# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'RSC Advances' _journal_coden_Cambridge 1500 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr M. Esther Garcia-Fernandez' _publ_contact_author_email mesther.garcia@usc.es _publ_section_title ; Transition of trigonal bipyramidal to square-planar geometries by oxidation of a coordinated tripodal polyphosphine in Pd(II) and Pt(II) complexes ; _publ_author_name M.E.Garcia-Fernandez # Attachment '- C1DT11353D_ccdc_835445_835447_cif.txt' #TrackingRef '- C1DT11353D_ccdc_835445_835447_cif.txt' # Attachment '- CIFS_oxid-V.New.cif' data_dami13* _database_code_depnum_ccdc_archive 'CCDC 835445' #TrackingRef '- CIFS_oxid-V.New.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Pd(PP3)2]Cl2.4CHCl3 ; _chemical_name_common (Pd(PP3)2)Cl2.4CHCl3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H84 Cl14 P8 Pd' _chemical_formula_weight 1992.01 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' 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 P21/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 14.942(2) _cell_length_b 18.073(3) _cell_length_c 17.298(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.440(4) _cell_angle_gamma 90.00 _cell_volume 4662.8(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 949 _cell_measurement_theta_min 2.358 _cell_measurement_theta_max 25.9965 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8919 _exptl_absorpt_correction_T_max 0.9474 _exptl_absorpt_process_details Sadabs _exptl_special_details ; [Pd(PP3)2]Cl2.4CHCl3 ; _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_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28588 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_av_sigmaI/netI 0.1638 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.41 _reflns_number_total 9528 _reflns_number_gt 3947 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction 'BRUKER Shelxtl' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, =999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR =nd 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 =s not relevant to the choice of reflections for refinement. R-factors =ased on F^2^ are statistically about twice as large as those based on F, and =- 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^)+(0.0927P)^2^+0.0000P] where ==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9528 _refine_ls_number_parameters 502 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1769 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1999 _refine_ls_wR_factor_gt 0.1506 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.0000 0.0000 0.5000 0.0321(2) Uani 1 2 d S . . P2 P 0.09435(12) 0.03415(10) 0.60561(11) 0.0347(4) Uani 1 1 d . . . P1 P -0.05754(12) 0.11928(10) 0.51297(11) 0.0356(4) Uani 1 1 d . . . P4 P 0.04749(14) 0.28899(11) 0.35221(12) 0.0471(5) Uani 1 1 d . . . P3 P -0.33301(14) 0.19032(12) 0.56843(13) 0.0492(6) Uani 1 1 d . . . Cl1 Cl 0.82947(16) 0.00143(14) 0.69280(14) 0.0752(7) Uani 1 1 d . . . Cl7 Cl 0.52399(19) 0.11660(19) 0.7217(2) 0.1211(12) Uani 1 1 d . . . Cl2 Cl 0.74609(17) 0.87206(15) 0.91320(15) 0.0817(8) Uani 1 1 d . . . Cl3 Cl 0.67557(17) 0.83334(17) 0.76077(17) 0.0938(9) Uani 1 1 d . . . Cl4 Cl 0.86068(16) 0.80751(15) 0.80331(17) 0.0876(8) Uani 1 1 d . . . Cl6 Cl 0.6290(2) 0.03050(17) 0.82829(19) 0.1073(10) Uani 1 1 d . . . Cl5 Cl 0.6861(2) 0.17776(15) 0.79250(18) 0.1051(10) Uani 1 1 d . . . C7 C 0.1311(5) -0.0349(4) 0.6742(4) 0.0416(18) Uani 1 1 d . . . C5 C -0.0449(4) 0.1878(4) 0.4372(4) 0.0417(18) Uani 1 1 d . . . H5A H -0.0777 0.1704 0.3906 0.050 Uiso 1 1 calc R . . H5B H -0.0734 0.2332 0.4528 0.050 Uiso 1 1 calc R . . C1 C -0.0038(5) 0.1612(4) 0.6000(4) 0.0449(19) Uani 1 1 d . . . H1A H 0.0452 0.1925 0.5855 0.054 Uiso 1 1 calc R . . H1B H -0.0469 0.1923 0.6245 0.054 Uiso 1 1 calc R . . C3 C -0.1770(4) 0.1214(4) 0.5275(4) 0.0407(18) Uani 1 1 d . . . H3A H -0.2079 0.0947 0.4852 0.049 Uiso 1 1 calc R . . H3B H -0.1872 0.0947 0.5749 0.049 Uiso 1 1 calc R . . C13 C 0.1937(4) 0.0801(4) 0.5753(4) 0.0374(17) Uani 1 1 d . . . C18 C 0.2187(5) 0.0727(4) 0.5002(5) 0.0459(19) Uani 1 1 d . . . H18 H 0.1825 0.0458 0.4648 0.055 Uiso 1 1 calc R . . C8 C 0.2190(5) -0.0602(4) 0.6799(5) 0.050(2) Uani 1 1 d . . . H8 H 0.2612 -0.0385 0.6497 0.060 Uiso 1 1 calc R . . C31 C 0.1609(5) 0.3242(4) 0.3658(4) 0.049(2) Uani 1 1 d . . . C14 C 0.2459(5) 0.1210(4) 0.6287(5) 0.054(2) Uani 1 1 d . . . H14 H 0.2296 0.1260 0.6795 0.064 Uiso 1 1 calc R . . C37 C -0.0117(5) 0.3545(4) 0.4114(5) 0.0449(19) Uani 1 1 d . . . C19 C -0.3919(5) 0.1534(4) 0.4833(5) 0.051(2) Uani 1 1 d . . . C4 C -0.2198(5) 0.1980(4) 0.5326(5) 0.048(2) Uani 1 1 d . . . H4A H -0.2233 0.2210 0.4819 0.057 Uiso 1 1 calc R . . H4B H -0.1829 0.2291 0.5674 0.057 Uiso 1 1 calc R . . C6 C 0.0507(5) 0.2065(4) 0.4164(5) 0.049(2) Uani 1 1 d . . . H6A H 0.0764 0.1649 0.3902 0.059 Uiso 1 1 calc R . . H6B H 0.0877 0.2167 0.4631 0.059 Uiso 1 1 calc R . . C25 C -0.3698(5) 0.2868(4) 0.5662(5) 0.048(2) Uani 1 1 d . . . C12 C 0.0680(5) -0.0685(4) 0.7203(4) 0.048(2) Uani 1 1 d . . . H12 H 0.0089 -0.0522 0.7177 0.057 Uiso 1 1 calc R . . C28 C -0.4397(6) 0.4296(5) 0.5733(6) 0.078(3) Uani 1 1 d . . . H28 H -0.4627 0.4773 0.5752 0.094 Uiso 1 1 calc R . . C20 C -0.4270(5) 0.1954(5) 0.4196(5) 0.059(2) Uani 1 1 d . . . H20 H -0.4219 0.2466 0.4215 0.071 Uiso 1 1 calc R . . C30 C -0.4478(5) 0.3016(5) 0.6052(6) 0.072(3) Uani 1 1 d . . . H30 H -0.4764 0.2633 0.6298 0.087 Uiso 1 1 calc R . . C101 C 0.6341(6) 0.0976(5) 0.7578(5) 0.063(2) Uani 1 1 d . . . C24 C -0.4058(5) 0.0773(5) 0.4773(6) 0.063(2) Uani 1 1 d . . . H24 H -0.3862 0.0470 0.5183 0.076 Uiso 1 1 calc R . . C26 C -0.3281(5) 0.3459(4) 0.5338(5) 0.061(2) Uani 1 1 d . . . H26 H -0.2751 0.3384 0.5094 0.073 Uiso 1 1 calc R . . C32 C 0.1782(6) 0.3979(5) 0.3494(5) 0.060(2) Uani 1 1 d . . . H32 H 0.1304 0.4290 0.3352 0.072 Uiso 1 1 calc R . . C2 C 0.0323(5) 0.1032(4) 0.6580(4) 0.0440(18) Uani 1 1 d . . . H2A H -0.0169 0.0798 0.6829 0.053 Uiso 1 1 calc R . . H2B H 0.0715 0.1263 0.6977 0.053 Uiso 1 1 calc R . . C38 C 0.0125(6) 0.3680(5) 0.4884(5) 0.062(2) Uani 1 1 d . . . H38 H 0.0634 0.3458 0.5116 0.074 Uiso 1 1 calc R . . C42 C -0.0857(6) 0.3900(5) 0.3785(6) 0.068(3) Uani 1 1 d . . . H42 H -0.1020 0.3823 0.3264 0.082 Uiso 1 1 calc R . . C100 C 0.7692(5) 0.8663(5) 0.8151(5) 0.058(2) Uani 1 1 d . . . C10 C 0.1828(7) -0.1503(5) 0.7734(5) 0.075(3) Uani 1 1 d . . . H10 H 0.1996 -0.1896 0.8058 0.090 Uiso 1 1 calc R . . C33 C 0.2635(8) 0.4263(6) 0.3534(5) 0.076(3) Uani 1 1 d . . . H33 H 0.2729 0.4757 0.3412 0.092 Uiso 1 1 calc R . . C11 C 0.0947(6) -0.1260(4) 0.7698(5) 0.063(2) Uani 1 1 d . . . H11 H 0.0533 -0.1483 0.8005 0.076 Uiso 1 1 calc R . . C17 C 0.2969(6) 0.1048(5) 0.4767(6) 0.066(3) Uani 1 1 d . . . H17 H 0.3145 0.0982 0.4265 0.079 Uiso 1 1 calc R . . C15 C 0.3241(6) 0.1550(5) 0.6044(7) 0.072(3) Uani 1 1 d . . . H15 H 0.3596 0.1830 0.6393 0.087 Uiso 1 1 calc R . . C9 C 0.2451(6) -0.1177(5) 0.7303(5) 0.065(2) Uani 1 1 d . . . H9 H 0.3044 -0.1335 0.7344 0.077 Uiso 1 1 calc R . . C21 C -0.4684(6) 0.1631(6) 0.3547(6) 0.083(3) Uani 1 1 d . . . H21 H -0.4886 0.1924 0.3130 0.099 Uiso 1 1 calc R . . C16 C 0.3485(6) 0.1471(5) 0.5297(7) 0.077(3) Uani 1 1 d . . . H16 H 0.4001 0.1702 0.5143 0.092 Uiso 1 1 calc R . . C27 C -0.3637(6) 0.4162(5) 0.5369(6) 0.069(3) Uani 1 1 d . . . H27 H -0.3348 0.4552 0.5136 0.083 Uiso 1 1 calc R . . C36 C 0.2344(5) 0.2806(5) 0.3862(6) 0.068(3) Uani 1 1 d . . . H36 H 0.2258 0.2308 0.3970 0.082 Uiso 1 1 calc R . . C22 C -0.4799(6) 0.0871(6) 0.3516(7) 0.080(3) Uani 1 1 d . . . H22 H -0.5093 0.0650 0.3087 0.096 Uiso 1 1 calc R . . C23 C -0.4475(6) 0.0457(6) 0.4123(7) 0.078(3) Uani 1 1 d . . . H23 H -0.4537 -0.0055 0.4100 0.093 Uiso 1 1 calc R . . C34 C 0.3350(7) 0.3818(7) 0.3752(7) 0.093(4) Uani 1 1 d . . . H34 H 0.3927 0.4013 0.3792 0.111 Uiso 1 1 calc R . . C29 C -0.4822(6) 0.3721(6) 0.6073(7) 0.094(4) Uani 1 1 d . . . H29 H -0.5348 0.3808 0.6321 0.113 Uiso 1 1 calc R . . C35 C 0.3211(6) 0.3093(6) 0.3910(7) 0.093(4) Uani 1 1 d . . . H35 H 0.3695 0.2787 0.4050 0.111 Uiso 1 1 calc R . . C39 C -0.0397(7) 0.4149(5) 0.5312(6) 0.076(3) Uani 1 1 d . . . H39 H -0.0248 0.4227 0.5836 0.091 Uiso 1 1 calc R . . C40 C -0.1135(8) 0.4498(6) 0.4957(9) 0.095(4) Uani 1 1 d . . . H40 H -0.1470 0.4823 0.5240 0.114 Uiso 1 1 calc R . . C41 C -0.1371(7) 0.4373(6) 0.4214(8) 0.095(4) Uani 1 1 d . . . H41 H -0.1877 0.4601 0.3982 0.114 Uiso 1 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 0.0300(4) 0.0318(4) 0.0345(4) -0.0027(4) 0.0032(3) 0.0021(4) P2 0.0317(10) 0.0388(10) 0.0335(11) -0.0025(8) 0.0009(8) 0.0016(8) P1 0.0346(10) 0.0309(10) 0.0416(12) -0.0028(8) 0.0052(9) 0.0011(8) P4 0.0535(13) 0.0410(12) 0.0475(13) 0.0053(10) 0.0100(10) -0.0011(10) P3 0.0439(12) 0.0500(13) 0.0547(14) 0.0027(10) 0.0126(10) 0.0099(10) Cl1 0.0786(16) 0.0835(16) 0.0636(15) 0.0190(14) 0.0059(12) -0.0105(14) Cl7 0.0689(19) 0.141(3) 0.152(3) 0.049(2) -0.0027(19) -0.0057(18) Cl2 0.0798(17) 0.102(2) 0.0641(17) 0.0052(14) 0.0072(13) -0.0047(15) Cl3 0.0612(16) 0.130(2) 0.088(2) -0.0149(18) -0.0108(14) 0.0019(16) Cl4 0.0633(16) 0.0922(19) 0.108(2) 0.0034(16) 0.0110(15) 0.0203(14) Cl6 0.105(2) 0.102(2) 0.116(3) 0.0431(19) 0.0149(19) -0.0026(17) Cl5 0.134(3) 0.0752(19) 0.104(2) -0.0190(17) -0.0095(19) -0.0143(18) C7 0.034(4) 0.047(4) 0.043(5) -0.004(4) 0.002(3) 0.002(3) C5 0.039(4) 0.037(4) 0.050(5) 0.003(3) 0.003(4) 0.005(3) C1 0.044(4) 0.033(4) 0.058(5) -0.007(4) 0.007(4) 0.006(3) C3 0.034(4) 0.043(4) 0.046(5) -0.006(4) 0.011(3) -0.003(3) C13 0.035(4) 0.039(4) 0.038(4) -0.003(3) -0.004(3) 0.001(3) C18 0.044(5) 0.037(4) 0.057(5) -0.001(4) 0.004(4) 0.004(4) C8 0.045(5) 0.049(5) 0.057(5) 0.010(4) 0.004(4) 0.004(4) C31 0.046(5) 0.052(5) 0.049(5) 0.000(4) 0.016(4) -0.002(4) C14 0.037(4) 0.066(6) 0.058(6) -0.007(4) -0.005(4) -0.007(4) C37 0.044(4) 0.034(4) 0.057(5) 0.010(4) 0.003(4) 0.003(3) C19 0.036(4) 0.048(5) 0.071(6) 0.003(4) 0.014(4) -0.001(4) C4 0.038(4) 0.042(5) 0.063(6) -0.010(4) 0.003(4) 0.008(3) C6 0.048(5) 0.040(5) 0.059(5) 0.003(4) 0.013(4) 0.007(4) C25 0.041(5) 0.054(5) 0.049(5) 0.002(4) -0.001(4) 0.015(4) C12 0.051(5) 0.050(5) 0.042(5) 0.006(4) 0.005(4) 0.003(4) C28 0.059(6) 0.063(6) 0.113(9) -0.011(6) 0.003(6) 0.023(5) C20 0.054(5) 0.052(5) 0.070(7) 0.003(5) -0.010(5) -0.004(4) C30 0.059(6) 0.052(6) 0.111(8) -0.007(5) 0.045(5) 0.008(4) C101 0.065(6) 0.056(5) 0.066(6) 0.002(5) -0.008(5) -0.009(4) C24 0.047(5) 0.059(6) 0.084(7) 0.009(5) 0.004(5) 0.002(4) C26 0.057(5) 0.047(5) 0.081(7) -0.005(5) 0.025(5) 0.008(4) C32 0.073(6) 0.057(6) 0.051(6) 0.000(4) 0.004(5) -0.013(5) C2 0.047(5) 0.049(5) 0.036(4) -0.003(4) -0.002(4) 0.004(4) C38 0.076(6) 0.055(5) 0.056(6) 0.000(4) 0.014(5) 0.004(5) C42 0.060(6) 0.057(6) 0.087(7) 0.000(5) -0.003(5) 0.016(5) C100 0.050(5) 0.069(6) 0.055(6) 0.001(4) 0.001(4) 0.010(4) C10 0.089(7) 0.071(7) 0.063(7) 0.028(5) 0.003(6) 0.015(6) C33 0.091(8) 0.066(7) 0.073(7) 0.002(5) 0.014(6) -0.036(6) C11 0.078(7) 0.056(6) 0.058(6) 0.020(5) 0.021(5) 0.001(5) C17 0.064(6) 0.054(6) 0.082(7) 0.020(5) 0.030(5) 0.007(5) C15 0.043(5) 0.062(6) 0.110(9) -0.006(6) -0.007(5) -0.017(4) C9 0.056(6) 0.067(6) 0.068(6) 0.013(5) -0.012(5) 0.022(5) C21 0.081(7) 0.068(7) 0.096(9) 0.001(6) -0.017(6) -0.009(6) C16 0.036(5) 0.069(7) 0.126(10) 0.017(7) 0.012(6) -0.009(5) C27 0.073(6) 0.046(5) 0.090(8) -0.003(5) 0.014(5) 0.002(5) C36 0.043(5) 0.056(6) 0.107(8) 0.006(5) 0.014(5) -0.006(4) C22 0.049(6) 0.089(8) 0.098(9) -0.022(7) -0.020(6) 0.001(5) C23 0.058(6) 0.058(6) 0.116(10) -0.015(6) -0.002(6) -0.006(5) C34 0.065(7) 0.109(10) 0.107(10) -0.013(8) 0.027(7) -0.035(7) C29 0.062(6) 0.070(7) 0.156(12) -0.016(7) 0.049(7) 0.015(5) C35 0.053(6) 0.084(8) 0.144(11) -0.005(7) 0.027(6) -0.014(6) C39 0.100(8) 0.067(7) 0.064(7) -0.015(5) 0.029(6) -0.019(6) C40 0.079(8) 0.069(8) 0.144(12) -0.039(8) 0.055(8) -0.009(6) C41 0.061(7) 0.070(7) 0.155(13) -0.027(8) 0.013(8) 0.020(5) _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 =aken into account individually in the estimation of esds in distances, =ngles and torsion angles; correlations between esds in cell parameters are =nly used when they are defined by crystal symmetry. An approximate =isotropic) treatment of cell esds is used for estimating esds involving l.s. =lanes. ; 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 P2 2.3231(19) . ? Pd1 P2 2.3231(19) 3_556 ? Pd1 P1 2.3366(18) 3_556 ? Pd1 P1 2.3366(18) . ? P2 C7 1.786(8) . ? P2 C13 1.806(7) . ? P2 C2 1.827(7) . ? P1 C3 1.818(6) . ? P1 C5 1.821(7) . ? P1 C1 1.828(7) . ? P4 C31 1.813(8) . ? P4 C37 1.829(8) . ? P4 C6 1.857(7) . ? P3 C19 1.798(9) . ? P3 C25 1.827(8) . ? P3 C4 1.841(7) . ? Cl7 C101 1.759(9) . ? Cl2 C100 1.755(9) . ? Cl3 C100 1.743(9) . ? Cl4 C100 1.753(8) . ? Cl6 C101 1.724(9) . ? Cl5 C101 1.734(8) . ? C7 C8 1.389(9) . ? C7 C12 1.407(9) . ? C5 C6 1.531(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C1 C2 1.528(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 C4 1.530(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C13 C18 1.378(10) . ? C13 C14 1.387(9) . ? C18 C17 1.387(10) . ? C18 H18 0.9300 . ? C8 C9 1.396(10) . ? C8 H8 0.9300 . ? C31 C36 1.380(10) . ? C31 C32 1.389(10) . ? C14 C15 1.405(11) . ? C14 H14 0.9300 . ? C37 C42 1.372(10) . ? C37 C38 1.379(11) . ? C19 C24 1.393(11) . ? C19 C20 1.413(11) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C25 C26 1.373(10) . ? C25 C30 1.406(10) . ? C12 C11 1.390(10) . ? C12 H12 0.9300 . ? C28 C27 1.353(11) . ? C28 C29 1.369(12) . ? C28 H28 0.9300 . ? C20 C21 1.378(12) . ? C20 H20 0.9300 . ? C30 C29 1.376(11) . ? C30 H30 0.9300 . ? C24 C23 1.376(13) . ? C24 H24 0.9300 . ? C26 C27 1.381(10) . ? C26 H26 0.9300 . ? C32 C33 1.373(11) . ? C32 H32 0.9300 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C38 C39 1.395(12) . ? C38 H38 0.9300 . ? C42 C41 1.392(12) . ? C42 H42 0.9300 . ? C10 C9 1.361(12) . ? C10 C11 1.385(11) . ? C10 H10 0.9300 . ? C33 C34 1.372(13) . ? C33 H33 0.9300 . ? C11 H11 0.9300 . ? C17 C16 1.391(13) . ? C17 H17 0.9300 . ? C15 C16 1.371(13) . ? C15 H15 0.9300 . ? C9 H9 0.9300 . ? C21 C22 1.384(13) . ? C21 H21 0.9300 . ? C16 H16 0.9300 . ? C27 H27 0.9300 . ? C36 C35 1.393(11) . ? C36 H36 0.9300 . ? C22 C23 1.355(13) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C34 C35 1.358(13) . ? C34 H34 0.9300 . ? C29 H29 0.9300 . ? C35 H35 0.9300 . ? C39 C40 1.382(14) . ? C39 H39 0.9300 . ? C40 C41 1.332(15) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? 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 P2 Pd1 P2 180.0 . 3_556 ? P2 Pd1 P1 96.38(7) . 3_556 ? P2 Pd1 P1 83.62(7) 3_556 3_556 ? P2 Pd1 P1 83.62(7) . . ? P2 Pd1 P1 96.38(7) 3_556 . ? P1 Pd1 P1 180.0 3_556 . ? C7 P2 C13 106.8(3) . . ? C7 P2 C2 107.0(3) . . ? C13 P2 C2 106.3(3) . . ? C7 P2 Pd1 119.0(3) . . ? C13 P2 Pd1 111.3(2) . . ? C2 P2 Pd1 105.6(2) . . ? C3 P1 C5 103.3(3) . . ? C3 P1 C1 105.3(3) . . ? C5 P1 C1 104.6(3) . . ? C3 P1 Pd1 113.7(2) . . ? C5 P1 Pd1 120.2(2) . . ? C1 P1 Pd1 108.4(2) . . ? C31 P4 C37 100.4(3) . . ? C31 P4 C6 102.4(4) . . ? C37 P4 C6 100.4(3) . . ? C19 P3 C25 101.8(4) . . ? C19 P3 C4 99.6(4) . . ? C25 P3 C4 101.7(3) . . ? C8 C7 C12 118.7(7) . . ? C8 C7 P2 121.9(6) . . ? C12 C7 P2 119.2(5) . . ? C6 C5 P1 117.3(5) . . ? C6 C5 H5A 108.0 . . ? P1 C5 H5A 108.0 . . ? C6 C5 H5B 108.0 . . ? P1 C5 H5B 108.0 . . ? H5A C5 H5B 107.2 . . ? C2 C1 P1 112.1(5) . . ? C2 C1 H1A 109.2 . . ? P1 C1 H1A 109.2 . . ? C2 C1 H1B 109.2 . . ? P1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C4 C3 P1 116.3(5) . . ? C4 C3 H3A 108.2 . . ? P1 C3 H3A 108.2 . . ? C4 C3 H3B 108.2 . . ? P1 C3 H3B 108.2 . . ? H3A C3 H3B 107.4 . . ? C18 C13 C14 120.3(7) . . ? C18 C13 P2 120.2(6) . . ? C14 C13 P2 119.4(6) . . ? C13 C18 C17 121.1(8) . . ? C13 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C7 C8 C9 121.1(8) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C36 C31 C32 116.4(8) . . ? C36 C31 P4 123.8(6) . . ? C32 C31 P4 119.6(6) . . ? C13 C14 C15 118.6(8) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C42 C37 C38 118.4(8) . . ? C42 C37 P4 118.4(7) . . ? C38 C37 P4 123.2(6) . . ? C24 C19 C20 115.1(8) . . ? C24 C19 P3 119.4(7) . . ? C20 C19 P3 125.4(6) . . ? C3 C4 P3 110.3(5) . . ? C3 C4 H4A 109.6 . . ? P3 C4 H4A 109.6 . . ? C3 C4 H4B 109.6 . . ? P3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C5 C6 P4 109.1(5) . . ? C5 C6 H6A 109.9 . . ? P4 C6 H6A 109.9 . . ? C5 C6 H6B 109.9 . . ? P4 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? C26 C25 C30 117.1(7) . . ? C26 C25 P3 127.4(6) . . ? C30 C25 P3 115.4(6) . . ? C11 C12 C7 119.6(7) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C27 C28 C29 119.3(9) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C21 C20 C19 122.4(9) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C29 C30 C25 120.8(8) . . ? C29 C30 H30 119.6 . . ? C25 C30 H30 119.6 . . ? Cl6 C101 Cl5 112.4(5) . . ? Cl6 C101 Cl7 108.0(5) . . ? Cl5 C101 Cl7 110.5(5) . . ? C23 C24 C19 121.9(9) . . ? C23 C24 H24 119.0 . . ? C19 C24 H24 119.0 . . ? C25 C26 C27 121.1(8) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C33 C32 C31 122.1(9) . . ? C33 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? C1 C2 P2 108.2(5) . . ? C1 C2 H2A 110.1 . . ? P2 C2 H2A 110.1 . . ? C1 C2 H2B 110.1 . . ? P2 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C37 C38 C39 119.9(9) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C37 C42 C41 121.5(10) . . ? C37 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? Cl3 C100 Cl4 109.6(5) . . ? Cl3 C100 Cl2 110.0(4) . . ? Cl4 C100 Cl2 110.4(5) . . ? C9 C10 C11 121.2(8) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C34 C33 C32 120.0(9) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C10 C11 C12 120.0(8) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C18 C17 C16 118.6(9) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C16 C15 C14 120.6(9) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C10 C9 C8 119.3(8) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C20 C21 C22 120.0(10) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C15 C16 C17 120.7(8) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C28 C27 C26 121.2(9) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C31 C36 C35 121.7(9) . . ? C31 C36 H36 119.1 . . ? C35 C36 H36 119.1 . . ? C23 C22 C21 118.7(10) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 121.8(9) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C35 C34 C33 119.7(10) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C28 C29 C30 120.4(8) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C34 C35 C36 120.0(10) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C40 C39 C38 119.8(10) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C41 C40 C39 120.7(10) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C40 C41 C42 119.7(11) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? 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 P2 C7 152(100) 3_556 . . . ? P1 Pd1 P2 C7 -32.3(3) 3_556 . . . ? P1 Pd1 P2 C7 147.7(3) . . . . ? P2 Pd1 P2 C13 -83(100) 3_556 . . . ? P1 Pd1 P2 C13 92.6(2) 3_556 . . . ? P1 Pd1 P2 C13 -87.4(2) . . . . ? P2 Pd1 P2 C2 32(100) 3_556 . . . ? P1 Pd1 P2 C2 -152.4(3) 3_556 . . . ? P1 Pd1 P2 C2 27.6(3) . . . . ? P2 Pd1 P1 C3 -122.2(3) . . . . ? P2 Pd1 P1 C3 57.8(3) 3_556 . . . ? P1 Pd1 P1 C3 7(5) 3_556 . . . ? P2 Pd1 P1 C5 114.6(3) . . . . ? P2 Pd1 P1 C5 -65.4(3) 3_556 . . . ? P1 Pd1 P1 C5 -116(5) 3_556 . . . ? P2 Pd1 P1 C1 -5.5(3) . . . . ? P2 Pd1 P1 C1 174.5(3) 3_556 . . . ? P1 Pd1 P1 C1 123(5) 3_556 . . . ? C13 P2 C7 C8 -18.3(7) . . . . ? C2 P2 C7 C8 -131.8(6) . . . . ? Pd1 P2 C7 C8 108.8(6) . . . . ? C13 P2 C7 C12 166.2(6) . . . . ? C2 P2 C7 C12 52.6(7) . . . . ? Pd1 P2 C7 C12 -66.8(6) . . . . ? C3 P1 C5 C6 173.5(6) . . . . ? C1 P1 C5 C6 63.6(6) . . . . ? Pd1 P1 C5 C6 -58.4(6) . . . . ? C3 P1 C1 C2 98.7(5) . . . . ? C5 P1 C1 C2 -152.7(5) . . . . ? Pd1 P1 C1 C2 -23.3(6) . . . . ? C5 P1 C3 C4 -45.2(6) . . . . ? C1 P1 C3 C4 64.2(6) . . . . ? Pd1 P1 C3 C4 -177.2(5) . . . . ? C7 P2 C13 C18 113.0(6) . . . . ? C2 P2 C13 C18 -133.0(6) . . . . ? Pd1 P2 C13 C18 -18.4(6) . . . . ? C7 P2 C13 C14 -65.2(7) . . . . ? C2 P2 C13 C14 48.8(7) . . . . ? Pd1 P2 C13 C14 163.4(5) . . . . ? C14 C13 C18 C17 1.1(11) . . . . ? P2 C13 C18 C17 -177.1(6) . . . . ? C12 C7 C8 C9 -0.1(12) . . . . ? P2 C7 C8 C9 -175.7(7) . . . . ? C37 P4 C31 C36 130.5(7) . . . . ? C6 P4 C31 C36 27.3(8) . . . . ? C37 P4 C31 C32 -54.8(7) . . . . ? C6 P4 C31 C32 -158.0(6) . . . . ? C18 C13 C14 C15 0.4(11) . . . . ? P2 C13 C14 C15 178.6(6) . . . . ? C31 P4 C37 C42 127.6(7) . . . . ? C6 P4 C37 C42 -127.6(6) . . . . ? C31 P4 C37 C38 -54.8(7) . . . . ? C6 P4 C37 C38 49.9(7) . . . . ? C25 P3 C19 C24 -159.0(6) . . . . ? C4 P3 C19 C24 96.9(6) . . . . ? C25 P3 C19 C20 20.9(8) . . . . ? C4 P3 C19 C20 -83.2(7) . . . . ? P1 C3 C4 P3 -167.5(4) . . . . ? C19 P3 C4 C3 -73.9(6) . . . . ? C25 P3 C4 C3 -178.3(5) . . . . ? P1 C5 C6 P4 -169.5(4) . . . . ? C31 P4 C6 C5 157.9(5) . . . . ? C37 P4 C6 C5 54.7(6) . . . . ? C19 P3 C25 C26 -93.0(8) . . . . ? C4 P3 C25 C26 9.5(9) . . . . ? C19 P3 C25 C30 89.8(7) . . . . ? C4 P3 C25 C30 -167.7(7) . . . . ? C8 C7 C12 C11 -0.4(11) . . . . ? P2 C7 C12 C11 175.3(6) . . . . ? C24 C19 C20 C21 -2.7(12) . . . . ? P3 C19 C20 C21 177.4(7) . . . . ? C26 C25 C30 C29 2.7(14) . . . . ? P3 C25 C30 C29 -179.8(8) . . . . ? C20 C19 C24 C23 2.5(12) . . . . ? P3 C19 C24 C23 -177.6(7) . . . . ? C30 C25 C26 C27 -2.5(13) . . . . ? P3 C25 C26 C27 -179.6(7) . . . . ? C36 C31 C32 C33 -0.3(12) . . . . ? P4 C31 C32 C33 -175.3(7) . . . . ? P1 C1 C2 P2 47.1(6) . . . . ? C7 P2 C2 C1 -177.4(5) . . . . ? C13 P2 C2 C1 68.8(6) . . . . ? Pd1 P2 C2 C1 -49.7(5) . . . . ? C42 C37 C38 C39 2.0(12) . . . . ? P4 C37 C38 C39 -175.6(6) . . . . ? C38 C37 C42 C41 -1.4(13) . . . . ? P4 C37 C42 C41 176.2(7) . . . . ? C31 C32 C33 C34 -0.9(14) . . . . ? C9 C10 C11 C12 1.5(15) . . . . ? C7 C12 C11 C10 -0.2(13) . . . . ? C13 C18 C17 C16 -2.3(12) . . . . ? C13 C14 C15 C16 -0.6(13) . . . . ? C11 C10 C9 C8 -2.0(15) . . . . ? C7 C8 C9 C10 1.3(13) . . . . ? C19 C20 C21 C22 2.5(15) . . . . ? C14 C15 C16 C17 -0.6(15) . . . . ? C18 C17 C16 C15 2.0(14) . . . . ? C29 C28 C27 C26 -0.3(16) . . . . ? C25 C26 C27 C28 1.3(15) . . . . ? C32 C31 C36 C35 0.9(13) . . . . ? P4 C31 C36 C35 175.7(8) . . . . ? C20 C21 C22 C23 -1.8(15) . . . . ? C21 C22 C23 C24 1.6(16) . . . . ? C19 C24 C23 C22 -2.0(15) . . . . ? C32 C33 C34 C35 1.6(16) . . . . ? C27 C28 C29 C30 0.6(17) . . . . ? C25 C30 C29 C28 -1.8(17) . . . . ? C33 C34 C35 C36 -1.1(17) . . . . ? C31 C36 C35 C34 -0.2(16) . . . . ? C37 C38 C39 C40 -2.3(13) . . . . ? C38 C39 C40 C41 2.1(16) . . . . ? C39 C40 C41 C42 -1.6(17) . . . . ? C37 C42 C41 C40 1.2(15) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.325 _refine_diff_density_min -2.433 _refine_diff_density_rms 0.108 #===END data_PdOCl13 _database_code_depnum_ccdc_archive 'CCDC 835446' #TrackingRef '- CIFS_oxid-V.New.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Pd(P(PO)2)2]Cl2.2MeOH.6H2O ; _chemical_name_common (Pd(P(PO)2)2)Cl2.2MeOH.6H2O _chemical_melting_point ? _chemical_formula_moiety 'C84 H84 Cl14 O4 P8 Pd1 Sn6' _chemical_formula_sum 'C86 H90 Cl2 O12 P8 Pd' _chemical_formula_weight 1740.64 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' 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 11.808(6) _cell_length_b 13.975(7) _cell_length_c 15.675(7) _cell_angle_alpha 105.495(7) _cell_angle_beta 98.909(7) _cell_angle_gamma 102.948(7) _cell_volume 2364.9(19) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 938 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 25.84 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 902 _exptl_absorpt_coefficient_mu 0.441 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8574 _exptl_absorpt_correction_T_max 0.9131 _exptl_absorpt_process_details sadabs _exptl_special_details ; [Pd(P(PO)2)2]Cl2.2MeOH.6H2O ; _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_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25012 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.43 _reflns_number_total 9623 _reflns_number_gt 7033 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction 'BRUKER Shelxtl' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, =999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR =nd 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 =s not relevant to the choice of reflections for refinement. R-factors =ased on F^2^ are statistically about twice as large as those based on F, and =- 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^)+(0.1384P)^2^+4.2383P] where ==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9623 _refine_ls_number_parameters 489 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.2402 _refine_ls_wR_factor_gt 0.2029 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.0000 0.0000 0.0000 0.03211(18) Uani 1 2 d S . . P2 P -0.12075(11) 0.08161(10) 0.08120(8) 0.0334(3) Uani 1 1 d . . . P1 P -0.09600(10) 0.04486(9) -0.11956(8) 0.0326(3) Uani 1 1 d . . . P3 P -0.41746(14) -0.19828(12) -0.29486(11) 0.0519(4) Uani 1 1 d . . . P4 P 0.0631(2) 0.25172(14) -0.27093(12) 0.0694(5) Uani 1 1 d . . . 01 O -0.4621(5) -0.1193(4) -0.3261(4) 0.0783(14) Uiso 1 1 d . . . C7 C -0.0669(4) 0.1491(4) 0.2026(3) 0.0407(11) Uani 1 1 d . . . O2 O 0.1393(7) 0.3405(5) -0.1926(4) 0.115(3) Uani 1 1 d . . . C13 C -0.2665(4) -0.0027(4) 0.0733(3) 0.0393(11) Uani 1 1 d . . . C5 C 0.0097(5) 0.1296(4) -0.1608(4) 0.0427(11) Uani 1 1 d . . . H5A H 0.0536 0.1908 -0.1102 0.051 Uiso 1 1 calc R . . H5B H 0.0668 0.0938 -0.1815 0.051 Uiso 1 1 calc R . . C3 C -0.1923(5) -0.0572(4) -0.2219(3) 0.0409(11) Uani 1 1 d . . . H3A H -0.2335 -0.0255 -0.2602 0.049 Uiso 1 1 calc R . . H3B H -0.1425 -0.0912 -0.2559 0.049 Uiso 1 1 calc R . . C1 C -0.1954(5) 0.1209(4) -0.0758(4) 0.0439(12) Uani 1 1 d . . . H1A H -0.2001 0.1711 -0.1077 0.053 Uiso 1 1 calc R . . H1B H -0.2750 0.0753 -0.0873 0.053 Uiso 1 1 calc R . . C18 C -0.2916(5) -0.1093(4) 0.0394(4) 0.0480(12) Uani 1 1 d . . . H18 H -0.2362 -0.1393 0.0149 0.058 Uiso 1 1 calc R . . C12 C -0.1052(5) 0.1039(5) 0.2658(4) 0.0508(13) Uani 1 1 d . . . H12 H -0.1623 0.0400 0.2462 0.061 Uiso 1 1 calc R . . C4 C -0.2856(5) -0.1393(4) -0.2014(4) 0.0446(12) Uani 1 1 d . . . H4A H -0.3090 -0.1073 -0.1465 0.053 Uiso 1 1 calc R . . H4B H -0.2502 -0.1925 -0.1907 0.053 Uiso 1 1 calc R . . C2 C -0.1500(5) 0.1768(4) 0.0256(3) 0.0428(11) Uani 1 1 d . . . H2A H -0.2092 0.2072 0.0496 0.051 Uiso 1 1 calc R . . H2B H -0.0773 0.2315 0.0368 0.051 Uiso 1 1 calc R . . C25 C -0.3823(6) -0.2900(6) -0.3863(4) 0.0637(17) Uani 1 1 d . . . C8 C 0.0177(5) 0.2452(5) 0.2331(4) 0.0515(13) Uani 1 1 d . . . H8 H 0.0453 0.2765 0.1919 0.062 Uiso 1 1 calc R . . C34 C -0.145(2) 0.3721(15) -0.4710(11) 0.171(10) Uani 1 1 d . . . H34 H -0.1853 0.3976 -0.5116 0.205 Uiso 1 1 calc R . . C19 C -0.5277(5) -0.2729(5) -0.2522(5) 0.0572(15) Uani 1 1 d . . . C17 C -0.4002(6) -0.1709(5) 0.0422(5) 0.0656(17) Uani 1 1 d . . . H17 H -0.4179 -0.2425 0.0188 0.079 Uiso 1 1 calc R . . C11 C -0.0585(7) 0.1537(7) 0.3583(4) 0.073(2) Uani 1 1 d . . . H11 H -0.0842 0.1223 0.3999 0.088 Uiso 1 1 calc R . . C14 C -0.3507(5) 0.0404(5) 0.1088(5) 0.0602(16) Uani 1 1 d . . . H14 H -0.3361 0.1118 0.1292 0.072 Uiso 1 1 calc R . . C9 C 0.0606(6) 0.2940(6) 0.3270(5) 0.071(2) Uani 1 1 d . . . H9 H 0.1150 0.3593 0.3482 0.085 Uiso 1 1 calc R . . C6 C -0.0473(6) 0.1637(5) -0.2382(4) 0.0562(15) Uani 1 1 d . . . H6A H -0.1066 0.1974 -0.2190 0.067 Uiso 1 1 calc R . . H6B H -0.0877 0.1032 -0.2905 0.067 Uiso 1 1 calc R . . C31 C -0.0212(10) 0.2932(6) -0.3535(5) 0.080(3) Uani 1 1 d . . . C20 C -0.6467(6) -0.2785(6) -0.2826(6) 0.081(2) Uani 1 1 d . . . H20 H -0.6674 -0.2435 -0.3228 0.098 Uiso 1 1 calc R . . C37 C 0.1521(7) 0.1786(6) -0.3281(5) 0.0682(19) Uani 1 1 d . . . C21 C -0.7350(8) -0.3365(8) -0.2527(10) 0.111(4) Uani 1 1 d . . . H21 H -0.8146 -0.3399 -0.2728 0.133 Uiso 1 1 calc R . . C38 C 0.1175(8) 0.1219(6) -0.4200(5) 0.077(2) Uani 1 1 d . . . H38 H 0.0455 0.1213 -0.4543 0.093 Uiso 1 1 calc R . . C16 C -0.4822(6) -0.1264(7) 0.0797(6) 0.076(2) Uani 1 1 d . . . H16 H -0.5549 -0.1681 0.0810 0.091 Uiso 1 1 calc R . . C10 C 0.0234(7) 0.2466(7) 0.3886(5) 0.078(2) Uani 1 1 d . . . H10 H 0.0548 0.2786 0.4506 0.093 Uiso 1 1 calc R . . C26 C -0.3726(7) -0.3873(6) -0.3802(6) 0.075(2) Uani 1 1 d . . . H26 H -0.3815 -0.4042 -0.3277 0.090 Uiso 1 1 calc R . . C30 C -0.3690(10) -0.2656(8) -0.4625(6) 0.100(3) Uani 1 1 d . . . H30 H -0.3742 -0.2013 -0.4661 0.120 Uiso 1 1 calc R . . C15 C -0.4570(6) -0.0227(7) 0.1142(6) 0.076(2) Uani 1 1 d . . . H15 H -0.5107 0.0068 0.1417 0.092 Uiso 1 1 calc R . . C24 C -0.4995(7) -0.3277(7) -0.1937(6) 0.079(2) Uani 1 1 d . . . H24 H -0.4205 -0.3265 -0.1745 0.095 Uiso 1 1 calc R . . C22 C -0.7055(11) -0.3887(10) -0.1937(9) 0.126(5) Uani 1 1 d . . . H22 H -0.7652 -0.4272 -0.1742 0.152 Uiso 1 1 calc R . . C42 C 0.2588(8) 0.1773(9) -0.2787(7) 0.100(3) Uani 1 1 d . . . H42 H 0.2841 0.2153 -0.2173 0.120 Uiso 1 1 calc R . . C32 C -0.1329(10) 0.2370(8) -0.4067(6) 0.094(3) Uani 1 1 d . . . H32 H -0.1674 0.1716 -0.4037 0.112 Uiso 1 1 calc R . . C28 C -0.3388(9) -0.4307(11) -0.5303(8) 0.118(4) Uani 1 1 d . . . H28 H -0.3251 -0.4776 -0.5794 0.142 Uiso 1 1 calc R . . C27 C -0.3500(8) -0.4578(8) -0.4523(7) 0.097(3) Uani 1 1 d . . . H27 H -0.3425 -0.5214 -0.4484 0.117 Uiso 1 1 calc R . . C39 C 0.1895(9) 0.0656(7) -0.4616(7) 0.093(3) Uani 1 1 d . . . H39 H 0.1658 0.0282 -0.5232 0.112 Uiso 1 1 calc R . . C33 C -0.1946(13) 0.2776(12) -0.4652(7) 0.133(5) Uani 1 1 d . . . H33 H -0.2704 0.2396 -0.5003 0.159 Uiso 1 1 calc R . . C29 C -0.3475(11) -0.3362(11) -0.5365(7) 0.124(4) Uani 1 1 d . . . H29 H -0.3393 -0.3192 -0.5890 0.148 Uiso 1 1 calc R . . C23 C -0.5897(10) -0.3846(8) -0.1636(7) 0.109(3) Uani 1 1 d . . . H23 H -0.5703 -0.4195 -0.1230 0.131 Uiso 1 1 calc R . . C36 C 0.0304(14) 0.3918(7) -0.3578(7) 0.122(4) Uani 1 1 d . . . H36 H 0.1056 0.4310 -0.3223 0.147 Uiso 1 1 calc R . . C40 C 0.2968(10) 0.0662(10) -0.4098(9) 0.111(3) Uani 1 1 d . . . H40 H 0.3458 0.0300 -0.4370 0.133 Uiso 1 1 calc R . . C41 C 0.3296(9) 0.1192(11) -0.3202(9) 0.118(4) Uani 1 1 d . . . H41 H 0.3999 0.1173 -0.2855 0.142 Uiso 1 1 calc R . . C35 C -0.036(2) 0.4300(10) -0.4182(10) 0.170(10) Uani 1 1 d . . . H35 H -0.0040 0.4958 -0.4215 0.204 Uiso 1 1 calc R . . Cl1 Cl 0.81998(19) 0.69114(18) 0.92128(14) 0.0812(6) Uani 1 1 d . . . O3 O 0.6491(9) 0.0586(7) 0.6368(6) 0.139(3) Uani 1 1 d . . . O5 O 0.3356(15) 0.4033(11) 0.9521(8) 0.249(8) Uani 1 1 d . . . C50 C 0.6997(10) 0.3489(6) 0.8077(8) 0.113(4) Uani 1 1 d . . . H50A H 0.6945 0.3764 0.8696 0.170 Uiso 1 1 calc R . . H50B H 0.6417 0.3656 0.7682 0.170 Uiso 1 1 calc R . . H50C H 0.7782 0.3786 0.8012 0.170 Uiso 1 1 calc R . . O50 O 0.6762(10) 0.2371(7) 0.7835(8) 0.167(4) Uani 1 1 d . . . 04 O -0.007(2) 0.3914(12) -0.0359(12) 0.302(10) Uani 1 1 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 0.0278(3) 0.0421(3) 0.0303(3) 0.0158(2) 0.00666(19) 0.0118(2) P2 0.0294(6) 0.0399(7) 0.0323(6) 0.0117(5) 0.0074(5) 0.0119(5) P1 0.0302(6) 0.0389(6) 0.0319(6) 0.0163(5) 0.0048(5) 0.0111(5) P3 0.0433(8) 0.0499(8) 0.0544(9) 0.0153(7) -0.0050(6) 0.0092(6) P4 0.1011(15) 0.0558(10) 0.0494(9) 0.0274(8) 0.0196(9) 0.0029(9) C7 0.034(3) 0.051(3) 0.036(2) 0.008(2) 0.006(2) 0.016(2) O2 0.165(7) 0.076(4) 0.063(3) 0.015(3) 0.013(4) -0.030(4) C13 0.032(2) 0.048(3) 0.037(2) 0.013(2) 0.0060(19) 0.011(2) C5 0.043(3) 0.049(3) 0.041(3) 0.022(2) 0.011(2) 0.011(2) C3 0.038(3) 0.043(3) 0.037(2) 0.014(2) 0.001(2) 0.008(2) C1 0.038(3) 0.051(3) 0.048(3) 0.022(2) 0.004(2) 0.019(2) C18 0.045(3) 0.050(3) 0.047(3) 0.016(2) 0.008(2) 0.011(2) C12 0.053(3) 0.063(4) 0.036(3) 0.013(2) 0.011(2) 0.019(3) C4 0.041(3) 0.045(3) 0.042(3) 0.014(2) 0.000(2) 0.007(2) C2 0.045(3) 0.044(3) 0.042(3) 0.013(2) 0.010(2) 0.017(2) C25 0.046(3) 0.071(4) 0.054(3) 0.009(3) 0.003(3) -0.004(3) C8 0.040(3) 0.056(3) 0.050(3) 0.009(3) 0.008(2) 0.009(2) C34 0.32(3) 0.205(19) 0.128(12) 0.129(13) 0.137(14) 0.21(2) C19 0.039(3) 0.053(3) 0.065(4) 0.004(3) 0.008(3) 0.006(3) C17 0.060(4) 0.053(4) 0.073(4) 0.022(3) 0.001(3) 0.001(3) C11 0.082(5) 0.100(6) 0.039(3) 0.018(3) 0.016(3) 0.029(4) C14 0.040(3) 0.065(4) 0.071(4) 0.009(3) 0.018(3) 0.016(3) C9 0.047(4) 0.070(4) 0.064(4) -0.013(3) -0.002(3) 0.007(3) C6 0.062(4) 0.065(4) 0.052(3) 0.037(3) 0.012(3) 0.015(3) C31 0.150(9) 0.057(4) 0.055(4) 0.031(3) 0.044(5) 0.040(5) C20 0.045(4) 0.066(4) 0.109(6) -0.004(4) 0.004(4) 0.015(3) C37 0.070(4) 0.073(4) 0.061(4) 0.039(3) 0.010(3) 0.000(3) C21 0.041(4) 0.083(6) 0.169(11) -0.015(7) 0.025(6) 0.005(4) C38 0.081(5) 0.080(5) 0.069(5) 0.026(4) 0.013(4) 0.017(4) C16 0.038(3) 0.094(6) 0.092(5) 0.038(5) 0.015(3) 0.001(3) C10 0.072(5) 0.099(6) 0.039(3) -0.005(4) 0.002(3) 0.019(4) C26 0.060(4) 0.074(5) 0.082(5) 0.011(4) 0.017(4) 0.015(4) C30 0.121(8) 0.093(6) 0.067(5) 0.026(5) 0.020(5) -0.004(5) C15 0.039(3) 0.088(5) 0.091(5) 0.012(4) 0.019(3) 0.013(3) C24 0.054(4) 0.092(5) 0.085(5) 0.034(4) 0.014(4) 0.001(4) C22 0.082(8) 0.106(8) 0.144(11) -0.015(7) 0.058(7) -0.024(6) C42 0.074(6) 0.146(9) 0.079(6) 0.054(6) 0.016(5) 0.010(6) C32 0.141(9) 0.114(7) 0.077(5) 0.065(6) 0.048(6) 0.077(7) C28 0.071(6) 0.130(9) 0.095(7) -0.031(7) 0.026(5) -0.010(6) C27 0.065(5) 0.086(6) 0.110(7) -0.007(5) 0.016(5) 0.007(4) C39 0.096(7) 0.089(6) 0.096(6) 0.032(5) 0.028(5) 0.023(5) C33 0.185(12) 0.207(13) 0.097(7) 0.100(8) 0.070(8) 0.142(11) C29 0.138(10) 0.135(10) 0.074(6) 0.015(7) 0.042(6) 0.000(8) C23 0.097(8) 0.108(7) 0.104(7) 0.036(6) 0.031(6) -0.016(6) C36 0.256(14) 0.062(5) 0.084(6) 0.046(5) 0.084(8) 0.054(7) C40 0.098(8) 0.135(9) 0.134(10) 0.074(8) 0.055(7) 0.043(7) C41 0.072(6) 0.190(12) 0.110(8) 0.075(9) 0.023(6) 0.036(7) C35 0.39(3) 0.096(9) 0.125(11) 0.086(9) 0.150(15) 0.140(14) Cl1 0.0860(13) 0.1016(14) 0.0812(12) 0.0419(11) 0.0333(10) 0.0496(12) O3 0.153(7) 0.133(6) 0.157(7) 0.084(6) 0.042(6) 0.040(6) O5 0.320(18) 0.206(12) 0.138(9) 0.060(9) -0.009(10) -0.052(12) C50 0.165(10) 0.047(4) 0.176(10) 0.073(6) 0.073(8) 0.055(5) O50 0.190(10) 0.130(7) 0.180(9) 0.056(7) 0.021(8) 0.046(7) 04 0.45(3) 0.201(13) 0.254(17) 0.051(12) -0.020(16) 0.188(16) _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 =aken into account individually in the estimation of esds in distances, =ngles and torsion angles; correlations between esds in cell parameters are =nly used when they are defined by crystal symmetry. An approximate =isotropic) treatment of cell esds is used for estimating esds involving l.s. =lanes. ; 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 P2 2.3386(14) 2 ? Pd1 P2 2.3386(14) . ? Pd1 P1 2.3406(13) 2 ? Pd1 P1 2.3406(13) . ? P2 C13 1.820(5) . ? P2 C7 1.821(5) . ? P2 C2 1.838(5) . ? P1 C5 1.837(5) . ? P1 C3 1.841(5) . ? P1 C1 1.842(5) . ? P3 01 1.485(6) . ? P3 C19 1.806(7) . ? P3 C25 1.819(7) . ? P3 C4 1.823(5) . ? P4 O2 1.484(6) . ? P4 C37 1.799(9) . ? P4 C31 1.807(9) . ? P4 C6 1.817(6) . ? C7 C12 1.389(8) . ? C7 C8 1.392(8) . ? C13 C18 1.386(8) . ? C13 C14 1.386(8) . ? C5 C6 1.534(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C3 C4 1.541(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C1 C2 1.520(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C18 C17 1.389(9) . ? C18 H18 0.9300 . ? C12 C11 1.389(9) . ? C12 H12 0.9300 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C25 C30 1.349(11) . ? C25 C26 1.417(11) . ? C8 C9 1.403(9) . ? C8 H8 0.9300 . ? C34 C33 1.35(2) . ? C34 C35 1.36(3) . ? C34 H34 0.9300 . ? C19 C24 1.390(11) . ? C19 C20 1.390(9) . ? C17 C16 1.387(11) . ? C17 H17 0.9300 . ? C11 C10 1.346(11) . ? C11 H11 0.9300 . ? C14 C15 1.391(10) . ? C14 H14 0.9300 . ? C9 C10 1.381(11) . ? C9 H9 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C31 C32 1.377(13) . ? C31 C36 1.400(11) . ? C20 C21 1.393(15) . ? C20 H20 0.9300 . ? C37 C42 1.379(12) . ? C37 C38 1.390(10) . ? C21 C22 1.373(17) . ? C21 H21 0.9300 . ? C38 C39 1.402(12) . ? C38 H38 0.9300 . ? C16 C15 1.348(11) . ? C16 H16 0.9300 . ? C10 H10 0.9300 . ? C26 C27 1.391(12) . ? C26 H26 0.9300 . ? C30 C29 1.405(15) . ? C30 H30 0.9300 . ? C15 H15 0.9300 . ? C24 C23 1.403(11) . ? C24 H24 0.9300 . ? C22 C23 1.358(16) . ? C22 H22 0.9300 . ? C42 C41 1.404(15) . ? C42 H42 0.9300 . ? C32 C33 1.396(12) . ? C32 H32 0.9300 . ? C28 C29 1.375(18) . ? C28 C27 1.389(16) . ? C28 H28 0.9300 . ? C27 H27 0.9300 . ? C39 C40 1.392(15) . ? C39 H39 0.9300 . ? C33 H33 0.9300 . ? C29 H29 0.9300 . ? C23 H23 0.9300 . ? C36 C35 1.42(2) . ? C36 H36 0.9300 . ? C40 C41 1.349(16) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C35 H35 0.9300 . ? C50 O50 1.456(11) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? 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 P2 Pd1 P2 180.00(8) 2 . ? P2 Pd1 P1 83.67(5) 2 2 ? P2 Pd1 P1 96.33(5) . 2 ? P2 Pd1 P1 96.33(5) 2 . ? P2 Pd1 P1 83.67(5) . . ? P1 Pd1 P1 180.00(5) 2 . ? C13 P2 C7 103.2(2) . . ? C13 P2 C2 105.8(2) . . ? C7 P2 C2 107.5(2) . . ? C13 P2 Pd1 114.53(17) . . ? C7 P2 Pd1 119.96(16) . . ? C2 P2 Pd1 104.85(17) . . ? C5 P1 C3 105.7(2) . . ? C5 P1 C1 105.8(3) . . ? C3 P1 C1 104.3(2) . . ? C5 P1 Pd1 112.05(17) . . ? C3 P1 Pd1 119.82(17) . . ? C1 P1 Pd1 108.16(17) . . ? 01 P3 C19 111.3(3) . . ? 01 P3 C25 112.1(3) . . ? C19 P3 C25 106.6(3) . . ? 01 P3 C4 111.8(3) . . ? C19 P3 C4 106.0(3) . . ? C25 P3 C4 108.8(3) . . ? O2 P4 C37 110.9(4) . . ? O2 P4 C31 111.8(4) . . ? C37 P4 C31 107.7(3) . . ? O2 P4 C6 112.9(3) . . ? C37 P4 C6 107.8(3) . . ? C31 P4 C6 105.4(4) . . ? C12 C7 C8 119.2(5) . . ? C12 C7 P2 120.8(4) . . ? C8 C7 P2 119.9(4) . . ? C18 C13 C14 119.3(5) . . ? C18 C13 P2 121.4(4) . . ? C14 C13 P2 119.1(4) . . ? C6 C5 P1 114.9(4) . . ? C6 C5 H5A 108.5 . . ? P1 C5 H5A 108.5 . . ? C6 C5 H5B 108.5 . . ? P1 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C4 C3 P1 113.7(4) . . ? C4 C3 H3A 108.8 . . ? P1 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? P1 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C2 C1 P1 111.0(3) . . ? C2 C1 H1A 109.4 . . ? P1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? P1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C13 C18 C17 119.4(6) . . ? C13 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C7 C12 C11 120.2(6) . . ? C7 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C3 C4 P3 111.6(4) . . ? C3 C4 H4A 109.3 . . ? P3 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? P3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C1 C2 P2 107.9(4) . . ? C1 C2 H2A 110.1 . . ? P2 C2 H2A 110.1 . . ? C1 C2 H2B 110.1 . . ? P2 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C30 C25 C26 119.6(8) . . ? C30 C25 P3 118.9(7) . . ? C26 C25 P3 121.4(6) . . ? C7 C8 C9 118.8(6) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C33 C34 C35 120.6(13) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C24 C19 C20 118.9(7) . . ? C24 C19 P3 123.2(5) . . ? C20 C19 P3 117.8(6) . . ? C16 C17 C18 120.4(6) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C10 C11 C12 121.1(7) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C13 C14 C15 120.4(6) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C10 C9 C8 121.0(7) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C5 C6 P4 111.8(4) . . ? C5 C6 H6A 109.3 . . ? P4 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? P4 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C32 C31 C36 119.8(9) . . ? C32 C31 P4 124.2(6) . . ? C36 C31 P4 115.9(9) . . ? C19 C20 C21 119.8(10) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C42 C37 C38 118.3(9) . . ? C42 C37 P4 118.8(7) . . ? C38 C37 P4 122.9(6) . . ? C22 C21 C20 120.6(9) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C37 C38 C39 120.9(8) . . ? C37 C38 H38 119.5 . . ? C39 C38 H38 119.5 . . ? C15 C16 C17 120.2(6) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C11 C10 C9 119.6(6) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C27 C26 C25 120.4(9) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C25 C30 C29 120.8(10) . . ? C25 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C16 C15 C14 120.2(7) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C19 C24 C23 120.3(8) . . ? C19 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C23 C22 C21 120.5(10) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C37 C42 C41 120.7(10) . . ? C37 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C31 C32 C33 120.3(11) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C29 C28 C27 121.4(10) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C28 C27 C26 118.4(10) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C40 C39 C38 119.3(10) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C34 C33 C32 120.4(15) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C28 C29 C30 119.3(10) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C22 C23 C24 119.9(11) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C31 C36 C35 117.9(14) . . ? C31 C36 H36 121.1 . . ? C35 C36 H36 121.1 . . ? C41 C40 C39 120.0(11) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 120.8(10) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C34 C35 C36 121.0(13) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? O50 C50 H50A 109.5 . . ? O50 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O50 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? 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 P2 Pd1 P2 C13 97(100) 2 . . . ? P1 Pd1 P2 C13 -91.49(18) 2 . . . ? P1 Pd1 P2 C13 88.51(18) . . . . ? P2 Pd1 P2 C7 -139(100) 2 . . . ? P1 Pd1 P2 C7 32.1(2) 2 . . . ? P1 Pd1 P2 C7 -147.9(2) . . . . ? P2 Pd1 P2 C2 -18(100) 2 . . . ? P1 Pd1 P2 C2 152.96(19) 2 . . . ? P1 Pd1 P2 C2 -27.04(19) . . . . ? P2 Pd1 P1 C5 -60.2(2) 2 . . . ? P2 Pd1 P1 C5 119.8(2) . . . . ? P1 Pd1 P1 C5 -26(100) 2 . . . ? P2 Pd1 P1 C3 64.4(2) 2 . . . ? P2 Pd1 P1 C3 -115.6(2) . . . . ? P1 Pd1 P1 C3 99(100) 2 . . . ? P2 Pd1 P1 C1 -176.40(19) 2 . . . ? P2 Pd1 P1 C1 3.60(19) . . . . ? P1 Pd1 P1 C1 -142(100) 2 . . . ? C13 P2 C7 C12 27.2(5) . . . . ? C2 P2 C7 C12 138.9(5) . . . . ? Pd1 P2 C7 C12 -101.6(4) . . . . ? C13 P2 C7 C8 -155.7(4) . . . . ? C2 P2 C7 C8 -44.1(5) . . . . ? Pd1 P2 C7 C8 75.4(5) . . . . ? C7 P2 C13 C18 -118.5(5) . . . . ? C2 P2 C13 C18 128.6(4) . . . . ? Pd1 P2 C13 C18 13.7(5) . . . . ? C7 P2 C13 C14 56.2(5) . . . . ? C2 P2 C13 C14 -56.6(5) . . . . ? Pd1 P2 C13 C14 -171.6(4) . . . . ? C3 P1 C5 C6 48.9(5) . . . . ? C1 P1 C5 C6 -61.4(5) . . . . ? Pd1 P1 C5 C6 -179.0(4) . . . . ? C5 P1 C3 C4 178.0(4) . . . . ? C1 P1 C3 C4 -70.7(4) . . . . ? Pd1 P1 C3 C4 50.4(4) . . . . ? C5 P1 C1 C2 -93.3(4) . . . . ? C3 P1 C1 C2 155.5(4) . . . . ? Pd1 P1 C1 C2 26.9(4) . . . . ? C14 C13 C18 C17 -0.5(9) . . . . ? P2 C13 C18 C17 174.2(5) . . . . ? C8 C7 C12 C11 -0.7(9) . . . . ? P2 C7 C12 C11 176.4(5) . . . . ? P1 C3 C4 P3 152.6(3) . . . . ? 01 P3 C4 C3 -48.0(5) . . . . ? C19 P3 C4 C3 -169.4(4) . . . . ? C25 P3 C4 C3 76.3(5) . . . . ? P1 C1 C2 P2 -50.6(4) . . . . ? C13 P2 C2 C1 -70.0(4) . . . . ? C7 P2 C2 C1 -179.8(4) . . . . ? Pd1 P2 C2 C1 51.5(4) . . . . ? 01 P3 C25 C30 16.8(8) . . . . ? C19 P3 C25 C30 138.7(7) . . . . ? C4 P3 C25 C30 -107.4(7) . . . . ? 01 P3 C25 C26 -161.1(6) . . . . ? C19 P3 C25 C26 -39.1(6) . . . . ? C4 P3 C25 C26 74.8(6) . . . . ? C12 C7 C8 C9 -0.8(8) . . . . ? P2 C7 C8 C9 -177.9(5) . . . . ? 01 P3 C19 C24 -159.0(6) . . . . ? C25 P3 C19 C24 78.5(7) . . . . ? C4 P3 C19 C24 -37.3(7) . . . . ? 01 P3 C19 C20 23.5(6) . . . . ? C25 P3 C19 C20 -99.0(6) . . . . ? C4 P3 C19 C20 145.2(5) . . . . ? C13 C18 C17 C16 -0.8(10) . . . . ? C7 C12 C11 C10 0.7(11) . . . . ? C18 C13 C14 C15 2.9(10) . . . . ? P2 C13 C14 C15 -171.9(6) . . . . ? C7 C8 C9 C10 2.4(10) . . . . ? P1 C5 C6 P4 177.4(3) . . . . ? O2 P4 C6 C5 -52.0(6) . . . . ? C37 P4 C6 C5 70.9(5) . . . . ? C31 P4 C6 C5 -174.3(5) . . . . ? O2 P4 C31 C32 -148.1(7) . . . . ? C37 P4 C31 C32 89.8(8) . . . . ? C6 P4 C31 C32 -25.1(8) . . . . ? O2 P4 C31 C36 28.1(8) . . . . ? C37 P4 C31 C36 -94.0(7) . . . . ? C6 P4 C31 C36 151.1(7) . . . . ? C24 C19 C20 C21 1.3(11) . . . . ? P3 C19 C20 C21 179.0(6) . . . . ? O2 P4 C37 C42 28.7(7) . . . . ? C31 P4 C37 C42 151.3(7) . . . . ? C6 P4 C37 C42 -95.4(7) . . . . ? O2 P4 C37 C38 -152.3(6) . . . . ? C31 P4 C37 C38 -29.6(7) . . . . ? C6 P4 C37 C38 83.7(6) . . . . ? C19 C20 C21 C22 -0.3(14) . . . . ? C42 C37 C38 C39 -0.6(11) . . . . ? P4 C37 C38 C39 -179.7(6) . . . . ? C18 C17 C16 C15 -0.4(12) . . . . ? C12 C11 C10 C9 0.9(12) . . . . ? C8 C9 C10 C11 -2.4(12) . . . . ? C30 C25 C26 C27 -0.2(11) . . . . ? P3 C25 C26 C27 177.6(6) . . . . ? C26 C25 C30 C29 0.9(14) . . . . ? P3 C25 C30 C29 -176.9(8) . . . . ? C17 C16 C15 C14 2.8(13) . . . . ? C13 C14 C15 C16 -4.2(12) . . . . ? C20 C19 C24 C23 -2.2(12) . . . . ? P3 C19 C24 C23 -179.6(7) . . . . ? C20 C21 C22 C23 0.0(17) . . . . ? C38 C37 C42 C41 -0.7(13) . . . . ? P4 C37 C42 C41 178.5(8) . . . . ? C36 C31 C32 C33 0.3(13) . . . . ? P4 C31 C32 C33 176.4(7) . . . . ? C29 C28 C27 C26 1.1(15) . . . . ? C25 C26 C27 C28 -0.8(12) . . . . ? C37 C38 C39 C40 0.4(13) . . . . ? C35 C34 C33 C32 -2(2) . . . . ? C31 C32 C33 C34 0.9(15) . . . . ? C27 C28 C29 C30 -0.4(17) . . . . ? C25 C30 C29 C28 -0.6(17) . . . . ? C21 C22 C23 C24 -0.8(17) . . . . ? C19 C24 C23 C22 1.9(15) . . . . ? C32 C31 C36 C35 -0.1(14) . . . . ? P4 C31 C36 C35 -176.5(8) . . . . ? C38 C39 C40 C41 1.1(15) . . . . ? C39 C40 C41 C42 -2.3(17) . . . . ? C37 C42 C41 C40 2.2(16) . . . . ? C33 C34 C35 C36 2(3) . . . . ? C31 C36 C35 C34 -1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.686 _refine_diff_density_min -1.268 _refine_diff_density_rms 0.138 #===END data_PdClSO7a _database_code_depnum_ccdc_archive 'CCDC 835447' #TrackingRef '- CIFS_oxid-V.New.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Pd(PP2PO)Cl][S(CH3)3(CH2)3(SO3)].4H2O ; _chemical_name_common (Pd(PP2PO)Cl)(S(CH3)3(CH2)3(SO3)).4H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H57 Cl O8 P4 Pd S2' _chemical_formula_weight 1091.79 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' 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' S S 0.1246 0.1234 '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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 36.211(5) _cell_length_b 14.7523(19) _cell_length_c 20.890(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.565(3) _cell_angle_gamma 90.00 _cell_volume 10696(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 884 _cell_measurement_theta_min 3,06 _cell_measurement_theta_max 25,91 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4512 _exptl_absorpt_coefficient_mu 0.642 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8507 _exptl_absorpt_correction_T_max 0.9564 _exptl_absorpt_process_details Sadabs _exptl_special_details ; [Pd(PP2PO)Cl][S(CH3)3(CH2)3(SO3)].4H2O ; _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_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33386 _diffrn_reflns_av_R_equivalents 0.0930 _diffrn_reflns_av_sigmaI/netI 0.1616 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 24.71 _reflns_number_total 9091 _reflns_number_gt 3787 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Shelxtl' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, =999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR =nd 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 =s not relevant to the choice of reflections for refinement. R-factors =ased on F^2^ are statistically about twice as large as those based on F, and =- 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^)+(0.0969P)^2^+0.0000P] where ==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9091 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1715 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.2015 _refine_ls_wR_factor_gt 0.1523 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.891 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.900416(19) 0.29677(4) 0.88943(3) 0.0443(2) Uani 1 1 d . . . P2 P 0.88822(7) 0.33786(17) 0.98882(13) 0.0542(7) Uani 1 1 d . . . Cl1 Cl 0.96523(6) 0.25296(16) 0.93513(12) 0.0592(7) Uani 1 1 d . . . P3 P 0.90370(7) 0.31359(15) 0.78088(12) 0.0501(6) Uani 1 1 d . . . P4 P 0.74112(7) 0.12676(17) 0.79144(13) 0.0534(7) Uani 1 1 d . . . P1 P 0.83808(7) 0.32303(15) 0.84487(13) 0.0506(7) Uani 1 1 d . . . C13 C 0.9099(2) 0.4485(6) 1.0099(4) 0.047(2) Uani 1 1 d . . . C19 C 0.9274(3) 0.4215(6) 0.7793(4) 0.049(2) Uani 1 1 d . . . C10 C 0.9378(7) 0.1765(11) 1.1807(10) 0.147(8) Uani 1 1 d . . . H10 H 0.9492 0.1444 1.2197 0.177 Uiso 1 1 calc R . . C12 C 0.8808(4) 0.2315(9) 1.0951(7) 0.125(5) Uani 1 1 d . . . H12 H 0.8542 0.2358 1.0780 0.150 Uiso 1 1 calc R . . C18 C 0.9388(2) 0.4797(6) 0.9847(5) 0.055(3) Uani 1 1 d . . . H18 H 0.9475 0.4434 0.9555 0.066 Uiso 1 1 calc R . . C20 C 0.9099(3) 0.4905(6) 0.7350(5) 0.056(3) Uani 1 1 d . . . H20 H 0.8860 0.4815 0.7039 0.067 Uiso 1 1 calc R . . C31 C 0.7024(2) 0.1280(5) 0.7155(5) 0.051(2) Uani 1 1 d . . . C7 C 0.9048(4) 0.2721(6) 1.0637(5) 0.065(3) Uani 1 1 d . . . C16 C 0.9433(3) 0.6177(6) 1.0440(5) 0.059(3) Uani 1 1 d . . . H16 H 0.9542 0.6747 1.0550 0.071 Uiso 1 1 calc R . . C14 C 0.8987(3) 0.5035(7) 1.0546(5) 0.058(3) Uani 1 1 d . . . H14 H 0.8801 0.4830 1.0740 0.070 Uiso 1 1 calc R . . C29 C 0.9326(5) 0.0728(9) 0.7174(8) 0.138(7) Uani 1 1 d . . . H29 H 0.9260 0.0125 0.7212 0.166 Uiso 1 1 calc R . . C25 C 0.9260(3) 0.2302(6) 0.7427(4) 0.057(3) Uani 1 1 d . . . C6 C 0.7719(2) 0.2197(5) 0.7836(5) 0.053(2) Uani 1 1 d . . . H6A H 0.7747 0.2194 0.7388 0.063 Uiso 1 1 calc R . . H6B H 0.7595 0.2762 0.7893 0.063 Uiso 1 1 calc R . . C21 C 0.9289(3) 0.5725(6) 0.7386(6) 0.072(3) Uani 1 1 d . . . H21 H 0.9177 0.6190 0.7095 0.086 Uiso 1 1 calc R . . C17 C 0.9553(3) 0.5647(7) 1.0022(5) 0.062(3) Uani 1 1 d . . . H17 H 0.9748 0.5846 0.9847 0.074 Uiso 1 1 calc R . . C1 C 0.8201(3) 0.3914(7) 0.9015(5) 0.067(3) Uani 1 1 d . . . H1A H 0.8277 0.4541 0.8994 0.080 Uiso 1 1 calc R . . H1B H 0.7921 0.3888 0.8888 0.080 Uiso 1 1 calc R . . C2 C 0.8368(3) 0.3547(7) 0.9729(6) 0.072(3) Uani 1 1 d . . . H2A H 0.8244 0.2977 0.9777 0.086 Uiso 1 1 calc R . . H2B H 0.8319 0.3975 1.0049 0.086 Uiso 1 1 calc R . . C37 C 0.7681(3) 0.0263(6) 0.7936(5) 0.055(2) Uani 1 1 d . . . C24 C 0.9632(3) 0.4366(6) 0.8238(5) 0.065(3) Uani 1 1 d . . . H24 H 0.9754 0.3906 0.8526 0.078 Uiso 1 1 calc R . . C38 C 0.7876(3) 0.0049(7) 0.7496(6) 0.072(3) Uiso 1 1 d . . . H38 H 0.7864 0.0446 0.7145 0.086 Uiso 1 1 calc R . . C26 C 0.9510(3) 0.2494(7) 0.7055(5) 0.065(3) Uani 1 1 d . . . H26 H 0.9577 0.3093 0.7004 0.078 Uiso 1 1 calc R . . C3 C 0.8309(3) 0.3738(6) 0.7637(4) 0.059(3) Uani 1 1 d . . . H3A H 0.8039 0.3702 0.7386 0.071 Uiso 1 1 calc R . . H3B H 0.8382 0.4372 0.7686 0.071 Uiso 1 1 calc R . . C42 C 0.7705(3) -0.0356(7) 0.8464(5) 0.069(3) Uani 1 1 d . . . H42 H 0.7579 -0.0224 0.8783 0.082 Uiso 1 1 calc R . . C23 C 0.9811(3) 0.5192(8) 0.8256(5) 0.075(3) Uani 1 1 d . . . H23 H 1.0053 0.5286 0.8556 0.090 Uiso 1 1 calc R . . C27 C 0.9665(4) 0.1790(9) 0.6751(6) 0.086(4) Uani 1 1 d . . . H27 H 0.9834 0.1934 0.6506 0.103 Uiso 1 1 calc R . . C9 C 0.9591(5) 0.2156(8) 1.1510(7) 0.107(5) Uani 1 1 d . . . H9 H 0.9857 0.2117 1.1682 0.128 Uiso 1 1 calc R . . C4 C 0.8551(3) 0.3244(6) 0.7264(5) 0.060(3) Uani 1 1 d . . . H4A H 0.8552 0.3581 0.6866 0.072 Uiso 1 1 calc R . . H4B H 0.8443 0.2649 0.7129 0.072 Uiso 1 1 calc R . . C39 C 0.8097(4) -0.0746(8) 0.7542(7) 0.100(4) Uani 1 1 d . . . H39 H 0.8233 -0.0872 0.7237 0.120 Uiso 1 1 calc R . . C28 C 0.9575(5) 0.0938(10) 0.6807(6) 0.109(5) Uani 1 1 d . . . H28 H 0.9677 0.0483 0.6602 0.131 Uiso 1 1 calc R . . C11 C 0.8988(7) 0.1799(10) 1.1576(8) 0.154(8) Uani 1 1 d . . . H11 H 0.8836 0.1506 1.1803 0.185 Uiso 1 1 calc R . . C41 C 0.7911(4) -0.1149(8) 0.8514(7) 0.100(4) Uani 1 1 d . . . H41 H 0.7920 -0.1560 0.8855 0.120 Uiso 1 1 calc R . . C5 C 0.8124(2) 0.2166(6) 0.8345(5) 0.058(3) Uani 1 1 d . . . H5A H 0.8277 0.1711 0.8202 0.069 Uiso 1 1 calc R . . H5B H 0.8098 0.1978 0.8775 0.069 Uiso 1 1 calc R . . C8 C 0.9435(4) 0.2642(8) 1.0931(6) 0.084(4) Uani 1 1 d . . . H8 H 0.9602 0.2929 1.0731 0.101 Uiso 1 1 calc R . . C15 C 0.9147(3) 0.5887(7) 1.0711(5) 0.069(3) Uani 1 1 d . . . H15 H 0.9063 0.6259 1.1001 0.083 Uiso 1 1 calc R . . C30 C 0.9168(4) 0.1399(7) 0.7493(7) 0.105(5) Uani 1 1 d . . . H30 H 0.9004 0.1241 0.7746 0.126 Uiso 1 1 calc R . . C22 C 0.9640(3) 0.5863(8) 0.7846(6) 0.079(3) Uani 1 1 d . . . H22 H 0.9760 0.6425 0.7872 0.094 Uiso 1 1 calc R . . C40 C 0.8102(4) -0.1319(8) 0.8049(8) 0.098(5) Uani 1 1 d . . . H40 H 0.8243 -0.1854 0.8084 0.118 Uiso 1 1 calc R . . O1 O 0.72705(19) 0.1357(5) 0.8519(3) 0.074(2) Uani 1 1 d . . . O2 O 0.67593(19) 0.0144(5) 0.8861(4) 0.088(2) Uani 1 1 d . . . C34 C 0.6403(4) 0.1400(7) 0.5997(8) 0.096(4) Uani 1 1 d . . . H34 H 0.6198 0.1446 0.5611 0.115 Uiso 1 1 calc R . . C32 C 0.7084(3) 0.1343(6) 0.6529(5) 0.064(3) Uani 1 1 d . . . H32 H 0.7334 0.1354 0.6492 0.077 Uiso 1 1 calc R . . C33 C 0.6773(3) 0.1389(7) 0.5954(6) 0.078(3) Uani 1 1 d . . . H33 H 0.6817 0.1413 0.5537 0.094 Uiso 1 1 calc R . . O4 O 0.7124(3) 0.8591(8) 0.9448(6) 0.174(5) Uani 1 1 d . . . C36 C 0.6638(3) 0.1289(6) 0.7178(6) 0.068(3) Uani 1 1 d . . . H36 H 0.6588 0.1256 0.7590 0.082 Uiso 1 1 calc R . . C35 C 0.6333(3) 0.1344(7) 0.6606(7) 0.088(4) Uani 1 1 d . . . H35 H 0.6082 0.1343 0.6633 0.106 Uiso 1 1 calc R . . S1 S 0.91691(10) 0.9574(2) 0.95346(18) 0.1005(11) Uani 1 1 d . . . C43 C 0.8454(3) 0.8439(9) 1.0573(6) 0.105(4) Uani 1 1 d . . . H43A H 0.8647 0.8146 1.0932 0.126 Uiso 1 1 calc R . . H43B H 0.8343 0.7980 1.0242 0.126 Uiso 1 1 calc R . . C45 C 0.8913(3) 0.8717(7) 0.9894(5) 0.081(3) Uani 1 1 d . . . H45A H 0.8762 0.8333 0.9538 0.097 Uiso 1 1 calc R . . H45B H 0.9101 0.8338 1.0203 0.097 Uiso 1 1 calc R . . C44 C 0.8650(4) 0.9145(8) 1.0257(6) 0.099(4) Uani 1 1 d . . . H44A H 0.8799 0.9548 1.0601 0.118 Uiso 1 1 calc R . . H44B H 0.8456 0.9505 0.9944 0.118 Uiso 1 1 calc R . . C47 C 0.9550(3) 1.0155(8) 1.0229(6) 0.107(4) Uani 1 1 d . . . H47A H 0.9730 0.9711 1.0473 0.160 Uiso 1 1 calc R . . H47B H 0.9429 1.0452 1.0526 0.160 Uiso 1 1 calc R . . H47C H 0.9684 1.0594 1.0040 0.160 Uiso 1 1 calc R . . C46 C 0.8850(4) 1.0489(8) 0.9090(7) 0.126(5) Uani 1 1 d . . . H46A H 0.8997 1.0914 0.8914 0.188 Uiso 1 1 calc R . . H46B H 0.8737 1.0795 0.9393 0.188 Uiso 1 1 calc R . . H46C H 0.8650 1.0235 0.8729 0.188 Uiso 1 1 calc R . . C48 C 0.9410(4) 0.8938(11) 0.8966(7) 0.161(7) Uani 1 1 d . . . H48A H 0.9576 0.8476 0.9217 0.241 Uiso 1 1 calc R . . H48B H 0.9559 0.9354 0.8787 0.241 Uiso 1 1 calc R . . H48C H 0.9216 0.8663 0.8606 0.241 Uiso 1 1 calc R . . S2 S 0.80922(13) 0.8861(4) 1.0892(2) 0.1337(17) Uani 1 1 d . . . O20 O 0.7964(3) 0.8192(8) 1.1222(6) 0.159(5) Uani 1 1 d . . . O21 O 0.7802(3) 0.9250(9) 1.0385(7) 0.198(6) Uani 1 1 d . . . O22 O 0.8308(5) 0.9559(15) 1.1396(9) 0.311(12) Uani 1 1 d . . . O3 O 0.7903(6) 0.1209(10) 0.9931(9) 0.300(10) Uani 1 1 d . . . O5 O 0.7421(8) 0.293(2) 0.9284(15) 0.68(4) Uani 1 1 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 0.0393(4) 0.0450(4) 0.0447(4) -0.0010(3) 0.0059(3) -0.0065(4) P2 0.0490(15) 0.0564(15) 0.0572(18) -0.0073(12) 0.0151(13) -0.0170(13) Cl1 0.0439(13) 0.0665(15) 0.0609(17) 0.0098(12) 0.0049(12) 0.0014(12) P3 0.0512(15) 0.0506(15) 0.0441(16) 0.0004(11) 0.0066(12) -0.0037(12) P4 0.0423(14) 0.0548(16) 0.0589(18) -0.0009(12) 0.0077(13) -0.0111(12) P1 0.0424(14) 0.0440(15) 0.0600(18) -0.0020(11) 0.0058(13) -0.0083(11) C13 0.044(5) 0.052(6) 0.043(6) -0.001(4) 0.009(5) -0.010(4) C19 0.060(6) 0.042(5) 0.043(6) 0.002(4) 0.013(5) 0.002(5) C10 0.21(2) 0.078(11) 0.116(16) -0.007(9) -0.014(16) -0.031(14) C12 0.125(12) 0.135(12) 0.114(13) 0.037(10) 0.032(10) -0.049(10) C18 0.044(6) 0.059(6) 0.069(7) -0.011(5) 0.027(5) -0.008(5) C20 0.049(6) 0.058(6) 0.061(7) 0.003(5) 0.014(5) -0.004(5) C31 0.040(5) 0.038(5) 0.069(7) 0.002(5) 0.006(5) -0.010(4) C7 0.100(9) 0.053(6) 0.050(7) -0.004(5) 0.036(7) -0.032(6) C16 0.042(6) 0.056(6) 0.070(8) -0.010(5) 0.001(5) -0.001(5) C14 0.055(6) 0.073(7) 0.054(7) -0.007(5) 0.025(5) -0.022(5) C29 0.24(2) 0.064(9) 0.131(14) -0.041(9) 0.085(14) 0.009(11) C25 0.079(7) 0.061(6) 0.033(6) -0.005(4) 0.022(5) -0.007(5) C6 0.043(5) 0.046(6) 0.058(6) 0.002(4) -0.002(5) -0.010(4) C21 0.083(8) 0.050(6) 0.094(9) 0.022(6) 0.046(8) 0.002(6) C17 0.050(6) 0.060(6) 0.076(8) -0.005(5) 0.020(6) -0.013(5) C1 0.040(6) 0.071(7) 0.086(9) -0.023(6) 0.014(6) -0.008(5) C2 0.058(7) 0.078(7) 0.090(9) -0.033(6) 0.039(7) -0.032(6) C37 0.054(6) 0.051(6) 0.056(7) 0.003(5) 0.012(5) -0.010(5) C24 0.068(7) 0.058(6) 0.062(7) 0.007(5) 0.007(6) -0.012(6) C26 0.063(7) 0.075(7) 0.052(7) 0.005(5) 0.009(6) 0.007(6) C3 0.045(6) 0.053(6) 0.066(7) 0.017(5) -0.005(5) -0.005(5) C42 0.057(7) 0.063(7) 0.073(8) 0.001(6) -0.002(6) -0.008(6) C23 0.056(7) 0.086(8) 0.074(8) 0.019(6) 0.003(6) -0.028(6) C27 0.089(9) 0.107(11) 0.063(9) -0.003(7) 0.022(7) 0.030(8) C9 0.150(14) 0.071(9) 0.091(11) 0.019(7) 0.020(10) -0.025(9) C4 0.063(7) 0.062(6) 0.052(7) 0.000(5) 0.012(5) -0.011(5) C39 0.103(10) 0.076(9) 0.122(13) -0.023(8) 0.035(9) 0.003(8) C28 0.174(16) 0.093(11) 0.074(10) -0.018(8) 0.058(10) 0.017(10) C11 0.25(2) 0.121(13) 0.101(14) 0.055(10) 0.071(15) -0.060(15) C41 0.097(11) 0.067(9) 0.114(13) 0.029(8) -0.004(9) -0.005(8) C5 0.049(6) 0.058(6) 0.059(7) -0.004(5) 0.002(5) -0.018(5) C8 0.090(9) 0.085(8) 0.065(9) 0.016(6) 0.001(7) -0.011(7) C15 0.072(7) 0.072(7) 0.061(7) -0.024(5) 0.014(6) -0.013(6) C30 0.146(13) 0.056(8) 0.131(12) -0.010(7) 0.071(10) -0.024(8) C22 0.077(8) 0.075(8) 0.084(9) 0.004(7) 0.022(7) -0.035(7) C40 0.092(10) 0.054(8) 0.127(14) 0.016(8) -0.005(9) 0.010(7) O1 0.072(5) 0.088(5) 0.066(5) 0.001(4) 0.024(4) -0.013(4) O2 0.063(5) 0.121(6) 0.083(6) 0.002(4) 0.024(4) -0.013(4) C34 0.065(9) 0.062(8) 0.137(14) 0.018(8) -0.013(9) -0.011(6) C32 0.057(7) 0.067(7) 0.062(8) -0.010(5) 0.005(6) 0.003(5) C33 0.075(8) 0.073(8) 0.067(8) -0.010(6) -0.011(7) -0.006(7) O4 0.106(8) 0.228(12) 0.180(11) 0.114(9) 0.029(8) 0.006(8) C36 0.055(7) 0.065(7) 0.077(8) 0.010(6) 0.008(6) -0.017(6) C35 0.054(7) 0.083(8) 0.110(12) 0.036(8) -0.004(8) -0.008(6) S1 0.101(3) 0.101(3) 0.090(3) 0.012(2) 0.010(2) -0.009(2) C43 0.088(9) 0.154(12) 0.081(10) 0.024(8) 0.038(8) 0.041(9) C45 0.093(9) 0.067(7) 0.081(9) 0.014(6) 0.023(7) 0.005(7) C44 0.105(10) 0.095(10) 0.096(11) 0.007(8) 0.029(9) -0.004(8) C47 0.086(9) 0.123(11) 0.102(11) -0.006(8) 0.011(8) -0.031(8) C46 0.110(11) 0.108(11) 0.138(13) 0.062(9) 0.003(10) -0.006(9) C48 0.155(15) 0.234(19) 0.122(14) -0.074(13) 0.085(13) -0.041(14) S2 0.084(3) 0.216(5) 0.106(4) 0.026(4) 0.035(3) 0.042(3) O20 0.127(9) 0.226(12) 0.160(10) 0.106(9) 0.100(8) 0.086(8) O21 0.111(8) 0.244(14) 0.239(15) 0.124(11) 0.052(10) 0.069(9) O22 0.213(16) 0.49(3) 0.269(19) -0.24(2) 0.131(15) -0.089(18) O3 0.40(3) 0.178(14) 0.267(19) -0.060(12) -0.002(17) 0.015(15) O5 0.59(4) 0.98(7) 0.69(5) -0.67(5) 0.54(4) -0.60(5) _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 =aken into account individually in the estimation of esds in distances, =ngles and torsion angles; correlations between esds in cell parameters are =nly used when they are defined by crystal symmetry. An approximate =isotropic) treatment of cell esds is used for estimating esds involving l.s. =lanes. ; 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 2.217(3) . ? Pd1 P3 2.318(3) . ? Pd1 P2 2.323(3) . ? Pd1 Cl1 2.358(2) . ? P2 C7 1.792(11) . ? P2 C13 1.810(9) . ? P2 C2 1.814(10) . ? P3 C25 1.780(9) . ? P3 C19 1.813(9) . ? P3 C4 1.811(9) . ? P4 O1 1.497(7) . ? P4 C37 1.770(9) . ? P4 C31 1.792(9) . ? P4 C6 1.804(8) . ? P1 C3 1.803(9) . ? P1 C5 1.806(8) . ? P1 C1 1.812(9) . ? C13 C14 1.383(11) . ? C13 C18 1.378(11) . ? C19 C24 1.382(12) . ? C19 C20 1.401(11) . ? C10 C9 1.26(2) . ? C10 C11 1.36(2) . ? C10 H10 0.9300 . ? C12 C7 1.366(14) . ? C12 C11 1.49(2) . ? C12 H12 0.9300 . ? C18 C17 1.392(11) . ? C18 H18 0.9300 . ? C20 C21 1.383(12) . ? C20 H20 0.9300 . ? C31 C32 1.388(12) . ? C31 C36 1.414(12) . ? C7 C8 1.365(14) . ? C16 C17 1.334(12) . ? C16 C15 1.380(12) . ? C16 H16 0.9300 . ? C14 C15 1.385(12) . ? C14 H14 0.9300 . ? C29 C28 1.374(17) . ? C29 C30 1.402(15) . ? C29 H29 0.9300 . ? C25 C26 1.380(12) . ? C25 C30 1.390(13) . ? C6 C5 1.548(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C21 C22 1.371(14) . ? C21 H21 0.9300 . ? C17 H17 0.9300 . ? C1 C2 1.540(13) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C37 C38 1.345(12) . ? C37 C42 1.416(12) . ? C24 C23 1.376(12) . ? C24 H24 0.9300 . ? C38 C39 1.408(14) . ? C38 H38 0.9300 . ? C26 C27 1.415(14) . ? C26 H26 0.9300 . ? C3 C4 1.514(12) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C42 C41 1.375(14) . ? C42 H42 0.9300 . ? C23 C22 1.340(14) . ? C23 H23 0.9300 . ? C27 C28 1.311(15) . ? C27 H27 0.9300 . ? C9 C8 1.380(15) . ? C9 H9 0.9300 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C39 C40 1.351(16) . ? C39 H39 0.9300 . ? C28 H28 0.9300 . ? C11 H11 0.9300 . ? C41 C40 1.367(16) . ? C41 H41 0.9300 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C8 H8 0.9300 . ? C15 H15 0.9300 . ? C30 H30 0.9300 . ? C22 H22 0.9300 . ? C40 H40 0.9300 . ? C34 C33 1.366(14) . ? C34 C35 1.367(16) . ? C34 H34 0.9300 . ? C32 C33 1.395(13) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C36 C35 1.378(14) . ? C36 H36 0.9300 . ? C35 H35 0.9300 . ? S1 C46 1.846(11) . ? S1 C45 1.848(10) . ? S1 C47 1.898(11) . ? S1 C48 1.909(12) . ? C43 C44 1.515(14) . ? C43 S2 1.744(11) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C45 C44 1.515(13) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? S2 O20 1.359(10) . ? S2 O21 1.385(11) . ? S2 O22 1.520(15) . ? 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 P3 84.29(10) . . ? P1 Pd1 P2 84.23(10) . . ? P3 Pd1 P2 157.28(9) . . ? P1 Pd1 Cl1 174.15(9) . . ? P3 Pd1 Cl1 95.89(9) . . ? P2 Pd1 Cl1 97.51(9) . . ? C7 P2 C13 105.1(4) . . ? C7 P2 C2 107.8(5) . . ? 13 P2 C2 105.9(4) . . ? C7 P2 Pd1 122.5(4) . . ? C13 P2 Pd1 105.8(3) . . ? C2 P2 Pd1 108.6(4) . . ? C25 P3 C19 108.8(4) . . ? C25 P3 C4 105.3(5) . . ? C19 P3 C4 106.9(4) . . ? C25 P3 Pd1 121.4(3) . . ? C19 P3 Pd1 105.5(3) . . ? C4 P3 Pd1 108.2(3) . . ? O1 P4 C37 111.8(4) . . ? O1 P4 C31 112.2(4) . . ? C37 P4 C31 108.5(4) . . ? O1 P4 C6 112.2(4) . . ? C37 P4 C6 106.7(4) . . ? C31 P4 C6 105.0(4) . . ? C3 P1 C5 108.5(4) . . ? C3 P1 C1 113.6(5) . . ? C5 P1 C1 107.1(4) . . ? C3 P1 Pd1 108.9(3) . . ? C5 P1 Pd1 109.0(3) . . ? C1 P1 Pd1 109.7(3) . . ? C14 C13 C18 117.6(8) . . ? C14 C13 P2 120.2(7) . . ? C18 C13 P2 122.2(7) . . ? C24 C19 C20 119.2(9) . . ? C24 C19 P3 119.2(7) . . ? C20 C19 P3 121.6(7) . . ? C9 C10 C11 122(2) . . ? C9 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C7 C12 C11 117.7(14) . . ? C7 C12 H12 121.1 . . ? C11 C12 H12 121.1 . . ? C13 C18 C17 121.0(9) . . ? C13 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C21 C20 C19 118.4(9) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? C32 C31 C36 116.9(9) . . ? C32 C31 P4 122.9(7) . . ? C36 C31 P4 120.1(8) . . ? C12 C7 C8 117.2(12) . . ? C12 C7 P2 123.8(11) . . ? C8 C7 P2 119.0(8) . . ? C17 C16 C15 120.5(9) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C13 C14 C15 121.2(9) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C28 C29 C30 121.8(13) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C26 C25 C30 117.9(10) . . ? C26 C25 P3 124.3(8) . . ? C30 C25 P3 117.8(8) . . ? C5 C6 P4 113.8(6) . . ? C5 C6 H6A 108.8 . . ? P4 C6 H6A 108.8 . . ? C5 C6 H6B 108.8 . . ? P4 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C22 C21 C20 121.0(10) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C16 C17 C18 120.4(9) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C2 C1 P1 108.8(7) . . ? C2 C1 H1A 109.9 . . ? P1 C1 H1A 109.9 . . ? C2 C1 H1B 109.9 . . ? P1 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? C1 C2 P2 108.9(6) . . ? C1 C2 H2A 109.9 . . ? P2 C2 H2A 109.9 . . ? C1 C2 H2B 109.9 . . ? P2 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C38 C37 C42 117.0(10) . . ? C38 C37 P4 124.9(8) . . ? C42 C37 P4 118.0(8) . . ? C23 C24 C19 120.4(9) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C37 C38 C39 123.2(11) . . ? C37 C38 H38 118.4 . . ? C39 C38 H38 118.4 . . ? C25 C26 C27 120.6(11) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C4 C3 P1 109.5(6) . . ? C4 C3 H3A 109.8 . . ? P1 C3 H3A 109.8 . . ? C4 C3 H3B 109.8 . . ? P1 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? C41 C42 C37 121.1(11) . . ? C41 C42 H42 119.4 . . ? C37 C42 H42 119.4 . . ? C22 C23 C24 120.5(10) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C28 C27 C26 121.5(13) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? C10 C9 C8 120.9(18) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C3 C4 P3 108.7(6) . . ? C3 C4 H4A 109.9 . . ? P3 C4 H4A 109.9 . . ? C3 C4 H4B 109.9 . . ? P3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C40 C39 C38 117.1(12) . . ? C40 C39 H39 121.4 . . ? C38 C39 H39 121.4 . . ? C27 C28 C29 119.0(13) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C10 C11 C12 118.7(16) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C42 C41 C40 118.5(13) . . ? C42 C41 H41 120.7 . . ? C40 C41 H41 120.7 . . ? C6 C5 P1 114.3(6) . . ? C6 C5 H5A 108.7 . . ? P1 C5 H5A 108.7 . . ? C6 C5 H5B 108.7 . . ? P1 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C7 C8 C9 123.4(13) . . ? C7 C8 H8 118.3 . . ? C9 C8 H8 118.3 . . ? C16 C15 C14 119.3(9) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C25 C30 C29 119.2(12) . . ? C25 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C23 C22 C21 120.4(10) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C39 C40 C41 123.0(13) . . ? C39 C40 H40 118.5 . . ? C41 C40 H40 118.5 . . ? C33 C34 C35 120.3(13) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C31 C32 C33 120.7(10) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C34 C33 C32 120.6(12) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C35 C36 C31 121.7(11) . . ? C35 C36 H36 119.2 . . ? C31 C36 H36 119.2 . . ? C34 C35 C36 119.7(12) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C46 S1 C45 113.0(5) . . ? C46 S1 C47 105.6(6) . . ? C45 S1 C47 109.7(5) . . ? C46 S1 C48 112.2(7) . . ? C45 S1 C48 106.7(6) . . ? C47 S1 C48 109.7(6) . . ? C44 C43 S2 114.7(10) . . ? C44 C43 H43A 108.6 . . ? S2 C43 H43A 108.6 . . ? C44 C43 H43B 108.6 . . ? S2 C43 H43B 108.6 . . ? H43A C43 H43B 107.6 . . ? C44 C45 S1 112.2(8) . . ? C44 C45 H45A 109.2 . . ? S1 C45 H45A 109.2 . . ? C44 C45 H45B 109.2 . . ? S1 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? C43 C44 C45 111.9(10) . . ? C43 C44 H44A 109.2 . . ? C45 C44 H44A 109.2 . . ? C43 C44 H44B 109.2 . . ? C45 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? S1 C47 H47A 109.5 . . ? S1 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? S1 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? S1 C46 H46A 109.5 . . ? S1 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? S1 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? S1 C48 H48A 109.5 . . ? S1 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? S1 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O20 S2 O21 113.2(8) . . ? O20 S2 O22 108.8(10) . . ? O21 S2 O22 112.1(12) . . ? O20 S2 C43 109.7(7) . . ? O21 S2 C43 110.1(7) . . ? O22 S2 C43 102.3(8) . . ? 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 P1 Pd1 P2 C7 132.1(4) . . . . ? P3 Pd1 P2 C7 -167.9(4) . . . . ? Cl1 Pd1 P2 C7 -42.3(4) . . . . ? P1 Pd1 P2 C13 -107.8(3) . . . . ? P3 Pd1 P2 C13 -47.8(4) . . . . ? Cl1 Pd1 P2 C13 77.9(3) . . . . ? P1 Pd1 P2 C2 5.5(4) . . . . ? P3 Pd1 P2 C2 65.5(4) . . . . ? Cl1 Pd1 P2 C2 -168.8(4) . . . . ? P1 Pd1 P3 C25 -127.9(4) . . . . ? P2 Pd1 P3 C25 172.1(4) . . . . ? Cl1 Pd1 P3 C25 46.2(4) . . . . ? P1 Pd1 P3 C19 108.0(3) . . . . ? P2 Pd1 P3 C19 48.0(4) . . . . ? Cl1 Pd1 P3 C19 -77.9(3) . . . . ? P1 Pd1 P3 C4 -6.2(3) . . . . ? P2 Pd1 P3 C4 -66.2(4) . . . . ? Cl1 Pd1 P3 C4 167.9(3) . . . . ? P3 Pd1 P1 C3 -17.4(3) . . . . ? P2 Pd1 P1 C3 143.0(3) . . . . ? Cl1 Pd1 P1 C3 -109.4(10) . . . . ? P3 Pd1 P1 C5 100.8(3) . . . . ? P2 Pd1 P1 C5 -98.8(3) . . . . ? Cl1 Pd1 P1 C5 8.7(11) . . . . ? P3 Pd1 P1 C1 -142.2(4) . . . . ? P2 Pd1 P1 C1 18.1(4) . . . . ? Cl1 Pd1 P1 C1 125.7(10) . . . . ? C7 P2 C13 C14 -68.0(9) . . . . ? C2 P2 C13 C14 45.9(9) . . . . ? Pd1 P2 C13 C14 161.1(7) . . . . ? C7 P2 C13 C18 109.5(8) . . . . ? C2 P2 C13 C18 -136.5(8) . . . . ? Pd1 P2 C13 C18 -21.4(8) . . . . ? C25 P3 C19 C24 -75.7(8) . . . . ? C4 P3 C19 C24 171.1(8) . . . . ? Pd1 P3 C19 C24 56.0(8) . . . . ? C25 P3 C19 C20 105.5(8) . . . . ? C4 P3 C19 C20 -7.7(9) . . . . ? Pd1 P3 C19 C20 -122.8(7) . . . . ? C14 C13 C18 C17 -1.8(14) . . . . ? P2 C13 C18 C17 -179.4(7) . . . . ? C24 C19 C20 C21 -1.6(14) . . . . ? P3 C19 C20 C21 177.2(7) . . . . ? O1 P4 C31 C32 170.1(7) . . . . ? C37 P4 C31 C32 -65.8(8) . . . . ? C6 P4 C31 C32 48.0(8) . . . . ? O1 P4 C31 C36 -5.4(8) . . . . ? C37 P4 C31 C36 118.6(8) . . . . ? C6 P4 C31 C36 -127.5(7) . . . . ? C11 C12 C7 C8 -1.6(19) . . . . ? C11 C12 C7 P2 -179.2(11) . . . . ? C13 P2 C7 C12 122.0(10) . . . . ? C2 P2 C7 C12 9.4(11) . . . . ? Pd1 P2 C7 C12 -117.6(10) . . . . ? C13 P2 C7 C8 -55.5(10) . . . . ? C2 P2 C7 C8 -168.1(9) . . . . ? Pd1 P2 C7 C8 64.9(10) . . . . ? C18 C13 C14 C15 2.9(15) . . . . ? P2 C13 C14 C15 -179.5(8) . . . . ? C19 P3 C25 C26 -13.1(10) . . . . ? C4 P3 C25 C26 101.3(9) . . . . ? Pd1 P3 C25 C26 -135.7(8) . . . . ? C19 P3 C25 C30 168.8(9) . . . . ? C4 P3 C25 C30 -76.9(9) . . . . ? Pd1 P3 C25 C30 46.2(10) . . . . ? O1 P4 C6 C5 73.2(7) . . . . ? C37 P4 C6 C5 -49.6(8) . . . . ? C31 P4 C6 C5 -164.7(7) . . . . ? C19 C20 C21 C22 -0.2(15) . . . . ? C15 C16 C17 C18 0.8(15) . . . . ? C13 C18 C17 C16 0.0(15) . . . . ? C3 P1 C1 C2 -165.5(6) . . . . ? C5 P1 C1 C2 74.8(7) . . . . ? Pd1 P1 C1 C2 -43.4(7) . . . . ? P1 C1 C2 P2 47.6(8) . . . . ? C7 P2 C2 C1 -167.2(6) . . . . ? C13 P2 C2 C1 80.8(7) . . . . ? Pd1 P2 C2 C1 -32.5(7) . . . . ? O1 P4 C37 C38 -172.8(8) . . . . ? C31 P4 C37 C38 62.9(10) . . . . ? C6 P4 C37 C38 -49.8(10) . . . . ? O1 P4 C37 C42 5.3(9) . . . . ? C31 P4 C37 C42 -119.0(8) . . . . ? C6 P4 C37 C42 128.3(8) . . . . ? C20 C19 C24 C23 1.6(15) . . . . ? P3 C19 C24 C23 -177.2(8) . . . . ? C42 C37 C38 C39 -0.1(16) . . . . ? P4 C37 C38 C39 178.1(9) . . . . ? C30 C25 C26 C27 0.1(15) . . . . ? P3 C25 C26 C27 -178.0(8) . . . . ? C5 P1 C3 C4 -75.0(7) . . . . ? C1 P1 C3 C4 166.1(6) . . . . ? Pd1 P1 C3 C4 43.6(7) . . . . ? C38 C37 C42 C41 -1.4(15) . . . . ? P4 C37 C42 C41 -179.8(8) . . . . ? C19 C24 C23 C22 0.2(17) . . . . ? C25 C26 C27 C28 0.6(18) . . . . ? C11 C10 C9 C8 0(3) . . . . ? P1 C3 C4 P3 -48.7(7) . . . . ? C25 P3 C4 C3 164.6(6) . . . . ? C19 P3 C4 C3 -79.8(7) . . . . ? Pd1 P3 C4 C3 33.5(7) . . . . ? C37 C38 C39 C40 1.4(18) . . . . ? C26 C27 C28 C29 0(2) . . . . ? C30 C29 C28 C27 0(2) . . . . ? C9 C10 C11 C12 0(3) . . . . ? C7 C12 C11 C10 1(2) . . . . ? C37 C42 C41 C40 1.6(18) . . . . ? P4 C6 C5 P1 -162.3(5) . . . . ? C3 P1 C5 C6 -41.9(8) . . . . ? C1 P1 C5 C6 81.0(8) . . . . ? Pd1 P1 C5 C6 -160.4(6) . . . . ? C12 C7 C8 C9 1.9(19) . . . . ? P2 C7 C8 C9 179.6(10) . . . . ? C10 C9 C8 C7 -1(2) . . . . ? C17 C16 C15 C14 0.3(15) . . . . ? C13 C14 C15 C16 -2.2(16) . . . . ? C26 C25 C30 C29 -1.0(18) . . . . ? P3 C25 C30 C29 177.3(11) . . . . ? C28 C29 C30 C25 1(2) . . . . ? C24 C23 C22 C21 -2.1(18) . . . . ? C20 C21 C22 C23 2.1(17) . . . . ? C38 C39 C40 C41 -1(2) . . . . ? C42 C41 C40 C39 0(2) . . . . ? C36 C31 C32 C33 -1.5(13) . . . . ? P4 C31 C32 C33 -177.2(7) . . . . ? C35 C34 C33 C32 -1.6(17) . . . . ? C31 C32 C33 C34 1.9(15) . . . . ? C32 C31 C36 C35 0.9(14) . . . . ? P4 C31 C36 C35 176.7(8) . . . . ? C33 C34 C35 C36 0.9(18) . . . . ? C31 C36 C35 C34 -0.6(17) . . . . ? C46 S1 C45 C44 -45.9(11) . . . . ? C47 S1 C45 C44 71.7(10) . . . . ? C48 S1 C45 C44 -169.6(9) . . . . ? S2 C43 C44 C45 -170.8(9) . . . . ? S1 C45 C44 C43 -177.7(9) . . . . ? C44 C43 S2 O20 -173.8(10) . . . . ? C44 C43 S2 O21 60.9(13) . . . . ? C44 C43 S2 O22 -58.4(14) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.596 _refine_diff_density_min -0.857 _refine_diff_density_rms 0.100