 1 d . . . Cl4 Cl 0.97999(15) 0.71912(14) 0.09410(9) 0.0855(5) Uani 1 1 d . . . P1 P -0.08227(12) 1.02971(10) 0.30457(7) 0.0540(3) Uani 1 1 d . . . P2 P 0.45905(12) 0.71912(11) 0.18100(8) 0.0591(4) Uani 1 1 d . . . P3 P 0.19592(12) 0.59322(10) 0.36728(7) 0.0536(3) Uani 1 1 d . . . N1 N 0.0883(3) 0.8773(3) 0.2360(2) 0.0515(10) Uani 1 1 d . . . N2 N 0.2098(3) 0.6773(3) 0.2138(2) 0.0498(10) Uani 1 1 d . . . C1 C -0.1573(4) 0.9244(4) 0.3121(2) 0.0539(13) Uani 1 1 d D . . C2 C -0.1062(4) 0.8455(3) 0.2741(2) 0.0543(13) Uani 1 1 d D . . C3 C -0.1683(4) 0.7670(4) 0.2749(3) 0.0653(15) Uani 1 1 d D . . H3 H -0.1375 0.7163 0.2479 0.078 Uiso 1 1 calc R . . C4 C -0.2734(5) 0.7649(4) 0.3153(3) 0.0728(17) Uani 1 1 d D . . H4 H -0.3117 0.7110 0.3171 0.087 Uiso 1 1 calc R . . C5 C -0.3228(5) 0.8412(4) 0.3529(3) 0.0729(17) Uani 1 1 d D . . H5 H -0.3946 0.8393 0.3795 0.087 Uiso 1 1 calc R . . C6 C -0.2658(5) 0.9210(4) 0.3514(3) 0.0669(16) Uani 1 1 d D . . H6 H -0.3000 0.9729 0.3768 0.080 Uiso 1 1 calc R . . C7 C -0.0853(4) 1.1015(4) 0.2207(3) 0.0597(14) Uani 1 1 d D . . C8 C -0.0138(5) 1.1748(4) 0.1968(3) 0.0693(16) Uani 1 1 d D . . H8 H 0.0355 1.1831 0.2226 0.083 Uiso 1 1 calc R . . C9 C -0.0171(6) 1.2357(5) 0.1336(3) 0.086(2) Uani 1 1 d D . . H9 H 0.0283 1.2866 0.1184 0.103 Uiso 1 1 calc R . . C10 C -0.0855(6) 1.2221(5) 0.0937(3) 0.094(2) Uani 1 1 d D . . H10 H -0.0859 1.2629 0.0515 0.113 Uiso 1 1 calc R . . C11 C -0.1539(6) 1.1479(6) 0.1162(3) 0.099(2) Uani 1 1 d D . . H11 H -0.2002 1.1378 0.0889 0.119 Uiso 1 1 calc R . . C12 C -0.1537(5) 1.0879(5) 0.1798(3) 0.0764(18) Uani 1 1 d D . . H12 H -0.2003 1.0379 0.1949 0.092 Uiso 1 1 calc R . . C13 C -0.1664(4) 1.1058(4) 0.3678(3) 0.0592(14) Uani 1 1 d D . . C14 C -0.1783(5) 1.0716(4) 0.4380(3) 0.0713(17) Uani 1 1 d D . . H14 H -0.1390 1.0112 0.4523 0.086 Uiso 1 1 calc R . . C15 C -0.2481(5) 1.1263(5) 0.4876(3) 0.0789(19) Uani 1 1 d D . . H15 H -0.2564 1.1017 0.5346 0.095 Uiso 1 1 calc R . . C16 C -0.3046(6) 1.2161(5) 0.4672(3) 0.087(2) Uani 1 1 d D . . H16 H -0.3511 1.2530 0.5002 0.104 Uiso 1 1 calc R . . C17 C -0.2923(6) 1.2513(5) 0.3980(4) 0.095(2) Uani 1 1 d D . . H17 H -0.3299 1.3129 0.3843 0.114 Uiso 1 1 calc R . . C18 C -0.2252(6) 1.1970(4) 0.3479(3) 0.0798(19) Uani 1 1 d D . . H18 H -0.2192 1.2214 0.3010 0.096 Uiso 1 1 calc R . . C19 C 0.4197(4) 0.7147(4) 0.1008(3) 0.0675(16) Uani 1 1 d D . . C20 C 0.3087(4) 0.7402(4) 0.0952(2) 0.0561(13) Uani 1 1 d D . . C21 C 0.2856(5) 0.7373(4) 0.0320(3) 0.0712(17) Uani 1 1 d D . . H21 H 0.2133 0.7546 0.0268 0.085 Uiso 1 1 calc R . . C22 C 0.3674(6) 0.7092(6) -0.0239(3) 0.095(2) Uani 1 1 d D . . H22 H 0.3494 0.7084 -0.0660 0.113 Uiso 1 1 calc R . . C23 C 0.4741(6) 0.6829(6) -0.0179(3) 0.101(2) Uani 1 1 d D . . H23 H 0.5282 0.6632 -0.0556 0.121 Uiso 1 1 calc R . . C24 C 0.5017(5) 0.6856(5) 0.0436(3) 0.084(2) Uani 1 1 d D . . H24 H 0.5746 0.6681 0.0476 0.100 Uiso 1 1 calc R . . C25 C 0.5104(5) 0.8401(4) 0.1660(3) 0.0661(16) Uani 1 1 d D . . C26 C 0.5252(5) 0.8803(4) 0.2214(3) 0.0779(18) Uani 1 1 d D . . H26 H 0.5110 0.8441 0.2658 0.093 Uiso 1 1 calc R . . C27 C 0.5611(6) 0.9741(5) 0.2113(4) 0.095(2) Uani 1 1 d D . . H27 H 0.5716 1.0004 0.2487 0.113 Uiso 1 1 calc R . . C28 C 0.5812(6) 1.0280(5) 0.1456(4) 0.093(2) Uani 1 1 d D . . H28 H 0.6039 1.0914 0.1392 0.112 Uiso 1 1 calc R . . C29 C 0.5684(6) 0.9904(5) 0.0902(4) 0.093(2) Uani 1 1 d D . . H29 H 0.5846 1.0266 0.0459 0.111 Uiso 1 1 calc R . . C30 C 0.5305(6) 0.8964(5) 0.1002(3) 0.086(2) Uani 1 1 d D . . H30 H 0.5188 0.8715 0.0627 0.104 Uiso 1 1 calc R . . C31 C 0.5752(4) 0.6225(4) 0.1834(3) 0.0685(16) Uani 1 1 d D . . C32 C 0.6832(5) 0.6417(5) 0.1696(3) 0.0784(19) Uani 1 1 d D . . H32 H 0.6999 0.7075 0.1587 0.094 Uiso 1 1 calc R . . C33 C 0.7678(6) 0.5629(5) 0.1719(4) 0.112(3) Uani 1 1 d D . . H33 H 0.8409 0.5761 0.1618 0.134 Uiso 1 1 calc R . . C34 C 0.7434(6) 0.4660(6) 0.1892(5) 0.124(3) Uani 1 1 d D . . H34 H 0.7998 0.4138 0.1925 0.148 Uiso 1 1 calc R . . C35 C 0.6382(7) 0.4456(6) 0.2013(5) 0.127(3) Uani 1 1 d D . . H35 H 0.6231 0.3794 0.2099 0.153 Uiso 1 1 calc R . . C36 C 0.5528(6) 0.5227(5) 0.2011(4) 0.099(3) Uani 1 1 d D . . H36 H 0.4800 0.5082 0.2128 0.119 Uiso 1 1 calc R . . C37 C 0.1403(4) 0.5030(3) 0.3338(3) 0.0569(14) Uani 1 1 d D . . C38 C 0.1162(4) 0.5245(4) 0.2682(3) 0.0603(14) Uani 1 1 d D . . C39 C 0.0554(5) 0.4607(4) 0.2480(3) 0.0795(19) Uani 1 1 d D . . H39 H 0.0385 0.4753 0.2045 0.095 Uiso 1 1 calc R . . C40 C 0.0206(6) 0.3763(5) 0.2926(3) 0.092(2) Uani 1 1 d D . . H40 H -0.0203 0.3349 0.2793 0.111 Uiso 1 1 calc R . . C41 C 0.0463(6) 0.3544(5) 0.3558(3) 0.089(2) Uani 1 1 d D . . H41 H 0.0254 0.2963 0.3847 0.107 Uiso 1 1 calc R . . C42 C 0.1037(5) 0.4177(4) 0.3782(3) 0.0727(18) Uani 1 1 d D . . H42 H 0.1176 0.4031 0.4225 0.087 Uiso 1 1 calc R . . C43 C 0.0758(4) 0.6697(4) 0.4081(2) 0.0547(13) Uani 1 1 d D . . C44 C -0.0320(4) 0.6479(4) 0.4176(3) 0.0618(14) Uani 1 1 d D . . H44 H -0.0451 0.5923 0.4011 0.074 Uiso 1 1 calc R . . C45 C -0.1196(4) 0.7091(4) 0.4515(3) 0.0641(15) Uani 1 1 d D . . H45 H -0.1914 0.6941 0.4580 0.077 Uiso 1 1 calc R . . C46 C -0.1017(5) 0.7906(4) 0.4754(3) 0.0680(16) Uani 1 1 d D . . H46 H -0.1612 0.8307 0.4986 0.082 Uiso 1 1 calc R . . C47 C 0.0028(5) 0.8144(4) 0.4658(3) 0.0737(18) Uani 1 1 d D . . H47 H 0.0137 0.8710 0.4821 0.088 Uiso 1 1 calc R . . C48 C 0.0928(5) 0.7557(4) 0.4320(3) 0.0618(14) Uani 1 1 d D . . H48 H 0.1638 0.7729 0.4252 0.074 Uiso 1 1 calc R . . C49 C 0.2583(4) 0.5230(4) 0.4356(3) 0.0627(15) Uani 1 1 d D . . C50 C 0.3463(5) 0.4494(5) 0.4181(3) 0.093(2) Uani 1 1 d D . . H50 H 0.3665 0.4325 0.3733 0.112 Uiso 1 1 calc R . . C51 C 0.4033(6) 0.4017(6) 0.4674(4) 0.123(3) Uani 1 1 d D . . H51 H 0.4632 0.3539 0.4550 0.148 Uiso 1 1 calc R . . C52 C 0.3742(6) 0.4228(6) 0.5333(4) 0.119(3) Uani 1 1 d D . . H52 H 0.4130 0.3892 0.5661 0.143 Uiso 1 1 calc R . . C53 C 0.2877(7) 0.4936(5) 0.5510(4) 0.112(3) Uani 1 1 d D . . H53 H 0.2684 0.5090 0.5962 0.134 Uiso 1 1 calc R . . C54 C 0.2272(6) 0.5435(4) 0.5033(3) 0.0776(18) Uani 1 1 d D . . H54 H 0.1666 0.5901 0.5167 0.093 Uiso 1 1 calc R . . C55 C 0.0050(4) 0.8395(4) 0.2304(3) 0.0538(13) Uani 1 1 d D . . H55 H 0.0170 0.8032 0.1935 0.065 Uiso 1 1 calc R . . C56 C 0.1953(4) 0.8621(4) 0.1808(3) 0.0545(13) Uani 1 1 d . . . H56 H 0.2566 0.8631 0.2027 0.065 Uiso 1 1 calc R . . C57 C 0.2122(4) 0.7605(4) 0.1539(2) 0.0520(13) Uani 1 1 d D . . H57 H 0.1464 0.7585 0.1365 0.062 Uiso 1 1 calc R . . C58 C 0.1441(5) 0.6140(4) 0.2162(3) 0.0555(13) Uani 1 1 d D . . H58 H 0.1079 0.6255 0.1799 0.067 Uiso 1 1 calc R . . C59 C 0.1975(4) 0.9518(4) 0.1238(3) 0.0563(14) Uani 1 1 d D . . C60 C 0.1335(5) 0.9648(4) 0.0759(3) 0.0688(16) Uani 1 1 d D . . H60 H 0.0880 0.9165 0.0772 0.083 Uiso 1 1 calc R . . C61 C 0.1355(6) 1.0485(5) 0.0254(3) 0.083(2) Uani 1 1 d D . . H61 H 0.0917 1.0557 -0.0067 0.100 Uiso 1 1 calc R . . C62 C 0.2018(6) 1.1206(5) 0.0227(3) 0.089(2) Uani 1 1 d D . . H62 H 0.2033 1.1767 -0.0112 0.107 Uiso 1 1 calc R . . C63 C 0.2652(6) 1.1090(5) 0.0700(4) 0.093(2) Uani 1 1 d D . . H63 H 0.3101 1.1580 0.0684 0.111 Uiso 1 1 calc R . . C64 C 0.2644(5) 1.0245(4) 0.1216(3) 0.0682(16) Uani 1 1 d D . . H64 H 0.3082 1.0176 0.1536 0.082 Uiso 1 1 calc R . . O1 O 1.0556(11) 0.4971(7) 0.0695(7) 0.123(4) Uani 0.50 1 d PDU . . H1 H 1.0397 0.5580 0.0621 0.184 Uiso 0.50 1 calc PR . . C65 C 1.1579(17) 0.470(2) 0.0275(12) 0.216(11) Uani 0.50 1 d PDU . . H65A H 1.1860 0.5283 -0.0012 0.324 Uiso 0.50 1 calc PR . . H65B H 1.1502 0.4232 -0.0014 0.324 Uiso 0.50 1 calc PR . . H65C H 1.2084 0.4387 0.0560 0.324 Uiso 0.50 1 calc PR . . O2 O 0.396(2) 1.2111(17) 0.2878(11) 0.308(12) Uani 0.50 1 d PDU . . H2 H 0.4118 1.2678 0.2860 0.463 Uiso 0.50 1 calc PR . . C66 C 0.391(2) 1.159(2) 0.3558(12) 0.225(10) Uani 0.50 1 d PDU . . H66A H 0.4640 1.1341 0.3614 0.337 Uiso 0.50 1 calc PR . . H66B H 0.3479 1.1041 0.3629 0.337 Uiso 0.50 1 calc PR . . H66C H 0.3563 1.2040 0.3891 0.337 Uiso 0.50 1 calc PR . . 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 0.0515(2) 0.0578(2) 0.0482(2) -0.00868(17) -0.01086(18) -0.00293(18) Pd2 0.0469(2) 0.0636(2) 0.0455(2) -0.00146(17) -0.01024(17) -0.00337(18) Cl1 0.0548(8) 0.0908(10) 0.0674(9) -0.0181(7) -0.0193(7) 0.0023(7) Cl2 0.0733(10) 0.0910(10) 0.0888(11) -0.0432(8) -0.0185(8) -0.0057(8) Cl3 0.0641(9) 0.0921(10) 0.0666(9) 0.0067(7) -0.0271(7) -0.0157(8) Cl4 0.0903(11) 0.1070(12) 0.0670(10) -0.0095(8) -0.0282(8) -0.0217(9) P1 0.0517(8) 0.0567(7) 0.0506(8) -0.0074(6) -0.0103(6) 0.0002(6) P2 0.0456(8) 0.0729(9) 0.0529(8) -0.0044(6) -0.0054(6) -0.0037(7) P3 0.0512(8) 0.0610(8) 0.0438(7) -0.0006(5) -0.0089(6) -0.0031(6) N1 0.044(2) 0.056(2) 0.052(2) -0.0034(18) -0.0128(18) 0.0002(19) N2 0.042(2) 0.056(2) 0.048(2) -0.0037(17) -0.0087(18) 0.0007(18) C1 0.051(3) 0.061(3) 0.045(3) -0.002(2) -0.009(2) -0.005(2) C2 0.052(3) 0.059(3) 0.049(3) -0.002(2) -0.009(2) -0.006(2) C3 0.061(4) 0.061(3) 0.077(4) -0.015(3) -0.019(3) -0.007(3) C4 0.059(3) 0.078(4) 0.082(4) -0.001(3) -0.011(3) -0.028(3) C5 0.047(3) 0.100(4) 0.066(4) -0.005(3) -0.001(3) -0.017(3) C6 0.066(4) 0.077(4) 0.056(3) -0.014(3) -0.012(3) -0.002(3) C7 0.059(3) 0.065(3) 0.048(3) -0.004(2) -0.007(3) 0.001(3) C8 0.075(4) 0.068(3) 0.058(3) -0.005(3) -0.008(3) -0.006(3) C9 0.093(5) 0.073(4) 0.076(4) 0.010(3) -0.002(4) -0.014(4) C10 0.108(6) 0.104(5) 0.056(4) 0.010(3) -0.017(4) 0.003(4) C11 0.095(5) 0.125(6) 0.079(5) 0.023(4) -0.040(4) -0.025(5) C12 0.066(4) 0.095(4) 0.065(4) 0.011(3) -0.020(3) -0.016(3) C13 0.055(3) 0.062(3) 0.061(3) -0.014(2) -0.012(3) -0.004(3) C14 0.076(4) 0.077(4) 0.062(4) -0.014(3) -0.014(3) -0.010(3) C15 0.073(4) 0.101(5) 0.062(4) -0.031(3) -0.001(3) -0.010(4) C16 0.075(5) 0.099(5) 0.086(5) -0.046(4) -0.003(4) 0.001(4) C17 0.093(5) 0.082(4) 0.099(5) -0.032(4) -0.013(4) 0.027(4) C18 0.083(5) 0.071(4) 0.076(4) -0.012(3) -0.015(3) 0.013(3) C19 0.066(4) 0.073(4) 0.058(3) -0.014(3) -0.004(3) -0.003(3) C20 0.055(3) 0.062(3) 0.045(3) -0.002(2) -0.008(2) 0.000(2) C21 0.065(4) 0.095(4) 0.048(3) -0.006(3) -0.013(3) 0.002(3) C22 0.090(5) 0.142(6) 0.050(4) -0.037(4) -0.013(3) 0.009(5) C23 0.083(5) 0.143(6) 0.063(4) -0.033(4) 0.003(4) 0.012(5) C24 0.060(4) 0.121(5) 0.061(4) -0.022(4) -0.006(3) 0.014(4) C25 0.049(3) 0.080(4) 0.065(4) -0.003(3) -0.014(3) -0.003(3) C26 0.070(4) 0.089(4) 0.074(4) 0.000(3) -0.019(3) -0.016(3) C27 0.102(5) 0.097(5) 0.091(5) -0.003(4) -0.024(4) -0.041(4) C28 0.072(4) 0.073(4) 0.124(6) 0.009(4) -0.012(4) -0.021(3) C29 0.089(5) 0.103(5) 0.074(5) 0.011(4) -0.009(4) -0.017(4) C30 0.090(5) 0.101(5) 0.063(4) 0.007(3) -0.011(3) -0.026(4) C31 0.051(3) 0.084(4) 0.067(4) -0.016(3) -0.005(3) -0.005(3) C32 0.054(4) 0.084(4) 0.094(5) -0.018(3) -0.013(3) 0.004(3) C33 0.057(4) 0.118(6) 0.158(8) -0.026(5) -0.031(5) 0.014(4) C34 0.081(6) 0.089(5) 0.191(10) -0.026(6) -0.033(6) 0.027(4) C35 0.111(7) 0.079(5) 0.189(10) -0.016(5) -0.045(7) 0.014(5) C36 0.069(5) 0.084(5) 0.141(7) -0.004(4) -0.029(4) 0.000(4) C37 0.062(3) 0.049(3) 0.056(3) -0.003(2) -0.013(3) -0.002(2) C38 0.065(3) 0.056(3) 0.064(3) -0.009(2) -0.021(3) -0.007(3) C39 0.099(5) 0.076(4) 0.071(4) -0.006(3) -0.029(4) -0.024(4) C40 0.128(6) 0.071(4) 0.086(5) -0.004(3) -0.025(4) -0.043(4) C41 0.120(6) 0.059(4) 0.083(5) -0.003(3) -0.014(4) -0.021(4) C42 0.097(5) 0.060(3) 0.055(3) -0.005(3) -0.011(3) -0.005(3) C43 0.056(3) 0.059(3) 0.045(3) -0.002(2) -0.012(2) -0.001(2) C44 0.066(4) 0.063(3) 0.057(3) -0.003(2) -0.016(3) -0.012(3) C45 0.047(3) 0.073(4) 0.068(4) -0.006(3) -0.009(3) -0.004(3) C46 0.067(4) 0.070(4) 0.058(3) -0.004(3) -0.006(3) 0.001(3) C47 0.095(5) 0.061(3) 0.061(4) -0.013(3) -0.010(3) -0.007(3) C48 0.059(3) 0.070(3) 0.059(3) -0.010(3) -0.014(3) -0.014(3) C49 0.057(3) 0.064(3) 0.060(3) 0.007(2) -0.011(3) -0.006(3) C50 0.067(4) 0.108(5) 0.085(5) 0.019(4) -0.011(4) 0.004(4) C51 0.069(5) 0.131(6) 0.138(7) 0.061(6) -0.031(5) 0.004(4) C52 0.103(6) 0.127(6) 0.132(7) 0.066(5) -0.073(5) -0.045(5) C53 0.166(7) 0.104(5) 0.087(5) 0.028(4) -0.076(5) -0.053(5) C54 0.107(5) 0.067(4) 0.067(4) 0.006(3) -0.037(3) -0.023(3) C55 0.050(3) 0.057(3) 0.053(3) -0.008(2) -0.008(2) -0.005(2) C56 0.046(3) 0.071(3) 0.042(3) -0.007(2) -0.003(2) -0.005(2) C57 0.056(3) 0.059(3) 0.040(3) -0.004(2) -0.012(2) -0.007(2) C58 0.059(3) 0.059(3) 0.047(3) -0.006(2) -0.014(2) -0.004(3) C59 0.049(3) 0.059(3) 0.053(3) -0.005(2) -0.003(2) 0.000(2) C60 0.067(4) 0.073(4) 0.062(4) -0.002(3) -0.013(3) -0.005(3) C61 0.087(5) 0.088(4) 0.060(4) 0.004(3) -0.009(3) 0.006(4) C62 0.085(5) 0.085(4) 0.074(4) 0.026(3) -0.005(4) -0.003(4) C63 0.093(5) 0.073(4) 0.096(5) 0.008(4) 0.002(4) -0.020(4) C64 0.059(4) 0.066(3) 0.070(4) -0.003(3) -0.003(3) -0.007(3) O1 0.142(9) 0.079(6) 0.135(10) -0.017(6) -0.017(7) 0.003(7) C65 0.191(17) 0.30(3) 0.140(18) -0.054(17) 0.072(14) -0.117(17) O2 0.30(2) 0.222(17) 0.302(16) -0.120(14) 0.174(18) -0.035(17) C66 0.128(19) 0.33(3) 0.268(19) -0.210(16) -0.023(19) -0.03(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.079(4) . ? Pd1 P1 2.2160(15) . ? Pd1 Cl2 2.2797(16) . ? Pd1 Cl1 2.3458(16) . ? Pd2 N2 2.059(4) . ? Pd2 Cl3 2.2976(16) . ? Pd2 P3 2.3044(13) . ? Pd2 P2 2.3404(14) . ? P1 C7 1.800(5) . ? P1 C1 1.803(5) . ? P1 C13 1.805(5) . ? P2 C19 1.810(6) . ? P2 C31 1.812(6) . ? P2 C25 1.814(6) . ? P3 C43 1.798(5) . ? P3 C37 1.800(5) . ? P3 C49 1.805(5) . ? N1 C55 1.272(6) . ? N1 C56 1.528(6) . ? N2 C58 1.271(6) . ? N2 C57 1.500(6) . ? C1 C6 1.400(6) . ? C1 C2 1.407(6) . ? C2 C3 1.416(6) . ? C2 C55 1.454(7) . ? C3 C4 1.369(7) . ? C4 C5 1.370(7) . ? C5 C6 1.386(7) . ? C7 C12 1.379(7) . ? C7 C8 1.392(7) . ? C8 C9 1.397(7) . ? C9 C10 1.363(8) . ? C10 C11 1.374(8) . ? C11 C12 1.392(7) . ? C13 C14 1.383(7) . ? C13 C18 1.392(7) . ? C14 C15 1.391(7) . ? C15 C16 1.368(8) . ? C16 C17 1.366(8) . ? C17 C18 1.383(8) . ? C19 C24 1.408(7) . ? C19 C20 1.412(7) . ? C20 C21 1.376(7) . ? C20 C57 1.496(7) . ? C21 C22 1.385(7) . ? C22 C23 1.364(8) . ? C23 C24 1.368(8) . ? C25 C26 1.384(7) . ? C25 C30 1.392(7) . ? C26 C27 1.388(7) . ? C27 C28 1.378(8) . ? C28 C29 1.354(8) . ? C29 C30 1.401(8) . ? C31 C32 1.374(7) . ? C31 C36 1.401(7) . ? C32 C33 1.392(8) . ? C33 C34 1.369(8) . ? C34 C35 1.348(9) . ? C35 C36 1.381(8) . ? C37 C38 1.395(7) . ? C37 C42 1.401(6) . ? C38 C39 1.411(7) . ? C38 C58 1.486(7) . ? C39 C40 1.387(7) . ? C40 C41 1.357(8) . ? C41 C42 1.399(8) . ? C43 C44 1.392(6) . ? C43 C48 1.406(7) . ? C44 C45 1.383(7) . ? C45 C46 1.353(7) . ? C46 C47 1.362(7) . ? C47 C48 1.380(7) . ? C49 C54 1.381(7) . ? C49 C50 1.392(7) . ? C50 C51 1.378(8) . ? C51 C52 1.349(9) . ? C52 C53 1.358(9) . ? C53 C54 1.390(8) . ? C56 C59 1.522(7) . ? C56 C57 1.538(7) . ? C59 C60 1.373(7) . ? C59 C64 1.384(7) . ? C60 C61 1.388(7) . ? C61 C62 1.370(8) . ? C62 C63 1.359(8) . ? C63 C64 1.408(7) . ? O1 C65 1.389(16) . ? O2 C66 1.414(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 P1 88.29(12) . . ? N1 Pd1 Cl2 175.96(12) . . ? P1 Pd1 Cl2 90.09(6) . . ? N1 Pd1 Cl1 92.81(12) . . ? P1 Pd1 Cl1 178.59(5) . . ? Cl2 Pd1 Cl1 88.87(6) . . ? N2 Pd2 Cl3 178.75(12) . . ? N2 Pd2 P3 89.10(11) . . ? Cl3 Pd2 P3 91.52(5) . . ? N2 Pd2 P2 91.61(11) . . ? Cl3 Pd2 P2 87.55(6) . . ? P3 Pd2 P2 166.68(5) . . ? C7 P1 C1 106.5(2) . . ? C7 P1 C13 106.2(2) . . ? C1 P1 C13 105.0(2) . . ? C7 P1 Pd1 109.27(18) . . ? C1 P1 Pd1 107.51(17) . . ? C13 P1 Pd1 121.48(19) . . ? C19 P2 C31 105.1(3) . . ? C19 P2 C25 103.1(3) . . ? C31 P2 C25 108.0(3) . . ? C19 P2 Pd2 110.53(18) . . ? C31 P2 Pd2 107.16(18) . . ? C25 P2 Pd2 121.72(19) . . ? C43 P3 C37 104.1(2) . . ? C43 P3 C49 107.0(2) . . ? C37 P3 C49 105.8(2) . . ? C43 P3 Pd2 116.26(16) . . ? C37 P3 Pd2 108.37(16) . . ? C49 P3 Pd2 114.35(18) . . ? C55 N1 C56 117.6(4) . . ? C55 N1 Pd1 126.5(4) . . ? C56 N1 Pd1 115.6(3) . . ? C58 N2 C57 114.1(4) . . ? C58 N2 Pd2 128.5(3) . . ? C57 N2 Pd2 117.3(3) . . ? C6 C1 C2 119.2(5) . . ? C6 C1 P1 122.4(4) . . ? C2 C1 P1 118.3(4) . . ? C1 C2 C3 118.5(4) . . ? C1 C2 C55 125.3(5) . . ? C3 C2 C55 116.1(5) . . ? C4 C3 C2 120.7(5) . . ? C3 C4 C5 120.8(5) . . ? C4 C5 C6 120.1(5) . . ? C5 C6 C1 120.6(5) . . ? C12 C7 C8 119.1(5) . . ? C12 C7 P1 123.9(4) . . ? C8 C7 P1 117.1(4) . . ? C7 C8 C9 119.1(6) . . ? C10 C9 C8 121.3(6) . . ? C9 C10 C11 119.7(6) . . ? C10 C11 C12 119.9(6) . . ? C7 C12 C11 120.9(6) . . ? C14 C13 C18 118.4(5) . . ? C14 C13 P1 120.0(4) . . ? C18 C13 P1 121.6(4) . . ? C13 C14 C15 120.9(6) . . ? C16 C15 C14 120.1(6) . . ? C17 C16 C15 119.5(6) . . ? C16 C17 C18 121.3(6) . . ? C17 C18 C13 119.9(6) . . ? C24 C19 C20 120.2(5) . . ? C24 C19 P2 118.9(5) . . ? C20 C19 P2 120.8(4) . . ? C21 C20 C19 117.4(5) . . ? C21 C20 C57 116.9(5) . . ? C19 C20 C57 125.4(5) . . ? C20 C21 C22 121.6(6) . . ? C23 C22 C21 120.7(6) . . ? C22 C23 C24 120.0(6) . . ? C23 C24 C19 120.0(6) . . ? C26 C25 C30 118.6(6) . . ? C26 C25 P2 119.7(4) . . ? C30 C25 P2 121.6(5) . . ? C25 C26 C27 120.6(6) . . ? C28 C27 C26 119.7(6) . . ? C29 C28 C27 121.2(6) . . ? C28 C29 C30 119.4(6) . . ? C25 C30 C29 120.5(6) . . ? C32 C31 C36 118.5(6) . . ? C32 C31 P2 123.9(5) . . ? C36 C31 P2 117.7(4) . . ? C31 C32 C33 120.2(6) . . ? C34 C33 C32 120.1(7) . . ? C35 C34 C33 120.5(7) . . ? C34 C35 C36 120.3(7) . . ? C35 C36 C31 120.3(7) . . ? C38 C37 C42 119.0(5) . . ? C38 C37 P3 120.7(3) . . ? C42 C37 P3 119.4(4) . . ? C37 C38 C39 119.6(5) . . ? C37 C38 C58 125.9(5) . . ? C39 C38 C58 114.4(5) . . ? C40 C39 C38 120.4(6) . . ? C41 C40 C39 119.8(6) . . ? C40 C41 C42 121.2(5) . . ? C41 C42 C37 119.9(5) . . ? C44 C43 C48 118.7(5) . . ? C44 C43 P3 123.7(4) . . ? C48 C43 P3 117.5(4) . . ? C45 C44 C43 119.9(5) . . ? C46 C45 C44 120.6(5) . . ? C45 C46 C47 120.6(5) . . ? C46 C47 C48 120.9(5) . . ? C47 C48 C43 119.2(5) . . ? C54 C49 C50 118.9(5) . . ? C54 C49 P3 122.8(4) . . ? C50 C49 P3 118.2(4) . . ? C51 C50 C49 119.7(7) . . ? C52 C51 C50 121.5(7) . . ? C51 C52 C53 119.2(7) . . ? C52 C53 C54 121.5(7) . . ? C49 C54 C53 119.2(6) . . ? N1 C55 C2 128.7(5) . . ? C59 C56 N1 108.1(4) . . ? C59 C56 C57 113.8(4) . . ? N1 C56 C57 113.0(4) . . ? C20 C57 N2 111.0(4) . . ? C20 C57 C56 118.3(4) . . ? N2 C57 C56 109.6(4) . . ? N2 C58 C38 130.0(5) . . ? C60 C59 C64 118.8(5) . . ? C60 C59 C56 122.5(5) . . ? C64 C59 C56 118.6(5) . . ? C59 C60 C61 121.2(5) . . ? C62 C61 C60 120.2(6) . . ? C63 C62 C61 119.2(5) . . ? C62 C63 C64 121.4(6) . . ? C59 C64 C63 119.1(6) . . ? _diffrn_measured_fraction_theta_max 0.754 _diffrn_reflns_theta_full 25.52 _diffrn_measured_fraction_theta_full 0.754 _refine_diff_density_max 0.794 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.108