Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'T.S. Andy Hor' _publ_contact_author_address ; Department of Chemistry National University of Singapore 3, Science Drive 3 Singapore Singapore 117543 SINGAPORE ; _publ_contact_author_email ANDYHOR@NUS.EDU.SG _publ_section_title ; Dinuclear PCP Pincer Complexes from Lewis Acidic [Pd(OTf)(PCP)] and Basic [Pd(4-Spy)(PCP)] (OTf = triflate; 4-Spy = 4-pyridinethiolate; PCP= -CH(CH2CH2PPh2)2) ; loop_ _publ_author_name 'Andy Hor' 'William Henderson' 'Han Vinh Huynh' 'Lip Lin Koh' 'Kian Eang Neo' # Attachment '2.CIF' data_5478 _database_code_depnum_ccdc_archive 'CCDC 654026' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H66 F6 N2 O6 P4 Pd2 S2' _chemical_formula_weight 1546.05 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' F F 0.0171 0.0103 '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' 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 10.0040(14) _cell_length_b 17.732(2) _cell_length_c 18.719(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.490(4) _cell_angle_gamma 90.00 _cell_volume 3253.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 723 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 21.29 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1572 _exptl_absorpt_coefficient_mu 0.788 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8214 _exptl_absorpt_correction_T_max 0.8712 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23012 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0813 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7463 _reflns_number_gt 5078 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+3.7177P] 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 constructed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7463 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1025 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1382 _refine_ls_wR_factor_gt 0.1244 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.36522(3) 0.75301(2) 0.05896(2) 0.02649(12) Uani 1 1 d . . . P1 P 0.57158(12) 0.69843(7) 0.04832(8) 0.0319(3) Uani 1 1 d . . . P2 P 0.19418(12) 0.83719(7) 0.07133(8) 0.0297(3) Uani 1 1 d . . . N1 N 0.2345(4) 0.6534(2) 0.0377(2) 0.0275(9) Uani 1 1 d . . . C1 C 0.4834(4) 0.8510(3) 0.0741(3) 0.0307(11) Uani 1 1 d . . . H1 H 0.5114 0.8558 0.1277 0.037 Uiso 1 1 calc R . . C2 C 0.6152(5) 0.8446(3) 0.0479(4) 0.0515(17) Uani 1 1 d . . . H21 H 0.5957 0.8466 -0.0055 0.062 Uiso 1 1 calc R . . H22 H 0.6725 0.8882 0.0658 0.062 Uiso 1 1 calc R . . C3 C 0.6910(5) 0.7761(3) 0.0711(4) 0.0443(15) Uani 1 1 d . . . H31 H 0.7275 0.7774 0.1238 0.053 Uiso 1 1 calc R . . H32 H 0.7673 0.7706 0.0458 0.053 Uiso 1 1 calc R . . C4 C 0.4032(5) 0.9209(3) 0.0511(4) 0.0492(16) Uani 1 1 d . . . H41 H 0.4620 0.9648 0.0649 0.059 Uiso 1 1 calc R . . H42 H 0.3746 0.9209 -0.0021 0.059 Uiso 1 1 calc R . . C5 C 0.2806(5) 0.9280(3) 0.0842(3) 0.0372(13) Uani 1 1 d . . . H51 H 0.2207 0.9681 0.0601 0.045 Uiso 1 1 calc R . . H52 H 0.3071 0.9399 0.1362 0.045 Uiso 1 1 calc R . . C6 C 0.1918(5) 0.6158(3) 0.0907(3) 0.0342(12) Uani 1 1 d . . . H6 H 0.2267 0.6301 0.1392 0.041 Uiso 1 1 calc R . . C7 C 0.0995(5) 0.5571(3) 0.0783(3) 0.0327(12) Uani 1 1 d . . . H7 H 0.0709 0.5337 0.1178 0.039 Uiso 1 1 calc R . . C8 C 0.0489(4) 0.5328(2) 0.0081(3) 0.0233(10) Uani 1 1 d . . . C9 C 0.0926(5) 0.5716(3) -0.0469(3) 0.0372(13) Uani 1 1 d . . . H9 H 0.0599 0.5581 -0.0958 0.045 Uiso 1 1 calc R . . C10 C 0.1847(5) 0.6305(3) -0.0302(3) 0.0395(13) Uani 1 1 d . . . H10 H 0.2135 0.6556 -0.0688 0.047 Uiso 1 1 calc R . . C1E C 0.6473(5) 0.6192(3) 0.1029(3) 0.0320(11) Uani 1 1 d . . . C2E C 0.5779(5) 0.5511(3) 0.0995(3) 0.0384(13) Uani 1 1 d . . . H2E H 0.4916 0.5466 0.0689 0.046 Uiso 1 1 calc R . . C3E C 0.6336(6) 0.4902(3) 0.1403(3) 0.0478(15) Uani 1 1 d . . . H3E H 0.5851 0.4445 0.1372 0.057 Uiso 1 1 calc R . . C4E C 0.7601(6) 0.4955(4) 0.1860(3) 0.0499(15) Uani 1 1 d . . . H4E H 0.7970 0.4540 0.2144 0.060 Uiso 1 1 calc R . . C5E C 0.8315(6) 0.5622(4) 0.1894(3) 0.0524(16) Uani 1 1 d . . . H5E H 0.9180 0.5661 0.2199 0.063 Uiso 1 1 calc R . . C6E C 0.7762(5) 0.6234(3) 0.1479(3) 0.0444(14) Uani 1 1 d . . . H6E H 0.8263 0.6685 0.1501 0.053 Uiso 1 1 calc R . . C1B C 0.5816(4) 0.6728(3) -0.0445(3) 0.0279(11) Uani 1 1 d . . . C2B C 0.5029(5) 0.7125(3) -0.1017(3) 0.0384(13) Uani 1 1 d . . . H2B H 0.4392 0.7480 -0.0919 0.046 Uiso 1 1 calc R . . C3B C 0.5165(5) 0.7007(3) -0.1727(3) 0.0453(15) Uani 1 1 d . . . H3B H 0.4645 0.7293 -0.2106 0.054 Uiso 1 1 calc R . . C4B C 0.6068(6) 0.6467(3) -0.1881(3) 0.0470(15) Uani 1 1 d . . . H4B H 0.6166 0.6388 -0.2365 0.056 Uiso 1 1 calc R . . C5B C 0.6822(6) 0.6048(3) -0.1324(3) 0.0414(13) Uani 1 1 d . . . H5B H 0.7405 0.5667 -0.1431 0.050 Uiso 1 1 calc R . . C6B C 0.6728(5) 0.6182(3) -0.0608(3) 0.0358(12) Uani 1 1 d . . . H6B H 0.7275 0.5907 -0.0230 0.043 Uiso 1 1 calc R . . C1C C 0.1023(4) 0.8303(3) 0.1449(3) 0.0284(11) Uani 1 1 d . . . C2C C -0.0068(5) 0.8784(3) 0.1480(3) 0.0305(11) Uani 1 1 d . . . H2C H -0.0371 0.9121 0.1094 0.037 Uiso 1 1 calc R . . C3C C -0.0708(5) 0.8773(3) 0.2067(3) 0.0350(12) Uani 1 1 d . . . H3C H -0.1430 0.9108 0.2083 0.042 Uiso 1 1 calc R . . C4C C -0.0294(6) 0.8273(3) 0.2631(3) 0.0411(13) Uani 1 1 d . . . H4C H -0.0738 0.8262 0.3029 0.049 Uiso 1 1 calc R . . C5C C 0.0780(6) 0.7787(3) 0.2609(3) 0.0484(15) Uani 1 1 d . . . H5C H 0.1062 0.7442 0.2991 0.058 Uiso 1 1 calc R . . C6C C 0.1435(5) 0.7807(3) 0.2029(3) 0.0416(14) Uani 1 1 d . . . H6C H 0.2174 0.7481 0.2024 0.050 Uiso 1 1 calc R . . C1D C 0.0599(5) 0.8450(3) -0.0100(3) 0.0312(11) Uani 1 1 d . . . C2D C -0.0288(5) 0.7846(3) -0.0278(3) 0.0350(12) Uani 1 1 d . . . H2D H -0.0193 0.7416 0.0022 0.042 Uiso 1 1 calc R . . C3D C -0.1310(5) 0.7876(3) -0.0894(3) 0.0423(14) Uani 1 1 d . . . H3D H -0.1924 0.7472 -0.1007 0.051 Uiso 1 1 calc R . . C4D C -0.1426(6) 0.8500(4) -0.1341(3) 0.0452(14) Uani 1 1 d . . . H4D H -0.2116 0.8520 -0.1763 0.054 Uiso 1 1 calc R . . C5D C -0.0543(7) 0.9089(3) -0.1172(3) 0.0530(16) Uani 1 1 d . . . H5D H -0.0624 0.9512 -0.1480 0.064 Uiso 1 1 calc R . . C6D C 0.0474(6) 0.9068(3) -0.0550(3) 0.0421(13) Uani 1 1 d . . . H6D H 0.1078 0.9477 -0.0436 0.051 Uiso 1 1 calc R . . S1 S 0.27939(13) 0.57862(8) 0.31884(8) 0.0368(3) Uani 1 1 d . . . O1 O 0.2793(4) 0.6513(2) 0.3517(2) 0.0543(11) Uani 1 1 d . . . O2 O 0.2857(4) 0.5164(2) 0.3679(2) 0.0453(10) Uani 1 1 d . . . O3 O 0.1856(4) 0.5693(3) 0.2508(2) 0.0677(14) Uani 1 1 d . . . C11 C 0.4444(6) 0.5764(4) 0.2924(4) 0.0498(15) Uani 1 1 d . . . F1 F 0.4536(4) 0.6285(2) 0.2423(2) 0.0688(11) Uani 1 1 d . . . F2 F 0.5450(3) 0.5895(2) 0.3490(2) 0.0659(11) Uani 1 1 d . . . F3 F 0.4689(5) 0.5097(2) 0.2659(3) 0.0910(14) 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 0.01877(17) 0.02351(19) 0.0383(2) -0.00562(17) 0.00847(14) -0.00482(15) P1 0.0194(6) 0.0288(7) 0.0480(9) -0.0095(6) 0.0077(6) -0.0036(5) P2 0.0199(6) 0.0268(6) 0.0435(8) -0.0045(6) 0.0089(6) -0.0020(5) N1 0.0188(18) 0.028(2) 0.036(3) -0.0008(18) 0.0065(18) 0.0000(16) C1 0.023(2) 0.029(3) 0.041(3) -0.010(2) 0.010(2) -0.0117(19) C2 0.033(3) 0.041(3) 0.081(5) -0.014(3) 0.011(3) -0.013(2) C3 0.025(2) 0.040(3) 0.071(4) -0.022(3) 0.018(3) -0.010(2) C4 0.036(3) 0.038(3) 0.073(5) -0.003(3) 0.008(3) -0.009(2) C5 0.030(3) 0.026(3) 0.057(4) -0.012(2) 0.012(3) -0.005(2) C6 0.035(3) 0.029(3) 0.034(3) -0.004(2) -0.004(2) -0.009(2) C7 0.032(3) 0.031(3) 0.035(3) 0.001(2) 0.006(2) -0.008(2) C8 0.020(2) 0.021(2) 0.029(3) 0.0009(19) 0.004(2) -0.0005(18) C9 0.040(3) 0.043(3) 0.031(3) -0.010(2) 0.013(2) -0.018(2) C10 0.044(3) 0.043(3) 0.036(3) -0.005(2) 0.019(3) -0.019(2) C1E 0.025(2) 0.046(3) 0.027(3) -0.010(2) 0.009(2) 0.000(2) C2E 0.024(2) 0.047(3) 0.042(3) -0.004(3) 0.002(2) 0.003(2) C3E 0.039(3) 0.048(3) 0.058(4) 0.008(3) 0.013(3) 0.008(3) C4E 0.043(3) 0.068(4) 0.041(4) 0.006(3) 0.013(3) 0.016(3) C5E 0.042(3) 0.080(5) 0.032(3) -0.005(3) 0.000(3) 0.016(3) C6E 0.032(3) 0.059(4) 0.040(3) -0.011(3) 0.003(3) -0.004(3) C1B 0.022(2) 0.025(2) 0.036(3) -0.004(2) 0.005(2) -0.0063(19) C2B 0.027(3) 0.027(3) 0.056(4) 0.003(3) -0.004(3) -0.002(2) C3B 0.034(3) 0.044(3) 0.051(4) 0.017(3) -0.009(3) -0.004(3) C4B 0.049(3) 0.056(4) 0.036(3) 0.004(3) 0.007(3) -0.014(3) C5B 0.044(3) 0.040(3) 0.042(4) 0.001(3) 0.014(3) 0.005(2) C6B 0.031(3) 0.032(3) 0.043(3) 0.002(2) 0.007(2) 0.004(2) C1C 0.022(2) 0.027(2) 0.034(3) -0.006(2) 0.001(2) -0.0030(19) C2C 0.029(2) 0.030(3) 0.030(3) 0.004(2) 0.002(2) 0.002(2) C3C 0.027(3) 0.035(3) 0.043(3) -0.004(2) 0.008(2) 0.003(2) C4C 0.047(3) 0.047(3) 0.032(3) 0.000(3) 0.016(3) 0.005(3) C5C 0.057(4) 0.047(3) 0.039(4) 0.003(3) 0.005(3) 0.015(3) C6C 0.037(3) 0.037(3) 0.050(4) -0.001(3) 0.004(3) 0.014(2) C1D 0.027(2) 0.032(3) 0.038(3) 0.001(2) 0.013(2) 0.005(2) C2D 0.030(3) 0.038(3) 0.039(3) 0.004(2) 0.010(2) 0.000(2) C3D 0.028(3) 0.057(4) 0.044(4) -0.009(3) 0.011(3) -0.011(2) C4D 0.040(3) 0.069(4) 0.027(3) 0.000(3) 0.009(3) 0.009(3) C5D 0.075(4) 0.046(4) 0.042(4) 0.002(3) 0.020(3) 0.006(3) C6D 0.054(3) 0.037(3) 0.037(3) -0.004(3) 0.011(3) -0.002(3) S1 0.0302(7) 0.0393(7) 0.0370(8) 0.0038(6) -0.0030(6) -0.0060(5) O1 0.049(2) 0.036(2) 0.079(3) -0.002(2) 0.016(2) 0.0014(18) O2 0.048(2) 0.039(2) 0.047(2) 0.0092(18) 0.0035(19) -0.0002(17) O3 0.048(2) 0.110(4) 0.035(2) 0.011(2) -0.015(2) -0.032(2) C11 0.049(4) 0.051(4) 0.053(4) -0.010(3) 0.019(3) -0.008(3) F1 0.064(2) 0.085(3) 0.062(3) 0.010(2) 0.024(2) -0.018(2) F2 0.0311(17) 0.077(3) 0.083(3) 0.001(2) -0.0046(19) -0.0072(17) F3 0.098(3) 0.069(3) 0.121(4) -0.032(3) 0.061(3) -0.003(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 C1 2.088(4) . ? Pd1 N1 2.187(4) . ? Pd1 P2 2.3168(13) . ? Pd1 P1 2.3242(13) . ? P1 C1E 1.812(5) . ? P1 C3 1.818(5) . ? P1 C1B 1.818(5) . ? P2 C1C 1.806(5) . ? P2 C5 1.821(5) . ? P2 C1D 1.824(5) . ? N1 C10 1.333(6) . ? N1 C6 1.334(6) . ? C1 C4 1.492(7) . ? C1 C2 1.499(7) . ? C2 C3 1.453(8) . ? C4 C5 1.486(8) . ? C6 C7 1.380(6) . ? C7 C8 1.381(7) . ? C8 C9 1.379(7) . ? C8 C8 1.511(8) 3_565 ? C9 C10 1.387(7) . ? C1E C2E 1.388(7) . ? C1E C6E 1.394(7) . ? C2E C3E 1.376(7) . ? C3E C4E 1.382(8) . ? C4E C5E 1.376(9) . ? C5E C6E 1.384(8) . ? C1B C2B 1.388(7) . ? C1B C6B 1.405(7) . ? C2B C3B 1.377(8) . ? C3B C4B 1.386(8) . ? C4B C5B 1.377(7) . ? C5B C6B 1.382(8) . ? C1C C6C 1.394(7) . ? C1C C2C 1.395(6) . ? C2C C3C 1.379(7) . ? C3C C4C 1.377(7) . ? C4C C5C 1.385(8) . ? C5C C6C 1.376(8) . ? C1D C6D 1.372(7) . ? C1D C2D 1.389(7) . ? C2D C3D 1.381(7) . ? C3D C4D 1.380(8) . ? C4D C5D 1.364(8) . ? C5D C6D 1.386(8) . ? S1 O1 1.427(4) . ? S1 O2 1.429(4) . ? S1 O3 1.433(4) . ? S1 C11 1.815(6) . ? C11 F3 1.324(7) . ? C11 F2 1.328(7) . ? C11 F1 1.332(7) . ? 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 C1 Pd1 N1 176.78(17) . . ? C1 Pd1 P2 81.95(13) . . ? N1 Pd1 P2 96.42(10) . . ? C1 Pd1 P1 82.50(13) . . ? N1 Pd1 P1 99.04(10) . . ? P2 Pd1 P1 164.40(5) . . ? C1E P1 C3 105.9(2) . . ? C1E P1 C1B 104.4(2) . . ? C3 P1 C1B 104.8(3) . . ? C1E P1 Pd1 123.59(17) . . ? C3 P1 Pd1 102.59(17) . . ? C1B P1 Pd1 113.89(15) . . ? C1C P2 C5 105.0(2) . . ? C1C P2 C1D 103.9(2) . . ? C5 P2 C1D 107.1(2) . . ? C1C P2 Pd1 122.05(16) . . ? C5 P2 Pd1 104.04(16) . . ? C1D P2 Pd1 113.66(16) . . ? C10 N1 C6 116.3(4) . . ? C10 N1 Pd1 121.0(3) . . ? C6 N1 Pd1 122.5(3) . . ? C4 C1 C2 115.2(5) . . ? C4 C1 Pd1 113.2(3) . . ? C2 C1 Pd1 113.8(3) . . ? C3 C2 C1 114.0(5) . . ? C2 C3 P1 106.5(4) . . ? C5 C4 C1 113.1(5) . . ? C4 C5 P2 106.2(4) . . ? N1 C6 C7 123.7(5) . . ? C6 C7 C8 120.1(5) . . ? C9 C8 C7 116.4(4) . . ? C9 C8 C8 121.6(5) . 3_565 ? C7 C8 C8 122.0(5) . 3_565 ? C8 C9 C10 120.2(5) . . ? N1 C10 C9 123.3(5) . . ? C2E C1E C6E 117.9(5) . . ? C2E C1E P1 119.9(4) . . ? C6E C1E P1 122.1(4) . . ? C3E C2E C1E 120.9(5) . . ? C2E C3E C4E 120.6(6) . . ? C5E C4E C3E 119.4(6) . . ? C4E C5E C6E 120.1(5) . . ? C5E C6E C1E 121.0(6) . . ? C2B C1B C6B 118.3(5) . . ? C2B C1B P1 118.7(4) . . ? C6B C1B P1 122.8(4) . . ? C3B C2B C1B 121.2(5) . . ? C2B C3B C4B 120.0(5) . . ? C5B C4B C3B 119.7(6) . . ? C4B C5B C6B 120.6(5) . . ? C5B C6B C1B 120.1(5) . . ? C6C C1C C2C 117.8(5) . . ? C6C C1C P2 121.3(4) . . ? C2C C1C P2 120.7(4) . . ? C3C C2C C1C 121.0(5) . . ? C4C C3C C2C 120.2(5) . . ? C3C C4C C5C 119.7(5) . . ? C6C C5C C4C 120.1(5) . . ? C5C C6C C1C 121.1(5) . . ? C6D C1D C2D 119.5(5) . . ? C6D C1D P2 122.4(4) . . ? C2D C1D P2 118.1(4) . . ? C3D C2D C1D 120.2(5) . . ? C4D C3D C2D 119.7(5) . . ? C5D C4D C3D 120.1(5) . . ? C4D C5D C6D 120.6(6) . . ? C1D C6D C5D 119.9(5) . . ? O1 S1 O2 115.1(3) . . ? O1 S1 O3 115.5(3) . . ? O2 S1 O3 114.8(3) . . ? O1 S1 C11 102.4(3) . . ? O2 S1 C11 103.4(3) . . ? O3 S1 C11 103.0(3) . . ? F3 C11 F2 106.7(5) . . ? F3 C11 F1 108.1(5) . . ? F2 C11 F1 107.0(5) . . ? F3 C11 S1 111.6(4) . . ? F2 C11 S1 111.4(4) . . ? F1 C11 S1 111.8(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.371 _refine_diff_density_min -0.680 _refine_diff_density_rms 0.107 # Attachment '3A.cif' data_5335a _database_code_depnum_ccdc_archive 'CCDC 654027' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H86 F6 Fe O6 P6 Pd2 S2' _chemical_formula_weight 1944.22 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' F F 0.0171 0.0103 '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' Fe Fe 0.3463 0.8444 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 21.0633(8) _cell_length_b 21.6510(8) _cell_length_c 39.0514(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17809.1(12) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Rectangular Plate' _exptl_crystal_colour Orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7936 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8348 _exptl_absorpt_correction_T_max 0.9260 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 101270 _diffrn_reflns_av_R_equivalents 0.1513 _diffrn_reflns_av_sigmaI/netI 0.0998 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15676 _reflns_number_gt 8906 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0881P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15676 _refine_ls_number_parameters 1053 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1336 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1768 _refine_ls_wR_factor_gt 0.1507 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.002 _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 0.77960(2) 0.80155(3) 0.715162(13) 0.03446(15) Uani 1 1 d . . . Pd2 Pd 0.38533(2) 0.72086(3) 0.536857(14) 0.04246(17) Uani 1 1 d . . . Fe1 Fe 0.56502(4) 0.72490(5) 0.64253(3) 0.0364(3) Uani 1 1 d . . . P1 P 0.69994(9) 0.85391(10) 0.74428(5) 0.0470(5) Uani 1 1 d . . . P2 P 0.87493(8) 0.75132(11) 0.70511(5) 0.0481(6) Uani 1 1 d . . . P3 P 0.32417(9) 0.80850(11) 0.52928(5) 0.0493(5) Uani 1 1 d . . . P4 P 0.44258(10) 0.63361(11) 0.52330(6) 0.0572(6) Uani 1 1 d . . . P5 P 0.72168(8) 0.77221(8) 0.66555(4) 0.0320(4) Uani 1 1 d . . . P6 P 0.42589(8) 0.74200(9) 0.59204(5) 0.0368(5) Uani 1 1 d . . . C1 C 0.8362(3) 0.8459(4) 0.75276(18) 0.0464(19) Uani 1 1 d . . . H1 H 0.8485 0.8850 0.7414 0.056 Uiso 1 1 calc R . . C2 C 0.8011(3) 0.8677(4) 0.78413(19) 0.061(2) Uani 1 1 d . . . H2A H 0.8290 0.8934 0.7983 0.073 Uiso 1 1 calc R . . H2B H 0.7875 0.8321 0.7978 0.073 Uiso 1 1 calc R . . C3 C 0.7435(3) 0.9049(4) 0.7730(2) 0.060(2) Uani 1 1 d . . . H3A H 0.7566 0.9426 0.7611 0.072 Uiso 1 1 calc R . . H3B H 0.7174 0.9162 0.7928 0.072 Uiso 1 1 calc R . . C4 C 0.9001(3) 0.8162(4) 0.76107(19) 0.051(2) Uani 1 1 d . . . H4A H 0.9267 0.8456 0.7736 0.061 Uiso 1 1 calc R . . H4B H 0.8935 0.7798 0.7756 0.061 Uiso 1 1 calc R . . C5 C 0.9330(3) 0.7972(4) 0.72805(18) 0.052(2) Uani 1 1 d . . . H5A H 0.9712 0.7729 0.7329 0.062 Uiso 1 1 calc R . . H5B H 0.9452 0.8337 0.7147 0.062 Uiso 1 1 calc R . . C6 C 0.3328(3) 0.6931(4) 0.49288(19) 0.058(2) Uani 1 1 d . . . H6 H 0.2970 0.6685 0.5022 0.069 Uiso 1 1 calc R . . C7 C 0.3020(4) 0.7435(4) 0.4735(2) 0.072(3) Uani 1 1 d . . . H7A H 0.2734 0.7260 0.4562 0.086 Uiso 1 1 calc R . . H7B H 0.3343 0.7680 0.4616 0.086 Uiso 1 1 calc R . . C8 C 0.2645(4) 0.7846(4) 0.4978(2) 0.067(3) Uani 1 1 d . . . H8A H 0.2299 0.7617 0.5087 0.080 Uiso 1 1 calc R . . H8B H 0.2468 0.8204 0.4857 0.080 Uiso 1 1 calc R . . C9 C 0.3685(4) 0.6481(5) 0.4695(2) 0.077(3) Uani 1 1 d . . . H9A H 0.3397 0.6319 0.4519 0.092 Uiso 1 1 calc R . . H9B H 0.4034 0.6697 0.4579 0.092 Uiso 1 1 calc R . . C10 C 0.3948(4) 0.5952(5) 0.4909(3) 0.081(3) Uani 1 1 d . . . H10A H 0.4208 0.5675 0.4769 0.098 Uiso 1 1 calc R . . H10B H 0.3604 0.5714 0.5014 0.098 Uiso 1 1 calc R . . C11 C 0.6357(3) 0.7666(3) 0.67024(16) 0.0285(15) Uani 1 1 d . . . C12 C 0.6020(3) 0.7232(3) 0.69080(17) 0.0388(17) Uani 1 1 d . . . H12 H 0.6203 0.6868 0.7025 0.047 Uiso 1 1 calc R . . C13 C 0.5376(3) 0.7418(4) 0.69149(18) 0.045(2) Uani 1 1 d . . . H13 H 0.5030 0.7202 0.7038 0.054 Uiso 1 1 calc R . . C14 C 0.5308(3) 0.7965(3) 0.67190(17) 0.0371(17) Uani 1 1 d . . . H14 H 0.4909 0.8197 0.6680 0.044 Uiso 1 1 calc R . . C15 C 0.5911(3) 0.8116(3) 0.65895(16) 0.0334(16) Uani 1 1 d . . . H15 H 0.6008 0.8471 0.6439 0.040 Uiso 1 1 calc R . . C16 C 0.5004(3) 0.7061(3) 0.60456(18) 0.0399(18) Uani 1 1 d . . . C17 C 0.5068(3) 0.6542(4) 0.6268(2) 0.053(2) Uani 1 1 d . . . H17 H 0.4724 0.6350 0.6404 0.064 Uiso 1 1 calc R . . C18 C 0.5722(4) 0.6354(4) 0.6264(2) 0.062(2) Uani 1 1 d . . . H18 H 0.5908 0.6008 0.6395 0.074 Uiso 1 1 calc R . . C19 C 0.6044(4) 0.6739(4) 0.6038(2) 0.060(3) Uani 1 1 d . . . H19 H 0.6503 0.6714 0.5986 0.072 Uiso 1 1 calc R . . C20 C 0.5616(3) 0.7177(4) 0.58949(19) 0.049(2) Uani 1 1 d . . . H20 H 0.5722 0.7505 0.5728 0.059 Uiso 1 1 calc R . . C1A C 0.6551(4) 0.8064(6) 0.7728(2) 0.069(3) Uani 1 1 d . . . C2A C 0.6167(4) 0.8308(7) 0.7992(2) 0.106(4) Uani 1 1 d . . . H2A1 H 0.6122 0.8738 0.8015 0.128 Uiso 1 1 calc R . . C3A C 0.5864(8) 0.7924(11) 0.8213(4) 0.167(11) Uani 1 1 d . . . H3A' H 0.5609 0.8105 0.8383 0.201 Uiso 1 1 calc R . . C4A C 0.5898(9) 0.7334(13) 0.8208(5) 0.186(14) Uani 1 1 d . . . H4A1 H 0.5684 0.7092 0.8371 0.223 Uiso 1 1 calc R . . C5A C 0.6258(6) 0.7067(8) 0.7954(4) 0.148(7) Uani 1 1 d . . . H5A1 H 0.6281 0.6634 0.7941 0.178 Uiso 1 1 calc R . . C6A C 0.6600(4) 0.7433(6) 0.7711(3) 0.088(4) Uani 1 1 d . . . H6A1 H 0.6853 0.7244 0.7542 0.105 Uiso 1 1 calc R . . C1B C 0.6435(3) 0.9029(4) 0.72206(18) 0.0449(19) Uani 1 1 d . . . C2B C 0.5779(4) 0.9005(4) 0.7270(2) 0.061(2) Uani 1 1 d . . . H2B1 H 0.5601 0.8715 0.7422 0.073 Uiso 1 1 calc R . . C3B C 0.5389(4) 0.9416(5) 0.7091(3) 0.074(3) Uani 1 1 d . . . H3B' H 0.4947 0.9405 0.7125 0.089 Uiso 1 1 calc R . . C4B C 0.5639(5) 0.9825(5) 0.6872(3) 0.078(3) Uani 1 1 d . . . H4B1 H 0.5371 1.0100 0.6755 0.094 Uiso 1 1 calc R . . C5B C 0.6293(5) 0.9848(4) 0.6817(2) 0.073(3) Uani 1 1 d . . . H5B1 H 0.6466 1.0132 0.6661 0.088 Uiso 1 1 calc R . . C6B C 0.6677(4) 0.9452(4) 0.6992(2) 0.057(2) Uani 1 1 d . . . H6B1 H 0.7118 0.9469 0.6956 0.069 Uiso 1 1 calc R . . C1C C 0.8764(4) 0.6769(4) 0.72636(19) 0.053(2) Uani 1 1 d . . . C2C C 0.9331(4) 0.6501(5) 0.7378(3) 0.078(3) Uani 1 1 d . . . H2C H 0.9719 0.6703 0.7338 0.094 Uiso 1 1 calc R . . C3C C 0.9325(6) 0.5955(6) 0.7547(3) 0.098(4) Uani 1 1 d . . . H3C H 0.9706 0.5787 0.7630 0.118 Uiso 1 1 calc R . . C4C C 0.8774(7) 0.5652(5) 0.7596(3) 0.097(4) Uani 1 1 d . . . H4C H 0.8776 0.5267 0.7707 0.117 Uiso 1 1 calc R . . C5C C 0.8212(5) 0.5895(4) 0.7486(3) 0.078(3) Uani 1 1 d . . . H5C H 0.7831 0.5678 0.7520 0.093 Uiso 1 1 calc R . . C6C C 0.8207(4) 0.6467(4) 0.7324(2) 0.051(2) Uani 1 1 d . . . H6C H 0.7820 0.6645 0.7257 0.062 Uiso 1 1 calc R . . C1D C 0.9104(3) 0.7396(6) 0.6633(2) 0.069(3) Uani 1 1 d . . . C2D C 0.9260(4) 0.6805(6) 0.6509(2) 0.093(4) Uani 1 1 d . . . H2D H 0.9169 0.6455 0.6643 0.112 Uiso 1 1 calc R . . C3D C 0.9545(5) 0.6737(7) 0.6194(3) 0.108(5) Uani 1 1 d . . . H3D H 0.9644 0.6341 0.6110 0.129 Uiso 1 1 calc R . . C4D C 0.9686(5) 0.7259(10) 0.6000(3) 0.139(8) Uani 1 1 d . . . H4D H 0.9902 0.7215 0.5791 0.167 Uiso 1 1 calc R . . C5D C 0.9517(5) 0.7826(8) 0.6110(3) 0.114(5) Uani 1 1 d . . . H5D H 0.9602 0.8171 0.5971 0.137 Uiso 1 1 calc R . . C6D C 0.9216(4) 0.7909(6) 0.6428(2) 0.088(4) Uani 1 1 d . . . H6D H 0.9094 0.8305 0.6501 0.106 Uiso 1 1 calc R . . C1E C 0.7319(3) 0.8314(3) 0.63310(16) 0.0310(15) Uani 1 1 d . . . C2E C 0.7729(3) 0.8800(3) 0.63879(18) 0.0425(18) Uani 1 1 d . . . H2E H 0.7958 0.8812 0.6594 0.051 Uiso 1 1 calc R . . C3E C 0.7815(4) 0.9263(4) 0.6155(2) 0.054(2) Uani 1 1 d . . . H3E H 0.8100 0.9587 0.6201 0.065 Uiso 1 1 calc R . . C4E C 0.7481(4) 0.9250(4) 0.5856(2) 0.058(2) Uani 1 1 d . . . H4E H 0.7534 0.9571 0.5696 0.070 Uiso 1 1 calc R . . C5E C 0.7067(4) 0.8774(4) 0.5782(2) 0.054(2) Uani 1 1 d . . . H5E H 0.6841 0.8767 0.5574 0.065 Uiso 1 1 calc R . . C6E C 0.6991(3) 0.8301(4) 0.60222(18) 0.0431(18) Uani 1 1 d . . . H6E H 0.6715 0.7971 0.5975 0.052 Uiso 1 1 calc R . . C1F C 0.7459(3) 0.7001(3) 0.64425(16) 0.0354(16) Uani 1 1 d . . . C2F C 0.7291(3) 0.6444(3) 0.65871(19) 0.0453(19) Uani 1 1 d . . . H2F H 0.7058 0.6439 0.6792 0.054 Uiso 1 1 calc R . . C3F C 0.7463(4) 0.5892(4) 0.6434(2) 0.057(2) Uani 1 1 d . . . H3F H 0.7343 0.5514 0.6534 0.068 Uiso 1 1 calc R . . C4F C 0.7810(4) 0.5902(4) 0.6137(2) 0.060(2) Uani 1 1 d . . . H4F H 0.7933 0.5528 0.6034 0.072 Uiso 1 1 calc R . . C5F C 0.7977(4) 0.6450(4) 0.5991(2) 0.055(2) Uani 1 1 d . . . H5F H 0.8210 0.6451 0.5785 0.066 Uiso 1 1 calc R . . C6F C 0.7809(3) 0.7007(3) 0.61412(17) 0.0424(18) Uani 1 1 d . . . H6F H 0.7930 0.7384 0.6041 0.051 Uiso 1 1 calc R . . C1G C 0.3681(3) 0.8691(4) 0.50725(18) 0.047(2) Uani 1 1 d . . . C2G C 0.4335(4) 0.8654(4) 0.5066(2) 0.072(3) Uani 1 1 d . . . H2G H 0.4541 0.8322 0.5174 0.086 Uiso 1 1 calc R . . C3G C 0.4692(5) 0.9103(5) 0.4900(3) 0.095(4) Uani 1 1 d . . . H3G H 0.5138 0.9079 0.4903 0.114 Uiso 1 1 calc R . . C4G C 0.4402(6) 0.9573(5) 0.4736(3) 0.092(3) Uani 1 1 d . . . H4G H 0.4646 0.9867 0.4618 0.110 Uiso 1 1 calc R . . C5G C 0.3752(6) 0.9622(5) 0.4742(2) 0.080(3) Uani 1 1 d . . . H5G H 0.3547 0.9953 0.4632 0.096 Uiso 1 1 calc R . . C6G C 0.3407(4) 0.9181(4) 0.4911(2) 0.070(3) Uani 1 1 d . . . H6G H 0.2962 0.9217 0.4915 0.084 Uiso 1 1 calc R . . C1H C 0.2817(3) 0.8433(4) 0.5645(2) 0.054(2) Uani 1 1 d . . . C2H C 0.2790(4) 0.9074(5) 0.5702(2) 0.065(2) Uani 1 1 d . . . H2H H 0.3001 0.9346 0.5553 0.078 Uiso 1 1 calc R . . C3H C 0.2444(4) 0.9307(5) 0.5986(3) 0.079(3) Uani 1 1 d . . . H3H H 0.2418 0.9735 0.6023 0.095 Uiso 1 1 calc R . . C4H C 0.2146(4) 0.8906(6) 0.6209(2) 0.077(3) Uani 1 1 d . . . H4H H 0.1930 0.9060 0.6401 0.093 Uiso 1 1 calc R . . C5H C 0.2165(4) 0.8278(5) 0.6148(2) 0.066(3) Uani 1 1 d . . . H5H H 0.1953 0.8009 0.6298 0.079 Uiso 1 1 calc R . . C6H C 0.2497(3) 0.8031(4) 0.5866(2) 0.058(2) Uani 1 1 d . . . H6H H 0.2503 0.7603 0.5827 0.070 Uiso 1 1 calc R . . C1I C 0.5128(4) 0.6583(5) 0.4994(2) 0.061(2) Uani 1 1 d . . . C2I C 0.5325(4) 0.7191(5) 0.5023(2) 0.064(2) Uani 1 1 d . . . H2I H 0.5116 0.7449 0.5181 0.077 Uiso 1 1 calc R . . C3I C 0.5815(4) 0.7434(5) 0.4830(2) 0.079(3) Uani 1 1 d . . . H3I H 0.5949 0.7845 0.4858 0.094 Uiso 1 1 calc R . . C4I C 0.6094(5) 0.7057(7) 0.4599(3) 0.108(4) Uani 1 1 d . . . H4I H 0.6413 0.7217 0.4456 0.130 Uiso 1 1 calc R . . C5I C 0.5928(5) 0.6442(7) 0.4566(3) 0.117(5) Uani 1 1 d . . . H5I H 0.6147 0.6186 0.4413 0.141 Uiso 1 1 calc R . . C6I C 0.5429(4) 0.6205(6) 0.4764(3) 0.097(4) Uani 1 1 d . . . H6I H 0.5302 0.5792 0.4739 0.116 Uiso 1 1 calc R . . C1J C 0.4650(5) 0.5737(4) 0.5530(2) 0.071(3) Uani 1 1 d . . . C2J C 0.5281(6) 0.5565(5) 0.5577(3) 0.096(4) Uani 1 1 d . . . H2J H 0.5610 0.5762 0.5457 0.116 Uiso 1 1 calc R . . C3J C 0.5412(9) 0.5066(7) 0.5821(4) 0.128(6) Uani 1 1 d . . . H3J H 0.5829 0.4927 0.5857 0.154 Uiso 1 1 calc R . . C4J C 0.4915(10) 0.4807(7) 0.5995(5) 0.140(7) Uani 1 1 d . . . H4J H 0.5002 0.4494 0.6155 0.168 Uiso 1 1 calc R . . C5J C 0.4312(10) 0.4980(7) 0.5948(4) 0.145(6) Uani 1 1 d . . . H5J H 0.3981 0.4787 0.6069 0.174 Uiso 1 1 calc R . . C6J C 0.4185(6) 0.5450(5) 0.5718(3) 0.097(4) Uani 1 1 d . . . H6J H 0.3762 0.5577 0.5689 0.116 Uiso 1 1 calc R . . C1K C 0.3694(3) 0.7082(3) 0.62254(17) 0.0377(17) Uani 1 1 d . . . C2K C 0.3726(4) 0.7179(4) 0.65727(19) 0.056(2) Uani 1 1 d . . . H2K H 0.4035 0.7448 0.6662 0.067 Uiso 1 1 calc R . . C3K C 0.3310(4) 0.6888(4) 0.6790(2) 0.074(3) Uani 1 1 d . . . H3K H 0.3350 0.6943 0.7028 0.089 Uiso 1 1 calc R . . C4K C 0.2843(4) 0.6521(4) 0.6665(2) 0.071(3) Uani 1 1 d . . . H4K H 0.2543 0.6343 0.6813 0.085 Uiso 1 1 calc R . . C5K C 0.2813(4) 0.6413(4) 0.6321(2) 0.063(2) Uani 1 1 d . . . H5K H 0.2502 0.6144 0.6234 0.076 Uiso 1 1 calc R . . C6K C 0.3235(3) 0.6693(3) 0.61022(18) 0.0445(19) Uani 1 1 d . . . H6K H 0.3208 0.6617 0.5866 0.053 Uiso 1 1 calc R . . C1L C 0.4352(3) 0.8229(3) 0.60369(17) 0.0393(17) Uani 1 1 d . . . C2L C 0.3935(4) 0.8549(4) 0.6242(2) 0.051(2) Uani 1 1 d . . . H2L H 0.3578 0.8344 0.6332 0.061 Uiso 1 1 calc R . . C3L C 0.4028(5) 0.9157(4) 0.6316(2) 0.068(3) Uani 1 1 d . . . H3L H 0.3736 0.9363 0.6457 0.081 Uiso 1 1 calc R . . C4L C 0.4539(5) 0.9475(4) 0.6189(3) 0.071(3) Uani 1 1 d . . . H4L H 0.4599 0.9894 0.6243 0.085 Uiso 1 1 calc R . . C5L C 0.4959(5) 0.9173(5) 0.5984(3) 0.076(3) Uani 1 1 d . . . H5L H 0.5311 0.9386 0.5893 0.092 Uiso 1 1 calc R . . C6L C 0.4872(4) 0.8563(4) 0.5908(2) 0.061(2) Uani 1 1 d . . . H6L H 0.5168 0.8361 0.5767 0.073 Uiso 1 1 calc R . . S2 S 0.6417(4) 0.5593(5) 0.7373(2) 0.101(3) Uani 0.407(4) 1 d PD A 1 O4 O 0.6712(8) 0.6154(7) 0.7454(5) 0.097(4) Uiso 0.407(4) 1 d PD A 1 O5 O 0.5809(6) 0.5655(9) 0.7219(5) 0.097(4) Uiso 0.407(4) 1 d PD A 1 O6 O 0.6818(8) 0.5110(7) 0.7236(5) 0.097(4) Uiso 0.407(4) 1 d PD A 1 C22 C 0.6288(8) 0.5327(8) 0.7774(4) 0.071(6) Uiso 0.407(4) 1 d PD A 1 F4 F 0.5798(8) 0.5674(8) 0.7888(5) 0.134(6) Uiso 0.407(4) 1 d PD A 1 F5 F 0.6727(7) 0.5331(8) 0.8016(4) 0.122(6) Uiso 0.407(4) 1 d PD A 1 F6 F 0.6040(8) 0.4772(7) 0.7811(5) 0.124(6) Uiso 0.407(4) 1 d PD A 1 S2A S 0.6210(2) 0.5179(2) 0.71907(15) 0.0766(16) Uani 0.593(4) 1 d PD A 2 O4A O 0.6765(6) 0.4883(7) 0.7064(4) 0.132(3) Uiso 0.593(4) 1 d PD A 2 O5A O 0.6171(8) 0.5821(4) 0.7144(4) 0.132(3) Uiso 0.593(4) 1 d PD A 2 O6A O 0.6057(7) 0.4951(7) 0.7525(3) 0.132(3) Uiso 0.593(4) 1 d PD A 2 C22A C 0.5727(7) 0.4909(7) 0.6934(4) 0.157(10) Uiso 0.593(4) 1 d PD A 2 F4A F 0.5838(8) 0.4989(8) 0.6602(3) 0.232(8) Uiso 0.593(4) 1 d PD A 2 F5A F 0.5636(7) 0.4318(6) 0.6908(4) 0.187(6) Uiso 0.593(4) 1 d PD A 2 F6A F 0.5137(6) 0.5102(8) 0.6929(5) 0.254(9) Uiso 0.593(4) 1 d PD A 2 S1 S 0.68907(11) 0.89381(12) 0.46315(7) 0.0661(6) Uani 1 1 d . . . O1 O 0.6544(3) 0.8867(3) 0.49447(17) 0.094(2) Uani 1 1 d . . . O2 O 0.7064(3) 0.8363(3) 0.44773(17) 0.0795(19) Uani 1 1 d . . . O3 O 0.7380(3) 0.9405(4) 0.4631(3) 0.130(3) Uani 1 1 d . . . C21 C 0.6308(4) 0.9255(5) 0.4348(2) 0.067(2) Uani 1 1 d . . . F1 F 0.5831(3) 0.8863(3) 0.42949(15) 0.0970(18) Uani 1 1 d . . . F2 F 0.6047(2) 0.9769(3) 0.44657(15) 0.0900(17) Uani 1 1 d . . . F3 F 0.6540(3) 0.9378(3) 0.40370(15) 0.113(2) 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 0.0246(3) 0.0550(4) 0.0239(3) -0.0003(3) -0.0018(2) -0.0065(2) Pd2 0.0340(3) 0.0663(4) 0.0272(3) -0.0059(3) 0.0003(2) -0.0167(3) Fe1 0.0262(5) 0.0453(6) 0.0376(6) -0.0102(5) -0.0039(4) -0.0026(5) P1 0.0353(10) 0.0757(15) 0.0300(11) -0.0126(10) 0.0019(8) -0.0061(10) P2 0.0242(9) 0.0897(17) 0.0305(11) -0.0050(10) -0.0020(7) -0.0007(10) P3 0.0392(11) 0.0742(15) 0.0344(12) 0.0053(10) -0.0096(8) -0.0132(10) P4 0.0510(13) 0.0743(16) 0.0464(13) -0.0251(12) 0.0045(10) -0.0130(11) P5 0.0259(9) 0.0429(11) 0.0273(10) -0.0018(8) -0.0025(7) -0.0015(8) P6 0.0269(9) 0.0561(13) 0.0273(10) -0.0042(9) -0.0010(7) -0.0078(8) C1 0.031(4) 0.072(6) 0.036(4) -0.002(4) -0.009(3) -0.017(4) C2 0.047(5) 0.104(7) 0.033(5) -0.008(5) -0.009(4) -0.006(5) C3 0.047(5) 0.092(7) 0.042(5) -0.032(5) 0.002(4) -0.001(5) C4 0.035(4) 0.071(6) 0.046(5) 0.005(4) -0.011(3) -0.012(4) C5 0.029(4) 0.092(6) 0.036(4) 0.007(4) -0.005(3) -0.011(4) C6 0.043(4) 0.094(7) 0.037(5) -0.017(5) -0.005(4) -0.028(5) C7 0.074(6) 0.102(8) 0.039(5) -0.002(5) -0.027(4) -0.040(6) C8 0.065(6) 0.090(7) 0.045(5) 0.005(5) -0.024(4) -0.028(5) C9 0.053(5) 0.137(9) 0.041(6) -0.039(6) 0.000(4) -0.021(6) C10 0.057(6) 0.106(8) 0.081(7) -0.055(7) 0.010(5) -0.022(6) C11 0.023(3) 0.038(4) 0.025(4) -0.002(3) 0.001(3) -0.003(3) C12 0.032(4) 0.051(5) 0.034(4) 0.002(4) -0.005(3) -0.003(3) C13 0.031(4) 0.072(6) 0.032(4) -0.010(4) 0.006(3) -0.016(4) C14 0.024(3) 0.058(5) 0.029(4) -0.017(4) -0.003(3) 0.005(3) C15 0.032(4) 0.040(4) 0.027(4) -0.004(3) -0.003(3) 0.003(3) C16 0.032(4) 0.051(5) 0.036(4) -0.012(4) -0.003(3) -0.009(3) C17 0.043(5) 0.048(5) 0.069(6) -0.016(4) -0.014(4) -0.006(4) C18 0.050(5) 0.045(5) 0.090(7) -0.021(5) -0.019(5) 0.002(4) C19 0.034(4) 0.090(7) 0.055(6) -0.046(5) -0.007(4) 0.004(5) C20 0.036(4) 0.070(6) 0.041(5) -0.024(4) -0.005(3) -0.008(4) C1A 0.032(4) 0.140(10) 0.036(5) 0.016(6) -0.007(3) -0.013(6) C2A 0.051(6) 0.233(14) 0.036(5) -0.020(7) 0.016(5) -0.034(7) C3A 0.058(8) 0.41(4) 0.032(7) 0.028(15) 0.003(5) -0.068(17) C4A 0.048(8) 0.41(4) 0.097(13) 0.14(2) -0.016(7) -0.084(17) C5A 0.068(8) 0.248(19) 0.130(12) 0.125(13) -0.034(8) -0.050(10) C6A 0.037(5) 0.153(11) 0.073(7) 0.063(8) -0.012(4) -0.024(6) C1B 0.042(4) 0.058(5) 0.034(5) -0.021(4) -0.005(3) -0.001(4) C2B 0.047(5) 0.076(6) 0.060(6) -0.025(5) -0.004(4) -0.011(5) C3B 0.036(5) 0.075(7) 0.112(9) -0.028(6) -0.019(5) 0.007(5) C4B 0.074(7) 0.060(7) 0.100(9) -0.004(6) -0.022(6) 0.001(5) C5B 0.069(7) 0.084(7) 0.068(7) -0.013(5) 0.008(5) 0.001(6) C6B 0.040(5) 0.084(7) 0.048(5) -0.014(5) -0.007(4) 0.009(5) C1C 0.046(5) 0.078(6) 0.036(5) -0.016(4) -0.005(3) 0.014(4) C2C 0.048(5) 0.102(8) 0.084(8) -0.029(6) -0.020(5) 0.028(6) C3C 0.104(9) 0.095(10) 0.095(9) -0.025(8) -0.038(7) 0.054(8) C4C 0.145(11) 0.065(8) 0.081(8) -0.010(6) -0.031(8) 0.033(8) C5C 0.097(8) 0.062(7) 0.074(7) -0.019(6) -0.004(6) 0.014(6) C6C 0.046(5) 0.056(6) 0.052(5) -0.006(4) -0.004(4) 0.019(4) C1D 0.022(4) 0.149(10) 0.035(5) -0.011(6) -0.005(3) 0.006(5) C2D 0.043(5) 0.189(13) 0.048(6) -0.031(7) 0.004(4) 0.005(7) C3D 0.060(7) 0.208(15) 0.055(7) -0.057(8) 0.003(5) 0.013(8) C4D 0.057(7) 0.32(3) 0.035(7) -0.013(11) 0.016(5) 0.005(11) C5D 0.043(6) 0.254(18) 0.046(7) 0.016(9) 0.008(5) 0.009(8) C6D 0.042(5) 0.179(12) 0.044(6) 0.022(7) -0.002(4) 0.006(6) C1E 0.024(3) 0.044(4) 0.025(4) -0.006(3) -0.002(3) 0.001(3) C2E 0.044(4) 0.047(5) 0.037(4) 0.000(4) 0.002(3) 0.004(4) C3E 0.058(5) 0.051(5) 0.054(6) 0.002(4) 0.011(4) -0.006(4) C4E 0.073(6) 0.053(5) 0.049(5) 0.023(4) 0.028(5) 0.021(5) C5E 0.048(5) 0.074(6) 0.041(5) 0.001(4) 0.010(4) 0.015(5) C6E 0.048(4) 0.051(5) 0.030(4) 0.000(4) -0.001(3) 0.007(4) C1F 0.034(4) 0.044(4) 0.028(4) -0.004(3) -0.005(3) 0.001(3) C2F 0.040(4) 0.051(5) 0.045(5) 0.005(4) 0.001(3) 0.005(4) C3F 0.058(5) 0.047(5) 0.066(6) -0.002(5) -0.001(4) 0.006(4) C4F 0.069(6) 0.049(6) 0.063(6) -0.015(5) -0.001(5) 0.021(5) C5F 0.054(5) 0.072(6) 0.038(5) -0.012(5) 0.002(4) 0.014(4) C6F 0.044(4) 0.048(5) 0.035(4) -0.013(4) 0.002(3) 0.000(4) C1G 0.048(5) 0.064(6) 0.030(4) -0.003(4) -0.008(3) -0.008(4) C2G 0.059(6) 0.074(7) 0.083(7) 0.011(5) 0.020(5) -0.008(5) C3G 0.081(8) 0.098(9) 0.104(9) 0.011(7) 0.029(7) -0.032(7) C4G 0.122(10) 0.086(9) 0.067(8) 0.016(6) 0.007(7) -0.029(8) C5G 0.103(9) 0.069(7) 0.068(7) 0.015(5) -0.012(6) -0.013(6) C6G 0.074(6) 0.080(7) 0.056(6) 0.008(5) -0.016(5) -0.007(6) C1H 0.032(4) 0.086(7) 0.043(5) 0.004(5) -0.015(3) -0.004(4) C2H 0.058(5) 0.086(7) 0.052(6) 0.007(5) -0.005(4) -0.005(5) C3H 0.071(6) 0.089(8) 0.078(7) -0.010(6) 0.002(5) 0.007(6) C4H 0.061(6) 0.115(9) 0.056(6) 0.007(6) 0.018(5) 0.004(6) C5H 0.050(5) 0.098(8) 0.051(6) 0.016(5) 0.004(4) -0.004(5) C6H 0.036(4) 0.081(6) 0.057(6) 0.012(5) -0.007(4) 0.001(4) C1I 0.038(4) 0.095(7) 0.050(5) -0.028(5) 0.005(4) 0.001(5) C2I 0.039(5) 0.101(8) 0.052(6) -0.007(5) 0.000(4) -0.004(5) C3I 0.053(6) 0.119(9) 0.063(7) -0.006(6) 0.011(5) -0.014(6) C4I 0.056(7) 0.163(13) 0.105(10) -0.031(9) 0.023(6) -0.027(8) C5I 0.069(7) 0.169(13) 0.113(10) -0.063(9) 0.051(7) -0.016(8) C6I 0.048(5) 0.134(10) 0.109(9) -0.046(8) 0.018(6) 0.002(6) C1J 0.092(7) 0.054(6) 0.068(7) -0.033(5) 0.002(6) -0.008(6) C2J 0.102(9) 0.088(9) 0.099(9) -0.058(8) -0.022(7) 0.012(7) C3J 0.194(18) 0.083(11) 0.107(12) -0.044(9) -0.063(11) 0.031(11) C4J 0.24(2) 0.065(10) 0.119(14) -0.014(9) -0.036(15) -0.008(13) C5J 0.23(2) 0.084(11) 0.125(14) 0.002(10) 0.005(14) 0.002(13) C6J 0.138(10) 0.074(8) 0.078(8) -0.009(6) 0.026(7) -0.011(8) C1K 0.028(3) 0.050(5) 0.035(4) -0.002(3) 0.004(3) -0.004(3) C2K 0.050(5) 0.084(6) 0.035(5) -0.008(4) -0.005(4) -0.018(4) C3K 0.077(6) 0.113(8) 0.033(5) 0.004(5) 0.000(4) -0.043(6) C4K 0.055(5) 0.105(8) 0.054(6) 0.010(5) 0.001(4) -0.041(5) C5K 0.051(5) 0.089(7) 0.049(5) -0.001(5) -0.002(4) -0.038(5) C6K 0.042(4) 0.058(5) 0.034(4) -0.004(4) -0.004(3) -0.015(4) C1L 0.041(4) 0.049(5) 0.028(4) 0.003(3) -0.008(3) 0.000(4) C2L 0.048(5) 0.057(6) 0.050(5) -0.004(4) -0.010(4) 0.002(4) C3L 0.076(7) 0.060(6) 0.067(7) -0.011(5) -0.021(5) 0.021(5) C4L 0.091(7) 0.052(6) 0.069(7) -0.001(5) -0.039(6) 0.009(6) C5L 0.079(7) 0.059(7) 0.090(8) 0.014(6) -0.011(6) -0.026(6) C6L 0.055(5) 0.070(6) 0.057(6) 0.002(5) 0.003(4) -0.003(5) S2 0.088(5) 0.113(7) 0.103(7) 0.022(6) -0.002(4) 0.045(5) S2A 0.079(3) 0.055(3) 0.096(4) 0.021(3) 0.034(3) 0.020(2) S1 0.0547(13) 0.0727(17) 0.0709(17) 0.0089(14) -0.0127(12) 0.0079(12) O1 0.109(5) 0.116(6) 0.056(5) 0.005(4) -0.006(4) 0.030(5) O2 0.074(4) 0.070(4) 0.094(5) 0.002(4) 0.006(3) 0.024(3) O3 0.076(5) 0.099(6) 0.216(10) 0.045(6) -0.053(5) -0.028(5) C21 0.054(6) 0.075(7) 0.072(7) 0.007(5) 0.008(5) 0.013(5) F1 0.073(4) 0.122(5) 0.096(5) -0.002(4) -0.027(3) -0.008(4) F2 0.083(4) 0.090(4) 0.097(4) 0.000(3) -0.003(3) 0.035(3) F3 0.101(4) 0.158(6) 0.081(4) 0.050(4) 0.032(3) 0.055(4) _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 C1 2.122(6) . ? Pd1 P2 2.317(2) . ? Pd1 P1 2.322(2) . ? Pd1 P5 2.3761(17) . ? Pd2 C6 2.130(7) . ? Pd2 P4 2.303(2) . ? Pd2 P3 2.313(2) . ? Pd2 P6 2.3628(18) . ? Fe1 C13 2.030(7) . ? Fe1 C12 2.040(7) . ? Fe1 C18 2.043(8) . ? Fe1 C19 2.049(7) . ? Fe1 C11 2.051(6) . ? Fe1 C16 2.053(7) . ? Fe1 C17 2.055(7) . ? Fe1 C15 2.058(7) . ? Fe1 C14 2.059(6) . ? Fe1 C20 2.078(7) . ? P1 C1A 1.786(10) . ? P1 C1B 1.814(8) . ? P1 C3 1.821(8) . ? P2 C1C 1.813(9) . ? P2 C5 1.813(7) . ? P2 C1D 1.815(9) . ? P3 C1H 1.807(9) . ? P3 C1G 1.822(8) . ? P3 C8 1.832(7) . ? P4 C1J 1.803(11) . ? P4 C10 1.819(8) . ? P4 C1I 1.828(8) . ? P5 C1E 1.815(7) . ? P5 C11 1.824(6) . ? P5 C1F 1.841(7) . ? P6 C16 1.819(7) . ? P6 C1L 1.820(7) . ? P6 C1K 1.836(7) . ? C1 C2 1.507(10) . ? C1 C4 1.526(9) . ? C2 C3 1.518(11) . ? C4 C5 1.521(10) . ? C6 C7 1.478(12) . ? C6 C9 1.533(11) . ? C7 C8 1.523(12) . ? C9 C10 1.522(13) . ? C11 C15 1.422(9) . ? C11 C12 1.427(9) . ? C12 C13 1.414(9) . ? C13 C14 1.418(10) . ? C14 C15 1.407(9) . ? C16 C17 1.427(10) . ? C16 C20 1.439(10) . ? C17 C18 1.436(10) . ? C18 C19 1.389(12) . ? C19 C20 1.423(11) . ? C1A C6A 1.372(14) . ? C1A C2A 1.413(13) . ? C2A C3A 1.359(18) . ? C3A C4A 1.28(3) . ? C4A C5A 1.37(3) . ? C5A C6A 1.433(14) . ? C1B C6B 1.377(11) . ? C1B C2B 1.397(10) . ? C2B C3B 1.398(12) . ? C3B C4B 1.340(13) . ? C4B C5B 1.395(13) . ? C5B C6B 1.362(12) . ? C1C C6C 1.364(11) . ? C1C C2C 1.402(11) . ? C2C C3C 1.354(15) . ? C3C C4C 1.348(15) . ? C4C C5C 1.364(13) . ? C5C C6C 1.390(12) . ? C1D C6D 1.388(13) . ? C1D C2D 1.406(14) . ? C2D C3D 1.380(13) . ? C3D C4D 1.392(19) . ? C4D C5D 1.35(2) . ? C5D C6D 1.409(13) . ? C1E C2E 1.379(9) . ? C1E C6E 1.390(9) . ? C2E C3E 1.365(10) . ? C3E C4E 1.366(11) . ? C4E C5E 1.381(11) . ? C5E C6E 1.398(10) . ? C1F C2F 1.377(9) . ? C1F C6F 1.388(9) . ? C2F C3F 1.384(10) . ? C3F C4F 1.372(11) . ? C4F C5F 1.365(11) . ? C5F C6F 1.388(10) . ? C1G C6G 1.362(11) . ? C1G C2G 1.381(11) . ? C2G C3G 1.388(12) . ? C3G C4G 1.348(14) . ? C4G C5G 1.375(14) . ? C5G C6G 1.369(12) . ? C1H C6H 1.398(11) . ? C1H C2H 1.405(12) . ? C2H C3H 1.421(12) . ? C3H C4H 1.380(12) . ? C4H C5H 1.382(13) . ? C5H C6H 1.408(11) . ? C1I C6I 1.371(11) . ? C1I C2I 1.385(12) . ? C2I C3I 1.384(11) . ? C3I C4I 1.351(14) . ? C4I C5I 1.381(16) . ? C5I C6I 1.401(14) . ? C1J C6J 1.373(13) . ? C1J C2J 1.392(13) . ? C2J C3J 1.466(17) . ? C3J C4J 1.37(2) . ? C4J C5J 1.34(2) . ? C5J C6J 1.383(17) . ? C1K C6K 1.369(9) . ? C1K C2K 1.375(10) . ? C2K C3K 1.372(10) . ? C3K C4K 1.357(11) . ? C4K C5K 1.362(11) . ? C5K C6K 1.375(10) . ? C1L C2L 1.375(10) . ? C1L C6L 1.406(10) . ? C2L C3L 1.364(11) . ? C3L C4L 1.371(12) . ? C4L C5L 1.360(13) . ? C5L C6L 1.366(12) . ? S2 O4 1.400(9) . ? S2 O5 1.421(9) . ? S2 O6 1.446(9) . ? S2 C22 1.693(15) . ? C22 F6 1.317(10) . ? C22 F5 1.322(10) . ? C22 F4 1.352(10) . ? S2A O5A 1.406(9) . ? S2A O4A 1.422(9) . ? S2A O6A 1.431(9) . ? S2A C22A 1.545(15) . ? C22A F5A 1.297(10) . ? C22A F6A 1.310(10) . ? C22A F4A 1.329(10) . ? S1 O2 1.431(6) . ? S1 O1 1.433(7) . ? S1 O3 1.444(7) . ? S1 C21 1.791(9) . ? C21 F2 1.324(10) . ? C21 F1 1.332(10) . ? C21 F3 1.335(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 C1 Pd1 P2 80.9(2) . . ? C1 Pd1 P1 81.2(2) . . ? P2 Pd1 P1 159.74(7) . . ? C1 Pd1 P5 166.9(2) . . ? P2 Pd1 P5 100.45(7) . . ? P1 Pd1 P5 99.13(6) . . ? C6 Pd2 P4 81.7(2) . . ? C6 Pd2 P3 80.7(3) . . ? P4 Pd2 P3 159.29(8) . . ? C6 Pd2 P6 167.9(2) . . ? P4 Pd2 P6 100.33(8) . . ? P3 Pd2 P6 99.16(7) . . ? C13 Fe1 C12 40.7(3) . . ? C13 Fe1 C18 118.9(4) . . ? C12 Fe1 C18 103.9(3) . . ? C13 Fe1 C19 155.2(4) . . ? C12 Fe1 C19 121.2(3) . . ? C18 Fe1 C19 39.7(3) . . ? C13 Fe1 C11 68.3(3) . . ? C12 Fe1 C11 40.8(2) . . ? C18 Fe1 C11 121.8(3) . . ? C19 Fe1 C11 109.5(3) . . ? C13 Fe1 C16 121.8(3) . . ? C12 Fe1 C16 156.4(3) . . ? C18 Fe1 C16 68.8(3) . . ? C19 Fe1 C16 68.1(3) . . ? C11 Fe1 C16 161.7(3) . . ? C13 Fe1 C17 104.2(3) . . ? C12 Fe1 C17 119.3(3) . . ? C18 Fe1 C17 41.0(3) . . ? C19 Fe1 C17 67.6(3) . . ? C11 Fe1 C17 156.8(3) . . ? C16 Fe1 C17 40.6(3) . . ? C13 Fe1 C15 67.6(3) . . ? C12 Fe1 C15 68.1(3) . . ? C18 Fe1 C15 160.3(3) . . ? C19 Fe1 C15 127.9(3) . . ? C11 Fe1 C15 40.5(2) . . ? C16 Fe1 C15 125.7(3) . . ? C17 Fe1 C15 158.7(3) . . ? C13 Fe1 C14 40.6(3) . . ? C12 Fe1 C14 68.4(3) . . ? C18 Fe1 C14 155.8(3) . . ? C19 Fe1 C14 163.6(4) . . ? C11 Fe1 C14 68.2(2) . . ? C16 Fe1 C14 108.6(3) . . ? C17 Fe1 C14 121.2(3) . . ? C15 Fe1 C14 40.0(2) . . ? C13 Fe1 C20 160.4(3) . . ? C12 Fe1 C20 158.9(3) . . ? C18 Fe1 C20 67.9(4) . . ? C19 Fe1 C20 40.3(3) . . ? C11 Fe1 C20 125.7(3) . . ? C16 Fe1 C20 40.8(3) . . ? C17 Fe1 C20 68.1(3) . . ? C15 Fe1 C20 112.8(3) . . ? C14 Fe1 C20 126.8(3) . . ? C1A P1 C1B 106.8(4) . . ? C1A P1 C3 103.4(4) . . ? C1B P1 C3 105.7(4) . . ? C1A P1 Pd1 114.0(4) . . ? C1B P1 Pd1 121.7(2) . . ? C3 P1 Pd1 103.5(2) . . ? C1C P2 C5 104.5(4) . . ? C1C P2 C1D 106.3(5) . . ? C5 P2 C1D 104.1(4) . . ? C1C P2 Pd1 110.7(3) . . ? C5 P2 Pd1 104.1(3) . . ? C1D P2 Pd1 125.1(3) . . ? C1H P3 C1G 108.1(4) . . ? C1H P3 C8 106.8(4) . . ? C1G P3 C8 103.6(4) . . ? C1H P3 Pd2 121.4(3) . . ? C1G P3 Pd2 111.6(3) . . ? C8 P3 Pd2 103.7(3) . . ? C1J P4 C10 105.3(5) . . ? C1J P4 C1I 109.1(5) . . ? C10 P4 C1I 103.1(4) . . ? C1J P4 Pd2 125.4(3) . . ? C10 P4 Pd2 104.2(3) . . ? C1I P4 Pd2 107.5(3) . . ? C1E P5 C11 103.5(3) . . ? C1E P5 C1F 104.5(3) . . ? C11 P5 C1F 105.3(3) . . ? C1E P5 Pd1 108.7(2) . . ? C11 P5 Pd1 116.5(2) . . ? C1F P5 Pd1 116.9(2) . . ? C16 P6 C1L 104.6(3) . . ? C16 P6 C1K 102.4(3) . . ? C1L P6 C1K 106.9(3) . . ? C16 P6 Pd2 118.3(2) . . ? C1L P6 Pd2 117.0(2) . . ? C1K P6 Pd2 106.3(2) . . ? C2 C1 C4 113.1(6) . . ? C2 C1 Pd1 115.3(5) . . ? C4 C1 Pd1 116.8(5) . . ? C1 C2 C3 109.0(6) . . ? C2 C3 P1 104.9(6) . . ? C5 C4 C1 109.6(6) . . ? C4 C5 P2 105.0(5) . . ? C7 C6 C9 112.2(7) . . ? C7 C6 Pd2 115.7(6) . . ? C9 C6 Pd2 113.9(5) . . ? C6 C7 C8 109.8(7) . . ? C7 C8 P3 103.2(6) . . ? C10 C9 C6 109.2(7) . . ? C9 C10 P4 103.9(6) . . ? C15 C11 C12 107.2(5) . . ? C15 C11 P5 125.4(5) . . ? C12 C11 P5 126.5(5) . . ? C15 C11 Fe1 70.0(4) . . ? C12 C11 Fe1 69.2(3) . . ? P5 C11 Fe1 134.2(3) . . ? C13 C12 C11 107.5(6) . . ? C13 C12 Fe1 69.3(4) . . ? C11 C12 Fe1 70.0(4) . . ? C12 C13 C14 109.0(6) . . ? C12 C13 Fe1 70.0(4) . . ? C14 C13 Fe1 70.8(4) . . ? C15 C14 C13 107.2(6) . . ? C15 C14 Fe1 70.0(4) . . ? C13 C14 Fe1 68.6(4) . . ? C14 C15 C11 109.1(6) . . ? C14 C15 Fe1 70.1(4) . . ? C11 C15 Fe1 69.5(4) . . ? C17 C16 C20 107.6(7) . . ? C17 C16 P6 125.5(5) . . ? C20 C16 P6 126.1(6) . . ? C17 C16 Fe1 69.7(4) . . ? C20 C16 Fe1 70.5(4) . . ? P6 C16 Fe1 132.9(4) . . ? C16 C17 C18 107.8(7) . . ? C16 C17 Fe1 69.6(4) . . ? C18 C17 Fe1 69.0(4) . . ? C19 C18 C17 107.8(8) . . ? C19 C18 Fe1 70.4(5) . . ? C17 C18 Fe1 70.0(4) . . ? C18 C19 C20 109.9(7) . . ? C18 C19 Fe1 69.9(5) . . ? C20 C19 Fe1 71.0(4) . . ? C19 C20 C16 106.8(7) . . ? C19 C20 Fe1 68.7(4) . . ? C16 C20 Fe1 68.7(4) . . ? C6A C1A C2A 116.8(10) . . ? C6A C1A P1 120.2(8) . . ? C2A C1A P1 122.9(10) . . ? C3A C2A C1A 120.3(16) . . ? C4A C3A C2A 125(2) . . ? C3A C4A C5A 117.5(17) . . ? C4A C5A C6A 121.6(18) . . ? C1A C6A C5A 118.7(13) . . ? C6B C1B C2B 118.7(8) . . ? C6B C1B P1 117.2(6) . . ? C2B C1B P1 124.0(7) . . ? C1B C2B C3B 119.2(9) . . ? C4B C3B C2B 120.6(9) . . ? C3B C4B C5B 120.7(9) . . ? C6B C5B C4B 119.1(10) . . ? C5B C6B C1B 121.6(8) . . ? C6C C1C C2C 118.7(9) . . ? C6C C1C P2 119.4(6) . . ? C2C C1C P2 121.9(8) . . ? C3C C2C C1C 120.5(10) . . ? C4C C3C C2C 120.2(10) . . ? C3C C4C C5C 121.0(11) . . ? C4C C5C C6C 119.6(10) . . ? C1C C6C C5C 120.0(8) . . ? C6D C1D C2D 119.5(9) . . ? C6D C1D P2 118.4(9) . . ? C2D C1D P2 122.1(8) . . ? C3D C2D C1D 120.4(12) . . ? C2D C3D C4D 119.4(13) . . ? C5D C4D C3D 120.7(12) . . ? C4D C5D C6D 121.1(14) . . ? C1D C6D C5D 118.8(12) . . ? C2E C1E C6E 117.8(7) . . ? C2E C1E P5 120.0(5) . . ? C6E C1E P5 122.2(5) . . ? C3E C2E C1E 122.4(7) . . ? C2E C3E C4E 119.1(8) . . ? C3E C4E C5E 121.3(8) . . ? C4E C5E C6E 118.6(8) . . ? C1E C6E C5E 120.7(7) . . ? C2F C1F C6F 119.5(7) . . ? C2F C1F P5 119.1(5) . . ? C6F C1F P5 121.4(6) . . ? C1F C2F C3F 120.8(7) . . ? C4F C3F C2F 119.4(8) . . ? C5F C4F C3F 120.4(8) . . ? C4F C5F C6F 120.8(8) . . ? C5F C6F C1F 119.1(7) . . ? C6G C1G C2G 117.4(8) . . ? C6G C1G P3 124.3(6) . . ? C2G C1G P3 118.3(6) . . ? C1G C2G C3G 120.5(9) . . ? C4G C3G C2G 120.3(10) . . ? C3G C4G C5G 120.1(10) . . ? C6G C5G C4G 118.8(10) . . ? C1G C6G C5G 122.8(9) . . ? C6H C1H C2H 119.9(8) . . ? C6H C1H P3 116.7(7) . . ? C2H C1H P3 123.5(7) . . ? C1H C2H C3H 119.6(9) . . ? C4H C3H C2H 120.2(10) . . ? C3H C4H C5H 119.8(9) . . ? C4H C5H C6H 121.5(9) . . ? C1H C6H C5H 119.0(9) . . ? C6I C1I C2I 118.8(9) . . ? C6I C1I P4 122.3(8) . . ? C2I C1I P4 118.6(6) . . ? C3I C2I C1I 122.8(9) . . ? C4I C3I C2I 117.3(11) . . ? C3I C4I C5I 122.3(11) . . ? C4I C5I C6I 119.5(10) . . ? C1I C6I C5I 119.3(11) . . ? C6J C1J C2J 119.3(11) . . ? C6J C1J P4 118.9(9) . . ? C2J C1J P4 121.8(9) . . ? C1J C2J C3J 117.6(13) . . ? C4J C3J C2J 118.7(17) . . ? C5J C4J C3J 123(2) . . ? C4J C5J C6J 118.6(19) . . ? C1J C6J C5J 122.8(14) . . ? C6K C1K C2K 118.4(6) . . ? C6K C1K P6 118.4(5) . . ? C2K C1K P6 123.2(5) . . ? C3K C2K C1K 120.5(7) . . ? C4K C3K C2K 120.7(8) . . ? C3K C4K C5K 119.2(8) . . ? C4K C5K C6K 120.5(7) . . ? C1K C6K C5K 120.6(7) . . ? C2L C1L C6L 116.5(7) . . ? C2L C1L P6 124.1(6) . . ? C6L C1L P6 119.3(6) . . ? C3L C2L C1L 121.2(8) . . ? C2L C3L C4L 121.5(9) . . ? C5L C4L C3L 118.8(9) . . ? C4L C5L C6L 120.3(9) . . ? C5L C6L C1L 121.7(8) . . ? O4 S2 O5 114.4(13) . . ? O4 S2 O6 116.9(12) . . ? O5 S2 O6 116.0(14) . . ? O4 S2 C22 99.0(11) . . ? O5 S2 C22 106.2(11) . . ? O6 S2 C22 101.0(11) . . ? F6 C22 F5 102.0(15) . . ? F6 C22 F4 99.7(15) . . ? F5 C22 F4 107.2(16) . . ? F6 C22 S2 118.3(14) . . ? F5 C22 S2 123.2(14) . . ? F4 C22 S2 103.7(13) . . ? O5A S2A O4A 116.6(10) . . ? O5A S2A O6A 116.5(10) . . ? O4A S2A O6A 110.4(9) . . ? O5A S2A C22A 104.5(10) . . ? O4A S2A C22A 98.4(9) . . ? O6A S2A C22A 108.2(9) . . ? F5A C22A F6A 100.1(13) . . ? F5A C22A F4A 94.6(12) . . ? F6A C22A F4A 96.4(13) . . ? F5A C22A S2A 121.3(12) . . ? F6A C22A S2A 120.8(13) . . ? F4A C22A S2A 117.9(12) . . ? O2 S1 O1 113.3(4) . . ? O2 S1 O3 115.2(5) . . ? O1 S1 O3 116.2(5) . . ? O2 S1 C21 104.4(4) . . ? O1 S1 C21 102.7(4) . . ? O3 S1 C21 102.7(5) . . ? F2 C21 F1 106.1(7) . . ? F2 C21 F3 107.5(8) . . ? F1 C21 F3 105.3(8) . . ? F2 C21 S1 113.0(7) . . ? F1 C21 S1 111.7(7) . . ? F3 C21 S1 112.8(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.064 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.106 # Attachment '4.CIF' data_6056 _database_code_depnum_ccdc_archive 'CCDC 654028' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35.50 H36 N O0.50 P2 Pd S' _chemical_formula_weight 685.05 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' Pd Pd -0.9988 1.0072 '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 22.749(3) _cell_length_b 9.4172(12) _cell_length_c 29.902(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.231(3) _cell_angle_gamma 90.00 _cell_volume 6355.2(14) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6841 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 24.91 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 0.778 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7671 _exptl_absorpt_correction_T_max 0.9263 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40276 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7280 _reflns_number_gt 6470 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+7.7895P] 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 constructed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7280 _refine_ls_number_parameters 388 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0897 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.004 _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 0.669273(8) 0.19303(2) 0.598901(7) 0.02127(7) Uani 1 1 d . . . S1 S 0.75871(3) 0.05463(8) 0.60800(3) 0.03213(17) Uani 1 1 d . . . P1 P 0.60535(3) 0.00494(7) 0.58347(2) 0.02341(15) Uani 1 1 d . . . P2 P 0.70263(3) 0.39803(7) 0.63410(2) 0.02412(15) Uani 1 1 d . . . N1 N 0.91820(15) 0.2694(4) 0.55748(14) 0.0659(10) Uani 1 1 d . . . C1 C 0.58962(12) 0.3112(3) 0.58781(10) 0.0271(6) Uani 1 1 d . . . H1 H 0.5863 0.3405 0.5558 0.033 Uiso 1 1 calc R . . C2 C 0.53391(12) 0.2236(3) 0.59147(10) 0.0310(6) Uani 1 1 d . . . H2A H 0.5318 0.2003 0.6232 0.037 Uiso 1 1 calc R . . H2B H 0.4988 0.2798 0.5805 0.037 Uiso 1 1 calc R . . C3 C 0.53391(12) 0.0870(3) 0.56421(10) 0.0313(6) Uani 1 1 d . . . H3A' H 0.5303 0.1075 0.5318 0.038 Uiso 1 1 calc R . . H3B' H 0.5012 0.0249 0.5701 0.038 Uiso 1 1 calc R . . C4 C 0.58871(13) 0.4494(3) 0.61413(10) 0.0323(6) Uani 1 1 d . . . H4A H 0.5562 0.5092 0.6002 0.039 Uiso 1 1 calc R . . H4B H 0.5813 0.4284 0.6450 0.039 Uiso 1 1 calc R . . C5 C 0.64657(13) 0.5300(3) 0.61540(10) 0.0315(6) Uani 1 1 d . . . H5A H 0.6481 0.6096 0.6366 0.038 Uiso 1 1 calc R . . H5B H 0.6519 0.5664 0.5855 0.038 Uiso 1 1 calc R . . C6 C 0.81799(12) 0.1420(3) 0.58864(10) 0.0297(6) Uani 1 1 d . . . C7 C 0.81249(15) 0.2471(4) 0.55559(11) 0.0402(7) Uani 1 1 d . . . H7 H 0.7748 0.2779 0.5427 0.048 Uiso 1 1 calc R . . C8 C 0.86276(18) 0.3054(4) 0.54205(14) 0.0584(11) Uani 1 1 d . . . H8 H 0.8575 0.3769 0.5200 0.070 Uiso 1 1 calc R . . C9 C 0.92244(15) 0.1685(4) 0.58884(15) 0.0546(10) Uani 1 1 d . . . H9 H 0.9608 0.1391 0.6005 0.065 Uiso 1 1 calc R . . C10 C 0.87614(13) 0.1038(4) 0.60556(12) 0.0396(8) Uani 1 1 d . . . H10 H 0.8832 0.0344 0.6282 0.048 Uiso 1 1 calc R . . C1A C 0.77494(12) 0.4796(3) 0.63415(9) 0.0284(6) Uani 1 1 d . . . C2A C 0.78255(15) 0.6055(3) 0.61145(11) 0.0405(8) Uani 1 1 d . . . H2A1 H 0.7496 0.6522 0.5960 0.049 Uiso 1 1 calc R . . C3A C 0.83870(18) 0.6624(4) 0.61162(13) 0.0529(10) Uani 1 1 d . . . H3A H 0.8436 0.7477 0.5962 0.063 Uiso 1 1 calc R . . C4A C 0.88723(16) 0.5950(4) 0.63407(13) 0.0522(10) Uani 1 1 d . . . H4A1 H 0.9253 0.6335 0.6337 0.063 Uiso 1 1 calc R . . C5A C 0.87997(15) 0.4708(4) 0.65715(12) 0.0461(8) Uani 1 1 d . . . H5A1 H 0.9131 0.4252 0.6729 0.055 Uiso 1 1 calc R . . C6A C 0.82400(13) 0.4132(3) 0.65722(10) 0.0349(7) Uani 1 1 d . . . H6A H 0.8193 0.3285 0.6730 0.042 Uiso 1 1 calc R . . C1B C 0.69640(12) 0.3829(3) 0.69413(9) 0.0267(6) Uani 1 1 d . . . C2B C 0.71215(14) 0.4960(3) 0.72290(10) 0.0344(7) Uani 1 1 d . . . H2B1 H 0.7277 0.5791 0.7116 0.041 Uiso 1 1 calc R . . C3B C 0.70506(15) 0.4872(4) 0.76813(10) 0.0408(8) Uani 1 1 d . . . H3B H 0.7156 0.5645 0.7874 0.049 Uiso 1 1 calc R . . C4B C 0.68273(15) 0.3659(4) 0.78480(11) 0.0429(8) Uani 1 1 d . . . H4B1 H 0.6781 0.3602 0.8155 0.051 Uiso 1 1 calc R . . C5B C 0.66709(16) 0.2527(4) 0.75705(11) 0.0451(8) Uani 1 1 d . . . H5B1 H 0.6519 0.1697 0.7687 0.054 Uiso 1 1 calc R . . C6B C 0.67380(15) 0.2609(3) 0.71135(10) 0.0363(7) Uani 1 1 d . . . H6B H 0.6630 0.1835 0.6923 0.044 Uiso 1 1 calc R . . C1C C 0.61192(12) -0.1445(3) 0.54586(9) 0.0261(6) Uani 1 1 d . . . C2C C 0.66558(14) -0.1754(3) 0.53046(10) 0.0343(7) Uani 1 1 d . . . H2C H 0.6985 -0.1160 0.5381 0.041 Uiso 1 1 calc R . . C3C C 0.67029(16) -0.2948(4) 0.50361(11) 0.0446(8) Uani 1 1 d . . . H3C H 0.7067 -0.3163 0.4933 0.054 Uiso 1 1 calc R . . C4C C 0.62203(16) -0.3817(4) 0.49199(11) 0.0455(8) Uani 1 1 d . . . H4C H 0.6256 -0.4631 0.4743 0.055 Uiso 1 1 calc R . . C5C C 0.56879(15) -0.3488(3) 0.50630(11) 0.0402(8) Uani 1 1 d . . . H5C H 0.5356 -0.4067 0.4977 0.048 Uiso 1 1 calc R . . C6C C 0.56325(14) -0.2320(3) 0.53317(10) 0.0328(7) Uani 1 1 d . . . H6C H 0.5265 -0.2111 0.5430 0.039 Uiso 1 1 calc R . . C1D C 0.59694(12) -0.0824(3) 0.63704(9) 0.0257(6) Uani 1 1 d . . . C2D C 0.54316(14) -0.1359(4) 0.64663(11) 0.0426(8) Uani 1 1 d . . . H2D H 0.5090 -0.1251 0.6257 0.051 Uiso 1 1 calc R . . C3D C 0.53958(17) -0.2053(4) 0.68704(13) 0.0562(10) Uani 1 1 d . . . H3D H 0.5031 -0.2429 0.6931 0.067 Uiso 1 1 calc R . . C4D C 0.58896(17) -0.2196(4) 0.71838(12) 0.0502(9) Uani 1 1 d . . . H4D H 0.5861 -0.2664 0.7458 0.060 Uiso 1 1 calc R . . C5D C 0.64227(15) -0.1657(3) 0.70960(11) 0.0388(7) Uani 1 1 d . . . H5D H 0.6759 -0.1745 0.7311 0.047 Uiso 1 1 calc R . . C6D C 0.64646(13) -0.0982(3) 0.66901(10) 0.0304(6) Uani 1 1 d . . . H6D H 0.6832 -0.0625 0.6630 0.036 Uiso 1 1 calc R . . O1 O 0.4828(5) 0.3648(14) 0.6970(4) 0.154(5) Uani 0.50 1 d PD A -1 C1S C 0.4957(6) 0.3234(15) 0.7326(5) 0.109(5) Uani 0.50 1 d PDU A -1 C2S C 0.5038(13) 0.1759(13) 0.7411(11) 0.180(12) Uani 0.50 1 d PDU A -1 H2S1 H 0.4949 0.1237 0.7131 0.270 Uiso 0.50 1 calc PR A -1 H2S2 H 0.4774 0.1451 0.7623 0.270 Uiso 0.50 1 calc PR A -1 H2S3 H 0.5445 0.1581 0.7537 0.270 Uiso 0.50 1 calc PR A -1 C3S C 0.5057(11) 0.4333(19) 0.7686(5) 0.160(9) Uani 0.50 1 d PDU A -1 H3S1 H 0.4985 0.5267 0.7554 0.239 Uiso 0.50 1 calc PR A -1 H3S2 H 0.5463 0.4277 0.7830 0.239 Uiso 0.50 1 calc PR A -1 H3S3 H 0.4789 0.4171 0.7908 0.239 Uiso 0.50 1 calc PR A -1 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 0.01855(11) 0.02105(11) 0.02413(11) 0.00063(8) 0.00236(7) -0.00081(8) S1 0.0217(3) 0.0300(4) 0.0450(4) 0.0044(3) 0.0056(3) 0.0024(3) P1 0.0199(3) 0.0240(3) 0.0260(4) 0.0001(3) 0.0014(3) -0.0022(3) P2 0.0255(4) 0.0211(3) 0.0257(4) 0.0003(3) 0.0027(3) -0.0014(3) N1 0.0429(19) 0.061(2) 0.100(3) -0.006(2) 0.0332(19) -0.0052(17) C1 0.0228(13) 0.0281(14) 0.0296(14) 0.0053(12) -0.0001(11) 0.0043(11) C2 0.0202(14) 0.0320(16) 0.0403(17) 0.0023(13) 0.0021(12) 0.0026(12) C3 0.0225(14) 0.0337(16) 0.0360(16) 0.0013(13) -0.0025(12) -0.0014(12) C4 0.0288(15) 0.0281(15) 0.0397(17) 0.0012(13) 0.0026(13) 0.0059(12) C5 0.0339(16) 0.0264(15) 0.0335(16) 0.0024(12) 0.0015(12) 0.0024(12) C6 0.0238(14) 0.0343(15) 0.0318(15) -0.0103(13) 0.0062(12) -0.0006(12) C7 0.0342(17) 0.0510(19) 0.0369(17) -0.0009(15) 0.0095(14) 0.0008(15) C8 0.059(3) 0.059(3) 0.063(3) 0.009(2) 0.031(2) -0.004(2) C9 0.0258(17) 0.050(2) 0.088(3) -0.023(2) 0.0070(18) -0.0024(15) C10 0.0298(16) 0.0405(18) 0.0476(19) -0.0131(15) 0.0010(14) 0.0032(14) C1A 0.0294(15) 0.0295(15) 0.0267(14) -0.0061(12) 0.0051(11) -0.0055(12) C2A 0.0421(19) 0.0364(17) 0.0427(18) 0.0042(14) 0.0040(15) -0.0133(15) C3A 0.060(2) 0.049(2) 0.052(2) 0.0004(17) 0.0169(19) -0.0255(19) C4A 0.039(2) 0.065(3) 0.055(2) -0.0156(19) 0.0188(17) -0.0237(19) C5A 0.0305(17) 0.058(2) 0.050(2) -0.0131(18) 0.0050(15) -0.0046(16) C6A 0.0349(17) 0.0349(16) 0.0352(16) -0.0044(13) 0.0057(13) -0.0022(13) C1B 0.0258(14) 0.0287(15) 0.0257(14) -0.0004(11) 0.0032(11) 0.0049(11) C2B 0.0406(17) 0.0315(16) 0.0307(16) 0.0000(13) 0.0027(13) -0.0020(13) C3B 0.0461(19) 0.0440(19) 0.0314(17) -0.0097(14) 0.0014(14) 0.0026(15) C4B 0.049(2) 0.053(2) 0.0273(16) 0.0032(15) 0.0096(14) 0.0080(17) C5B 0.055(2) 0.0425(19) 0.0397(19) 0.0121(16) 0.0148(16) 0.0017(17) C6B 0.0464(19) 0.0312(16) 0.0323(16) -0.0005(13) 0.0085(14) -0.0020(14) C1C 0.0288(15) 0.0277(14) 0.0214(13) 0.0009(11) 0.0014(11) -0.0037(11) C2C 0.0313(16) 0.0391(17) 0.0335(16) -0.0072(13) 0.0073(13) -0.0090(13) C3C 0.045(2) 0.049(2) 0.0433(19) -0.0127(16) 0.0164(15) -0.0053(16) C4C 0.065(2) 0.0410(19) 0.0317(17) -0.0147(14) 0.0087(16) -0.0104(17) C5C 0.048(2) 0.0368(17) 0.0341(17) -0.0037(14) -0.0026(14) -0.0177(15) C6C 0.0330(16) 0.0338(16) 0.0309(15) 0.0011(12) 0.0012(12) -0.0068(13) C1D 0.0270(14) 0.0230(13) 0.0274(14) -0.0020(11) 0.0046(11) -0.0030(11) C2D 0.0318(17) 0.056(2) 0.0412(19) 0.0097(16) 0.0077(14) -0.0062(15) C3D 0.042(2) 0.074(3) 0.056(2) 0.022(2) 0.0191(18) -0.0107(19) C4D 0.059(2) 0.059(2) 0.0343(18) 0.0159(16) 0.0150(17) -0.0028(19) C5D 0.0464(19) 0.0364(17) 0.0325(16) 0.0028(13) 0.0006(14) 0.0013(14) C6D 0.0311(15) 0.0276(15) 0.0324(15) 0.0021(12) 0.0033(12) -0.0039(12) O1 0.126(9) 0.222(14) 0.117(9) 0.043(9) 0.024(8) -0.032(9) C1S 0.068(7) 0.158(12) 0.107(11) 0.022(9) 0.039(9) -0.015(9) C2S 0.098(10) 0.173(14) 0.26(3) -0.103(18) -0.021(14) -0.054(14) C3S 0.167(17) 0.154(14) 0.16(2) -0.009(13) 0.03(2) 0.050(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 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 C1 2.117(3) . ? Pd1 P2 2.2824(8) . ? Pd1 P1 2.3013(7) . ? Pd1 S1 2.4027(8) . ? S1 C6 1.740(3) . ? P1 C1C 1.820(3) . ? P1 C3 1.826(3) . ? P1 C1D 1.832(3) . ? P2 C1A 1.816(3) . ? P2 C5 1.818(3) . ? P2 C1B 1.824(3) . ? N1 C9 1.330(5) . ? N1 C8 1.331(5) . ? C1 C4 1.522(4) . ? C1 C2 1.528(4) . ? C2 C3 1.523(4) . ? C4 C5 1.516(4) . ? C6 C7 1.393(5) . ? C6 C10 1.402(4) . ? C7 C8 1.375(5) . ? C9 C10 1.365(5) . ? C1A C6A 1.385(4) . ? C1A C2A 1.388(4) . ? C2A C3A 1.384(5) . ? C3A C4A 1.373(6) . ? C4A C5A 1.378(5) . ? C5A C6A 1.384(4) . ? C1B C6B 1.384(4) . ? C1B C2B 1.387(4) . ? C2B C3B 1.384(4) . ? C3B C4B 1.370(5) . ? C4B C5B 1.370(5) . ? C5B C6B 1.396(4) . ? C1C C2C 1.388(4) . ? C1C C6C 1.394(4) . ? C2C C3C 1.394(4) . ? C3C C4C 1.378(5) . ? C4C C5C 1.370(5) . ? C5C C6C 1.378(4) . ? C1D C2D 1.386(4) . ? C1D C6D 1.391(4) . ? C2D C3D 1.385(5) . ? C3D C4D 1.376(5) . ? C4D C5D 1.370(5) . ? C5D C6D 1.384(4) . ? O1 C1S 1.137(12) . ? C1S C2S 1.420(15) . ? C1S C3S 1.489(14) . ? 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 C1 Pd1 P2 81.71(8) . . ? C1 Pd1 P1 82.33(8) . . ? P2 Pd1 P1 155.29(3) . . ? C1 Pd1 S1 177.35(8) . . ? P2 Pd1 S1 100.31(3) . . ? P1 Pd1 S1 96.31(3) . . ? C6 S1 Pd1 112.73(11) . . ? C1C P1 C3 105.75(13) . . ? C1C P1 C1D 102.64(12) . . ? C3 P1 C1D 106.20(13) . . ? C1C P1 Pd1 128.34(9) . . ? C3 P1 Pd1 104.62(10) . . ? C1D P1 Pd1 107.65(9) . . ? C1A P2 C5 108.15(14) . . ? C1A P2 C1B 102.41(13) . . ? C5 P2 C1B 102.59(13) . . ? C1A P2 Pd1 127.37(9) . . ? C5 P2 Pd1 104.88(10) . . ? C1B P2 Pd1 108.97(10) . . ? C9 N1 C8 114.1(3) . . ? C4 C1 C2 111.1(2) . . ? C4 C1 Pd1 115.83(19) . . ? C2 C1 Pd1 113.96(18) . . ? C3 C2 C1 111.2(2) . . ? C2 C3 P1 104.38(19) . . ? C5 C4 C1 111.9(2) . . ? C4 C5 P2 103.82(19) . . ? C7 C6 C10 115.8(3) . . ? C7 C6 S1 124.6(2) . . ? C10 C6 S1 119.6(3) . . ? C8 C7 C6 119.3(3) . . ? N1 C8 C7 125.7(4) . . ? N1 C9 C10 125.9(4) . . ? C9 C10 C6 119.3(3) . . ? C6A C1A C2A 119.2(3) . . ? C6A C1A P2 118.8(2) . . ? C2A C1A P2 122.0(2) . . ? C3A C2A C1A 120.0(3) . . ? C4A C3A C2A 120.5(3) . . ? C3A C4A C5A 119.8(3) . . ? C4A C5A C6A 120.1(3) . . ? C5A C6A C1A 120.4(3) . . ? C6B C1B C2B 119.0(3) . . ? C6B C1B P2 120.6(2) . . ? C2B C1B P2 120.3(2) . . ? C3B C2B C1B 120.5(3) . . ? C4B C3B C2B 120.0(3) . . ? C3B C4B C5B 120.6(3) . . ? C4B C5B C6B 119.9(3) . . ? C1B C6B C5B 120.1(3) . . ? C2C C1C C6C 119.2(3) . . ? C2C C1C P1 120.7(2) . . ? C6C C1C P1 120.1(2) . . ? C1C C2C C3C 119.6(3) . . ? C4C C3C C2C 120.5(3) . . ? C5C C4C C3C 119.6(3) . . ? C4C C5C C6C 120.8(3) . . ? C5C C6C C1C 120.2(3) . . ? C2D C1D C6D 118.6(3) . . ? C2D C1D P1 122.4(2) . . ? C6D C1D P1 119.0(2) . . ? C3D C2D C1D 120.2(3) . . ? C4D C3D C2D 120.5(3) . . ? C5D C4D C3D 120.0(3) . . ? C4D C5D C6D 119.9(3) . . ? C5D C6D C1D 120.8(3) . . ? O1 C1S C2S 121.0(13) . . ? O1 C1S C3S 115.9(12) . . ? C2S C1S C3S 123.1(16) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.746 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.081 # Attachment '6.CIF' data_6146 _database_code_depnum_ccdc_archive 'CCDC 654029' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H62 F6 N P5 Pd2 S' _chemical_formula_weight 1346.85 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' F F 0.0171 0.0103 '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' 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 12.9468(5) _cell_length_b 17.4888(7) _cell_length_c 26.5948(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.3880(10) _cell_angle_gamma 90.00 _cell_volume 6019.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7672 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 26.31 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 0.824 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7341 _exptl_absorpt_correction_T_max 0.8934 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77929 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.50 _reflns_number_total 13826 _reflns_number_gt 12171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+4.3536P] 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 constructed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13826 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.182 _refine_ls_restrained_S_all 1.182 _refine_ls_shift/su_max 0.002 _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 0.232725(17) 0.670601(12) 0.554696(8) 0.02649(6) Uani 1 1 d . . . Pd2 Pd 0.358998(18) 0.489317(13) 0.811560(9) 0.03209(7) Uani 1 1 d . . . S1 S 0.26486(7) 0.74696(4) 0.62978(3) 0.03522(17) Uani 1 1 d . . . P1 P 0.39670(6) 0.66653(4) 0.52444(3) 0.03133(17) Uani 1 1 d . . . P2 P 0.05737(6) 0.66948(4) 0.56092(3) 0.03085(17) Uani 1 1 d . . . P3 P 0.53325(7) 0.47506(5) 0.79868(4) 0.0391(2) Uani 1 1 d . . . P4 P 0.19582(6) 0.48531(5) 0.84215(3) 0.03496(18) Uani 1 1 d . . . N1 N 0.32626(19) 0.57162(14) 0.75377(9) 0.0328(5) Uani 1 1 d . . . C1 C 0.2015(2) 0.59750(17) 0.49359(11) 0.0314(6) Uani 1 1 d . . . H1 H 0.2095 0.5452 0.5074 0.038 Uiso 1 1 calc R . . C2 C 0.2795(3) 0.6027(2) 0.45192(12) 0.0395(7) Uani 1 1 d . . . H2A H 0.2716 0.6518 0.4344 0.047 Uiso 1 1 calc R . . H2B H 0.2667 0.5617 0.4275 0.047 Uiso 1 1 calc R . . C3 C 0.3889(3) 0.5959(2) 0.47364(13) 0.0419(8) Uani 1 1 d . . . H3A H 0.4397 0.6071 0.4479 0.050 Uiso 1 1 calc R . . H3B H 0.4016 0.5443 0.4867 0.050 Uiso 1 1 calc R . . C4 C 0.0903(2) 0.60157(18) 0.47386(12) 0.0368(7) Uani 1 1 d . . . H4A H 0.0773 0.5600 0.4498 0.044 Uiso 1 1 calc R . . H4B H 0.0788 0.6502 0.4563 0.044 Uiso 1 1 calc R . . C5 C 0.0159(2) 0.59486(18) 0.51726(12) 0.0352(7) Uani 1 1 d . . . H5A H 0.0210 0.5443 0.5331 0.042 Uiso 1 1 calc R . . H5B H -0.0556 0.6032 0.5056 0.042 Uiso 1 1 calc R . . C6 C 0.3896(3) 0.4149(2) 0.87110(15) 0.0506(9) Uani 1 1 d . . . H6 H 0.4113 0.4491 0.8991 0.061 Uiso 1 1 calc R . . C7 C 0.4847(3) 0.3650(2) 0.86264(15) 0.0544(10) Uani 1 1 d . . . H7A H 0.4999 0.3341 0.8927 0.065 Uiso 1 1 calc R . . H7B H 0.4715 0.3303 0.8343 0.065 Uiso 1 1 calc R . . C8 C 0.5755(3) 0.4162(2) 0.85174(15) 0.0529(10) Uani 1 1 d . . . H8A H 0.6361 0.3857 0.8431 0.063 Uiso 1 1 calc R . . H8B H 0.5932 0.4481 0.8810 0.063 Uiso 1 1 calc R . . C9 C 0.2960(4) 0.3749(3) 0.89036(18) 0.0699(13) Uani 1 1 d . . . H9A H 0.2719 0.3371 0.8655 0.084 Uiso 1 1 calc R . . H9B H 0.3145 0.3477 0.9215 0.084 Uiso 1 1 calc R . . C10 C 0.2106(3) 0.4303(2) 0.90031(13) 0.0482(9) Uani 1 1 d . . . H10A H 0.2291 0.4638 0.9287 0.058 Uiso 1 1 calc R . . H10B H 0.1465 0.4033 0.9078 0.058 Uiso 1 1 calc R . . C11 C 0.3051(3) 0.55069(18) 0.70603(12) 0.0369(7) Uani 1 1 d . . . H11 H 0.3046 0.4982 0.6984 0.044 Uiso 1 1 calc R . . C12 C 0.2841(3) 0.60119(17) 0.66785(12) 0.0360(7) Uani 1 1 d . . . H12 H 0.2683 0.5828 0.6354 0.043 Uiso 1 1 calc R . . C13 C 0.2859(2) 0.68016(16) 0.67676(11) 0.0297(6) Uani 1 1 d . . . C14 C 0.3076(3) 0.70160(18) 0.72657(12) 0.0380(7) Uani 1 1 d . . . H14 H 0.3094 0.7537 0.7352 0.046 Uiso 1 1 calc R . . C15 C 0.3261(3) 0.64749(19) 0.76282(12) 0.0401(7) Uani 1 1 d . . . H15 H 0.3395 0.6642 0.7959 0.048 Uiso 1 1 calc R . . C1A C 0.5068(2) 0.63813(18) 0.56369(12) 0.0352(7) Uani 1 1 d . . . C2A C 0.5979(3) 0.6770(2) 0.56691(18) 0.0631(12) Uani 1 1 d . . . H2A1 H 0.6068 0.7223 0.5485 0.076 Uiso 1 1 calc R . . C3A C 0.6775(4) 0.6492(3) 0.5977(2) 0.0833(16) Uani 1 1 d . . . H3A1 H 0.7407 0.6756 0.5995 0.100 Uiso 1 1 calc R . . C4A C 0.6658(4) 0.5846(3) 0.62518(18) 0.0702(13) Uani 1 1 d . . . H4A1 H 0.7204 0.5667 0.6460 0.084 Uiso 1 1 calc R . . C5A C 0.5746(3) 0.5457(3) 0.62253(17) 0.0627(11) Uani 1 1 d . . . H5A1 H 0.5658 0.5011 0.6417 0.075 Uiso 1 1 calc R . . C6A C 0.4948(3) 0.5720(2) 0.59157(14) 0.0503(9) Uani 1 1 d . . . H6A H 0.4322 0.5449 0.5895 0.060 Uiso 1 1 calc R . . C1B C 0.4334(2) 0.75617(19) 0.49499(12) 0.0370(7) Uani 1 1 d . . . C2B C 0.5068(3) 0.7585(2) 0.45779(16) 0.0594(11) Uani 1 1 d . . . H2B1 H 0.5375 0.7128 0.4470 0.071 Uiso 1 1 calc R . . C3B C 0.5351(4) 0.8270(3) 0.4366(2) 0.0755(14) Uani 1 1 d . . . H3B1 H 0.5850 0.8280 0.4115 0.091 Uiso 1 1 calc R . . C4B C 0.4904(4) 0.8937(3) 0.45213(19) 0.0736(14) Uani 1 1 d . . . H4B1 H 0.5096 0.9405 0.4376 0.088 Uiso 1 1 calc R . . C5B C 0.4169(4) 0.8926(2) 0.48929(18) 0.0646(12) Uani 1 1 d . . . H5B1 H 0.3866 0.9385 0.5000 0.077 Uiso 1 1 calc R . . C6B C 0.3882(3) 0.82352(19) 0.51055(14) 0.0461(8) Uani 1 1 d . . . H6B H 0.3380 0.8225 0.5355 0.055 Uiso 1 1 calc R . . C1C C 0.0013(3) 0.75707(18) 0.53506(12) 0.0380(7) Uani 1 1 d . . . C2C C -0.0950(3) 0.7578(2) 0.51140(16) 0.0580(10) Uani 1 1 d . . . H2C H -0.1362 0.7135 0.5118 0.070 Uiso 1 1 calc R . . C3C C -0.1314(5) 0.8224(3) 0.48719(18) 0.0789(16) Uani 1 1 d . . . H3C H -0.1968 0.8218 0.4711 0.095 Uiso 1 1 calc R . . C4C C -0.0733(5) 0.8866(3) 0.48652(18) 0.0812(16) Uani 1 1 d . . . H4C H -0.0979 0.9303 0.4695 0.097 Uiso 1 1 calc R . . C5C C 0.0208(5) 0.8879(3) 0.5105(2) 0.0847(16) Uani 1 1 d . . . H5C H 0.0606 0.9329 0.5104 0.102 Uiso 1 1 calc R . . C6C C 0.0584(3) 0.8234(2) 0.53519(18) 0.0604(11) Uani 1 1 d . . . H6C H 0.1231 0.8251 0.5520 0.073 Uiso 1 1 calc R . . C1D C -0.0069(2) 0.65176(18) 0.61978(12) 0.0336(7) Uani 1 1 d . . . C2D C -0.0589(3) 0.7080(2) 0.64498(13) 0.0419(8) Uani 1 1 d . . . H2D H -0.0632 0.7575 0.6314 0.050 Uiso 1 1 calc R . . C3D C -0.1051(3) 0.6918(2) 0.69032(14) 0.0510(9) Uani 1 1 d . . . H3D H -0.1402 0.7307 0.7073 0.061 Uiso 1 1 calc R . . C4D C -0.1000(3) 0.6201(2) 0.71043(14) 0.0517(9) Uani 1 1 d . . . H4D H -0.1331 0.6092 0.7407 0.062 Uiso 1 1 calc R . . C5D C -0.0465(3) 0.5641(2) 0.68628(15) 0.0576(11) Uani 1 1 d . . . H5D H -0.0414 0.5151 0.7006 0.069 Uiso 1 1 calc R . . C6D C 0.0003(3) 0.5788(2) 0.64107(14) 0.0517(9) Uani 1 1 d . . . H6D H 0.0368 0.5399 0.6247 0.062 Uiso 1 1 calc R . . C1E C 0.6130(3) 0.5603(2) 0.79693(16) 0.0542(10) Uani 1 1 d . . . C2E C 0.5921(3) 0.6133(2) 0.7593(2) 0.0781(15) Uani 1 1 d . . . H2E H 0.5421 0.6024 0.7341 0.094 Uiso 1 1 calc R . . C3E C 0.6452(4) 0.6827(3) 0.7587(3) 0.105(2) Uani 1 1 d . . . H3E H 0.6316 0.7187 0.7332 0.126 Uiso 1 1 calc R . . C4E C 0.7173(6) 0.6976(4) 0.7958(3) 0.121(3) Uani 1 1 d . . . H4E H 0.7523 0.7447 0.7957 0.146 Uiso 1 1 calc R . . C5E C 0.7396(5) 0.6468(5) 0.8324(3) 0.120(3) Uani 1 1 d . . . H5E H 0.7894 0.6585 0.8576 0.144 Uiso 1 1 calc R . . C6E C 0.6880(4) 0.5763(4) 0.83285(19) 0.0880(18) Uani 1 1 d . . . H6E H 0.7048 0.5398 0.8577 0.106 Uiso 1 1 calc R . . C1F C 0.5677(2) 0.42028(18) 0.74342(12) 0.0369(7) Uani 1 1 d . . . C2F C 0.6685(3) 0.4190(2) 0.72627(13) 0.0414(8) Uani 1 1 d . . . H2F H 0.7198 0.4494 0.7419 0.050 Uiso 1 1 calc R . . C3F C 0.6926(3) 0.3727(2) 0.68603(13) 0.0447(8) Uani 1 1 d . . . H3F H 0.7603 0.3723 0.6741 0.054 Uiso 1 1 calc R . . C4F C 0.6184(3) 0.3270(2) 0.66326(13) 0.0477(9) Uani 1 1 d . . . H4F H 0.6361 0.2948 0.6365 0.057 Uiso 1 1 calc R . . C5F C 0.5183(3) 0.3288(2) 0.67973(14) 0.0487(9) Uani 1 1 d . . . H5F H 0.4673 0.2985 0.6638 0.058 Uiso 1 1 calc R . . C6F C 0.4930(3) 0.3749(2) 0.71954(13) 0.0425(8) Uani 1 1 d . . . H6F H 0.4247 0.3758 0.7307 0.051 Uiso 1 1 calc R . . C1G C 0.0971(2) 0.43426(18) 0.80601(13) 0.0385(7) Uani 1 1 d . . . C2G C 0.0011(3) 0.4177(2) 0.82639(17) 0.0552(10) Uani 1 1 d . . . H2G H -0.0148 0.4357 0.8586 0.066 Uiso 1 1 calc R . . C3G C -0.0706(3) 0.3748(3) 0.7991(2) 0.0656(12) Uani 1 1 d . . . H3G H -0.1345 0.3629 0.8132 0.079 Uiso 1 1 calc R . . C4G C -0.0489(3) 0.3496(2) 0.75190(19) 0.0623(11) Uani 1 1 d . . . H4G H -0.0982 0.3206 0.7337 0.075 Uiso 1 1 calc R . . C5G C 0.0444(3) 0.3662(2) 0.73074(17) 0.0553(10) Uani 1 1 d . . . H5G H 0.0584 0.3493 0.6981 0.066 Uiso 1 1 calc R . . C6G C 0.1180(3) 0.40829(19) 0.75797(14) 0.0443(8) Uani 1 1 d . . . H6G H 0.1821 0.4192 0.7438 0.053 Uiso 1 1 calc R . . C1H C 0.1407(2) 0.57770(18) 0.85675(12) 0.0365(7) Uani 1 1 d . . . C2H C 0.0634(3) 0.6096(2) 0.82743(16) 0.0609(11) Uani 1 1 d . . . H2H H 0.0338 0.5814 0.8006 0.073 Uiso 1 1 calc R . . C3H C 0.0285(4) 0.6831(2) 0.8370(2) 0.0711(14) Uani 1 1 d . . . H3H H -0.0240 0.7045 0.8164 0.085 Uiso 1 1 calc R . . C4H C 0.0695(3) 0.7245(2) 0.87572(17) 0.0598(11) Uani 1 1 d . . . H4H H 0.0442 0.7738 0.8825 0.072 Uiso 1 1 calc R . . C5H C 0.1483(4) 0.6940(2) 0.90492(16) 0.0631(11) Uani 1 1 d . . . H5H H 0.1781 0.7228 0.9314 0.076 Uiso 1 1 calc R . . C6H C 0.1838(3) 0.6210(2) 0.89532(14) 0.0542(10) Uani 1 1 d . . . H6H H 0.2379 0.6006 0.9153 0.065 Uiso 1 1 calc R . . P5 P 0.76052(7) 0.62159(5) 0.40242(4) 0.0419(2) Uani 1 1 d . . . F1 F 0.7117(2) 0.70356(15) 0.40644(11) 0.0859(9) Uani 1 1 d . . . F2 F 0.7510(2) 0.62694(16) 0.34267(9) 0.0774(8) Uani 1 1 d . . . F3 F 0.8056(3) 0.53890(16) 0.39845(14) 0.1131(12) Uani 1 1 d . . . F4 F 0.7666(2) 0.61671(17) 0.46183(9) 0.0822(8) Uani 1 1 d . . . F5 F 0.6490(2) 0.58515(19) 0.40296(11) 0.0960(10) Uani 1 1 d . . . F6 F 0.8705(2) 0.6584(2) 0.40129(12) 0.0990(11) 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 0.02848(12) 0.02437(11) 0.02672(11) -0.00056(8) 0.00262(8) -0.00318(8) Pd2 0.02992(13) 0.02971(13) 0.03665(13) 0.00421(9) 0.00081(10) 0.00451(9) S1 0.0496(5) 0.0251(4) 0.0309(4) -0.0014(3) -0.0017(3) -0.0038(3) P1 0.0301(4) 0.0295(4) 0.0345(4) -0.0007(3) 0.0037(3) -0.0005(3) P2 0.0299(4) 0.0284(4) 0.0344(4) -0.0017(3) 0.0026(3) -0.0036(3) P3 0.0309(4) 0.0394(5) 0.0471(5) -0.0031(4) 0.0009(4) 0.0051(3) P4 0.0337(4) 0.0350(4) 0.0363(4) 0.0056(3) 0.0037(3) 0.0035(3) N1 0.0337(14) 0.0317(13) 0.0330(13) 0.0010(11) 0.0018(11) 0.0011(11) C1 0.0411(17) 0.0254(14) 0.0277(15) -0.0015(11) 0.0015(12) -0.0049(12) C2 0.0450(19) 0.0427(19) 0.0309(16) -0.0046(14) 0.0033(14) -0.0017(15) C3 0.0431(19) 0.0415(19) 0.0416(18) -0.0099(15) 0.0096(15) 0.0014(15) C4 0.0431(18) 0.0327(16) 0.0345(16) -0.0024(13) -0.0009(14) -0.0087(14) C5 0.0338(16) 0.0320(16) 0.0398(17) -0.0041(13) 0.0006(13) -0.0081(13) C6 0.050(2) 0.051(2) 0.050(2) 0.0172(17) -0.0030(17) 0.0101(17) C7 0.057(2) 0.051(2) 0.055(2) 0.0129(18) -0.0045(18) 0.0193(19) C8 0.044(2) 0.064(2) 0.050(2) -0.0036(18) -0.0062(17) 0.0190(18) C9 0.076(3) 0.064(3) 0.070(3) 0.031(2) 0.008(2) 0.020(2) C10 0.052(2) 0.053(2) 0.0405(19) 0.0169(16) 0.0069(16) 0.0046(17) C11 0.0455(19) 0.0252(15) 0.0398(18) -0.0027(13) -0.0002(14) -0.0005(13) C12 0.0454(18) 0.0298(16) 0.0326(16) -0.0049(13) -0.0021(13) -0.0025(13) C13 0.0291(15) 0.0278(15) 0.0323(15) -0.0010(12) 0.0014(12) -0.0006(12) C14 0.053(2) 0.0269(15) 0.0344(17) -0.0062(13) -0.0045(14) 0.0006(14) C15 0.053(2) 0.0346(17) 0.0322(16) -0.0038(13) -0.0037(14) 0.0005(15) C1A 0.0310(16) 0.0337(16) 0.0410(17) -0.0022(13) 0.0022(13) 0.0050(13) C2A 0.047(2) 0.055(2) 0.087(3) 0.012(2) -0.011(2) -0.0095(19) C3A 0.045(2) 0.084(4) 0.119(4) 0.004(3) -0.030(3) -0.010(2) C4A 0.062(3) 0.072(3) 0.076(3) -0.007(2) -0.027(2) 0.023(2) C5A 0.068(3) 0.056(2) 0.064(3) 0.011(2) -0.006(2) 0.018(2) C6A 0.048(2) 0.046(2) 0.056(2) 0.0066(17) -0.0010(17) 0.0043(17) C1B 0.0327(16) 0.0376(17) 0.0407(18) 0.0076(14) 0.0019(13) -0.0028(13) C2B 0.056(2) 0.056(2) 0.067(3) 0.011(2) 0.026(2) 0.0048(19) C3B 0.075(3) 0.067(3) 0.086(3) 0.028(3) 0.031(3) -0.005(2) C4B 0.072(3) 0.056(3) 0.093(4) 0.038(3) 0.004(3) -0.014(2) C5B 0.070(3) 0.038(2) 0.086(3) 0.013(2) 0.002(2) 0.0009(19) C6B 0.046(2) 0.0390(19) 0.054(2) 0.0052(16) 0.0076(16) -0.0025(15) C1C 0.0452(19) 0.0339(17) 0.0352(17) -0.0021(13) 0.0046(14) 0.0041(14) C2C 0.064(3) 0.046(2) 0.062(3) -0.0106(19) -0.017(2) 0.0105(19) C3C 0.108(4) 0.065(3) 0.063(3) -0.019(2) -0.032(3) 0.038(3) C4C 0.126(5) 0.058(3) 0.060(3) 0.007(2) 0.004(3) 0.038(3) C5C 0.096(4) 0.040(2) 0.120(5) 0.018(3) 0.027(4) 0.006(2) C6C 0.053(2) 0.037(2) 0.091(3) 0.006(2) 0.007(2) 0.0024(17) C1D 0.0229(14) 0.0415(17) 0.0365(16) 0.0023(13) 0.0018(12) -0.0021(13) C2D 0.0409(19) 0.0381(18) 0.047(2) -0.0070(15) 0.0045(15) -0.0057(15) C3D 0.047(2) 0.056(2) 0.051(2) -0.0163(18) 0.0134(17) -0.0031(18) C4D 0.041(2) 0.076(3) 0.0381(19) 0.0023(18) 0.0079(15) -0.0009(19) C5D 0.058(2) 0.064(3) 0.052(2) 0.0211(19) 0.0142(19) 0.015(2) C6D 0.053(2) 0.052(2) 0.051(2) 0.0103(17) 0.0151(17) 0.0156(18) C1E 0.039(2) 0.051(2) 0.073(3) -0.024(2) 0.0189(18) -0.0082(17) C2E 0.048(2) 0.043(2) 0.145(5) 0.000(3) 0.026(3) -0.0012(19) C3E 0.075(4) 0.042(3) 0.201(7) -0.010(3) 0.070(4) -0.001(2) C4E 0.101(5) 0.097(5) 0.170(7) -0.094(5) 0.089(5) -0.055(4) C5E 0.107(5) 0.165(7) 0.091(4) -0.078(5) 0.057(4) -0.083(5) C6E 0.066(3) 0.133(5) 0.067(3) -0.049(3) 0.027(2) -0.044(3) C1F 0.0351(17) 0.0324(16) 0.0432(18) 0.0019(14) 0.0018(14) 0.0069(13) C2F 0.0356(18) 0.0426(19) 0.0460(19) 0.0008(15) -0.0008(14) 0.0050(14) C3F 0.0376(18) 0.054(2) 0.0430(19) 0.0133(16) 0.0107(15) 0.0114(16) C4F 0.065(2) 0.046(2) 0.0326(17) 0.0042(15) 0.0070(16) 0.0047(18) C5F 0.057(2) 0.046(2) 0.043(2) 0.0022(16) 0.0008(17) -0.0065(17) C6F 0.0360(18) 0.0421(19) 0.049(2) -0.0004(15) 0.0040(15) -0.0016(14) C1G 0.0338(17) 0.0287(16) 0.053(2) 0.0064(14) 0.0012(14) 0.0020(13) C2G 0.045(2) 0.053(2) 0.068(3) 0.006(2) 0.0078(19) 0.0008(18) C3G 0.033(2) 0.063(3) 0.101(4) 0.016(3) 0.002(2) -0.0105(18) C4G 0.048(2) 0.047(2) 0.091(3) 0.005(2) -0.017(2) -0.0107(18) C5G 0.056(2) 0.043(2) 0.066(3) -0.0037(18) -0.012(2) -0.0024(18) C6G 0.0419(19) 0.0373(18) 0.054(2) 0.0002(16) 0.0003(16) -0.0035(15) C1H 0.0363(17) 0.0369(17) 0.0364(17) 0.0037(13) 0.0061(13) 0.0024(14) C2H 0.071(3) 0.044(2) 0.067(3) -0.0084(19) -0.027(2) 0.0097(19) C3H 0.070(3) 0.046(2) 0.096(4) -0.007(2) -0.028(3) 0.020(2) C4H 0.070(3) 0.040(2) 0.070(3) -0.0061(19) 0.006(2) 0.0124(19) C5H 0.085(3) 0.050(2) 0.054(2) -0.0155(19) -0.005(2) 0.008(2) C6H 0.059(2) 0.055(2) 0.048(2) -0.0040(18) -0.0113(18) 0.0123(19) P5 0.0401(5) 0.0335(4) 0.0517(5) -0.0038(4) -0.0061(4) -0.0036(4) F1 0.102(2) 0.0555(15) 0.101(2) 0.0006(15) 0.0248(17) 0.0248(15) F2 0.100(2) 0.0810(18) 0.0515(14) -0.0071(13) 0.0020(13) -0.0170(16) F3 0.147(3) 0.0553(17) 0.135(3) -0.0195(18) -0.028(2) 0.0421(19) F4 0.102(2) 0.090(2) 0.0532(15) 0.0042(14) -0.0154(14) -0.0255(16) F5 0.0723(18) 0.119(2) 0.096(2) 0.0196(18) -0.0145(15) -0.0540(18) F6 0.0521(16) 0.136(3) 0.109(2) -0.033(2) 0.0112(15) -0.0411(17) _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 C1 2.099(3) . ? Pd1 P2 2.2804(8) . ? Pd1 P1 2.2896(8) . ? Pd1 S1 2.4298(8) . ? Pd2 C6 2.080(3) . ? Pd2 N1 2.140(3) . ? Pd2 P4 2.2832(9) . ? Pd2 P3 2.3036(9) . ? S1 C13 1.727(3) . ? P1 C1A 1.815(3) . ? P1 C1B 1.821(3) . ? P1 C3 1.831(3) . ? P2 C1D 1.817(3) . ? P2 C5 1.819(3) . ? P2 C1C 1.823(3) . ? P3 C1E 1.815(4) . ? P3 C1F 1.819(3) . ? P3 C8 1.820(4) . ? P4 C1H 1.813(3) . ? P4 C1G 1.815(3) . ? P4 C10 1.827(3) . ? N1 C11 1.343(4) . ? N1 C15 1.349(4) . ? C1 C2 1.520(4) . ? C1 C4 1.522(4) . ? C2 C3 1.522(5) . ? C4 C5 1.525(4) . ? C6 C9 1.501(6) . ? C6 C7 1.530(5) . ? C7 C8 1.512(6) . ? C9 C10 1.498(5) . ? C11 C12 1.368(4) . ? C12 C13 1.401(4) . ? C13 C14 1.399(4) . ? C14 C15 1.368(4) . ? C1A C2A 1.363(5) . ? C1A C6A 1.384(5) . ? C2A C3A 1.389(6) . ? C3A C4A 1.356(7) . ? C4A C5A 1.363(6) . ? C5A C6A 1.384(5) . ? C1B C6B 1.383(5) . ? C1B C2B 1.389(5) . ? C2B C3B 1.378(6) . ? C3B C4B 1.371(7) . ? C4B C5B 1.389(6) . ? C5B C6B 1.388(5) . ? C1C C6C 1.377(5) . ? C1C C2C 1.382(5) . ? C2C C3C 1.378(6) . ? C3C C4C 1.352(7) . ? C4C C5C 1.363(8) . ? C5C C6C 1.387(6) . ? C1D C2D 1.375(5) . ? C1D C6D 1.399(5) . ? C2D C3D 1.388(5) . ? C3D C4D 1.365(6) . ? C4D C5D 1.369(5) . ? C5D C6D 1.383(5) . ? C1E C6E 1.375(6) . ? C1E C2E 1.385(7) . ? C2E C3E 1.396(6) . ? C3E C4E 1.366(10) . ? C4E C5E 1.345(11) . ? C5E C6E 1.403(8) . ? C1F C6F 1.392(5) . ? C1F C2F 1.393(5) . ? C2F C3F 1.384(5) . ? C3F C4F 1.377(5) . ? C4F C5F 1.378(5) . ? C5F C6F 1.377(5) . ? C1G C6G 1.389(5) . ? C1G C2G 1.398(5) . ? C2G C3G 1.385(6) . ? C3G C4G 1.366(6) . ? C4G C5G 1.376(6) . ? C5G C6G 1.393(5) . ? C1H C2H 1.372(5) . ? C1H C6H 1.382(5) . ? C2H C3H 1.389(5) . ? C3H C4H 1.356(6) . ? C4H C5H 1.375(6) . ? C5H C6H 1.382(5) . ? P5 F6 1.564(3) . ? P5 F3 1.564(3) . ? P5 F1 1.571(3) . ? P5 F5 1.579(3) . ? P5 F4 1.583(3) . ? P5 F2 1.593(3) . ? 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 C1 Pd1 P2 82.97(9) . . ? C1 Pd1 P1 82.64(9) . . ? P2 Pd1 P1 163.43(3) . . ? C1 Pd1 S1 175.45(8) . . ? P2 Pd1 S1 95.51(3) . . ? P1 Pd1 S1 99.45(3) . . ? C6 Pd2 N1 176.31(13) . . ? C6 Pd2 P4 82.57(11) . . ? N1 Pd2 P4 96.18(7) . . ? C6 Pd2 P3 82.88(11) . . ? N1 Pd2 P3 98.26(7) . . ? P4 Pd2 P3 165.37(3) . . ? C13 S1 Pd1 104.10(10) . . ? C1A P1 C1B 105.89(15) . . ? C1A P1 C3 105.54(15) . . ? C1B P1 C3 105.89(16) . . ? C1A P1 Pd1 121.87(11) . . ? C1B P1 Pd1 112.22(11) . . ? C3 P1 Pd1 104.20(11) . . ? C1D P2 C5 107.06(15) . . ? C1D P2 C1C 106.37(15) . . ? C5 P2 C1C 104.68(15) . . ? C1D P2 Pd1 122.78(10) . . ? C5 P2 Pd1 103.80(11) . . ? C1C P2 Pd1 110.71(11) . . ? C1E P3 C1F 105.16(16) . . ? C1E P3 C8 108.9(2) . . ? C1F P3 C8 104.69(16) . . ? C1E P3 Pd2 118.32(13) . . ? C1F P3 Pd2 115.93(11) . . ? C8 P3 Pd2 102.88(13) . . ? C1H P4 C1G 106.03(15) . . ? C1H P4 C10 108.75(16) . . ? C1G P4 C10 104.32(17) . . ? C1H P4 Pd2 114.94(11) . . ? C1G P4 Pd2 118.17(12) . . ? C10 P4 Pd2 103.83(12) . . ? C11 N1 C15 115.8(3) . . ? C11 N1 Pd2 121.9(2) . . ? C15 N1 Pd2 122.3(2) . . ? C2 C1 C4 112.7(3) . . ? C2 C1 Pd1 114.1(2) . . ? C4 C1 Pd1 113.7(2) . . ? C1 C2 C3 110.3(3) . . ? C2 C3 P1 105.1(2) . . ? C1 C4 C5 110.2(3) . . ? C4 C5 P2 104.2(2) . . ? C9 C6 C7 116.3(3) . . ? C9 C6 Pd2 114.2(3) . . ? C7 C6 Pd2 112.6(3) . . ? C8 C7 C6 108.7(3) . . ? C7 C8 P3 105.3(2) . . ? C10 C9 C6 111.4(4) . . ? C9 C10 P4 104.7(3) . . ? N1 C11 C12 123.9(3) . . ? C11 C12 C13 120.6(3) . . ? C14 C13 C12 115.2(3) . . ? C14 C13 S1 121.9(2) . . ? C12 C13 S1 122.9(2) . . ? C15 C14 C13 120.7(3) . . ? N1 C15 C14 123.8(3) . . ? C2A C1A C6A 119.4(3) . . ? C2A C1A P1 124.5(3) . . ? C6A C1A P1 116.1(3) . . ? C1A C2A C3A 119.4(4) . . ? C4A C3A C2A 121.3(4) . . ? C3A C4A C5A 119.7(4) . . ? C4A C5A C6A 119.9(4) . . ? C5A C6A C1A 120.3(4) . . ? C6B C1B C2B 119.3(3) . . ? C6B C1B P1 119.2(3) . . ? C2B C1B P1 121.5(3) . . ? C3B C2B C1B 120.7(4) . . ? C4B C3B C2B 119.9(4) . . ? C3B C4B C5B 120.3(4) . . ? C6B C5B C4B 119.8(4) . . ? C1B C6B C5B 120.0(4) . . ? C6C C1C C2C 118.2(3) . . ? C6C C1C P2 119.9(3) . . ? C2C C1C P2 121.7(3) . . ? C3C C2C C1C 120.9(4) . . ? C4C C3C C2C 120.2(5) . . ? C3C C4C C5C 120.0(4) . . ? C4C C5C C6C 120.5(5) . . ? C1C C6C C5C 120.1(4) . . ? C2D C1D C6D 118.9(3) . . ? C2D C1D P2 122.5(3) . . ? C6D C1D P2 118.5(3) . . ? C1D C2D C3D 120.3(3) . . ? C4D C3D C2D 120.6(3) . . ? C3D C4D C5D 119.6(3) . . ? C4D C5D C6D 120.8(4) . . ? C5D C6D C1D 119.7(3) . . ? C6E C1E C2E 119.3(4) . . ? C6E C1E P3 122.8(4) . . ? C2E C1E P3 117.8(3) . . ? C1E C2E C3E 120.1(6) . . ? C4E C3E C2E 119.1(7) . . ? C5E C4E C3E 121.8(6) . . ? C4E C5E C6E 119.5(7) . . ? C1E C6E C5E 120.1(6) . . ? C6F C1F C2F 119.2(3) . . ? C6F C1F P3 119.2(2) . . ? C2F C1F P3 121.5(3) . . ? C3F C2F C1F 119.5(3) . . ? C4F C3F C2F 120.8(3) . . ? C3F C4F C5F 119.9(3) . . ? C6F C5F C4F 120.1(4) . . ? C5F C6F C1F 120.6(3) . . ? C6G C1G C2G 118.9(3) . . ? C6G C1G P4 119.9(3) . . ? C2G C1G P4 121.2(3) . . ? C3G C2G C1G 120.0(4) . . ? C4G C3G C2G 120.4(4) . . ? C3G C4G C5G 120.6(4) . . ? C4G C5G C6G 119.7(4) . . ? C1G C6G C5G 120.3(4) . . ? C2H C1H C6H 118.3(3) . . ? C2H C1H P4 121.7(3) . . ? C6H C1H P4 119.6(3) . . ? C1H C2H C3H 120.5(4) . . ? C4H C3H C2H 120.7(4) . . ? C3H C4H C5H 119.5(4) . . ? C4H C5H C6H 119.9(4) . . ? C1H C6H C5H 120.9(4) . . ? F6 P5 F3 92.1(2) . . ? F6 P5 F1 89.65(18) . . ? F3 P5 F1 178.2(2) . . ? F6 P5 F5 179.3(2) . . ? F3 P5 F5 88.3(2) . . ? F1 P5 F5 89.91(19) . . ? F6 P5 F4 91.01(17) . . ? F3 P5 F4 90.44(18) . . ? F1 P5 F4 89.52(17) . . ? F5 P5 F4 89.59(16) . . ? F6 P5 F2 90.29(17) . . ? F3 P5 F2 90.41(18) . . ? F1 P5 F2 89.59(16) . . ? F5 P5 F2 89.10(15) . . ? F4 P5 F2 178.42(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.928 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.088 data_5095 _database_code_depnum_ccdc_archive 'CCDC 661013' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H29 F3 O3 P2 Pd S' _chemical_formula_weight 694.93 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' S S 0.1246 0.1234 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 9.4270(7) _cell_length_b 10.6781(8) _cell_length_c 15.8613(12) _cell_angle_alpha 98.489(2) _cell_angle_beta 93.482(2) _cell_angle_gamma 114.8970(10) _cell_volume 1418.89(18) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6913 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 28.91 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.892 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7168 _exptl_absorpt_correction_T_max 0.9161 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18705 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6515 _reflns_number_gt 5966 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+1.0197P] 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 constructed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6515 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _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 0.350893(19) 0.107741(17) 0.243060(11) 0.02150(6) Uani 1 1 d . . . P1 P 0.50606(7) -0.01109(6) 0.23713(4) 0.02297(13) Uani 1 1 d . . . P2 P 0.25171(7) 0.27372(6) 0.26198(4) 0.02496(13) Uani 1 1 d . . . C1 C 0.5670(3) 0.2832(3) 0.26590(16) 0.0288(5) Uani 1 1 d . . . H1 H 0.5926 0.3025 0.2082 0.035 Uiso 1 1 calc R . . C2 C 0.7003(3) 0.2555(3) 0.30392(17) 0.0329(6) Uani 1 1 d . . . H2A H 0.8010 0.3385 0.3074 0.039 Uiso 1 1 calc R . . H2B H 0.6844 0.2380 0.3623 0.039 Uiso 1 1 calc R . . C3 C 0.7059(3) 0.1296(3) 0.24888(16) 0.0294(5) Uani 1 1 d . . . H3A' H 0.7821 0.1035 0.2771 0.035 Uiso 1 1 calc R . . H3B' H 0.7359 0.1501 0.1926 0.035 Uiso 1 1 calc R . . C4 C 0.5603(3) 0.4160(3) 0.31295(17) 0.0309(5) Uani 1 1 d . . . H4A H 0.5414 0.4070 0.3723 0.037 Uiso 1 1 calc R . . H4B H 0.6614 0.4978 0.3146 0.037 Uiso 1 1 calc R . . C5 C 0.4286(3) 0.4372(3) 0.26677(18) 0.0312(5) Uani 1 1 d . . . H5A H 0.4500 0.4541 0.2088 0.037 Uiso 1 1 calc R . . H5B H 0.4166 0.5172 0.2988 0.037 Uiso 1 1 calc R . . C1A C 0.5067(3) -0.0963(2) 0.32808(15) 0.0265(5) Uani 1 1 d . . . C2A C 0.6224(3) -0.1413(3) 0.34465(18) 0.0368(6) Uani 1 1 d . . . H2A1 H 0.6980 -0.1317 0.3070 0.044 Uiso 1 1 calc R . . C3A C 0.6268(4) -0.2001(3) 0.4162(2) 0.0452(7) Uani 1 1 d . . . H3A H 0.7057 -0.2299 0.4273 0.054 Uiso 1 1 calc R . . C4A C 0.5155(4) -0.2151(3) 0.47117(19) 0.0469(8) Uani 1 1 d . . . H4A1 H 0.5192 -0.2540 0.5202 0.056 Uiso 1 1 calc R . . C5A C 0.3996(4) -0.1734(3) 0.45447(19) 0.0452(7) Uani 1 1 d . . . H5A1 H 0.3230 -0.1852 0.4918 0.054 Uiso 1 1 calc R . . C6A C 0.3938(3) -0.1139(3) 0.38317(16) 0.0322(5) Uani 1 1 d . . . H6A H 0.3138 -0.0856 0.3722 0.039 Uiso 1 1 calc R . . C1B C 0.4814(3) -0.1409(3) 0.14268(15) 0.0244(5) Uani 1 1 d . . . C2B C 0.3935(3) -0.2834(3) 0.14072(17) 0.0323(5) Uani 1 1 d . . . H2B1 H 0.3454 -0.3136 0.1888 0.039 Uiso 1 1 calc R . . C3B C 0.3761(4) -0.3816(3) 0.06817(18) 0.0390(6) Uani 1 1 d . . . H3B H 0.3166 -0.4780 0.0674 0.047 Uiso 1 1 calc R . . C4B C 0.4457(3) -0.3382(3) -0.00285(18) 0.0403(7) Uani 1 1 d . . . H4B1 H 0.4357 -0.4049 -0.0514 0.048 Uiso 1 1 calc R . . C5B C 0.5299(3) -0.1970(3) -0.00243(17) 0.0410(7) Uani 1 1 d . . . H5B1 H 0.5759 -0.1672 -0.0511 0.049 Uiso 1 1 calc R . . C6B C 0.5469(3) -0.0985(3) 0.06980(16) 0.0327(6) Uani 1 1 d . . . H6B H 0.6033 -0.0021 0.0694 0.039 Uiso 1 1 calc R . . C1C C 0.1738(3) 0.2934(3) 0.36278(16) 0.0277(5) Uani 1 1 d . . . C2C C 0.2047(4) 0.4238(3) 0.41129(19) 0.0419(7) Uani 1 1 d . . . H2C H 0.2699 0.5064 0.3928 0.050 Uiso 1 1 calc R . . C3C C 0.1402(4) 0.4329(3) 0.4865(2) 0.0478(7) Uani 1 1 d . . . H3C H 0.1624 0.5217 0.5189 0.057 Uiso 1 1 calc R . . C4C C 0.0442(4) 0.3136(4) 0.51433(19) 0.0436(7) Uani 1 1 d . . . H4C H 0.0010 0.3204 0.5657 0.052 Uiso 1 1 calc R . . C5C C 0.0116(4) 0.1840(3) 0.46657(19) 0.0429(7) Uani 1 1 d . . . H5C H -0.0553 0.1020 0.4851 0.051 Uiso 1 1 calc R . . C6C C 0.0765(3) 0.1732(3) 0.39154(18) 0.0348(6) Uani 1 1 d . . . H6C H 0.0546 0.0840 0.3598 0.042 Uiso 1 1 calc R . . C1D C 0.1069(3) 0.2691(2) 0.17952(16) 0.0265(5) Uani 1 1 d . . . C2D C 0.0633(3) 0.3786(3) 0.18086(19) 0.0347(6) Uani 1 1 d . . . H2D H 0.1050 0.4556 0.2271 0.042 Uiso 1 1 calc R . . C3D C -0.0410(3) 0.3745(3) 0.1143(2) 0.0397(6) Uani 1 1 d . . . H3D H -0.0695 0.4491 0.1153 0.048 Uiso 1 1 calc R . . C4D C -0.1035(3) 0.2617(3) 0.04659(18) 0.0396(6) Uani 1 1 d . . . H4D H -0.1735 0.2600 0.0011 0.048 Uiso 1 1 calc R . . C5D C -0.0634(3) 0.1515(3) 0.04539(18) 0.0400(6) Uani 1 1 d . . . H5D H -0.1073 0.0738 -0.0004 0.048 Uiso 1 1 calc R . . C6D C 0.0419(3) 0.1552(3) 0.11190(17) 0.0330(6) Uani 1 1 d . . . H6D H 0.0691 0.0799 0.1110 0.040 Uiso 1 1 calc R . . C6 C -0.1531(3) -0.2720(3) 0.16089(18) 0.0385(6) Uani 1 1 d . . . F1 F -0.2701(2) -0.3714(2) 0.18752(14) 0.0730(7) Uani 1 1 d . . . F2 F -0.1340(2) -0.3274(2) 0.08492(11) 0.0630(6) Uani 1 1 d . . . F3 F -0.1973(2) -0.1727(3) 0.15088(16) 0.0744(7) Uani 1 1 d . . . S1 S 0.02589(7) -0.20035(6) 0.23731(4) 0.02968(14) Uani 1 1 d . . . O1 O 0.1282(2) -0.0850(2) 0.19945(13) 0.0422(5) Uani 1 1 d . . . O2 O 0.0695(3) -0.3126(2) 0.23556(17) 0.0605(7) Uani 1 1 d . . . O3 O -0.0202(3) -0.1574(2) 0.31620(13) 0.0518(6) 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 0.01890(9) 0.01840(9) 0.02669(10) 0.00441(7) 0.00268(6) 0.00767(7) P1 0.0211(3) 0.0247(3) 0.0252(3) 0.0052(2) 0.0036(2) 0.0117(2) P2 0.0248(3) 0.0191(3) 0.0312(3) 0.0046(2) 0.0039(2) 0.0099(2) C1 0.0241(12) 0.0256(12) 0.0313(13) 0.0049(10) 0.0018(10) 0.0062(10) C2 0.0258(12) 0.0331(13) 0.0336(13) 0.0024(11) 0.0015(10) 0.0085(11) C3 0.0207(11) 0.0330(13) 0.0325(13) 0.0044(10) 0.0036(10) 0.0103(10) C4 0.0280(13) 0.0239(12) 0.0344(13) 0.0045(10) 0.0010(10) 0.0058(10) C5 0.0300(13) 0.0202(11) 0.0414(14) 0.0079(10) 0.0042(11) 0.0085(10) C1A 0.0307(12) 0.0246(12) 0.0234(11) 0.0034(9) 0.0000(9) 0.0120(10) C2A 0.0393(15) 0.0399(15) 0.0382(15) 0.0069(12) 0.0033(12) 0.0244(13) C3A 0.0517(18) 0.0389(16) 0.0490(17) 0.0101(13) -0.0109(14) 0.0253(14) C4A 0.0571(19) 0.0380(16) 0.0368(16) 0.0163(13) -0.0059(14) 0.0110(14) C5A 0.0429(17) 0.0521(18) 0.0331(15) 0.0162(13) 0.0057(12) 0.0108(14) C6A 0.0295(13) 0.0366(14) 0.0289(13) 0.0072(11) 0.0024(10) 0.0127(11) C1B 0.0234(11) 0.0298(12) 0.0235(11) 0.0039(9) 0.0005(9) 0.0158(10) C2B 0.0352(14) 0.0319(13) 0.0300(13) 0.0075(10) 0.0040(11) 0.0146(11) C3B 0.0467(16) 0.0298(14) 0.0372(15) 0.0006(11) -0.0027(12) 0.0166(12) C4B 0.0423(16) 0.0459(17) 0.0311(14) -0.0071(12) -0.0027(12) 0.0234(14) C5B 0.0407(16) 0.0530(18) 0.0263(13) 0.0051(12) 0.0073(11) 0.0179(14) C6B 0.0340(14) 0.0341(14) 0.0286(13) 0.0073(11) 0.0042(10) 0.0131(11) C1C 0.0276(12) 0.0274(12) 0.0297(12) 0.0041(10) 0.0015(10) 0.0143(10) C2C 0.0493(17) 0.0302(14) 0.0433(16) 0.0039(12) 0.0127(13) 0.0147(13) C3C 0.0539(19) 0.0415(17) 0.0439(17) -0.0067(13) 0.0060(14) 0.0218(15) C4C 0.0436(16) 0.063(2) 0.0329(15) 0.0064(14) 0.0069(12) 0.0318(16) C5C 0.0427(16) 0.0454(17) 0.0454(17) 0.0184(14) 0.0130(13) 0.0199(14) C6C 0.0373(14) 0.0285(13) 0.0399(15) 0.0072(11) 0.0064(11) 0.0152(11) C1D 0.0244(12) 0.0256(12) 0.0321(13) 0.0087(10) 0.0070(10) 0.0118(10) C2D 0.0324(13) 0.0242(12) 0.0472(16) 0.0053(11) 0.0036(12) 0.0126(11) C3D 0.0382(15) 0.0360(15) 0.0531(17) 0.0151(13) 0.0041(13) 0.0220(13) C4D 0.0356(15) 0.0526(18) 0.0366(15) 0.0163(13) 0.0033(12) 0.0227(14) C5D 0.0429(16) 0.0471(17) 0.0308(14) -0.0001(12) 0.0020(12) 0.0231(14) C6D 0.0396(14) 0.0323(13) 0.0327(13) 0.0040(11) 0.0058(11) 0.0214(12) C6 0.0259(13) 0.0404(15) 0.0402(15) 0.0111(12) 0.0041(11) 0.0050(12) F1 0.0353(10) 0.0798(15) 0.0633(13) 0.0232(11) 0.0058(9) -0.0166(10) F2 0.0577(12) 0.0701(13) 0.0351(10) -0.0024(9) 0.0030(8) 0.0076(10) F3 0.0508(12) 0.0837(16) 0.0997(17) 0.0240(13) -0.0111(11) 0.0403(12) S1 0.0259(3) 0.0216(3) 0.0385(3) 0.0034(2) -0.0016(2) 0.0090(2) O1 0.0289(10) 0.0307(10) 0.0520(12) 0.0067(9) -0.0014(9) 0.0001(8) O2 0.0629(15) 0.0386(12) 0.0862(18) 0.0050(12) -0.0104(13) 0.0328(12) O3 0.0626(15) 0.0490(13) 0.0353(11) 0.0010(10) 0.0061(10) 0.0187(11) _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 C1 2.071(2) . ? Pd1 O1 2.2106(18) . ? Pd1 P1 2.3028(6) . ? Pd1 P2 2.3190(6) . ? P1 C1B 1.815(2) . ? P1 C1A 1.817(2) . ? P1 C3 1.826(2) . ? P2 C1D 1.812(3) . ? P2 C1C 1.820(3) . ? P2 C5 1.824(2) . ? C1 C2 1.517(4) . ? C1 C4 1.530(3) . ? C2 C3 1.514(4) . ? C4 C5 1.518(4) . ? C1A C6A 1.387(4) . ? C1A C2A 1.391(4) . ? C2A C3A 1.382(4) . ? C3A C4A 1.377(5) . ? C4A C5A 1.368(5) . ? C5A C6A 1.385(4) . ? C1B C2B 1.387(3) . ? C1B C6B 1.389(3) . ? C2B C3B 1.388(4) . ? C3B C4B 1.379(4) . ? C4B C5B 1.376(4) . ? C5B C6B 1.387(4) . ? C1C C6C 1.389(4) . ? C1C C2C 1.390(4) . ? C2C C3C 1.380(4) . ? C3C C4C 1.372(5) . ? C4C C5C 1.374(4) . ? C5C C6C 1.382(4) . ? C1D C6D 1.383(4) . ? C1D C2D 1.391(3) . ? C2D C3D 1.381(4) . ? C3D C4D 1.377(4) . ? C4D C5D 1.378(4) . ? C5D C6D 1.388(4) . ? C6 F1 1.313(3) . ? C6 F3 1.319(4) . ? C6 F2 1.319(3) . ? C6 S1 1.814(3) . ? S1 O2 1.419(2) . ? S1 O3 1.425(2) . ? S1 O1 1.448(2) . ? 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 C1 Pd1 O1 171.66(9) . . ? C1 Pd1 P1 83.05(7) . . ? O1 Pd1 P1 94.02(6) . . ? C1 Pd1 P2 83.46(7) . . ? O1 Pd1 P2 99.71(6) . . ? P1 Pd1 P2 166.24(2) . . ? C1B P1 C1A 105.33(11) . . ? C1B P1 C3 107.74(11) . . ? C1A P1 C3 104.48(12) . . ? C1B P1 Pd1 120.49(8) . . ? C1A P1 Pd1 114.29(8) . . ? C3 P1 Pd1 103.24(8) . . ? C1D P2 C1C 105.24(11) . . ? C1D P2 C5 106.65(11) . . ? C1C P2 C5 106.03(12) . . ? C1D P2 Pd1 119.82(8) . . ? C1C P2 Pd1 115.94(8) . . ? C5 P2 Pd1 101.98(8) . . ? C2 C1 C4 114.3(2) . . ? C2 C1 Pd1 113.12(17) . . ? C4 C1 Pd1 113.40(17) . . ? C3 C2 C1 110.4(2) . . ? C2 C3 P1 105.11(16) . . ? C5 C4 C1 109.7(2) . . ? C4 C5 P2 104.88(16) . . ? C6A C1A C2A 119.2(2) . . ? C6A C1A P1 120.22(19) . . ? C2A C1A P1 120.5(2) . . ? C3A C2A C1A 120.3(3) . . ? C4A C3A C2A 119.9(3) . . ? C5A C4A C3A 120.1(3) . . ? C4A C5A C6A 120.7(3) . . ? C5A C6A C1A 119.8(3) . . ? C2B C1B C6B 118.7(2) . . ? C2B C1B P1 121.03(19) . . ? C6B C1B P1 120.22(19) . . ? C1B C2B C3B 120.4(2) . . ? C4B C3B C2B 120.2(3) . . ? C5B C4B C3B 119.9(3) . . ? C4B C5B C6B 120.1(3) . . ? C5B C6B C1B 120.6(3) . . ? C6C C1C C2C 118.5(2) . . ? C6C C1C P2 118.74(19) . . ? C2C C1C P2 122.7(2) . . ? C3C C2C C1C 120.4(3) . . ? C4C C3C C2C 120.6(3) . . ? C3C C4C C5C 119.5(3) . . ? C4C C5C C6C 120.5(3) . . ? C5C C6C C1C 120.4(3) . . ? C6D C1D C2D 119.2(2) . . ? C6D C1D P2 118.82(19) . . ? C2D C1D P2 121.9(2) . . ? C3D C2D C1D 120.1(3) . . ? C4D C3D C2D 120.3(3) . . ? C3D C4D C5D 120.0(3) . . ? C4D C5D C6D 119.9(3) . . ? C1D C6D C5D 120.4(2) . . ? F1 C6 F3 107.4(3) . . ? F1 C6 F2 107.2(2) . . ? F3 C6 F2 108.4(2) . . ? F1 C6 S1 111.5(2) . . ? F3 C6 S1 110.3(2) . . ? F2 C6 S1 112.0(2) . . ? O2 S1 O3 115.53(15) . . ? O2 S1 O1 115.19(15) . . ? O3 S1 O1 114.10(13) . . ? O2 S1 C6 104.65(14) . . ? O3 S1 C6 104.10(14) . . ? O1 S1 C6 100.85(12) . . ? S1 O1 Pd1 136.27(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.924 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.082