# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2000 # CCDC Number: 440/158 data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common - _chemical_formula_moiety 'C27 H26 Cl2 N2 O P2 Pd' _chemical_formula_structural 'C27 H26 Cl2 N2 O P2 Pd' _chemical_formula_analytical 'C27 H26 Cl2 N2 O P2 Pd' _chemical_formula_sum 'C27 H26 Cl2 N2 O P2 Pd' _chemical_formula_weight 633.74 _chemical_melting_point - _chemical_compound_source - 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.90760(10) _cell_length_b 14.6999(2) _cell_length_c 19.0506(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.70 _cell_angle_gamma 90.00 _cell_volume 2716.94(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 57 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max .05 _exptl_crystal_size_mid .05 _exptl_crystal_size_min .1 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method - _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 1.021 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.864823 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 11787 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 23.27 _reflns_number_total 3916 _reflns_number_observed 3178 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.7524P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3866 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_obs 0.0263 _refine_ls_wR_factor_all 0.0690 _refine_ls_wR_factor_obs 0.0576 _refine_ls_goodness_of_fit_all 0.964 _refine_ls_goodness_of_fit_obs 0.985 _refine_ls_restrained_S_all 1.061 _refine_ls_restrained_S_obs 0.985 _refine_ls_shift/esd_max -0.003 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.15257(2) 0.672025(14) 0.295752(11) 0.02905(10) Uani 1 d . . Cl1 Cl 0.19327(9) 0.67203(5) 0.42152(4) 0.0459(2) Uani 1 d . . Cl2 Cl -0.08251(8) 0.70045(6) 0.28820(5) 0.0546(2) Uani 1 d . . P1 P 0.37538(8) 0.64966(5) 0.30634(4) 0.0302(2) Uani 1 d . . C1 C 0.4314(4) 0.5420(2) 0.3494(2) 0.0413(8) Uani 1 d . . C2 C 0.3388(4) 0.4705(2) 0.3351(2) 0.0514(9) Uani 1 d . . H2A H 0.2501(4) 0.4806(2) 0.3089(2) 0.062 Uiso 1 calc R . C3 C 0.3784(6) 0.3841(3) 0.3599(2) 0.0768(14) Uani 1 d . . H3A H 0.3166(6) 0.3360(3) 0.3499(2) 0.092 Uiso 1 calc R . C4 C 0.5089(7) 0.3693(3) 0.3993(2) 0.087(2) Uani 1 d . . H4A H 0.5353(7) 0.3111(3) 0.4157(2) 0.104 Uiso 1 calc R . C5 C 0.5993(6) 0.4394(4) 0.4142(3) 0.092(2) Uani 1 d . . H5A H 0.6872(6) 0.4289(4) 0.4411(3) 0.110 Uiso 1 calc R . C6 C 0.5616(4) 0.5266(3) 0.3895(2) 0.0734(12) Uani 1 d . . H6A H 0.6239(4) 0.5744(3) 0.4001(2) 0.088 Uiso 1 calc R . C7 C 0.4716(3) 0.7427(2) 0.3546(2) 0.0353(7) Uani 1 d . . C8 C 0.5132(3) 0.7428(2) 0.4284(2) 0.0487(9) Uani 1 d . . H8A H 0.4977(3) 0.6920(2) 0.4548(2) 0.058 Uiso 1 calc R . C9 C 0.5778(4) 0.8185(3) 0.4631(2) 0.0679(12) Uani 1 d . . H9A H 0.6047(4) 0.8187(3) 0.5127(2) 0.081 Uiso 1 calc R . C10 C 0.6024(4) 0.8934(3) 0.4246(2) 0.0728(12) Uani 1 d . . H10A H 0.6470(4) 0.9439(3) 0.4481(2) 0.087 Uiso 1 calc R . C11 C 0.5614(4) 0.8935(2) 0.3521(2) 0.0657(11) Uani 1 d . . H11A H 0.5780(4) 0.9445(2) 0.3262(2) 0.079 Uiso 1 calc R . C12 C 0.4956(4) 0.8195(2) 0.3162(2) 0.0481(8) Uani 1 d . . H12A H 0.4674(4) 0.8208(2) 0.2666(2) 0.058 Uiso 1 calc R . N1 N 0.4404(3) 0.6468(2) 0.23052(13) 0.0374(6) Uani 1 d . . C13 C 0.3789(3) 0.6419(2) 0.1588(2) 0.0335(7) Uani 1 d . . O13 O 0.4526(2) 0.6340(2) 0.11483(11) 0.0499(6) Uani 1 d . . N2 N 0.2382(3) 0.6444(2) 0.13469(12) 0.0344(6) Uani 1 d . . P2 P 0.10729(8) 0.66881(5) 0.17746(4) 0.0302(2) Uani 1 d . . C14 C -0.0128(3) 0.5777(2) 0.14656(15) 0.0323(7) Uani 1 d . . C15 C 0.0386(3) 0.4893(2) 0.1451(2) 0.0420(8) Uani 1 d . . H15A H 0.1333(3) 0.4794(2) 0.1555(2) 0.050 Uiso 1 calc R . C16 C -0.0505(4) 0.4166(2) 0.1281(2) 0.0513(9) Uani 1 d . . H16A H -0.0156(4) 0.3580(2) 0.1274(2) 0.062 Uiso 1 calc R . C17 C -0.1907(4) 0.4308(2) 0.1123(2) 0.0485(9) Uani 1 d . . H17A H -0.2503(4) 0.3817(2) 0.1010(2) 0.058 Uiso 1 calc R . C18 C -0.2427(4) 0.5170(2) 0.1132(2) 0.0482(9) Uani 1 d . . H18A H -0.3375(4) 0.5262(2) 0.1021(2) 0.058 Uiso 1 calc R . C19 C -0.1547(3) 0.5905(2) 0.1304(2) 0.0386(7) Uani 1 d . . H19A H -0.1908(3) 0.6488(2) 0.1312(2) 0.046 Uiso 1 calc R . C20 C 0.0400(3) 0.7765(2) 0.1390(2) 0.0414(8) Uani 1 d . . C21 C 0.0818(4) 0.8540(2) 0.1796(2) 0.0581(10) Uani 1 d . . H21A H 0.1354(4) 0.8485(2) 0.2256(2) 0.070 Uiso 1 calc R . C22 C 0.0434(5) 0.9392(3) 0.1515(3) 0.084(2) Uani 1 d . . H22A H 0.0713(5) 0.9911(3) 0.1785(3) 0.101 Uiso 1 calc R . C23 C -0.0351(6) 0.9468(3) 0.0844(4) 0.100(2) Uani 1 d . . H23A H -0.0607(6) 1.0042(3) 0.0658(4) 0.120 Uiso 1 calc R . C24 C -0.0771(5) 0.8710(4) 0.0437(3) 0.091(2) Uani 1 d . . H24A H -0.1300(5) 0.8773(4) -0.0023(3) 0.109 Uiso 1 calc R . C25 C -0.0407(4) 0.7850(3) 0.0710(2) 0.0625(10) Uani 1 d . . H25A H -0.0702(4) 0.7334(3) 0.0439(2) 0.075 Uiso 1 calc R . C26 C 0.5937(3) 0.6389(3) 0.2428(2) 0.0581(10) Uani 1 d . . H26A H 0.6319(3) 0.6428(3) 0.2932(2) 0.087 Uiso 1 calc R . H26B H 0.6298(3) 0.6873(3) 0.2182(2) 0.087 Uiso 1 calc R . H26C H 0.6181(3) 0.5815(3) 0.2248(2) 0.087 Uiso 1 calc R . C27 C 0.1971(4) 0.6371(2) 0.0554(2) 0.0505(9) Uani 1 d . . H27A H 0.0985(4) 0.6393(2) 0.0414(2) 0.076 Uiso 1 calc R . H27B H 0.2300(4) 0.5806(2) 0.0400(2) 0.076 Uiso 1 calc R . H27C H 0.2364(4) 0.6867(2) 0.0336(2) 0.076 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02532(15) 0.03248(15) 0.02969(14) -0.00591(10) 0.00637(9) -0.00356(10) Cl1 0.0550(5) 0.0514(5) 0.0328(4) -0.0045(4) 0.0126(4) -0.0075(4) Cl2 0.0281(5) 0.0755(6) 0.0609(6) -0.0244(5) 0.0111(4) -0.0043(4) P1 0.0280(4) 0.0316(4) 0.0298(4) -0.0017(3) 0.0028(3) -0.0013(3) C1 0.047(2) 0.035(2) 0.042(2) 0.0012(14) 0.009(2) 0.008(2) C2 0.059(2) 0.040(2) 0.060(2) 0.003(2) 0.022(2) 0.002(2) C3 0.117(4) 0.038(2) 0.088(3) 0.006(2) 0.052(3) 0.003(2) C4 0.143(5) 0.052(3) 0.079(3) 0.025(2) 0.053(4) 0.040(3) C5 0.100(4) 0.083(4) 0.086(3) 0.025(3) -0.001(3) 0.046(3) C6 0.067(3) 0.062(3) 0.079(3) 0.010(2) -0.014(2) 0.016(2) C7 0.027(2) 0.039(2) 0.039(2) -0.0019(14) 0.0043(14) -0.0017(13) C8 0.048(2) 0.057(2) 0.038(2) -0.004(2) 0.002(2) -0.016(2) C9 0.068(3) 0.081(3) 0.050(2) -0.018(2) -0.001(2) -0.024(2) C10 0.076(3) 0.060(3) 0.080(3) -0.022(2) 0.009(2) -0.030(2) C11 0.075(3) 0.043(2) 0.079(3) -0.002(2) 0.015(2) -0.022(2) C12 0.052(2) 0.046(2) 0.045(2) -0.004(2) 0.007(2) -0.012(2) N1 0.0253(14) 0.051(2) 0.0360(15) -0.0066(12) 0.0060(11) -0.0008(12) C13 0.036(2) 0.028(2) 0.038(2) 0.0013(13) 0.013(2) 0.0027(13) O13 0.0415(14) 0.071(2) 0.0433(13) -0.0009(11) 0.0218(12) 0.0070(12) N2 0.036(2) 0.0403(14) 0.0267(13) 0.0009(11) 0.0054(11) 0.0069(11) P2 0.0276(4) 0.0299(4) 0.0316(4) -0.0015(3) 0.0028(3) 0.0016(3) C14 0.032(2) 0.035(2) 0.026(2) -0.0003(12) -0.0009(13) -0.0003(13) C15 0.038(2) 0.034(2) 0.048(2) -0.0003(15) -0.0048(15) 0.0046(15) C16 0.077(3) 0.031(2) 0.044(2) 0.0009(15) 0.006(2) 0.000(2) C17 0.064(3) 0.047(2) 0.033(2) -0.010(2) 0.008(2) -0.021(2) C18 0.037(2) 0.064(2) 0.043(2) -0.010(2) 0.007(2) -0.010(2) C19 0.037(2) 0.040(2) 0.037(2) -0.0053(14) 0.0038(14) 0.0018(15) C20 0.038(2) 0.035(2) 0.053(2) 0.006(2) 0.014(2) 0.0058(15) C21 0.064(3) 0.035(2) 0.082(3) -0.001(2) 0.031(2) 0.005(2) C22 0.104(4) 0.034(2) 0.132(4) 0.007(3) 0.066(4) 0.011(2) C23 0.120(5) 0.058(3) 0.147(5) 0.053(4) 0.081(4) 0.048(3) C24 0.093(4) 0.090(4) 0.092(4) 0.049(3) 0.025(3) 0.048(3) C25 0.061(3) 0.059(2) 0.064(3) 0.020(2) 0.006(2) 0.023(2) C26 0.027(2) 0.091(3) 0.057(2) -0.012(2) 0.008(2) 0.001(2) C27 0.053(2) 0.071(2) 0.028(2) 0.002(2) 0.007(2) 0.013(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 P1 2.2003(8) . ? Pd1 P2 2.2072(8) . ? Pd1 Cl2 2.3418(9) . ? Pd1 Cl1 2.3476(8) . ? P1 N1 1.697(2) . ? P1 C7 1.808(3) . ? P1 C1 1.816(3) . ? C1 C2 1.386(5) . ? C1 C6 1.378(5) . ? C2 C3 1.384(5) . ? C3 C4 1.374(7) . ? C4 C5 1.357(7) . ? C5 C6 1.391(6) . ? C7 C8 1.383(4) . ? C7 C12 1.391(4) . ? C8 C9 1.383(5) . ? C9 C10 1.371(5) . ? C10 C11 1.359(5) . ? C11 C12 1.377(5) . ? N1 C13 1.380(4) . ? N1 C26 1.494(4) . ? C13 O13 1.224(3) . ? C13 N2 1.377(4) . ? N2 C27 1.486(4) . ? N2 P2 1.704(2) . ? P2 C14 1.809(3) . ? P2 C20 1.814(3) . ? C14 C19 1.390(4) . ? C14 C15 1.397(4) . ? C15 C16 1.382(4) . ? C16 C17 1.376(5) . ? C17 C18 1.369(5) . ? C18 C19 1.386(4) . ? C20 C25 1.383(5) . ? C20 C21 1.391(5) . ? C21 C22 1.386(5) . ? C22 C23 1.359(7) . ? C23 C24 1.374(7) . ? C24 C25 1.387(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 P2 94.76(3) . . ? P1 Pd1 Cl2 177.62(3) . . ? P2 Pd1 Cl2 86.98(3) . . ? P1 Pd1 Cl1 86.84(3) . . ? P2 Pd1 Cl1 177.82(3) . . ? Cl2 Pd1 Cl1 91.47(3) . . ? N1 P1 C7 101.51(13) . . ? N1 P1 C1 103.24(13) . . ? C7 P1 C1 110.34(14) . . ? N1 P1 Pd1 118.19(9) . . ? C7 P1 Pd1 110.47(10) . . ? C1 P1 Pd1 112.36(11) . . ? C2 C1 C6 119.5(3) . . ? C2 C1 P1 116.3(3) . . ? C6 C1 P1 124.0(3) . . ? C1 C2 C3 119.9(4) . . ? C4 C3 C2 120.2(4) . . ? C5 C4 C3 120.1(4) . . ? C4 C5 C6 120.6(5) . . ? C1 C6 C5 119.7(4) . . ? C8 C7 C12 119.1(3) . . ? C8 C7 P1 122.4(2) . . ? C12 C7 P1 118.4(2) . . ? C9 C8 C7 120.0(3) . . ? C10 C9 C8 120.4(4) . . ? C9 C10 C11 119.7(3) . . ? C10 C11 C12 121.1(4) . . ? C11 C12 C7 119.7(3) . . ? C13 N1 C26 112.4(2) . . ? C13 N1 P1 132.6(2) . . ? C26 N1 P1 114.7(2) . . ? O13 C13 N2 118.5(3) . . ? O13 C13 N1 118.6(3) . . ? N2 C13 N1 122.9(3) . . ? C13 N2 C27 112.8(2) . . ? C13 N2 P2 131.5(2) . . ? C27 N2 P2 115.0(2) . . ? N2 P2 C14 101.67(13) . . ? N2 P2 C20 104.14(13) . . ? C14 P2 C20 110.58(14) . . ? N2 P2 Pd1 118.41(9) . . ? C14 P2 Pd1 109.41(9) . . ? C20 P2 Pd1 112.04(11) . . ? C19 C14 C15 118.6(3) . . ? C19 C14 P2 122.7(2) . . ? C15 C14 P2 118.5(2) . . ? C16 C15 C14 120.3(3) . . ? C17 C16 C15 120.2(3) . . ? C18 C17 C16 120.2(3) . . ? C17 C18 C19 120.3(3) . . ? C14 C19 C18 120.4(3) . . ? C25 C20 C21 119.9(3) . . ? C25 C20 P2 123.5(3) . . ? C21 C20 P2 116.5(3) . . ? C20 C21 C22 119.8(4) . . ? C23 C22 C21 119.9(5) . . ? C22 C23 C24 120.9(4) . . ? C23 C24 C25 120.1(5) . . ? C24 C25 C20 119.4(4) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pd1 P1 N1 4.98(10) . . . . ? Cl2 Pd1 P1 N1 -131.8(8) . . . . ? Cl1 Pd1 P1 N1 -176.51(10) . . . . ? P2 Pd1 P1 C7 121.19(11) . . . . ? Cl2 Pd1 P1 C7 -15.6(8) . . . . ? Cl1 Pd1 P1 C7 -60.30(11) . . . . ? P2 Pd1 P1 C1 -115.12(11) . . . . ? Cl2 Pd1 P1 C1 108.1(8) . . . . ? Cl1 Pd1 P1 C1 63.39(11) . . . . ? N1 P1 C1 C2 -94.1(3) . . . . ? C7 P1 C1 C2 158.1(2) . . . . ? Pd1 P1 C1 C2 34.3(3) . . . . ? N1 P1 C1 C6 80.4(3) . . . . ? C7 P1 C1 C6 -27.4(4) . . . . ? Pd1 P1 C1 C6 -151.1(3) . . . . ? C6 C1 C2 C3 -1.3(5) . . . . ? P1 C1 C2 C3 173.6(3) . . . . ? C1 C2 C3 C4 0.6(6) . . . . ? C2 C3 C4 C5 0.2(7) . . . . ? C3 C4 C5 C6 -0.4(7) . . . . ? C2 C1 C6 C5 1.1(6) . . . . ? P1 C1 C6 C5 -173.3(3) . . . . ? C4 C5 C6 C1 -0.2(7) . . . . ? N1 P1 C7 C8 -144.4(3) . . . . ? C1 P1 C7 C8 -35.4(3) . . . . ? Pd1 P1 C7 C8 89.4(3) . . . . ? N1 P1 C7 C12 40.4(3) . . . . ? C1 P1 C7 C12 149.4(3) . . . . ? Pd1 P1 C7 C12 -85.8(3) . . . . ? C12 C7 C8 C9 -0.1(5) . . . . ? P1 C7 C8 C9 -175.3(3) . . . . ? C7 C8 C9 C10 -0.7(6) . . . . ? C8 C9 C10 C11 0.9(7) . . . . ? C9 C10 C11 C12 -0.2(7) . . . . ? C10 C11 C12 C7 -0.6(6) . . . . ? C8 C7 C12 C11 0.7(5) . . . . ? P1 C7 C12 C11 176.1(3) . . . . ? C7 P1 N1 C13 -132.7(3) . . . . ? C1 P1 N1 C13 113.0(3) . . . . ? Pd1 P1 N1 C13 -11.8(3) . . . . ? C7 P1 N1 C26 54.3(3) . . . . ? C1 P1 N1 C26 -60.0(3) . . . . ? Pd1 P1 N1 C26 175.3(2) . . . . ? C26 N1 C13 O13 -1.5(4) . . . . ? P1 N1 C13 O13 -174.6(2) . . . . ? C26 N1 C13 N2 177.7(3) . . . . ? P1 N1 C13 N2 4.6(4) . . . . ? O13 C13 N2 C27 -0.3(4) . . . . ? N1 C13 N2 C27 -179.4(3) . . . . ? O13 C13 N2 P2 -170.4(2) . . . . ? N1 C13 N2 P2 10.4(4) . . . . ? C13 N2 P2 C14 -134.0(3) . . . . ? C27 N2 P2 C14 56.0(2) . . . . ? C13 N2 P2 C20 111.0(3) . . . . ? C27 N2 P2 C20 -59.0(2) . . . . ? C13 N2 P2 Pd1 -14.2(3) . . . . ? C27 N2 P2 Pd1 175.9(2) . . . . ? P1 Pd1 P2 N2 4.46(10) . . . . ? Cl2 Pd1 P2 N2 -177.17(10) . . . . ? Cl1 Pd1 P2 N2 -132.6(8) . . . . ? P1 Pd1 P2 C14 120.22(10) . . . . ? Cl2 Pd1 P2 C14 -61.42(11) . . . . ? Cl1 Pd1 P2 C14 -16.8(8) . . . . ? P1 Pd1 P2 C20 -116.78(12) . . . . ? Cl2 Pd1 P2 C20 61.59(12) . . . . ? Cl1 Pd1 P2 C20 106.2(8) . . . . ? N2 P2 C14 C19 -141.8(2) . . . . ? C20 P2 C14 C19 -31.7(3) . . . . ? Pd1 P2 C14 C19 92.2(2) . . . . ? N2 P2 C14 C15 44.1(3) . . . . ? C20 P2 C14 C15 154.3(2) . . . . ? Pd1 P2 C14 C15 -81.9(2) . . . . ? C19 C14 C15 C16 -0.2(4) . . . . ? P2 C14 C15 C16 174.1(2) . . . . ? C14 C15 C16 C17 0.3(5) . . . . ? C15 C16 C17 C18 0.1(5) . . . . ? C16 C17 C18 C19 -0.4(5) . . . . ? C15 C14 C19 C18 -0.1(4) . . . . ? P2 C14 C19 C18 -174.2(2) . . . . ? C17 C18 C19 C14 0.4(5) . . . . ? N2 P2 C20 C25 74.8(3) . . . . ? C14 P2 C20 C25 -33.7(4) . . . . ? Pd1 P2 C20 C25 -156.1(3) . . . . ? N2 P2 C20 C21 -100.6(3) . . . . ? C14 P2 C20 C21 150.9(2) . . . . ? Pd1 P2 C20 C21 28.6(3) . . . . ? C25 C20 C21 C22 -0.6(5) . . . . ? P2 C20 C21 C22 175.0(3) . . . . ? C20 C21 C22 C23 0.1(6) . . . . ? C21 C22 C23 C24 -0.1(7) . . . . ? C22 C23 C24 C25 0.6(7) . . . . ? C23 C24 C25 C20 -1.1(6) . . . . ? C21 C20 C25 C24 1.0(6) . . . . ? P2 C20 C25 C24 -174.2(3) . . . . ? _refine_diff_density_max 0.380 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.054 #---end data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common - _chemical_formula_moiety 'C18 H23 Cl5 N2 O P Pt S2' _chemical_formula_structural 'C18 H23 Cl5 N2 O P Pt S2' _chemical_formula_analytical 'C18 H23 Cl5 N2 O P Pt S2' _chemical_formula_sum 'C18 H23 Cl5 N2 O P Pt S2' _chemical_formula_weight 750.81 _chemical_melting_point - _chemical_compound_source - loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'Pt' 'Pt' -1.7033 8.3905 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4044(5) _cell_length_b 11.5628(5) _cell_length_c 11.9275(5) _cell_angle_alpha 69.23 _cell_angle_beta 71.9290(10) _cell_angle_gamma 74.8710(10) _cell_volume 1377.76(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 83 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max .16 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .06 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.810 _exptl_crystal_density_method - _exptl_crystal_F_000 726 _exptl_absorpt_coefficient_mu 5.800 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.386898 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 5986 _diffrn_reflns_av_R_equivalents 0.1137 _diffrn_reflns_av_sigmaI/netI 0.2434 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 23.15 _reflns_number_total 3885 _reflns_number_observed 2231 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 56 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0587P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3829 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1161 _refine_ls_R_factor_obs 0.0503 _refine_ls_wR_factor_all 0.3141 _refine_ls_wR_factor_obs 0.1149 _refine_ls_goodness_of_fit_all 0.622 _refine_ls_goodness_of_fit_obs 0.654 _refine_ls_restrained_S_all 1.330 _refine_ls_restrained_S_obs 0.654 _refine_ls_shift/esd_max -0.237 _refine_ls_shift/esd_mean 0.008 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.04633(5) 0.08026(5) 0.26501(5) 0.0376(3) Uani 1 d . . Cl1 Cl 0.1880(4) 0.2044(3) 0.1140(4) 0.0620(11) Uani 1 d . . Cl2 Cl -0.1110(4) 0.2613(3) 0.2746(3) 0.0526(10) Uani 1 d . . P1 P 0.1858(3) -0.0908(3) 0.2671(3) 0.0337(9) Uani 1 d . . C1 C 0.3306(13) -0.0942(11) 0.3001(12) 0.038(3) Uani 1 d . . C2 C 0.3440(15) -0.1275(13) 0.4214(13) 0.048(4) Uani 1 d . . H2A H 0.2792(15) -0.1572(13) 0.4876(13) 0.057 Uiso 1 calc R . C3 C 0.4484(17) -0.1171(16) 0.4432(17) 0.063(5) Uani 1 d . . H3A H 0.4547(17) -0.1386(16) 0.5243(17) 0.076 Uiso 1 calc R . C4 C 0.5481(19) -0.0745(18) 0.3460(22) 0.083(6) Uani 1 d . . H4A H 0.6207(19) -0.0683(18) 0.3620(22) 0.099 Uiso 1 calc R . C5 C 0.5378(17) -0.0412(18) 0.2241(20) 0.085(6) Uani 1 d . . H5A H 0.6040(17) -0.0147(18) 0.1581(20) 0.102 Uiso 1 calc R . C6 C 0.4294(15) -0.0482(16) 0.2039(15) 0.064(5) Uani 1 d . . H6A H 0.4207(15) -0.0215(16) 0.1232(15) 0.077 Uiso 1 calc R . C7 C 0.2299(13) -0.1384(13) 0.1283(12) 0.041(4) Uani 1 d . . C8 C 0.3309(15) -0.2303(14) 0.1060(13) 0.058(5) Uani 1 d . . H8A H 0.3831(15) -0.2651(14) 0.1603(13) 0.069 Uiso 1 calc R . C9 C 0.3562(17) -0.2721(15) 0.0024(16) 0.071(5) Uani 1 d . . H9A H 0.4211(17) -0.3381(15) -0.0091(16) 0.085 Uiso 1 calc R . C10 C 0.2829(15) -0.2135(17) -0.0824(15) 0.066(5) Uani 1 d . . H10A H 0.3011(15) -0.2378(17) -0.1532(15) 0.079 Uiso 1 calc R . C11 C 0.1859(15) -0.1221(16) -0.0630(14) 0.055(4) Uani 1 d . . H11A H 0.1356(15) -0.0856(16) -0.1189(14) 0.066 Uiso 1 calc R . C12 C 0.1598(13) -0.0811(14) 0.0410(12) 0.045(4) Uani 1 d . . H12A H 0.0949(13) -0.0149(14) 0.0513(12) 0.054 Uiso 1 calc R . N1 N 0.1192(10) -0.2121(9) 0.3855(9) 0.034(3) Uani 1 d . . C13 C -0.0024(13) -0.1901(13) 0.4403(12) 0.040(4) Uani 1 d . . S13 S -0.0916(3) -0.0410(3) 0.4051(3) 0.0400(9) Uani 1 d . . N2 N -0.0560(10) -0.2853(11) 0.5258(10) 0.044(3) Uani 1 d . . C14 C 0.1921(14) -0.3418(13) 0.4158(14) 0.058(4) Uani 1 d . . H14A H 0.2773(14) -0.3410(13) 0.3689(14) 0.087 Uiso 1 calc R . H14B H 0.1562(14) -0.3961(13) 0.3956(14) 0.087 Uiso 1 calc R . H14C H 0.1896(14) -0.3719(13) 0.5024(14) 0.087 Uiso 1 calc R . C15 C -0.1912(13) -0.2715(15) 0.5918(15) 0.063(5) Uani 1 d . . H15A H -0.2095(13) -0.3510(15) 0.6490(15) 0.094 Uiso 1 calc R . H15B H -0.2417(13) -0.2432(15) 0.5329(15) 0.094 Uiso 1 calc R . H15C H -0.2094(13) -0.2113(15) 0.6360(15) 0.094 Uiso 1 calc R . C20 C -0.3889(16) 0.4886(16) 0.2593(16) 0.080(6) Uani 1 d . . H20A H -0.3211(16) 0.4218(16) 0.2856(16) 0.095 Uiso 1 calc R . Cl3 Cl -0.5177(5) 0.4215(5) 0.2831(6) 0.117(2) Uani 1 d . . Cl4 Cl -0.4261(5) 0.5947(6) 0.3466(6) 0.112(2) Uani 1 d . . Cl5 Cl -0.3367(5) 0.5690(5) 0.1021(5) 0.100(2) Uani 1 d . . S30 S -0.0777(4) 0.5749(4) 0.2430(4) 0.0615(12) Uani 1 d . . O30 O -0.0164(11) 0.5367(10) 0.3502(9) 0.069(3) Uani 1 d . . C31 C 0.0443(19) 0.5629(18) 0.1097(16) 0.093(7) Uani 1 d . . H31A H 0.0778(19) 0.4761(18) 0.1167(16) 0.140 Uiso 1 calc R . H31B H 0.1094(19) 0.6052(18) 0.1030(16) 0.140 Uiso 1 calc R . H31C H 0.0115(19) 0.6010(18) 0.0374(16) 0.140 Uiso 1 calc R . C32 C -0.1209(15) 0.7437(12) 0.2047(19) 0.078(6) Uani 1 d . . H32A H -0.1877(15) 0.7655(12) 0.2700(19) 0.117 Uiso 1 calc R . H32B H -0.1480(15) 0.7757(12) 0.1291(19) 0.117 Uiso 1 calc R . H32C H -0.0499(15) 0.7796(12) 0.1947(19) 0.117 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0493(4) 0.0386(4) 0.0208(3) -0.0101(2) -0.0094(2) 0.0022(2) Cl1 0.072(3) 0.043(2) 0.055(3) 0.000(2) -0.005(2) -0.016(2) Cl2 0.063(3) 0.038(2) 0.054(2) -0.017(2) -0.020(2) 0.008(2) P1 0.037(2) 0.037(2) 0.025(2) -0.009(2) -0.007(2) -0.004(2) C1 0.053(9) 0.023(7) 0.037(8) -0.010(6) -0.013(7) -0.003(7) C2 0.058(10) 0.053(10) 0.036(9) -0.022(7) -0.017(8) 0.004(8) C3 0.066(12) 0.079(13) 0.066(12) -0.038(10) -0.039(11) 0.006(10) C4 0.069(14) 0.084(15) 0.116(19) -0.047(13) -0.049(15) 0.009(12) C5 0.047(11) 0.104(17) 0.101(17) -0.022(13) -0.016(11) -0.023(11) C6 0.060(11) 0.082(13) 0.045(10) 0.001(9) -0.014(9) -0.026(10) C7 0.045(9) 0.044(9) 0.027(8) -0.010(6) -0.012(7) 0.006(7) C8 0.064(11) 0.068(11) 0.038(9) -0.024(8) -0.021(8) 0.015(9) C9 0.087(13) 0.065(12) 0.067(12) -0.046(10) -0.029(11) 0.026(10) C10 0.064(11) 0.092(14) 0.051(11) -0.043(10) -0.006(9) -0.005(11) C11 0.055(11) 0.080(12) 0.040(9) -0.025(8) -0.012(8) -0.017(10) C12 0.032(8) 0.067(10) 0.041(9) -0.028(8) -0.011(7) 0.004(7) N1 0.035(7) 0.028(6) 0.034(7) -0.006(5) -0.005(5) -0.004(5) C13 0.041(9) 0.045(9) 0.027(8) -0.008(7) -0.015(7) 0.008(7) S13 0.038(2) 0.037(2) 0.039(2) -0.013(2) -0.006(2) -0.001(2) N2 0.050(7) 0.053(8) 0.030(7) -0.009(6) -0.009(6) -0.016(6) C14 0.059(10) 0.045(10) 0.052(10) -0.003(7) -0.010(8) 0.002(8) C15 0.048(10) 0.067(11) 0.058(11) -0.002(8) -0.002(9) -0.021(9) C20 0.064(12) 0.072(13) 0.066(13) -0.007(10) -0.005(10) 0.016(10) Cl3 0.092(4) 0.089(4) 0.141(6) -0.028(4) 0.013(4) -0.026(3) Cl4 0.090(4) 0.143(5) 0.102(5) -0.066(4) -0.001(3) -0.004(4) Cl5 0.086(4) 0.122(5) 0.058(3) -0.002(3) 0.000(3) -0.017(3) S30 0.073(3) 0.054(3) 0.055(3) -0.011(2) -0.016(2) -0.011(2) O30 0.101(9) 0.066(7) 0.043(7) -0.001(5) -0.033(6) -0.020(7) C31 0.112(16) 0.099(15) 0.047(12) -0.033(10) -0.006(11) 0.017(13) C32 0.069(11) 0.009(8) 0.169(19) 0.005(9) -0.075(12) -0.017(8) _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 Pt1 P1 2.188(3) . ? Pt1 S13 2.256(4) . ? Pt1 Cl1 2.342(4) . ? Pt1 Cl2 2.387(3) . ? P1 N1 1.739(10) . ? P1 C1 1.801(14) . ? P1 C7 1.811(14) . ? C1 C6 1.39(2) . ? C1 C2 1.41(2) . ? C2 C3 1.34(2) . ? C3 C4 1.40(2) . ? C4 C5 1.40(3) . ? C5 C6 1.36(2) . ? C7 C8 1.38(2) . ? C7 C12 1.38(2) . ? C8 C9 1.40(2) . ? C9 C10 1.39(2) . ? C10 C11 1.34(2) . ? C11 C12 1.40(2) . ? N1 C13 1.34(2) . ? N1 C14 1.49(2) . ? C13 N2 1.34(2) . ? C13 S13 1.737(13) . ? N2 C15 1.49(2) . ? C20 Cl3 1.74(2) . ? C20 Cl5 1.76(2) . ? C20 Cl4 1.77(2) . ? S30 O30 1.520(10) . ? S30 C31 1.78(2) . ? S30 C32 1.807(13) . ? 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 P1 Pt1 S13 88.02(13) . . ? P1 Pt1 Cl1 91.71(14) . . ? S13 Pt1 Cl1 177.98(15) . . ? P1 Pt1 Cl2 176.78(13) . . ? S13 Pt1 Cl2 89.23(13) . . ? Cl1 Pt1 Cl2 91.10(14) . . ? N1 P1 C1 105.3(5) . . ? N1 P1 C7 105.9(6) . . ? C1 P1 C7 105.7(6) . . ? N1 P1 Pt1 106.8(4) . . ? C1 P1 Pt1 116.8(4) . . ? C7 P1 Pt1 115.4(4) . . ? C6 C1 C2 117.4(14) . . ? C6 C1 P1 119.7(11) . . ? C2 C1 P1 122.4(11) . . ? C3 C2 C1 121.0(15) . . ? C2 C3 C4 120.9(16) . . ? C3 C4 C5 119.3(18) . . ? C6 C5 C4 118.8(18) . . ? C5 C6 C1 122.3(15) . . ? C8 C7 C12 118.2(13) . . ? C8 C7 P1 122.6(10) . . ? C12 C7 P1 119.2(10) . . ? C7 C8 C9 121.0(14) . . ? C10 C9 C8 119.0(15) . . ? C11 C10 C9 120.5(15) . . ? C10 C11 C12 120.6(15) . . ? C7 C12 C11 120.6(14) . . ? C13 N1 C14 120.2(11) . . ? C13 N1 P1 118.7(8) . . ? C14 N1 P1 120.7(9) . . ? N2 C13 N1 118.9(11) . . ? N2 C13 S13 119.3(10) . . ? N1 C13 S13 121.7(10) . . ? C13 S13 Pt1 104.0(5) . . ? C13 N2 C15 123.4(12) . . ? Cl3 C20 Cl5 110.9(11) . . ? Cl3 C20 Cl4 110.8(10) . . ? Cl5 C20 Cl4 109.0(10) . . ? O30 S30 C31 107.0(8) . . ? O30 S30 C32 105.1(7) . . ? C31 S30 C32 99.6(9) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S13 Pt1 P1 N1 -7.8(4) . . . . ? Cl1 Pt1 P1 N1 174.2(4) . . . . ? Cl2 Pt1 P1 N1 23.4(26) . . . . ? S13 Pt1 P1 C1 -125.2(5) . . . . ? Cl1 Pt1 P1 C1 56.8(5) . . . . ? Cl2 Pt1 P1 C1 -94.0(25) . . . . ? S13 Pt1 P1 C7 109.6(5) . . . . ? Cl1 Pt1 P1 C7 -68.4(5) . . . . ? Cl2 Pt1 P1 C7 140.8(24) . . . . ? N1 P1 C1 C6 153.6(13) . . . . ? C7 P1 C1 C6 41.8(14) . . . . ? Pt1 P1 C1 C6 -88.1(13) . . . . ? N1 P1 C1 C2 -34.3(12) . . . . ? C7 P1 C1 C2 -146.1(11) . . . . ? Pt1 P1 C1 C2 84.0(11) . . . . ? C6 C1 C2 C3 -1.0(22) . . . . ? P1 C1 C2 C3 -173.2(12) . . . . ? C1 C2 C3 C4 -0.9(25) . . . . ? C2 C3 C4 C5 0.6(29) . . . . ? C3 C4 C5 C6 1.7(30) . . . . ? C4 C5 C6 C1 -3.7(30) . . . . ? C2 C1 C6 C5 3.3(25) . . . . ? P1 C1 C6 C5 175.8(15) . . . . ? N1 P1 C7 C8 -73.6(14) . . . . ? C1 P1 C7 C8 37.8(14) . . . . ? Pt1 P1 C7 C8 168.5(11) . . . . ? N1 P1 C7 C12 106.2(12) . . . . ? C1 P1 C7 C12 -142.4(12) . . . . ? Pt1 P1 C7 C12 -11.7(14) . . . . ? C12 C7 C8 C9 -5.1(24) . . . . ? P1 C7 C8 C9 174.7(13) . . . . ? C7 C8 C9 C10 4.4(28) . . . . ? C8 C9 C10 C11 -2.9(28) . . . . ? C9 C10 C11 C12 2.3(26) . . . . ? C8 C7 C12 C11 4.5(22) . . . . ? P1 C7 C12 C11 -175.3(12) . . . . ? C10 C11 C12 C7 -3.1(24) . . . . ? C1 P1 N1 C13 134.2(11) . . . . ? C7 P1 N1 C13 -114.1(11) . . . . ? Pt1 P1 N1 C13 9.4(11) . . . . ? C1 P1 N1 C14 -52.6(11) . . . . ? C7 P1 N1 C14 59.1(11) . . . . ? Pt1 P1 N1 C14 -177.3(9) . . . . ? C14 N1 C13 N2 2.4(20) . . . . ? P1 N1 C13 N2 175.6(9) . . . . ? C14 N1 C13 S13 -178.5(10) . . . . ? P1 N1 C13 S13 -5.3(16) . . . . ? N2 C13 S13 Pt1 177.6(10) . . . . ? N1 C13 S13 Pt1 -1.6(12) . . . . ? P1 Pt1 S13 C13 5.6(5) . . . . ? Cl1 Pt1 S13 C13 88.0(39) . . . . ? Cl2 Pt1 S13 C13 -172.8(5) . . . . ? N1 C13 N2 C15 -179.3(13) . . . . ? S13 C13 N2 C15 1.6(19) . . . . ? _refine_diff_density_max 2.564 _refine_diff_density_min -4.492 _refine_diff_density_rms 0.347 #---end data_3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common - _chemical_formula_moiety 'C56 H58 Cl4 N4 O5 P4 Pd2' _chemical_formula_structural 'C56 H58 Cl4 N4 O5 P4 Pd2' _chemical_formula_analytical 'C56 H58 Cl4 N4 O5 P4 Pd2' _chemical_formula_sum 'C56 H58 Cl4 N4 O5 P4 Pd2' _chemical_formula_weight 1345.54 _chemical_melting_point - _chemical_compound_source - 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 11.6946(3) _cell_length_b 15.4866(4) _cell_length_c 18.5407(3) _cell_angle_alpha 76.1840(10) _cell_angle_beta 71.8340(10) _cell_angle_gamma 72.8060(10) _cell_volume 3007.91(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .06 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .2 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method - _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 0.930 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.773652 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time ? _diffrn_standards_decay_% - _diffrn_reflns_number 14316 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 23.25 _reflns_number_total 8562 _reflns_number_observed 6340 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+2.8900P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0007(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8512 _refine_ls_number_parameters 668 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_obs 0.0430 _refine_ls_wR_factor_all 0.1503 _refine_ls_wR_factor_obs 0.1130 _refine_ls_goodness_of_fit_all 1.022 _refine_ls_goodness_of_fit_obs 1.072 _refine_ls_restrained_S_all 1.221 _refine_ls_restrained_S_obs 1.072 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.15944(4) 0.13502(3) 0.26937(2) 0.03054(14) Uani 1 d . . P1 P 0.20325(14) 0.26876(9) 0.25176(8) 0.0356(3) Uani 1 d . . C1 C 0.2871(6) 0.2863(4) 0.3130(3) 0.0413(14) Uani 1 d . . C2 C 0.4128(6) 0.2823(4) 0.2901(4) 0.056(2) Uani 1 d . . H2A H 0.4594(6) 0.2709(4) 0.2411(4) 0.067 Uiso 1 calc R . C3 C 0.4684(8) 0.2958(5) 0.3421(6) 0.084(3) Uani 1 d . . H3A H 0.5531(8) 0.2922(5) 0.3275(6) 0.101 Uiso 1 calc R . C4 C 0.4004(10) 0.3141(6) 0.4140(6) 0.087(3) Uani 1 d . . H4A H 0.4383(10) 0.3249(6) 0.4472(6) 0.105 Uiso 1 calc R . C5 C 0.2780(10) 0.3165(5) 0.4365(5) 0.083(3) Uani 1 d . . H5A H 0.2324(10) 0.3278(5) 0.4857(5) 0.100 Uiso 1 calc R . C6 C 0.2199(7) 0.3024(4) 0.3875(4) 0.058(2) Uani 1 d . . H6A H 0.1358(7) 0.3037(4) 0.4040(4) 0.069 Uiso 1 calc R . C7 C 0.2712(6) 0.3160(4) 0.1539(3) 0.0424(14) Uani 1 d . . C8 C 0.2415(6) 0.2904(5) 0.0960(4) 0.055(2) Uani 1 d . . H8A H 0.1931(6) 0.2483(5) 0.1080(4) 0.066 Uiso 1 calc R . C9 C 0.2861(8) 0.3294(6) 0.0194(4) 0.079(2) Uani 1 d . . H9A H 0.2670(8) 0.3126(6) -0.0196(4) 0.095 Uiso 1 calc R . C10 C 0.3559(8) 0.3904(6) 0.0012(5) 0.080(2) Uani 1 d . . H10A H 0.3854(8) 0.4148(6) -0.0500(5) 0.096 Uiso 1 calc R . C11 C 0.3831(9) 0.4164(6) 0.0574(5) 0.090(3) Uani 1 d . . H11A H 0.4309(9) 0.4590(6) 0.0445(5) 0.107 Uiso 1 calc R . C12 C 0.3404(7) 0.3801(4) 0.1340(4) 0.067(2) Uani 1 d . . H12A H 0.3586(7) 0.3992(4) 0.1721(4) 0.080 Uiso 1 calc R . N1 N 0.0629(4) 0.3390(3) 0.2768(3) 0.0438(12) Uani 1 d . . C13 C -0.0443(5) 0.3028(4) 0.3017(3) 0.0387(13) Uani 1 d . . O13 O -0.1463(4) 0.3558(3) 0.3217(2) 0.0557(11) Uani 1 d . . N2 N -0.0211(4) 0.2140(3) 0.3010(3) 0.0383(11) Uani 1 d . . C26 C 0.0479(6) 0.4382(4) 0.2664(4) 0.061(2) Uani 1 d . . H26A H 0.1280(6) 0.4517(4) 0.2496(4) 0.092 Uiso 1 calc R . H26B H 0.0033(6) 0.4595(4) 0.3144(4) 0.092 Uiso 1 calc R . H26C H 0.0025(6) 0.4683(4) 0.2285(4) 0.092 Uiso 1 calc R . C27 C -0.1281(5) 0.1746(4) 0.3293(4) 0.056(2) Uani 1 d . . H27A H -0.1020(5) 0.1104(4) 0.3265(4) 0.083 Uiso 1 calc R . H27B H -0.1854(5) 0.2043(4) 0.2984(4) 0.083 Uiso 1 calc R . H27C H -0.1676(5) 0.1831(4) 0.3817(4) 0.083 Uiso 1 calc R . P2 P 0.35328(13) 0.04209(9) 0.24006(9) 0.0359(4) Uani 1 d . . C14 C 0.4853(5) 0.0919(4) 0.1856(4) 0.048(2) Uani 1 d . . C15 C 0.4925(6) 0.1258(4) 0.1073(5) 0.065(2) Uani 1 d . . H15A H 0.4314(6) 0.1226(4) 0.0864(5) 0.077 Uiso 1 calc R . C16 C 0.5892(8) 0.1638(5) 0.0610(6) 0.089(3) Uani 1 d . . H16A H 0.5916(8) 0.1880(5) 0.0097(6) 0.106 Uiso 1 calc R . C17 C 0.6811(9) 0.1658(6) 0.0906(8) 0.104(4) Uani 1 d . . H17A H 0.7470(9) 0.1903(6) 0.0591(8) 0.125 Uiso 1 calc R . C18 C 0.6773(7) 0.1325(6) 0.1652(8) 0.094(3) Uani 1 d . . H18A H 0.7404(7) 0.1347(6) 0.1847(8) 0.112 Uiso 1 calc R . C19 C 0.5782(6) 0.0939(5) 0.2146(5) 0.073(2) Uani 1 d . . H19A H 0.5768(6) 0.0704(5) 0.2658(5) 0.088 Uiso 1 calc R . C20 C 0.3815(5) -0.0144(4) 0.3328(4) 0.0438(14) Uani 1 d . . C21 C 0.3659(7) 0.0381(5) 0.3881(4) 0.069(2) Uani 1 d . . H21A H 0.3459(7) 0.1017(5) 0.3765(4) 0.083 Uiso 1 calc R . C22 C 0.3802(8) -0.0048(6) 0.4607(5) 0.089(3) Uani 1 d . . H22A H 0.3705(8) 0.0304(6) 0.4974(5) 0.107 Uiso 1 calc R . C23 C 0.4084(7) -0.0984(6) 0.4789(5) 0.076(2) Uani 1 d . . H23A H 0.4150(7) -0.1263(6) 0.5282(5) 0.091 Uiso 1 calc R . C24 C 0.4271(6) -0.1511(5) 0.4244(4) 0.064(2) Uani 1 d . . H24A H 0.4487(6) -0.2147(5) 0.4361(4) 0.076 Uiso 1 calc R . C25 C 0.4134(5) -0.1089(4) 0.3521(4) 0.051(2) Uani 1 d . . H25A H 0.4260(5) -0.1449(4) 0.3154(4) 0.061 Uiso 1 calc R . O2 O 0.3665(3) -0.0293(2) 0.1912(2) 0.0410(9) Uani 1 d . . Pd2 Pd 0.30108(4) -0.14583(3) 0.21055(2) 0.03122(15) Uani 1 d . . P31 P 0.25172(13) -0.27864(9) 0.23949(8) 0.0341(3) Uani 1 d . . C31 C 0.1602(6) -0.3069(3) 0.1899(3) 0.0410(14) Uani 1 d . . C32 C 0.2172(7) -0.3294(5) 0.1156(4) 0.057(2) Uani 1 d . . H32A H 0.3002(7) -0.3291(5) 0.0931(4) 0.068 Uiso 1 calc R . C33 C 0.1510(9) -0.3519(5) 0.0764(4) 0.074(2) Uani 1 d . . H33A H 0.1895(9) -0.3662(5) 0.0272(4) 0.089 Uiso 1 calc R . C34 C 0.0300(8) -0.3535(5) 0.1083(5) 0.069(2) Uani 1 d . . H34A H -0.0129(8) -0.3706(5) 0.0816(5) 0.082 Uiso 1 calc R . C35 C -0.0288(7) -0.3299(4) 0.1795(5) 0.062(2) Uani 1 d . . H35A H -0.1124(7) -0.3290(4) 0.2005(5) 0.075 Uiso 1 calc R . C36 C 0.0361(6) -0.3074(4) 0.2207(4) 0.050(2) Uani 1 d . . H36A H -0.0042(6) -0.2925(4) 0.2695(4) 0.060 Uiso 1 calc R . C37 C 0.1893(5) -0.3133(4) 0.3414(3) 0.0396(14) Uani 1 d . . C38 C 0.1982(6) -0.2660(5) 0.3933(4) 0.056(2) Uani 1 d . . H38A H 0.2226(6) -0.2110(5) 0.3752(4) 0.067 Uiso 1 calc R . C39 C 0.1718(7) -0.2984(6) 0.4715(4) 0.068(2) Uani 1 d . . H39A H 0.1795(7) -0.2655(6) 0.5049(4) 0.082 Uiso 1 calc R . C40 C 0.1354(8) -0.3766(7) 0.4996(4) 0.082(2) Uani 1 d . . H40A H 0.1195(8) -0.3984(7) 0.5522(4) 0.098 Uiso 1 calc R . C41 C 0.1214(8) -0.4253(6) 0.4504(5) 0.089(3) Uani 1 d . . H41A H 0.0933(8) -0.4786(6) 0.4701(5) 0.107 Uiso 1 calc R . C42 C 0.1494(7) -0.3941(4) 0.3710(4) 0.068(2) Uani 1 d . . H42A H 0.1414(7) -0.4273(4) 0.3379(4) 0.081 Uiso 1 calc R . N31 N 0.3904(4) -0.3518(3) 0.2163(3) 0.0418(12) Uani 1 d . . C43 C 0.4989(5) -0.3188(4) 0.1949(3) 0.0417(14) Uani 1 d . . O43 O 0.6011(4) -0.3745(3) 0.1840(3) 0.0554(11) Uani 1 d . . N32 N 0.4779(4) -0.2284(3) 0.1868(3) 0.0441(12) Uani 1 d . . C56 C 0.4041(6) -0.4513(4) 0.2318(4) 0.063(2) Uani 1 d . . H56A H 0.3239(6) -0.4642(4) 0.2457(4) 0.095 Uiso 1 calc R . H56B H 0.4428(6) -0.4779(4) 0.2733(4) 0.095 Uiso 1 calc R . H56C H 0.4547(6) -0.4769(4) 0.1866(4) 0.095 Uiso 1 calc R . C57 C 0.5885(6) -0.1924(5) 0.1617(5) 0.081(3) Uani 1 d . . H57A H 0.5646(6) -0.1269(5) 0.1574(5) 0.121 Uiso 1 calc R . H57B H 0.6370(6) -0.2091(5) 0.1125(5) 0.121 Uiso 1 calc R . H57C H 0.6368(6) -0.2176(5) 0.1986(5) 0.121 Uiso 1 calc R . P32 P 0.11405(12) -0.04502(9) 0.22890(8) 0.0305(3) Uani 1 d . . C44 C -0.0272(5) -0.0846(4) 0.2602(4) 0.0388(14) Uani 1 d . . C45 C -0.0915(6) -0.0851(4) 0.2084(4) 0.060(2) Uani 1 d . . H45A H -0.0605(6) -0.0663(4) 0.1560(4) 0.072 Uiso 1 calc R . C46 C -0.2010(8) -0.1133(5) 0.2344(7) 0.092(3) Uani 1 d . . H46A H -0.2441(8) -0.1127(5) 0.1997(7) 0.110 Uiso 1 calc R . C47 C -0.2455(7) -0.1419(6) 0.3103(8) 0.090(3) Uani 1 d . . H47A H -0.3186(7) -0.1616(6) 0.3270(8) 0.109 Uiso 1 calc R . C48 C -0.1851(8) -0.1424(5) 0.3635(5) 0.084(3) Uani 1 d . . H48A H -0.2173(8) -0.1614(5) 0.4156(5) 0.101 Uiso 1 calc R . C49 C -0.0712(6) -0.1129(5) 0.3367(4) 0.060(2) Uani 1 d . . H49A H -0.0281(6) -0.1132(5) 0.3713(4) 0.072 Uiso 1 calc R . C50 C 0.1075(5) 0.0246(4) 0.1354(3) 0.0369(13) Uani 1 d . . C51 C 0.1738(8) -0.0098(5) 0.0687(4) 0.089(3) Uani 1 d . . H51A H 0.2223(8) -0.0695(5) 0.0714(4) 0.106 Uiso 1 calc R . C52 C 0.1695(11) 0.0431(6) -0.0025(4) 0.120(4) Uani 1 d . . H52A H 0.2171(11) 0.0194(6) -0.0471(4) 0.144 Uiso 1 calc R . C53 C 0.0958(8) 0.1299(5) -0.0076(4) 0.083(3) Uani 1 d . . H53A H 0.0909(8) 0.1648(5) -0.0554(4) 0.100 Uiso 1 calc R . C54 C 0.0296(6) 0.1648(4) 0.0581(4) 0.054(2) Uani 1 d . . H54A H -0.0199(6) 0.2242(4) 0.0551(4) 0.065 Uiso 1 calc R . C55 C 0.0354(5) 0.1125(4) 0.1290(3) 0.0401(14) Uani 1 d . . H55A H -0.0103(5) 0.1373(4) 0.1733(3) 0.048 Uiso 1 calc R . O32 O 0.0951(3) 0.0171(2) 0.2873(2) 0.0347(8) Uani 1 d . . C80 C -0.2182(7) 0.4341(5) 0.1616(4) 0.073(2) Uani 1 d . . H80A H -0.2668(7) 0.4970(5) 0.1597(4) 0.088 Uiso 1 calc R . H80B H -0.2057(7) 0.4125(5) 0.2128(4) 0.088 Uiso 1 calc R . Cl1 Cl -0.2992(2) 0.3664(2) 0.14321(15) 0.1051(8) Uani 1 d . . Cl2 Cl -0.0744(2) 0.4299(2) 0.0940(2) 0.1141(9) Uani 1 d . . C90 C -0.3414(9) -0.4491(7) 0.3543(7) 0.124(4) Uani 1 d . . H90A H -0.3083(9) -0.5141(7) 0.3688(7) 0.148 Uiso 1 calc R . H90B H -0.3319(9) -0.4371(7) 0.2992(7) 0.148 Uiso 1 calc R . Cl3 Cl -0.2571(3) -0.3887(2) 0.3757(2) 0.1289(10) Uani 1 d . . Cl4 Cl -0.4995(3) -0.4205(3) 0.4016(2) 0.1610(14) Uani 1 d . . O91 O -0.0462 -0.0914 0.5244 0.068 Uani 1 d D . H91A H 0.0416 -0.1093 0.4971 0.050 Uiso 1 d D . H91B H -0.0970 -0.1349 0.5328 0.050 Uiso 1 d D . 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 0.0323(3) 0.0218(2) 0.0385(3) -0.0071(2) -0.0085(2) -0.0069(2) P1 0.0433(9) 0.0242(7) 0.0390(8) -0.0073(6) -0.0077(7) -0.0092(6) C1 0.055(4) 0.026(3) 0.043(4) -0.008(3) -0.010(3) -0.010(3) C2 0.060(4) 0.043(4) 0.072(5) -0.016(3) -0.022(4) -0.013(3) C3 0.084(6) 0.060(5) 0.129(8) -0.005(5) -0.062(6) -0.021(4) C4 0.117(8) 0.079(6) 0.091(7) -0.012(5) -0.066(6) -0.022(6) C5 0.126(8) 0.070(5) 0.064(5) -0.018(4) -0.042(6) -0.015(5) C6 0.078(5) 0.055(4) 0.044(4) -0.008(3) -0.019(4) -0.017(4) C7 0.056(4) 0.030(3) 0.038(3) -0.008(3) -0.004(3) -0.011(3) C8 0.061(4) 0.063(4) 0.045(4) -0.014(3) -0.016(3) -0.012(3) C9 0.091(6) 0.093(6) 0.053(5) -0.023(4) -0.019(4) -0.011(5) C10 0.096(6) 0.077(6) 0.049(5) 0.008(4) -0.002(4) -0.027(5) C11 0.132(8) 0.072(6) 0.060(5) 0.002(4) -0.002(5) -0.054(6) C12 0.107(6) 0.046(4) 0.050(4) -0.004(3) -0.005(4) -0.043(4) N1 0.049(3) 0.023(2) 0.054(3) -0.009(2) -0.009(2) -0.004(2) C13 0.043(3) 0.034(3) 0.036(3) -0.007(3) -0.014(3) -0.001(3) O13 0.047(3) 0.042(2) 0.066(3) -0.017(2) -0.010(2) 0.008(2) N2 0.037(3) 0.029(3) 0.046(3) -0.009(2) -0.007(2) -0.005(2) C26 0.070(5) 0.026(3) 0.081(5) -0.013(3) -0.014(4) -0.002(3) C27 0.042(4) 0.049(4) 0.070(5) -0.021(3) -0.002(3) -0.006(3) P2 0.0326(8) 0.0228(7) 0.0542(9) -0.0081(6) -0.0111(7) -0.0079(6) C14 0.033(3) 0.028(3) 0.083(5) -0.021(3) -0.004(3) -0.008(3) C15 0.050(4) 0.044(4) 0.084(6) -0.014(4) 0.008(4) -0.014(3) C16 0.067(5) 0.052(5) 0.118(7) -0.016(5) 0.026(5) -0.023(4) C17 0.067(6) 0.062(6) 0.158(11) -0.025(6) 0.030(7) -0.034(5) C18 0.040(4) 0.060(5) 0.183(11) -0.038(6) -0.010(6) -0.021(4) C19 0.047(4) 0.048(4) 0.129(7) -0.021(4) -0.019(4) -0.015(3) C20 0.039(3) 0.036(3) 0.060(4) -0.009(3) -0.019(3) -0.006(3) C21 0.087(5) 0.046(4) 0.078(5) -0.014(4) -0.039(4) 0.002(4) C22 0.108(7) 0.084(6) 0.079(6) -0.031(5) -0.050(5) 0.015(5) C23 0.080(5) 0.074(6) 0.067(5) 0.009(4) -0.035(4) -0.008(4) C24 0.068(5) 0.042(4) 0.077(5) 0.011(4) -0.033(4) -0.008(3) C25 0.042(4) 0.041(4) 0.075(5) -0.012(3) -0.022(3) -0.009(3) O2 0.038(2) 0.030(2) 0.054(2) -0.013(2) -0.001(2) -0.014(2) Pd2 0.0302(2) 0.0217(2) 0.0422(3) -0.0080(2) -0.0066(2) -0.0076(2) P31 0.0381(8) 0.0234(7) 0.0416(9) -0.0084(6) -0.0085(7) -0.0081(6) C31 0.055(4) 0.023(3) 0.049(4) -0.003(3) -0.017(3) -0.012(3) C32 0.067(4) 0.062(4) 0.046(4) -0.009(3) -0.014(3) -0.021(4) C33 0.116(7) 0.061(5) 0.060(5) -0.010(4) -0.045(5) -0.020(5) C34 0.102(6) 0.042(4) 0.085(6) -0.001(4) -0.057(5) -0.024(4) C35 0.066(5) 0.045(4) 0.090(6) -0.003(4) -0.040(4) -0.019(3) C36 0.047(4) 0.040(4) 0.069(4) -0.016(3) -0.017(3) -0.011(3) C37 0.043(3) 0.033(3) 0.039(3) -0.003(3) -0.004(3) -0.013(3) C38 0.070(4) 0.054(4) 0.049(4) -0.017(3) -0.012(3) -0.020(4) C39 0.080(5) 0.085(6) 0.040(4) -0.014(4) -0.005(4) -0.027(5) C40 0.084(6) 0.098(7) 0.043(4) -0.003(5) -0.008(4) -0.007(5) C41 0.106(7) 0.059(5) 0.076(6) 0.022(4) 0.005(5) -0.036(5) C42 0.087(5) 0.046(4) 0.066(5) -0.006(4) 0.002(4) -0.036(4) N31 0.046(3) 0.021(2) 0.057(3) -0.010(2) -0.011(2) -0.005(2) C43 0.044(4) 0.036(3) 0.046(4) -0.016(3) -0.013(3) -0.001(3) O43 0.044(2) 0.042(2) 0.076(3) -0.025(2) -0.016(2) 0.010(2) N32 0.034(3) 0.030(3) 0.067(3) -0.014(2) -0.008(2) -0.006(2) C56 0.065(4) 0.029(3) 0.089(5) -0.016(3) -0.012(4) -0.006(3) C57 0.034(4) 0.064(5) 0.146(8) -0.049(5) 0.002(4) -0.018(3) P32 0.0320(7) 0.0223(7) 0.0391(8) -0.0055(6) -0.0096(6) -0.0084(6) C44 0.029(3) 0.026(3) 0.061(4) -0.013(3) -0.007(3) -0.006(2) C45 0.057(4) 0.049(4) 0.091(5) -0.004(4) -0.039(4) -0.020(3) C46 0.062(5) 0.061(5) 0.172(11) -0.011(6) -0.055(6) -0.024(4) C47 0.039(4) 0.067(6) 0.169(11) -0.030(6) -0.015(6) -0.021(4) C48 0.067(5) 0.075(6) 0.096(6) -0.025(5) 0.027(5) -0.035(4) C49 0.049(4) 0.065(4) 0.070(5) -0.021(4) 0.001(4) -0.029(4) C50 0.046(3) 0.029(3) 0.037(3) -0.005(2) -0.013(3) -0.008(3) C51 0.131(7) 0.046(4) 0.053(5) -0.010(4) -0.021(5) 0.031(5) C52 0.182(10) 0.086(7) 0.042(5) -0.015(4) -0.030(6) 0.045(7) C53 0.118(7) 0.062(5) 0.048(5) 0.001(4) -0.026(5) 0.006(5) C54 0.069(4) 0.035(3) 0.056(4) 0.002(3) -0.029(4) -0.002(3) C55 0.041(3) 0.032(3) 0.045(4) -0.008(3) -0.010(3) -0.004(3) O32 0.039(2) 0.031(2) 0.035(2) -0.009(2) -0.003(2) -0.014(2) C80 0.082(5) 0.063(5) 0.069(5) -0.026(4) -0.031(4) 0.013(4) Cl1 0.110(2) 0.098(2) 0.107(2) -0.0417(14) 0.0058(15) -0.0419(15) Cl2 0.094(2) 0.129(2) 0.131(2) -0.060(2) -0.005(2) -0.037(2) C90 0.128(8) 0.099(7) 0.146(9) -0.067(7) -0.068(8) 0.042(6) Cl3 0.176(3) 0.108(2) 0.112(2) -0.038(2) -0.032(2) -0.037(2) Cl4 0.127(3) 0.204(4) 0.137(3) -0.053(3) -0.025(2) -0.009(2) O91 0.073 0.097 0.019 -0.011 -0.008 -0.003 _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 N2 2.083(4) . ? Pd1 O32 2.092(3) . ? Pd1 P1 2.2043(14) . ? Pd1 P2 2.2764(14) . ? P1 N1 1.674(5) . ? P1 C7 1.808(6) . ? P1 C1 1.823(6) . ? C1 C2 1.383(9) . ? C1 C6 1.401(8) . ? C2 C3 1.402(10) . ? C3 C4 1.371(12) . ? C4 C5 1.352(12) . ? C5 C6 1.379(10) . ? C7 C12 1.375(8) . ? C7 C8 1.394(8) . ? C8 C9 1.404(10) . ? C9 C10 1.343(11) . ? C10 C11 1.354(11) . ? C11 C12 1.388(10) . ? N1 C13 1.424(7) . ? N1 C26 1.466(7) . ? C13 O13 1.235(6) . ? C13 N2 1.323(7) . ? N2 C27 1.449(7) . ? P2 O2 1.536(4) . ? P2 C20 1.815(6) . ? P2 C14 1.833(6) . ? C14 C19 1.364(9) . ? C14 C15 1.406(10) . ? C15 C16 1.382(10) . ? C16 C17 1.361(14) . ? C17 C18 1.347(14) . ? C18 C19 1.422(11) . ? C20 C25 1.386(8) . ? C20 C21 1.394(9) . ? C21 C22 1.389(10) . ? C22 C23 1.370(11) . ? C23 C24 1.374(10) . ? C24 C25 1.379(9) . ? O2 Pd2 2.075(3) . ? Pd2 N32 2.059(4) . ? Pd2 P31 2.1985(14) . ? Pd2 P32 2.2600(14) . ? P31 N31 1.676(5) . ? P31 C31 1.807(6) . ? P31 C37 1.811(6) . ? C31 C36 1.386(8) . ? C31 C32 1.408(8) . ? C32 C33 1.372(9) . ? C33 C34 1.358(11) . ? C34 C35 1.366(10) . ? C35 C36 1.386(9) . ? C37 C38 1.386(8) . ? C37 C42 1.393(8) . ? C38 C39 1.384(9) . ? C39 C40 1.335(11) . ? C40 C41 1.387(12) . ? C41 C42 1.401(10) . ? N31 C43 1.414(7) . ? N31 C56 1.469(7) . ? C43 O43 1.240(6) . ? C43 N32 1.328(7) . ? N32 C57 1.458(7) . ? P32 O32 1.539(3) . ? P32 C44 1.809(5) . ? P32 C50 1.821(6) . ? C44 C49 1.361(9) . ? C44 C45 1.394(8) . ? C45 C46 1.382(10) . ? C46 C47 1.353(13) . ? C47 C48 1.378(13) . ? C48 C49 1.438(10) . ? C50 C55 1.372(7) . ? C50 C51 1.375(8) . ? C51 C52 1.384(10) . ? C52 C53 1.366(10) . ? C53 C54 1.361(9) . ? C54 C55 1.380(8) . ? C80 Cl2 1.751(8) . ? C80 Cl1 1.753(8) . ? C90 Cl3 1.724(11) . ? C90 Cl4 1.754(10) . ? 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 N2 Pd1 O32 91.3(2) . . ? N2 Pd1 P1 81.81(13) . . ? O32 Pd1 P1 172.93(10) . . ? N2 Pd1 P2 176.72(13) . . ? O32 Pd1 P2 86.10(10) . . ? P1 Pd1 P2 100.87(5) . . ? N1 P1 C7 105.2(3) . . ? N1 P1 C1 103.6(2) . . ? C7 P1 C1 107.7(3) . . ? N1 P1 Pd1 102.6(2) . . ? C7 P1 Pd1 116.6(2) . . ? C1 P1 Pd1 119.2(2) . . ? C2 C1 C6 119.2(6) . . ? C2 C1 P1 123.4(5) . . ? C6 C1 P1 117.4(5) . . ? C1 C2 C3 118.7(7) . . ? C4 C3 C2 121.3(8) . . ? C5 C4 C3 119.7(8) . . ? C4 C5 C6 120.9(8) . . ? C5 C6 C1 120.2(7) . . ? C12 C7 C8 118.8(6) . . ? C12 C7 P1 124.3(5) . . ? C8 C7 P1 116.6(5) . . ? C7 C8 C9 118.7(7) . . ? C10 C9 C8 121.3(7) . . ? C9 C10 C11 120.1(8) . . ? C10 C11 C12 120.5(8) . . ? C7 C12 C11 120.5(7) . . ? C13 N1 C26 119.4(5) . . ? C13 N1 P1 119.4(3) . . ? C26 N1 P1 120.9(4) . . ? O13 C13 N2 127.5(6) . . ? O13 C13 N1 117.9(5) . . ? N2 C13 N1 114.6(5) . . ? C13 N2 C27 115.7(5) . . ? C13 N2 Pd1 121.6(4) . . ? C27 N2 Pd1 122.6(3) . . ? O2 P2 C20 110.2(2) . . ? O2 P2 C14 101.3(2) . . ? C20 P2 C14 107.0(3) . . ? O2 P2 Pd1 113.9(2) . . ? C20 P2 Pd1 104.4(2) . . ? C14 P2 Pd1 119.8(2) . . ? C19 C14 C15 118.8(6) . . ? C19 C14 P2 124.9(6) . . ? C15 C14 P2 116.2(5) . . ? C16 C15 C14 120.7(8) . . ? C17 C16 C15 119.9(10) . . ? C18 C17 C16 120.5(9) . . ? C17 C18 C19 121.0(9) . . ? C14 C19 C18 119.1(9) . . ? C25 C20 C21 118.2(6) . . ? C25 C20 P2 122.3(5) . . ? C21 C20 P2 119.5(5) . . ? C22 C21 C20 119.8(7) . . ? C23 C22 C21 120.7(7) . . ? C22 C23 C24 120.2(7) . . ? C23 C24 C25 119.4(6) . . ? C24 C25 C20 121.7(6) . . ? P2 O2 Pd2 134.8(2) . . ? N32 Pd2 O2 92.3(2) . . ? N32 Pd2 P31 81.90(13) . . ? O2 Pd2 P31 172.11(12) . . ? N32 Pd2 P32 174.81(13) . . ? O2 Pd2 P32 83.30(10) . . ? P31 Pd2 P32 102.75(5) . . ? N31 P31 C31 103.9(2) . . ? N31 P31 C37 105.3(3) . . ? C31 P31 C37 107.0(3) . . ? N31 P31 Pd2 102.3(2) . . ? C31 P31 Pd2 122.4(2) . . ? C37 P31 Pd2 113.9(2) . . ? C36 C31 C32 117.6(6) . . ? C36 C31 P31 123.7(5) . . ? C32 C31 P31 118.6(5) . . ? C33 C32 C31 120.3(7) . . ? C34 C33 C32 120.9(7) . . ? C33 C34 C35 120.2(7) . . ? C34 C35 C36 120.1(7) . . ? C35 C36 C31 120.8(6) . . ? C38 C37 C42 117.6(6) . . ? C38 C37 P31 119.2(4) . . ? C42 C37 P31 122.5(5) . . ? C39 C38 C37 121.6(6) . . ? C40 C39 C38 120.8(7) . . ? C39 C40 C41 120.0(7) . . ? C40 C41 C42 120.0(7) . . ? C37 C42 C41 120.1(7) . . ? C43 N31 C56 118.0(5) . . ? C43 N31 P31 119.2(3) . . ? C56 N31 P31 121.7(4) . . ? O43 C43 N32 127.0(6) . . ? O43 C43 N31 118.8(5) . . ? N32 C43 N31 114.2(5) . . ? C43 N32 C57 115.2(5) . . ? C43 N32 Pd2 121.9(4) . . ? C57 N32 Pd2 122.8(4) . . ? O32 P32 C44 103.5(2) . . ? O32 P32 C50 109.6(2) . . ? C44 P32 C50 103.5(3) . . ? O32 P32 Pd2 112.8(2) . . ? C44 P32 Pd2 120.6(2) . . ? C50 P32 Pd2 106.2(2) . . ? C49 C44 C45 120.2(6) . . ? C49 C44 P32 118.0(5) . . ? C45 C44 P32 121.8(5) . . ? C46 C45 C44 120.3(8) . . ? C47 C46 C45 120.0(9) . . ? C46 C47 C48 121.6(8) . . ? C47 C48 C49 118.6(8) . . ? C44 C49 C48 119.3(7) . . ? C55 C50 C51 117.7(5) . . ? C55 C50 P32 121.5(4) . . ? C51 C50 P32 120.8(4) . . ? C50 C51 C52 121.0(6) . . ? C53 C52 C51 120.3(7) . . ? C54 C53 C52 119.2(7) . . ? C53 C54 C55 120.4(6) . . ? C50 C55 C54 121.3(5) . . ? P32 O32 Pd1 128.4(2) . . ? Cl2 C80 Cl1 110.8(4) . . ? Cl3 C90 Cl4 112.7(5) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pd1 P1 N1 0.6(2) . . . . ? O32 Pd1 P1 N1 12.3(9) . . . . ? P2 Pd1 P1 N1 -177.4(2) . . . . ? N2 Pd1 P1 C7 -113.8(3) . . . . ? O32 Pd1 P1 C7 -102.1(8) . . . . ? P2 Pd1 P1 C7 68.1(2) . . . . ? N2 Pd1 P1 C1 114.3(3) . . . . ? O32 Pd1 P1 C1 126.0(8) . . . . ? P2 Pd1 P1 C1 -63.8(2) . . . . ? N1 P1 C1 C2 -146.2(5) . . . . ? C7 P1 C1 C2 -35.0(6) . . . . ? Pd1 P1 C1 C2 100.7(5) . . . . ? N1 P1 C1 C6 35.3(5) . . . . ? C7 P1 C1 C6 146.5(5) . . . . ? Pd1 P1 C1 C6 -77.8(5) . . . . ? C6 C1 C2 C3 -0.8(9) . . . . ? P1 C1 C2 C3 -179.3(5) . . . . ? C1 C2 C3 C4 -1.1(11) . . . . ? C2 C3 C4 C5 2.1(13) . . . . ? C3 C4 C5 C6 -1.2(13) . . . . ? C4 C5 C6 C1 -0.7(11) . . . . ? C2 C1 C6 C5 1.7(9) . . . . ? P1 C1 C6 C5 -179.8(5) . . . . ? N1 P1 C7 C12 89.4(6) . . . . ? C1 P1 C7 C12 -20.7(6) . . . . ? Pd1 P1 C7 C12 -157.7(5) . . . . ? N1 P1 C7 C8 -85.0(5) . . . . ? C1 P1 C7 C8 164.9(5) . . . . ? Pd1 P1 C7 C8 27.9(5) . . . . ? C12 C7 C8 C9 1.6(9) . . . . ? P1 C7 C8 C9 176.4(5) . . . . ? C7 C8 C9 C10 -0.2(11) . . . . ? C8 C9 C10 C11 -0.9(13) . . . . ? C9 C10 C11 C12 0.5(14) . . . . ? C8 C7 C12 C11 -2.0(11) . . . . ? P1 C7 C12 C11 -176.3(6) . . . . ? C10 C11 C12 C7 1.0(13) . . . . ? C7 P1 N1 C13 122.6(4) . . . . ? C1 P1 N1 C13 -124.4(4) . . . . ? Pd1 P1 N1 C13 0.2(4) . . . . ? C7 P1 N1 C26 -51.5(5) . . . . ? C1 P1 N1 C26 61.4(5) . . . . ? Pd1 P1 N1 C26 -174.0(4) . . . . ? C26 N1 C13 O13 -7.6(8) . . . . ? P1 N1 C13 O13 178.2(4) . . . . ? C26 N1 C13 N2 172.8(5) . . . . ? P1 N1 C13 N2 -1.4(7) . . . . ? O13 C13 N2 C27 -2.1(9) . . . . ? N1 C13 N2 C27 177.4(5) . . . . ? O13 C13 N2 Pd1 -177.4(5) . . . . ? N1 C13 N2 Pd1 2.2(7) . . . . ? O32 Pd1 N2 C13 179.8(4) . . . . ? P1 Pd1 N2 C13 -1.7(4) . . . . ? P2 Pd1 N2 C13 143.3(20) . . . . ? O32 Pd1 N2 C27 4.8(5) . . . . ? P1 Pd1 N2 C27 -176.6(5) . . . . ? P2 Pd1 N2 C27 -31.6(25) . . . . ? N2 Pd1 P2 O2 77.6(22) . . . . ? O32 Pd1 P2 O2 41.0(2) . . . . ? P1 Pd1 P2 O2 -137.8(2) . . . . ? N2 Pd1 P2 C20 -42.7(22) . . . . ? O32 Pd1 P2 C20 -79.2(2) . . . . ? P1 Pd1 P2 C20 102.0(2) . . . . ? N2 Pd1 P2 C14 -162.4(22) . . . . ? O32 Pd1 P2 C14 161.1(3) . . . . ? P1 Pd1 P2 C14 -17.7(3) . . . . ? O2 P2 C14 C19 -122.3(5) . . . . ? C20 P2 C14 C19 -6.9(6) . . . . ? Pd1 P2 C14 C19 111.5(5) . . . . ? O2 P2 C14 C15 54.2(5) . . . . ? C20 P2 C14 C15 169.7(4) . . . . ? Pd1 P2 C14 C15 -71.9(5) . . . . ? C19 C14 C15 C16 -2.5(9) . . . . ? P2 C14 C15 C16 -179.3(5) . . . . ? C14 C15 C16 C17 2.3(11) . . . . ? C15 C16 C17 C18 -1.3(13) . . . . ? C16 C17 C18 C19 0.5(14) . . . . ? C15 C14 C19 C18 1.7(9) . . . . ? P2 C14 C19 C18 178.2(5) . . . . ? C17 C18 C19 C14 -0.8(12) . . . . ? O2 P2 C20 C25 1.6(6) . . . . ? C14 P2 C20 C25 -107.8(5) . . . . ? Pd1 P2 C20 C25 124.3(5) . . . . ? O2 P2 C20 C21 -175.7(5) . . . . ? C14 P2 C20 C21 75.0(6) . . . . ? Pd1 P2 C20 C21 -53.0(6) . . . . ? C25 C20 C21 C22 -1.2(11) . . . . ? P2 C20 C21 C22 176.2(6) . . . . ? C20 C21 C22 C23 -0.6(13) . . . . ? C21 C22 C23 C24 2.2(14) . . . . ? C22 C23 C24 C25 -1.9(12) . . . . ? C23 C24 C25 C20 0.1(11) . . . . ? C21 C20 C25 C24 1.4(10) . . . . ? P2 C20 C25 C24 -175.9(5) . . . . ? C20 P2 O2 Pd2 47.4(4) . . . . ? C14 P2 O2 Pd2 160.5(3) . . . . ? Pd1 P2 O2 Pd2 -69.5(3) . . . . ? P2 O2 Pd2 N32 -119.3(3) . . . . ? P2 O2 Pd2 P31 -77.1(8) . . . . ? P2 O2 Pd2 P32 63.4(3) . . . . ? N32 Pd2 P31 N31 -3.7(2) . . . . ? O2 Pd2 P31 N31 -46.4(8) . . . . ? P32 Pd2 P31 N31 174.0(2) . . . . ? N32 Pd2 P31 C31 -119.1(3) . . . . ? O2 Pd2 P31 C31 -161.8(8) . . . . ? P32 Pd2 P31 C31 58.6(2) . . . . ? N32 Pd2 P31 C37 109.4(3) . . . . ? O2 Pd2 P31 C37 66.7(8) . . . . ? P32 Pd2 P31 C37 -72.9(2) . . . . ? N31 P31 C31 C36 141.5(5) . . . . ? C37 P31 C31 C36 30.4(6) . . . . ? Pd2 P31 C31 C36 -103.8(5) . . . . ? N31 P31 C31 C32 -38.6(5) . . . . ? C37 P31 C31 C32 -149.8(5) . . . . ? Pd2 P31 C31 C32 76.0(5) . . . . ? C36 C31 C32 C33 -0.7(9) . . . . ? P31 C31 C32 C33 179.5(5) . . . . ? C31 C32 C33 C34 -0.5(11) . . . . ? C32 C33 C34 C35 1.9(11) . . . . ? C33 C34 C35 C36 -2.3(10) . . . . ? C34 C35 C36 C31 1.1(10) . . . . ? C32 C31 C36 C35 0.3(9) . . . . ? P31 C31 C36 C35 -179.9(5) . . . . ? N31 P31 C37 C38 99.5(5) . . . . ? C31 P31 C37 C38 -150.4(5) . . . . ? Pd2 P31 C37 C38 -11.8(6) . . . . ? N31 P31 C37 C42 -70.6(6) . . . . ? C31 P31 C37 C42 39.5(6) . . . . ? Pd2 P31 C37 C42 178.1(5) . . . . ? C42 C37 C38 C39 1.7(10) . . . . ? P31 C37 C38 C39 -168.8(5) . . . . ? C37 C38 C39 C40 -0.7(11) . . . . ? C38 C39 C40 C41 -1.3(13) . . . . ? C39 C40 C41 C42 2.2(13) . . . . ? C38 C37 C42 C41 -0.8(10) . . . . ? P31 C37 C42 C41 169.4(6) . . . . ? C40 C41 C42 C37 -1.1(13) . . . . ? C31 P31 N31 C43 135.5(4) . . . . ? C37 P31 N31 C43 -112.2(5) . . . . ? Pd2 P31 N31 C43 7.2(5) . . . . ? C31 P31 N31 C56 -56.6(5) . . . . ? C37 P31 N31 C56 55.8(5) . . . . ? Pd2 P31 N31 C56 175.2(5) . . . . ? C56 N31 C43 O43 5.7(8) . . . . ? P31 N31 C43 O43 174.1(4) . . . . ? C56 N31 C43 N32 -175.9(5) . . . . ? P31 N31 C43 N32 -7.5(7) . . . . ? O43 C43 N32 C57 0.6(10) . . . . ? N31 C43 N32 C57 -177.6(6) . . . . ? O43 C43 N32 Pd2 -178.1(5) . . . . ? N31 C43 N32 Pd2 3.7(7) . . . . ? O2 Pd2 N32 C43 175.2(5) . . . . ? P31 Pd2 N32 C43 0.5(4) . . . . ? P32 Pd2 N32 C43 -153.3(13) . . . . ? O2 Pd2 N32 C57 -3.4(6) . . . . ? P31 Pd2 N32 C57 -178.0(6) . . . . ? P32 Pd2 N32 C57 28.2(19) . . . . ? N32 Pd2 P32 O32 -83.7(15) . . . . ? O2 Pd2 P32 O32 -52.0(2) . . . . ? P31 Pd2 P32 O32 122.9(2) . . . . ? N32 Pd2 P32 C44 153.3(15) . . . . ? O2 Pd2 P32 C44 -174.9(3) . . . . ? P31 Pd2 P32 C44 -0.1(2) . . . . ? N32 Pd2 P32 C50 36.3(16) . . . . ? O2 Pd2 P32 C50 68.1(2) . . . . ? P31 Pd2 P32 C50 -117.1(2) . . . . ? O32 P32 C44 C49 -44.6(5) . . . . ? C50 P32 C44 C49 -158.9(5) . . . . ? Pd2 P32 C44 C49 82.7(5) . . . . ? O32 P32 C44 C45 134.3(5) . . . . ? C50 P32 C44 C45 20.0(5) . . . . ? Pd2 P32 C44 C45 -98.3(5) . . . . ? C49 C44 C45 C46 0.7(9) . . . . ? P32 C44 C45 C46 -178.2(5) . . . . ? C44 C45 C46 C47 -0.9(11) . . . . ? C45 C46 C47 C48 1.0(13) . . . . ? C46 C47 C48 C49 -0.9(13) . . . . ? C45 C44 C49 C48 -0.6(9) . . . . ? P32 C44 C49 C48 178.3(5) . . . . ? C47 C48 C49 C44 0.7(11) . . . . ? O32 P32 C50 C55 -30.9(5) . . . . ? C44 P32 C50 C55 79.0(5) . . . . ? Pd2 P32 C50 C55 -153.1(4) . . . . ? O32 P32 C50 C51 149.8(6) . . . . ? C44 P32 C50 C51 -100.3(6) . . . . ? Pd2 P32 C50 C51 27.7(6) . . . . ? C55 C50 C51 C52 1.1(13) . . . . ? P32 C50 C51 C52 -179.7(8) . . . . ? C50 C51 C52 C53 -2.1(17) . . . . ? C51 C52 C53 C54 2.0(17) . . . . ? C52 C53 C54 C55 -1.0(13) . . . . ? C51 C50 C55 C54 0.0(10) . . . . ? P32 C50 C55 C54 -179.3(5) . . . . ? C53 C54 C55 C50 0.0(10) . . . . ? C44 P32 O32 Pd1 -147.2(3) . . . . ? C50 P32 O32 Pd1 -37.3(3) . . . . ? Pd2 P32 O32 Pd1 80.7(3) . . . . ? N2 Pd1 O32 P32 119.8(3) . . . . ? P1 Pd1 O32 P32 108.3(8) . . . . ? P2 Pd1 O32 P32 -62.1(3) . . . . ? _refine_diff_density_max 2.305 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.093 #---ENd