# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Brian R. James' _publ_contact_author_email brj@chem.ubc.ca loop_ _publ_author_name C.B.Pamplin S.J.Rettig B.O.Patrick B.R.James data_bj245 _database_code_depnum_ccdc_archive 'CCDC 849399' #TrackingRef '- bj245_267_bj244_Oct27.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H28 Cl2 P4 Pd2 Se' _chemical_formula_weight 634.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.1062(7) _cell_length_b 8.5205(13) _cell_length_c 15.3582(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.5110(10) _cell_angle_gamma 90.00 _cell_volume 1058.78(19) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8010 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.05 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 3.959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.329 _exptl_absorpt_correction_T_max 0.453 _exptl_absorpt_process_details 'd*TREK (MSC, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Rigaku/ADSC CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9175 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 30.03 _reflns_number_total 4623 _reflns_number_gt 4366 _reflns_threshold_expression >2\s(I) _computing_data_collection 'd*TREK (MSC, 1998)' _computing_cell_refinement 'd*TREK (MSC, 1998)' _computing_data_reduction 'teXsan (MSC, 1992)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0321P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.046(7) _refine_ls_number_reflns 4623 _refine_ls_number_parameters 180 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0234 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0532 _refine_ls_wR_factor_gt 0.0528 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 C1 C 0.8662(4) 0.6375(5) 0.1114(2) 0.0202(8) Uani 1 1 d . . . H1A H 0.8722 0.7298 0.0726 0.024 Uiso 1 1 calc R . . H1B H 0.9751 0.5847 0.1135 0.024 Uiso 1 1 calc R . . C2 C 0.8270(5) 0.3753(6) -0.0032(3) 0.0337(10) Uani 1 1 d . . . H2A H 0.7513 0.3049 -0.0366 0.051 Uiso 1 1 calc R . . H2B H 0.9053 0.3131 0.0337 0.051 Uiso 1 1 calc R . . H2C H 0.8878 0.4392 -0.0436 0.051 Uiso 1 1 calc R . . C3 C 0.5918(5) 0.6225(6) -0.0149(3) 0.0321(10) Uani 1 1 d . . . H3A H 0.6669 0.6692 -0.0553 0.048 Uiso 1 1 calc R . . H3B H 0.5347 0.7059 0.0152 0.048 Uiso 1 1 calc R . . H3C H 0.5104 0.5567 -0.0476 0.048 Uiso 1 1 calc R . . C4 C 0.6483(6) 0.8338(5) 0.2041(3) 0.0316(10) Uani 1 1 d . . . H4A H 0.6189 0.8764 0.2604 0.047 Uiso 1 1 calc R . . H4B H 0.5545 0.7745 0.1776 0.047 Uiso 1 1 calc R . . H4C H 0.6755 0.9202 0.1654 0.047 Uiso 1 1 calc R . . C5 C 0.9971(6) 0.8366(5) 0.2473(3) 0.0344(10) Uani 1 1 d . . . H5A H 1.1016 0.7812 0.2407 0.052 Uiso 1 1 calc R . . H5B H 0.9923 0.8726 0.3077 0.052 Uiso 1 1 calc R . . H5C H 0.9900 0.9271 0.2079 0.052 Uiso 1 1 calc R . . C6 C 0.5609(4) 0.1986(5) 0.3778(3) 0.0194(7) Uani 1 1 d . . . H6A H 0.5991 0.0972 0.3548 0.023 Uiso 1 1 calc R . . H6B H 0.4917 0.1754 0.4271 0.023 Uiso 1 1 calc R . . C7 C 0.3254(5) 0.4460(5) 0.3511(3) 0.0290(9) Uani 1 1 d . . . H7A H 0.2367 0.4911 0.3128 0.043 Uiso 1 1 calc R . . H7B H 0.4032 0.5290 0.3703 0.043 Uiso 1 1 calc R . . H7C H 0.2781 0.3985 0.4021 0.043 Uiso 1 1 calc R . . C8 C 0.2756(4) 0.1516(5) 0.2641(3) 0.0255(9) Uani 1 1 d . . . H8A H 0.2186 0.1234 0.3164 0.038 Uiso 1 1 calc R . . H8B H 0.3272 0.0578 0.2408 0.038 Uiso 1 1 calc R . . H8C H 0.1958 0.1949 0.2200 0.038 Uiso 1 1 calc R . . C9 C 0.6902(6) 0.3710(6) 0.5284(3) 0.0318(10) Uani 1 1 d . . . H9A H 0.5881 0.4328 0.5246 0.048 Uiso 1 1 calc R . . H9B H 0.7802 0.4345 0.5554 0.048 Uiso 1 1 calc R . . H9C H 0.6744 0.2772 0.5640 0.048 Uiso 1 1 calc R . . C10 C 0.9016(5) 0.1654(5) 0.4414(3) 0.0310(10) Uani 1 1 d . . . H10A H 0.9967 0.2141 0.4734 0.047 Uiso 1 1 calc R . . H10B H 0.9364 0.1221 0.3863 0.047 Uiso 1 1 calc R . . H10C H 0.8580 0.0809 0.4766 0.047 Uiso 1 1 calc R . . P1 P 0.70971(10) 0.50261(13) 0.06483(6) 0.01693(18) Uani 1 1 d . . . P2 P 0.82583(11) 0.70478(11) 0.22068(7) 0.0171(2) Uani 1 1 d . . . P3 P 0.43351(10) 0.29703(11) 0.29228(6) 0.01528(18) Uani 1 1 d . . . P4 P 0.74215(11) 0.31199(12) 0.41888(6) 0.01721(19) Uani 1 1 d . . . Cl1 Cl 0.30116(10) 0.50233(15) 0.12131(7) 0.0306(2) Uani 1 1 d . . . Cl2 Cl 0.72275(12) 0.72181(11) 0.42307(6) 0.0264(2) Uani 1 1 d . . . Se1 Se 0.82830(4) 0.30238(4) 0.22588(2) 0.01672(8) Uani 1 1 d . . . Pd1 Pd 0.55996(3) 0.39612(3) 0.172256(16) 0.01256(6) Uani 1 1 d . . . Pd2 Pd 0.78989(3) 0.51560(3) 0.326560(16) 0.01382(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 C1 0.0217(17) 0.0184(19) 0.0210(19) 0.0012(15) 0.0058(13) -0.0056(15) C2 0.035(2) 0.033(3) 0.036(2) -0.012(2) 0.0172(17) -0.004(2) C3 0.030(2) 0.039(3) 0.027(2) 0.006(2) -0.0031(16) -0.002(2) C4 0.043(2) 0.019(2) 0.033(2) -0.0015(18) -0.0002(18) 0.0098(18) C5 0.040(2) 0.027(2) 0.036(3) -0.0012(19) -0.0028(19) -0.0194(19) C6 0.0214(17) 0.0146(18) 0.0221(19) 0.0008(15) 0.0010(13) -0.0054(14) C7 0.029(2) 0.027(2) 0.032(2) -0.0044(18) 0.0106(16) 0.0074(17) C8 0.0174(17) 0.025(2) 0.034(2) 0.0055(18) 0.0008(14) -0.0104(15) C9 0.044(2) 0.031(3) 0.021(2) -0.0019(18) 0.0026(16) -0.007(2) C10 0.0235(18) 0.029(2) 0.040(2) 0.0114(19) -0.0048(16) 0.0035(17) P1 0.0170(4) 0.0185(5) 0.0157(4) -0.0010(4) 0.0046(3) -0.0024(4) P2 0.0180(4) 0.0111(5) 0.0220(5) -0.0001(4) 0.0001(3) -0.0041(3) P3 0.0115(4) 0.0149(5) 0.0196(4) 0.0001(4) 0.0031(3) -0.0016(3) P4 0.0183(4) 0.0160(5) 0.0171(5) 0.0011(4) -0.0014(3) -0.0023(4) Cl1 0.0153(4) 0.0367(6) 0.0396(5) 0.0128(5) 0.0010(3) 0.0059(4) Cl2 0.0324(5) 0.0220(5) 0.0250(5) -0.0099(4) 0.0018(4) -0.0007(4) Se1 0.01343(16) 0.01392(18) 0.0228(2) -0.00300(14) 0.00140(13) 0.00317(13) Pd1 0.01020(10) 0.01162(12) 0.01599(12) -0.00120(11) 0.00183(7) -0.00090(9) Pd2 0.01292(11) 0.01149(12) 0.01691(12) -0.00178(11) -0.00027(8) -0.00238(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 P1 1.825(4) . ? C1 P2 1.822(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 P1 1.815(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 P1 1.820(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 P2 1.817(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 P2 1.813(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 P3 1.824(4) . ? C6 P4 1.838(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 P3 1.815(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 P3 1.815(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 P4 1.830(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 P4 1.816(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? P1 Pd1 2.2944(9) . ? P2 Pd2 2.3207(10) . ? P3 Pd1 2.3222(10) . ? P4 Pd2 2.2885(10) . ? Cl1 Pd1 2.3730(9) . ? Cl2 Pd2 2.3831(10) . ? Se1 Pd1 2.4142(4) . ? Se1 Pd2 2.4182(5) . ? Pd1 Pd2 3.0961(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 P1 C1 P2 113.53(19) . . ? P1 C1 H1A 108.9 . . ? P2 C1 H1A 108.9 . . ? P1 C1 H1B 108.9 . . ? P2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P3 C6 P4 114.3(2) . . ? P3 C6 H6A 108.7 . . ? P4 C6 H6A 108.7 . . ? P3 C6 H6B 108.7 . . ? P4 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P4 C9 H9A 109.5 . . ? P4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P4 C10 H10A 109.5 . . ? P4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 P1 C3 102.7(2) . . ? C2 P1 C1 103.06(19) . . ? C3 P1 C1 103.5(2) . . ? C2 P1 Pd1 119.78(17) . . ? C3 P1 Pd1 115.25(14) . . ? C1 P1 Pd1 110.67(13) . . ? C5 P2 C4 104.2(2) . . ? C5 P2 C1 102.97(19) . . ? C4 P2 C1 104.3(2) . . ? C5 P2 Pd2 113.54(15) . . ? C4 P2 Pd2 112.71(16) . . ? C1 P2 Pd2 117.68(13) . . ? C8 P3 C7 104.0(2) . . ? C8 P3 C6 102.56(18) . . ? C7 P3 C6 103.4(2) . . ? C8 P3 Pd1 113.48(14) . . ? C7 P3 Pd1 113.01(15) . . ? C6 P3 Pd1 118.71(13) . . ? C10 P4 C9 102.4(2) . . ? C10 P4 C6 104.4(2) . . ? C9 P4 C6 103.66(19) . . ? C10 P4 Pd2 119.60(15) . . ? C9 P4 Pd2 114.75(15) . . ? C6 P4 Pd2 110.33(13) . . ? Pd1 Se1 Pd2 79.687(14) . . ? P1 Pd1 P3 173.35(3) . . ? P1 Pd1 Cl1 96.20(3) . . ? P3 Pd1 Cl1 88.63(3) . . ? P1 Pd1 Se1 82.58(3) . . ? P3 Pd1 Se1 92.36(2) . . ? Cl1 Pd1 Se1 176.89(3) . . ? P1 Pd1 Pd2 95.75(2) . . ? P3 Pd1 Pd2 77.66(2) . . ? Cl1 Pd1 Pd2 127.27(3) . . ? Se1 Pd1 Pd2 50.213(12) . . ? P4 Pd2 P2 173.70(4) . . ? P4 Pd2 Cl2 96.88(4) . . ? P2 Pd2 Cl2 88.11(4) . . ? P4 Pd2 Se1 81.95(3) . . ? P2 Pd2 Se1 92.70(3) . . ? Cl2 Pd2 Se1 174.21(3) . . ? P4 Pd2 Pd1 96.21(3) . . ? P2 Pd2 Pd1 77.73(2) . . ? Cl2 Pd2 Pd1 124.67(3) . . ? Se1 Pd2 Pd1 50.101(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 C1 P1 C2 -148.1(2) . . . . ? P2 C1 P1 C3 105.2(2) . . . . ? P2 C1 P1 Pd1 -18.8(2) . . . . ? P1 C1 P2 C5 -179.0(2) . . . . ? P1 C1 P2 C4 -70.4(3) . . . . ? P1 C1 P2 Pd2 55.3(2) . . . . ? P4 C6 P3 C8 177.4(2) . . . . ? P4 C6 P3 C7 -74.7(3) . . . . ? P4 C6 P3 Pd1 51.4(3) . . . . ? P3 C6 P4 C10 -144.2(2) . . . . ? P3 C6 P4 C9 108.9(2) . . . . ? P3 C6 P4 Pd2 -14.5(2) . . . . ? C2 P1 Pd1 P3 100.8(4) . . . . ? C3 P1 Pd1 P3 -135.9(4) . . . . ? C1 P1 Pd1 P3 -18.9(4) . . . . ? C2 P1 Pd1 Cl1 -122.85(17) . . . . ? C3 P1 Pd1 Cl1 0.51(19) . . . . ? C1 P1 Pd1 Cl1 117.54(14) . . . . ? C2 P1 Pd1 Se1 60.03(17) . . . . ? C3 P1 Pd1 Se1 -176.61(19) . . . . ? C1 P1 Pd1 Se1 -59.58(14) . . . . ? C2 P1 Pd1 Pd2 108.60(17) . . . . ? C3 P1 Pd1 Pd2 -128.04(19) . . . . ? C1 P1 Pd1 Pd2 -11.02(14) . . . . ? C8 P3 Pd1 P1 -159.5(3) . . . . ? C7 P3 Pd1 P1 82.4(4) . . . . ? C6 P3 Pd1 P1 -38.9(4) . . . . ? C8 P3 Pd1 Cl1 63.79(16) . . . . ? C7 P3 Pd1 Cl1 -54.28(16) . . . . ? C6 P3 Pd1 Cl1 -175.65(15) . . . . ? C8 P3 Pd1 Se1 -119.15(15) . . . . ? C7 P3 Pd1 Se1 122.77(15) . . . . ? C6 P3 Pd1 Se1 1.40(15) . . . . ? C8 P3 Pd1 Pd2 -167.50(16) . . . . ? C7 P3 Pd1 Pd2 74.43(16) . . . . ? C6 P3 Pd1 Pd2 -46.94(15) . . . . ? Pd2 Se1 Pd1 P1 103.89(3) . . . . ? Pd2 Se1 Pd1 P3 -71.78(3) . . . . ? Pd2 Se1 Pd1 Cl1 36.8(5) . . . . ? C10 P4 Pd2 P2 91.0(4) . . . . ? C9 P4 Pd2 P2 -146.6(3) . . . . ? C6 P4 Pd2 P2 -30.0(4) . . . . ? C10 P4 Pd2 Cl2 -126.77(18) . . . . ? C9 P4 Pd2 Cl2 -4.45(16) . . . . ? C6 P4 Pd2 Cl2 112.18(14) . . . . ? C10 P4 Pd2 Se1 58.95(18) . . . . ? C9 P4 Pd2 Se1 -178.73(16) . . . . ? C6 P4 Pd2 Se1 -62.10(14) . . . . ? C10 P4 Pd2 Pd1 107.11(18) . . . . ? C9 P4 Pd2 Pd1 -130.57(16) . . . . ? C6 P4 Pd2 Pd1 -13.94(14) . . . . ? C5 P2 Pd2 P4 -152.2(4) . . . . ? C4 P2 Pd2 P4 89.5(4) . . . . ? C1 P2 Pd2 P4 -31.9(4) . . . . ? C5 P2 Pd2 Cl2 65.30(18) . . . . ? C4 P2 Pd2 Cl2 -52.94(16) . . . . ? C1 P2 Pd2 Cl2 -174.38(13) . . . . ? C5 P2 Pd2 Se1 -120.45(18) . . . . ? C4 P2 Pd2 Se1 121.32(16) . . . . ? C1 P2 Pd2 Se1 -0.12(13) . . . . ? C5 P2 Pd2 Pd1 -168.58(18) . . . . ? C4 P2 Pd2 Pd1 73.19(16) . . . . ? C1 P2 Pd2 Pd1 -48.26(13) . . . . ? Pd1 Se1 Pd2 P4 105.12(3) . . . . ? Pd1 Se1 Pd2 P2 -71.54(2) . . . . ? Pd1 Se1 Pd2 Cl2 26.4(3) . . . . ? P1 Pd1 Pd2 P4 -149.41(4) . . . . ? P3 Pd1 Pd2 P4 29.66(4) . . . . ? Cl1 Pd1 Pd2 P4 108.28(4) . . . . ? Se1 Pd1 Pd2 P4 -74.06(3) . . . . ? P1 Pd1 Pd2 P2 28.81(4) . . . . ? P3 Pd1 Pd2 P2 -152.12(4) . . . . ? Cl1 Pd1 Pd2 P2 -73.50(4) . . . . ? Se1 Pd1 Pd2 P2 104.16(3) . . . . ? P1 Pd1 Pd2 Cl2 107.77(4) . . . . ? P3 Pd1 Pd2 Cl2 -73.16(4) . . . . ? Cl1 Pd1 Pd2 Cl2 5.46(5) . . . . ? Se1 Pd1 Pd2 Cl2 -176.88(4) . . . . ? P1 Pd1 Pd2 Se1 -75.35(3) . . . . ? P3 Pd1 Pd2 Se1 103.72(3) . . . . ? Cl1 Pd1 Pd2 Se1 -177.66(4) . . . . ? _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.556 _refine_diff_density_min -1.363 _refine_diff_density_rms 0.142 data_bj267 _database_code_depnum_ccdc_archive 'CCDC 849400' #TrackingRef '- bj245_267_bj244_Oct27.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H31 Cl2 F3 O3 P4 Pd2 S2' _chemical_formula_weight 752.07 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2968(2) _cell_length_b 15.17220(10) _cell_length_c 27.7363(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5174.75(11) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 32524 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.05 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.931 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 2.039 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.459 _exptl_absorpt_correction_T_max 0.541 _exptl_absorpt_process_details 'd*TREK (MSC, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Rigaku/ADSC CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42219 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 30.49 _reflns_number_total 7431 _reflns_number_gt 6229 _reflns_threshold_expression >2\s(I) _computing_data_collection 'd*TREK (MSC, 1998)' _computing_cell_refinement 'd*TREK (MSC, 1998)' _computing_data_reduction 'teXsan (MSC, 1992)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0489P)^2^+4.7334P] 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 7431 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0.003 _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 C1 C 1.1777(2) 0.89130(16) 0.38749(10) 0.0176(5) Uani 1 1 d . . . H1A H 1.2371 0.9295 0.3755 0.021 Uiso 1 1 calc R . . H1B H 1.1644 0.9070 0.4216 0.021 Uiso 1 1 calc R . . C2 C 1.1032(2) 0.9079(2) 0.29099(10) 0.0270(6) Uani 1 1 d . . . H2A H 1.0472 0.9295 0.2688 0.041 Uiso 1 1 calc R . . H2B H 1.1203 0.8464 0.2834 0.041 Uiso 1 1 calc R . . H2C H 1.1689 0.9439 0.2876 0.041 Uiso 1 1 calc R . . C3 C 1.0319(2) 1.03154(17) 0.36389(11) 0.0250(6) Uani 1 1 d . . . H3A H 1.0988 1.0642 0.3569 0.037 Uiso 1 1 calc R . . H3B H 1.0119 1.0401 0.3978 0.037 Uiso 1 1 calc R . . H3C H 0.9731 1.0532 0.3432 0.037 Uiso 1 1 calc R . . C4 C 1.3299(2) 0.7785(2) 0.33908(13) 0.0318(7) Uani 1 1 d . . . H4A H 1.3869 0.8199 0.3490 0.048 Uiso 1 1 calc R . . H4B H 1.2991 0.7974 0.3082 0.048 Uiso 1 1 calc R . . H4C H 1.3612 0.7194 0.3356 0.048 Uiso 1 1 calc R . . C5 C 1.3004(3) 0.7593(2) 0.43975(13) 0.0325(7) Uani 1 1 d . . . H5A H 1.3256 0.6981 0.4412 0.049 Uiso 1 1 calc R . . H5B H 1.2540 0.7716 0.4677 0.049 Uiso 1 1 calc R . . H5C H 1.3631 0.7991 0.4401 0.049 Uiso 1 1 calc R . . C6 C 0.7967(2) 0.61701(17) 0.36492(10) 0.0184(5) Uani 1 1 d . . . H6A H 0.7974 0.6012 0.3995 0.022 Uiso 1 1 calc R . . H6B H 0.7438 0.5779 0.3486 0.022 Uiso 1 1 calc R . . C7 C 0.6568(2) 0.74856(18) 0.40851(11) 0.0252(6) Uani 1 1 d . . . H7A H 0.6262 0.8081 0.4068 0.038 Uiso 1 1 calc R . . H7B H 0.6956 0.7412 0.4391 0.038 Uiso 1 1 calc R . . H7C H 0.5979 0.7052 0.4065 0.038 Uiso 1 1 calc R . . C8 C 0.6630(2) 0.73202(19) 0.30590(11) 0.0266(6) Uani 1 1 d . . . H8A H 0.6024 0.6912 0.3111 0.040 Uiso 1 1 calc R . . H8B H 0.7049 0.7132 0.2777 0.040 Uiso 1 1 calc R . . H8C H 0.6345 0.7915 0.3005 0.040 Uiso 1 1 calc R . . C9 C 0.9168(2) 0.6163(2) 0.27524(10) 0.0268(6) Uani 1 1 d . . . H9A H 0.9828 0.5975 0.2583 0.040 Uiso 1 1 calc R . . H9B H 0.9046 0.6793 0.2695 0.040 Uiso 1 1 calc R . . H9C H 0.8545 0.5826 0.2633 0.040 Uiso 1 1 calc R . . C10 C 0.9494(3) 0.47861(18) 0.34556(12) 0.0274(6) Uani 1 1 d . . . H10A H 0.8858 0.4487 0.3319 0.041 Uiso 1 1 calc R . . H10B H 0.9563 0.4634 0.3798 0.041 Uiso 1 1 calc R . . H10C H 1.0150 0.4598 0.3283 0.041 Uiso 1 1 calc R . . C11 C 1.0107(2) 0.8032(2) 0.47027(10) 0.0245(6) Uani 1 1 d . . . H11A H 1.0630 0.7673 0.4883 0.037 Uiso 1 1 calc R . . H11B H 0.9510 0.8206 0.4917 0.037 Uiso 1 1 calc R . . H11C H 1.0471 0.8560 0.4579 0.037 Uiso 1 1 calc R . . C12 C 1.1578(3) 0.5231(2) 0.49819(11) 0.0297(6) Uani 1 1 d . . . O1 O 1.35941(19) 0.54271(16) 0.47480(8) 0.0350(5) Uani 1 1 d . . . O2 O 1.3088(2) 0.55890(18) 0.55927(9) 0.0421(6) Uani 1 1 d . . . O3 O 1.3077(2) 0.41477(15) 0.52146(9) 0.0367(5) Uani 1 1 d . . . F1 F 1.1306(2) 0.60666(16) 0.49317(10) 0.0599(7) Uani 1 1 d . . . F2 F 1.09163(16) 0.4887(2) 0.53157(9) 0.0556(7) Uani 1 1 d . . . F3 F 1.13538(17) 0.48345(16) 0.45661(8) 0.0473(5) Uani 1 1 d . . . P1 P 1.05360(5) 0.91525(4) 0.35253(2) 0.01394(13) Uani 1 1 d . . . P2 P 1.22287(5) 0.77624(4) 0.38469(3) 0.01715(14) Uani 1 1 d . . . P3 P 0.75052(5) 0.73217(4) 0.35874(2) 0.01535(13) Uani 1 1 d . . . P4 P 0.93304(5) 0.59694(4) 0.33947(2) 0.01570(13) Uani 1 1 d . . . S1 S 0.95695(5) 0.73978(4) 0.42041(2) 0.01500(12) Uani 1 1 d . . . S2 S 1.30052(6) 0.50851(5) 0.51555(2) 0.02196(14) Uani 1 1 d . . . Cl1 Cl 0.82610(6) 0.91114(5) 0.29492(3) 0.02624(15) Uani 1 1 d . . . Cl2 Cl 1.18681(6) 0.59992(5) 0.31342(3) 0.02694(15) Uani 1 1 d . . . Pd1 Pd 0.896850(15) 0.828500(12) 0.359021(7) 0.01268(6) Uani 1 1 d . . . Pd2 Pd 1.079682(15) 0.679891(12) 0.367782(7) 0.01293(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 C1 0.0188(11) 0.0124(10) 0.0214(13) -0.0010(9) -0.0027(10) -0.0025(9) C2 0.0282(14) 0.0361(16) 0.0167(14) 0.0042(12) 0.0035(11) 0.0009(12) C3 0.0252(14) 0.0130(11) 0.0366(17) -0.0008(11) -0.0018(12) 0.0024(10) C4 0.0243(14) 0.0258(14) 0.045(2) -0.0017(14) 0.0088(13) 0.0000(11) C5 0.0315(15) 0.0256(14) 0.0402(19) -0.0008(13) -0.0204(14) 0.0033(12) C6 0.0199(12) 0.0134(11) 0.0218(13) 0.0038(9) 0.0018(10) -0.0022(9) C7 0.0238(13) 0.0234(13) 0.0283(15) -0.0002(11) 0.0104(12) 0.0044(11) C8 0.0265(14) 0.0273(14) 0.0261(15) 0.0011(12) -0.0105(12) -0.0031(11) C9 0.0299(15) 0.0357(16) 0.0147(14) -0.0053(12) -0.0017(11) 0.0036(12) C10 0.0281(14) 0.0152(12) 0.0389(17) -0.0048(12) -0.0006(13) 0.0030(11) C11 0.0296(14) 0.0300(14) 0.0140(13) -0.0065(11) -0.0026(11) 0.0034(12) C12 0.0314(15) 0.0374(16) 0.0204(14) -0.0011(13) 0.0020(12) 0.0076(13) O1 0.0342(12) 0.0437(13) 0.0272(12) 0.0022(10) 0.0048(9) -0.0118(10) O2 0.0464(15) 0.0538(15) 0.0260(12) -0.0164(11) -0.0028(11) -0.0066(12) O3 0.0368(13) 0.0294(11) 0.0441(14) 0.0068(10) 0.0055(11) 0.0081(9) F1 0.0686(16) 0.0437(13) 0.0673(17) -0.0001(12) -0.0142(13) 0.0307(12) F2 0.0256(10) 0.101(2) 0.0402(13) 0.0175(13) 0.0065(9) 0.0044(11) F3 0.0329(10) 0.0756(16) 0.0334(11) -0.0185(11) -0.0073(9) 0.0031(10) P1 0.0150(3) 0.0122(3) 0.0147(3) 0.0014(2) 0.0003(2) -0.0003(2) P2 0.0143(3) 0.0145(3) 0.0226(4) 0.0003(3) -0.0026(2) 0.0004(2) P3 0.0141(3) 0.0154(3) 0.0165(3) 0.0008(2) -0.0002(2) -0.0008(2) P4 0.0170(3) 0.0137(3) 0.0164(3) -0.0025(2) -0.0014(2) 0.0007(2) S1 0.0177(3) 0.0157(3) 0.0116(3) 0.0005(2) 0.0005(2) 0.0016(2) S2 0.0244(3) 0.0234(3) 0.0181(3) -0.0021(3) -0.0003(3) -0.0016(3) Cl1 0.0242(3) 0.0299(3) 0.0246(4) 0.0113(3) -0.0081(3) 0.0001(3) Cl2 0.0219(3) 0.0299(3) 0.0290(4) -0.0107(3) 0.0057(3) 0.0044(3) Pd1 0.01327(9) 0.01265(9) 0.01214(11) 0.00087(6) -0.00114(6) 0.00026(6) Pd2 0.01359(9) 0.01239(9) 0.01280(11) -0.00095(7) -0.00051(6) 0.00136(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 P2 1.834(2) . ? C1 P1 1.844(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 P1 1.816(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 P1 1.812(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 P2 1.826(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 P2 1.818(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 P4 1.844(3) . ? C6 P3 1.845(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 P3 1.816(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 P3 1.818(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 P4 1.817(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 P4 1.815(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 S1 1.809(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 F1 1.318(4) . ? C12 F3 1.330(4) . ? C12 F2 1.339(4) . ? C12 S2 1.833(3) . ? O1 S2 1.439(2) . ? O2 S2 1.437(2) . ? O3 S2 1.434(2) . ? P1 Pd1 2.3410(7) . ? P2 Pd2 2.3361(7) . ? P3 Pd1 2.3181(7) . ? P4 Pd2 2.3350(7) . ? S1 Pd2 2.2879(6) . ? S1 Pd1 2.2929(6) . ? Cl1 Pd1 2.3430(7) . ? Cl2 Pd2 2.3412(7) . ? Pd1 Pd2 3.1933(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 P2 C1 P1 114.59(13) . . ? P2 C1 H1A 108.6 . . ? P1 C1 H1A 108.6 . . ? P2 C1 H1B 108.6 . . ? P1 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P4 C6 P3 113.60(13) . . ? P4 C6 H6A 108.8 . . ? P3 C6 H6A 108.8 . . ? P4 C6 H6B 108.8 . . ? P3 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P4 C9 H9A 109.5 . . ? P4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P4 C10 H10A 109.5 . . ? P4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? S1 C11 H11A 109.5 . . ? S1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? F1 C12 F3 106.9(3) . . ? F1 C12 F2 107.0(3) . . ? F3 C12 F2 107.3(3) . . ? F1 C12 S2 112.8(2) . . ? F3 C12 S2 111.8(2) . . ? F2 C12 S2 110.7(2) . . ? C3 P1 C2 105.84(15) . . ? C3 P1 C1 102.85(13) . . ? C2 P1 C1 101.78(13) . . ? C3 P1 Pd1 114.37(10) . . ? C2 P1 Pd1 108.32(11) . . ? C1 P1 Pd1 122.00(8) . . ? C5 P2 C4 101.94(17) . . ? C5 P2 C1 104.92(13) . . ? C4 P2 C1 103.30(13) . . ? C5 P2 Pd2 118.38(11) . . ? C4 P2 Pd2 114.59(11) . . ? C1 P2 Pd2 112.08(8) . . ? C7 P3 C8 103.72(15) . . ? C7 P3 C6 104.74(12) . . ? C8 P3 C6 104.82(13) . . ? C7 P3 Pd1 113.82(10) . . ? C8 P3 Pd1 117.58(10) . . ? C6 P3 Pd1 110.97(9) . . ? C10 P4 C9 105.28(15) . . ? C10 P4 C6 103.22(13) . . ? C9 P4 C6 104.42(13) . . ? C10 P4 Pd2 114.60(10) . . ? C9 P4 Pd2 109.10(11) . . ? C6 P4 Pd2 118.97(9) . . ? C11 S1 Pd2 117.26(10) . . ? C11 S1 Pd1 111.91(10) . . ? Pd2 S1 Pd1 88.39(2) . . ? O3 S2 O2 115.26(16) . . ? O3 S2 O1 114.62(15) . . ? O2 S2 O1 115.79(15) . . ? O3 S2 C12 102.04(15) . . ? O2 S2 C12 103.03(15) . . ? O1 S2 C12 103.40(15) . . ? S1 Pd1 P3 83.26(2) . . ? S1 Pd1 P1 97.00(2) . . ? P3 Pd1 P1 173.38(2) . . ? S1 Pd1 Cl1 175.81(2) . . ? P3 Pd1 Cl1 92.67(2) . . ? P1 Pd1 Cl1 86.93(2) . . ? S1 Pd1 Pd2 45.740(16) . . ? P3 Pd1 Pd2 95.831(18) . . ? P1 Pd1 Pd2 79.815(16) . . ? Cl1 Pd1 Pd2 134.19(2) . . ? S1 Pd2 P4 85.37(2) . . ? S1 Pd2 P2 96.93(2) . . ? P4 Pd2 P2 170.70(3) . . ? S1 Pd2 Cl2 171.10(3) . . ? P4 Pd2 Cl2 86.48(2) . . ? P2 Pd2 Cl2 91.69(3) . . ? S1 Pd2 Pd1 45.870(16) . . ? P4 Pd2 Pd1 79.120(17) . . ? P2 Pd2 Pd1 95.974(17) . . ? Cl2 Pd2 Pd1 135.49(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 C1 P1 C3 179.21(15) . . . . ? P2 C1 P1 C2 -71.31(18) . . . . ? P2 C1 P1 Pd1 49.28(18) . . . . ? P1 C1 P2 C5 -154.94(17) . . . . ? P1 C1 P2 C4 98.63(18) . . . . ? P1 C1 P2 Pd2 -25.24(17) . . . . ? P4 C6 P3 C7 -152.90(16) . . . . ? P4 C6 P3 C8 98.24(17) . . . . ? P4 C6 P3 Pd1 -29.66(16) . . . . ? P3 C6 P4 C10 -174.67(16) . . . . ? P3 C6 P4 C9 -64.80(18) . . . . ? P3 C6 P4 Pd2 57.10(17) . . . . ? F1 C12 S2 O3 176.6(2) . . . . ? F3 C12 S2 O3 -62.8(3) . . . . ? F2 C12 S2 O3 56.7(3) . . . . ? F1 C12 S2 O2 56.8(3) . . . . ? F3 C12 S2 O2 177.4(2) . . . . ? F2 C12 S2 O2 -63.1(3) . . . . ? F1 C12 S2 O1 -64.1(3) . . . . ? F3 C12 S2 O1 56.4(3) . . . . ? F2 C12 S2 O1 176.0(2) . . . . ? C11 S1 Pd1 P3 -136.19(11) . . . . ? Pd2 S1 Pd1 P3 104.96(2) . . . . ? C11 S1 Pd1 P1 50.47(11) . . . . ? Pd2 S1 Pd1 P1 -68.38(2) . . . . ? C11 S1 Pd1 Cl1 -150.1(4) . . . . ? Pd2 S1 Pd1 Cl1 91.1(4) . . . . ? C11 S1 Pd1 Pd2 118.86(11) . . . . ? C7 P3 Pd1 S1 75.19(11) . . . . ? C8 P3 Pd1 S1 -163.26(12) . . . . ? C6 P3 Pd1 S1 -42.65(10) . . . . ? C7 P3 Pd1 P1 167.8(2) . . . . ? C8 P3 Pd1 P1 -70.7(3) . . . . ? C6 P3 Pd1 P1 50.0(2) . . . . ? C7 P3 Pd1 Cl1 -105.82(11) . . . . ? C8 P3 Pd1 Cl1 15.73(12) . . . . ? C6 P3 Pd1 Cl1 136.34(10) . . . . ? C7 P3 Pd1 Pd2 119.26(11) . . . . ? C8 P3 Pd1 Pd2 -119.19(12) . . . . ? C6 P3 Pd1 Pd2 1.42(9) . . . . ? C3 P1 Pd1 S1 -119.10(11) . . . . ? C2 P1 Pd1 S1 123.15(11) . . . . ? C1 P1 Pd1 S1 5.73(10) . . . . ? C3 P1 Pd1 P3 149.1(2) . . . . ? C2 P1 Pd1 P3 31.4(3) . . . . ? C1 P1 Pd1 P3 -86.1(2) . . . . ? C3 P1 Pd1 Cl1 62.38(11) . . . . ? C2 P1 Pd1 Cl1 -55.37(11) . . . . ? C1 P1 Pd1 Cl1 -172.79(10) . . . . ? C3 P1 Pd1 Pd2 -161.67(11) . . . . ? C2 P1 Pd1 Pd2 80.58(11) . . . . ? C1 P1 Pd1 Pd2 -36.84(10) . . . . ? C11 S1 Pd2 P4 166.75(11) . . . . ? Pd1 S1 Pd2 P4 -79.33(2) . . . . ? C11 S1 Pd2 P2 -22.30(11) . . . . ? Pd1 S1 Pd2 P2 91.62(2) . . . . ? C11 S1 Pd2 Cl2 142.98(19) . . . . ? Pd1 S1 Pd2 Cl2 -103.10(17) . . . . ? C11 S1 Pd2 Pd1 -113.92(11) . . . . ? C10 P4 Pd2 S1 -119.08(12) . . . . ? C9 P4 Pd2 S1 123.19(11) . . . . ? C6 P4 Pd2 S1 3.66(10) . . . . ? C10 P4 Pd2 P2 136.21(18) . . . . ? C9 P4 Pd2 P2 18.5(2) . . . . ? C6 P4 Pd2 P2 -101.04(18) . . . . ? C10 P4 Pd2 Cl2 57.33(12) . . . . ? C9 P4 Pd2 Cl2 -60.39(11) . . . . ? C6 P4 Pd2 Cl2 -179.92(10) . . . . ? C10 P4 Pd2 Pd1 -164.99(12) . . . . ? C9 P4 Pd2 Pd1 77.28(11) . . . . ? C6 P4 Pd2 Pd1 -42.25(10) . . . . ? C5 P2 Pd2 S1 77.33(13) . . . . ? C4 P2 Pd2 S1 -162.29(12) . . . . ? C1 P2 Pd2 S1 -45.00(10) . . . . ? C5 P2 Pd2 P4 -178.88(18) . . . . ? C4 P2 Pd2 P4 -58.5(2) . . . . ? C1 P2 Pd2 P4 58.79(19) . . . . ? C5 P2 Pd2 Cl2 -100.42(13) . . . . ? C4 P2 Pd2 Cl2 19.96(12) . . . . ? C1 P2 Pd2 Cl2 137.25(10) . . . . ? C5 P2 Pd2 Pd1 123.50(13) . . . . ? C4 P2 Pd2 Pd1 -116.12(12) . . . . ? C1 P2 Pd2 Pd1 1.17(10) . . . . ? P3 Pd1 Pd2 S1 -74.67(3) . . . . ? P1 Pd1 Pd2 S1 110.36(3) . . . . ? Cl1 Pd1 Pd2 S1 -174.15(3) . . . . ? S1 Pd1 Pd2 P4 94.12(3) . . . . ? P3 Pd1 Pd2 P4 19.45(2) . . . . ? P1 Pd1 Pd2 P4 -155.52(2) . . . . ? Cl1 Pd1 Pd2 P4 -80.03(3) . . . . ? S1 Pd1 Pd2 P2 -93.87(3) . . . . ? P3 Pd1 Pd2 P2 -168.54(3) . . . . ? P1 Pd1 Pd2 P2 16.49(3) . . . . ? Cl1 Pd1 Pd2 P2 91.99(3) . . . . ? S1 Pd1 Pd2 Cl2 167.58(4) . . . . ? P3 Pd1 Pd2 Cl2 92.91(3) . . . . ? P1 Pd1 Pd2 Cl2 -82.06(3) . . . . ? Cl1 Pd1 Pd2 Cl2 -6.56(4) . . . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 1.553 _refine_diff_density_min -1.267 _refine_diff_density_rms 0.146 data_bj244 _database_code_depnum_ccdc_archive 'CCDC 849401' #TrackingRef '- bj245_267_bj244_Oct27.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H28 Br2 O P4 Pd2 S' _chemical_formula_weight 692.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 'P 212121' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.7943(11) _cell_length_b 13.7756(3) _cell_length_c 14.8223(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2204.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(1) _cell_measurement_reflns_used 16508 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.05 _exptl_crystal_description irregular _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.088 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 5.636 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.106 _exptl_absorpt_correction_T_max 0.139 _exptl_absorpt_process_details 'd*TREK (MSC, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(1) _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 'Rigaku/ADSC CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16735 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 30.06 _reflns_number_total 5409 _reflns_number_gt 5121 _reflns_threshold_expression >2\s(I) _computing_data_collection 'd*TREK (MSC, 1998)' _computing_cell_refinement 'd*TREK (MSC, 1998)' _computing_data_reduction 'teXsan (MSC, 1992)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0392P)^2^+3.4804P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.130(8) _refine_ls_number_reflns 5409 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 C1 C 0.3692(4) 0.3205(3) 0.0117(3) 0.0213(8) Uani 1 1 d . . . H1A H 0.2839 0.2945 0.0079 0.026 Uiso 1 1 calc R . . H1B H 0.4207 0.2711 0.0424 0.026 Uiso 1 1 calc R . . C2 C 0.2220(5) 0.4905(4) 0.0487(5) 0.0377(13) Uani 1 1 d . . . H2A H 0.2316 0.5184 -0.0117 0.057 Uiso 1 1 calc R . . H2B H 0.2038 0.5425 0.0919 0.057 Uiso 1 1 calc R . . H2C H 0.1537 0.4436 0.0485 0.057 Uiso 1 1 calc R . . C3 C 0.3341(6) 0.3804(5) 0.1933(4) 0.0457(16) Uani 1 1 d . . . H3A H 0.3308 0.4337 0.2370 0.068 Uiso 1 1 calc R . . H3B H 0.3998 0.3350 0.2104 0.068 Uiso 1 1 calc R . . H3C H 0.2543 0.3465 0.1926 0.068 Uiso 1 1 calc R . . C4 C 0.2925(5) 0.3705(5) -0.1674(4) 0.0431(15) Uani 1 1 d . . . H4A H 0.3127 0.3699 -0.2319 0.065 Uiso 1 1 calc R . . H4B H 0.2660 0.4358 -0.1497 0.065 Uiso 1 1 calc R . . H4C H 0.2254 0.3243 -0.1556 0.065 Uiso 1 1 calc R . . C5 C 0.4569(6) 0.2122(4) -0.1372(4) 0.0442(14) Uani 1 1 d . . . H5A H 0.3839 0.1724 -0.1239 0.066 Uiso 1 1 calc R . . H5B H 0.5285 0.1868 -0.1041 0.066 Uiso 1 1 calc R . . H5C H 0.4740 0.2103 -0.2021 0.066 Uiso 1 1 calc R . . C6 C 0.8232(4) 0.5914(3) -0.0351(3) 0.0169(7) Uani 1 1 d . . . H6A H 0.8687 0.5538 0.0112 0.020 Uiso 1 1 calc R . . H6B H 0.8770 0.6457 -0.0545 0.020 Uiso 1 1 calc R . . C7 C 0.6108(4) 0.7143(3) -0.0727(3) 0.0262(9) Uani 1 1 d . . . H7A H 0.6716 0.7605 -0.0965 0.039 Uiso 1 1 calc R . . H7B H 0.5401 0.7498 -0.0476 0.039 Uiso 1 1 calc R . . H7C H 0.5822 0.6719 -0.1215 0.039 Uiso 1 1 calc R . . C8 C 0.7412(5) 0.7319(4) 0.0943(4) 0.0326(11) Uani 1 1 d . . . H8A H 0.7888 0.7809 0.0611 0.049 Uiso 1 1 calc R . . H8B H 0.7949 0.7004 0.1388 0.049 Uiso 1 1 calc R . . H8C H 0.6716 0.7633 0.1251 0.049 Uiso 1 1 calc R . . C9 C 0.8147(5) 0.5906(4) -0.2288(3) 0.0313(11) Uani 1 1 d . . . H9A H 0.7438 0.6346 -0.2346 0.047 Uiso 1 1 calc R . . H9B H 0.8217 0.5509 -0.2834 0.047 Uiso 1 1 calc R . . H9C H 0.8906 0.6286 -0.2207 0.047 Uiso 1 1 calc R . . C10 C 0.9298(5) 0.4362(4) -0.1361(4) 0.0353(11) Uani 1 1 d . . . H10A H 1.0040 0.4769 -0.1318 0.053 Uiso 1 1 calc R . . H10B H 0.9312 0.4002 -0.1931 0.053 Uiso 1 1 calc R . . H10C H 0.9281 0.3904 -0.0855 0.053 Uiso 1 1 calc R . . O1 O 0.6271(3) 0.3074(2) 0.0607(2) 0.0286(7) Uani 1 1 d . . . P1 P 0.36613(10) 0.42902(8) 0.08155(7) 0.0180(2) Uani 1 1 d . . . P2 P 0.42800(10) 0.33622(8) -0.10290(7) 0.0183(2) Uani 1 1 d . . . P3 P 0.68232(10) 0.64111(7) 0.01554(7) 0.01429(19) Uani 1 1 d . . . P4 P 0.79235(10) 0.51262(7) -0.13224(7) 0.0164(2) Uani 1 1 d . . . S1 S 0.66230(9) 0.40532(7) 0.02431(6) 0.01551(18) Uani 1 1 d . . . Br1 Br 0.42218(4) 0.66900(3) 0.13842(3) 0.02597(10) Uani 1 1 d . . . Br2 Br 0.55190(5) 0.45393(4) -0.28537(3) 0.03578(13) Uani 1 1 d . . . Pd1 Pd 0.53640(3) 0.52969(2) 0.066123(18) 0.01169(6) Uani 1 1 d . . . Pd2 Pd 0.60619(3) 0.42892(2) -0.121696(18) 0.01330(7) 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 C1 0.025(2) 0.0166(17) 0.0221(19) 0.0009(15) -0.0035(17) -0.0084(17) C2 0.014(2) 0.037(3) 0.062(4) -0.009(3) 0.001(2) 0.001(2) C3 0.048(4) 0.064(4) 0.025(2) 0.001(2) 0.006(2) -0.030(3) C4 0.023(3) 0.076(4) 0.030(3) 0.015(3) -0.011(2) -0.004(3) C5 0.052(3) 0.025(2) 0.055(4) -0.019(2) 0.017(3) -0.013(3) C6 0.0142(18) 0.0182(17) 0.0184(17) 0.0010(14) 0.0034(15) -0.0028(15) C7 0.021(2) 0.026(2) 0.032(2) 0.0102(18) 0.002(2) 0.0013(19) C8 0.035(3) 0.026(2) 0.037(3) -0.021(2) 0.003(2) -0.005(2) C9 0.041(3) 0.032(2) 0.020(2) 0.0035(18) 0.007(2) -0.011(2) C10 0.032(3) 0.030(2) 0.044(3) -0.005(2) 0.014(2) 0.004(2) O1 0.0328(18) 0.0213(14) 0.0316(16) 0.0041(13) -0.0041(15) 0.0020(13) P1 0.0141(5) 0.0215(5) 0.0183(5) 0.0006(4) 0.0035(4) -0.0052(4) P2 0.0182(5) 0.0192(4) 0.0174(5) -0.0024(4) -0.0045(4) -0.0047(4) P3 0.0150(5) 0.0122(4) 0.0157(4) -0.0016(3) 0.0015(4) -0.0013(4) P4 0.0168(5) 0.0174(4) 0.0149(4) -0.0014(4) 0.0050(4) -0.0019(4) S1 0.0179(5) 0.0157(4) 0.0129(4) -0.0001(3) -0.0004(4) 0.0061(4) Br1 0.0267(2) 0.02049(18) 0.0307(2) -0.00067(16) 0.00943(17) 0.00961(17) Br2 0.0445(3) 0.0487(3) 0.01414(18) 0.00660(18) -0.00652(18) -0.0118(3) Pd1 0.01165(13) 0.01156(11) 0.01186(12) 0.00027(10) 0.00207(10) 0.00136(11) Pd2 0.01681(14) 0.01297(12) 0.01012(11) -0.00057(10) 0.00021(11) -0.00129(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 P1 1.819(4) . ? C1 P2 1.826(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 P1 1.837(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 P1 1.819(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 P2 1.810(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 P2 1.809(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 P3 1.829(4) . ? C6 P4 1.834(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 P3 1.824(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 P3 1.825(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 P4 1.805(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 P4 1.820(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? O1 S1 1.502(3) . ? P1 Pd1 2.3137(11) . ? P2 Pd2 2.3255(11) . ? P3 Pd1 2.3236(11) . ? P4 Pd2 2.3221(11) . ? S1 Pd2 2.2706(10) . ? S1 Pd1 2.2729(10) . ? Br1 Pd1 2.5202(5) . ? Br2 Pd2 2.5195(5) . ? Pd1 Pd2 3.2007(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 C1 P2 116.0(2) . . ? P1 C1 H1A 108.3 . . ? P2 C1 H1A 108.3 . . ? P1 C1 H1B 108.3 . . ? P2 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P3 C6 P4 113.1(2) . . ? P3 C6 H6A 109.0 . . ? P4 C6 H6A 109.0 . . ? P3 C6 H6B 109.0 . . ? P4 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P4 C9 H9A 109.5 . . ? P4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P4 C10 H10A 109.5 . . ? P4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C1 P1 C3 102.7(3) . . ? C1 P1 C2 104.1(2) . . ? C3 P1 C2 104.5(3) . . ? C1 P1 Pd1 114.94(15) . . ? C3 P1 Pd1 117.5(2) . . ? C2 P1 Pd1 111.72(18) . . ? C5 P2 C4 103.7(3) . . ? C5 P2 C1 102.1(2) . . ? C4 P2 C1 104.0(2) . . ? C5 P2 Pd2 110.0(2) . . ? C4 P2 Pd2 117.5(2) . . ? C1 P2 Pd2 117.64(14) . . ? C7 P3 C8 103.1(2) . . ? C7 P3 C6 105.4(2) . . ? C8 P3 C6 103.3(2) . . ? C7 P3 Pd1 108.04(16) . . ? C8 P3 Pd1 118.86(19) . . ? C6 P3 Pd1 116.65(13) . . ? C9 P4 C10 102.1(3) . . ? C9 P4 C6 104.3(2) . . ? C10 P4 C6 102.6(2) . . ? C9 P4 Pd2 117.67(19) . . ? C10 P4 Pd2 114.86(18) . . ? C6 P4 Pd2 113.45(13) . . ? O1 S1 Pd2 113.82(15) . . ? O1 S1 Pd1 115.32(15) . . ? Pd2 S1 Pd1 89.57(3) . . ? S1 Pd1 P1 92.87(4) . . ? S1 Pd1 P3 90.26(4) . . ? P1 Pd1 P3 165.08(4) . . ? S1 Pd1 Br1 169.24(3) . . ? P1 Pd1 Br1 91.48(3) . . ? P3 Pd1 Br1 88.04(3) . . ? S1 Pd1 Pd2 45.19(2) . . ? P1 Pd1 Pd2 90.74(3) . . ? P3 Pd1 Pd2 81.16(3) . . ? Br1 Pd1 Pd2 144.610(16) . . ? S1 Pd2 P4 84.51(4) . . ? S1 Pd2 P2 91.59(4) . . ? P4 Pd2 P2 175.21(4) . . ? S1 Pd2 Br2 177.93(3) . . ? P4 Pd2 Br2 93.93(3) . . ? P2 Pd2 Br2 89.89(3) . . ? S1 Pd2 Pd1 45.24(2) . . ? P4 Pd2 Pd1 92.69(3) . . ? P2 Pd2 Pd1 86.52(3) . . ? Br2 Pd2 Pd1 136.341(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 C1 P1 C3 -168.8(3) . . . . ? P2 C1 P1 C2 82.5(3) . . . . ? P2 C1 P1 Pd1 -40.0(3) . . . . ? P1 C1 P2 C5 164.6(3) . . . . ? P1 C1 P2 C4 -87.8(3) . . . . ? P1 C1 P2 Pd2 44.1(3) . . . . ? P4 C6 P3 C7 -61.9(3) . . . . ? P4 C6 P3 C8 -169.8(3) . . . . ? P4 C6 P3 Pd1 57.9(2) . . . . ? P3 C6 P4 C9 97.5(3) . . . . ? P3 C6 P4 C10 -156.3(2) . . . . ? P3 C6 P4 Pd2 -31.7(2) . . . . ? O1 S1 Pd1 P1 -28.12(16) . . . . ? Pd2 S1 Pd1 P1 88.19(4) . . . . ? O1 S1 Pd1 P3 166.46(16) . . . . ? Pd2 S1 Pd1 P3 -77.22(4) . . . . ? O1 S1 Pd1 Br1 85.6(2) . . . . ? Pd2 S1 Pd1 Br1 -158.06(14) . . . . ? O1 S1 Pd1 Pd2 -116.32(16) . . . . ? C1 P1 Pd1 S1 -27.02(16) . . . . ? C3 P1 Pd1 S1 94.0(3) . . . . ? C2 P1 Pd1 S1 -145.3(2) . . . . ? C1 P1 Pd1 P3 74.9(2) . . . . ? C3 P1 Pd1 P3 -164.1(3) . . . . ? C2 P1 Pd1 P3 -43.4(3) . . . . ? C1 P1 Pd1 Br1 162.82(16) . . . . ? C3 P1 Pd1 Br1 -76.2(3) . . . . ? C2 P1 Pd1 Br1 44.5(2) . . . . ? C1 P1 Pd1 Pd2 18.14(16) . . . . ? C3 P1 Pd1 Pd2 139.1(3) . . . . ? C2 P1 Pd1 Pd2 -100.2(2) . . . . ? C7 P3 Pd1 S1 119.83(17) . . . . ? C8 P3 Pd1 S1 -123.3(2) . . . . ? C6 P3 Pd1 S1 1.46(15) . . . . ? C7 P3 Pd1 P1 17.6(2) . . . . ? C8 P3 Pd1 P1 134.5(2) . . . . ? C6 P3 Pd1 P1 -100.8(2) . . . . ? C7 P3 Pd1 Br1 -70.79(17) . . . . ? C8 P3 Pd1 Br1 46.1(2) . . . . ? C6 P3 Pd1 Br1 170.83(15) . . . . ? C7 P3 Pd1 Pd2 75.39(17) . . . . ? C8 P3 Pd1 Pd2 -167.7(2) . . . . ? C6 P3 Pd1 Pd2 -42.98(15) . . . . ? O1 S1 Pd2 P4 -143.05(16) . . . . ? Pd1 S1 Pd2 P4 99.30(4) . . . . ? O1 S1 Pd2 P2 34.15(16) . . . . ? Pd1 S1 Pd2 P2 -83.50(4) . . . . ? O1 S1 Pd2 Br2 -101.7(9) . . . . ? Pd1 S1 Pd2 Br2 140.7(8) . . . . ? O1 S1 Pd2 Pd1 117.66(16) . . . . ? C9 P4 Pd2 S1 -164.4(2) . . . . ? C10 P4 Pd2 S1 75.2(2) . . . . ? C6 P4 Pd2 S1 -42.41(15) . . . . ? C9 P4 Pd2 P2 159.8(5) . . . . ? C10 P4 Pd2 P2 39.5(5) . . . . ? C6 P4 Pd2 P2 -78.2(5) . . . . ? C9 P4 Pd2 Br2 16.9(2) . . . . ? C10 P4 Pd2 Br2 -103.4(2) . . . . ? C6 P4 Pd2 Br2 138.96(15) . . . . ? C9 P4 Pd2 Pd1 -119.9(2) . . . . ? C10 P4 Pd2 Pd1 119.8(2) . . . . ? C6 P4 Pd2 Pd1 2.14(15) . . . . ? C5 P2 Pd2 S1 -94.7(2) . . . . ? C4 P2 Pd2 S1 147.0(3) . . . . ? C1 P2 Pd2 S1 21.55(17) . . . . ? C5 P2 Pd2 P4 -59.1(5) . . . . ? C4 P2 Pd2 P4 -177.4(5) . . . . ? C1 P2 Pd2 P4 57.2(5) . . . . ? C5 P2 Pd2 Br2 83.9(2) . . . . ? C4 P2 Pd2 Br2 -34.5(3) . . . . ? C1 P2 Pd2 Br2 -159.89(17) . . . . ? C5 P2 Pd2 Pd1 -139.7(2) . . . . ? C4 P2 Pd2 Pd1 102.0(3) . . . . ? C1 P2 Pd2 Pd1 -23.42(17) . . . . ? P1 Pd1 Pd2 S1 -93.31(5) . . . . ? P3 Pd1 Pd2 S1 99.27(5) . . . . ? Br1 Pd1 Pd2 S1 173.09(5) . . . . ? S1 Pd1 Pd2 P4 -79.55(5) . . . . ? P1 Pd1 Pd2 P4 -172.87(4) . . . . ? P3 Pd1 Pd2 P4 19.72(4) . . . . ? Br1 Pd1 Pd2 P4 93.53(4) . . . . ? S1 Pd1 Pd2 P2 95.71(5) . . . . ? P1 Pd1 Pd2 P2 2.40(4) . . . . ? P3 Pd1 Pd2 P2 -165.02(4) . . . . ? Br1 Pd1 Pd2 P2 -91.20(4) . . . . ? S1 Pd1 Pd2 Br2 -178.10(5) . . . . ? P1 Pd1 Pd2 Br2 88.59(4) . . . . ? P3 Pd1 Pd2 Br2 -78.83(4) . . . . ? Br1 Pd1 Pd2 Br2 -5.01(4) . . . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 1.008 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.137