# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1882 data_shel _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C29 H30 P2 Pd S2' _chemical_formula_weight 610.99 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.354(2) _cell_length_b 25.041(5) _cell_length_c 11.332(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.87(3) _cell_angle_gamma 90.00 _cell_volume 2796.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method ? _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.944 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5285 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.01 _reflns_number_total 5010 _reflns_number_observed 4188 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.2006P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5010 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_obs 0.0357 _refine_ls_wR_factor_all 0.1024 _refine_ls_wR_factor_obs 0.1006 _refine_ls_goodness_of_fit_all 1.056 _refine_ls_goodness_of_fit_obs 1.143 _refine_ls_restrained_S_all 1.056 _refine_ls_restrained_S_obs 1.143 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd Pd 0.19697(2) 0.824354(10) 0.32171(2) 0.03812(10) Uani 1 d . . S1 S 0.06119(10) 0.75293(4) 0.22883(10) 0.0570(3) Uani 1 d . . S2 S 0.01016(12) 0.86421(5) 0.35534(14) 0.0786(4) Uani 1 d . . P1 P 0.37828(8) 0.78553(3) 0.28172(8) 0.0379(2) Uani 1 d . . P2 P 0.31826(9) 0.90005(3) 0.39331(8) 0.0424(2) Uani 1 d . . C01 C -0.1089(4) 0.7761(2) 0.2225(6) 0.090(2) Uani 1 d . . C02 C -0.1066(7) 0.8055(4) 0.3298(8) 0.088(2) Uani 0.70 d P . C1 C 0.5430(3) 0.79977(14) 0.3955(3) 0.0472(8) Uani 1 d . . H1A H 0.5437(3) 0.78461(14) 0.4745(3) 0.057 Uiso 1 calc R . H1B H 0.6127(3) 0.78168(14) 0.3697(3) 0.057 Uiso 1 calc R . C2 C 0.5807(3) 0.85885(14) 0.4151(4) 0.0543(9) Uani 1 d . . H2A H 0.5690(3) 0.87527(14) 0.3350(4) 0.065 Uiso 1 calc R . H2B H 0.6758(3) 0.86168(14) 0.4627(4) 0.065 Uiso 1 calc R . C3 C 0.4965(4) 0.89003(15) 0.4822(3) 0.0545(9) Uani 1 d . . H3A H 0.5382(4) 0.92474(15) 0.5054(3) 0.065 Uiso 1 calc R . H3B H 0.5005(4) 0.87125(15) 0.5581(3) 0.065 Uiso 1 calc R . C11 C 0.3833(3) 0.71288(14) 0.2789(3) 0.0463(8) Uani 1 d . . C12 C 0.4118(5) 0.6845(2) 0.1851(4) 0.0692(12) Uani 1 d . . H12A H 0.4262(5) 0.7024(2) 0.1183(4) 0.083 Uiso 1 calc R . C13 C 0.4188(6) 0.6291(2) 0.1910(5) 0.091(2) Uani 1 d . . H13A H 0.4364(6) 0.6102(2) 0.1269(5) 0.109 Uiso 1 calc R . C14 C 0.4006(6) 0.6023(2) 0.2878(5) 0.090(2) Uani 1 d . . H14A H 0.4052(6) 0.5652(2) 0.2901(5) 0.108 Uiso 1 calc R . C15 C 0.3755(6) 0.6300(2) 0.3826(6) 0.092(2) Uani 1 d . . H15A H 0.3650(6) 0.6119(2) 0.4507(6) 0.111 Uiso 1 calc R . C16 C 0.3659(6) 0.6853(2) 0.3760(5) 0.0795(15) Uani 1 d . . H16A H 0.3470(6) 0.7039(2) 0.4399(5) 0.095 Uiso 1 calc R . C21 C 0.3922(3) 0.80712(14) 0.1327(3) 0.0422(7) Uani 1 d . . C22 C 0.5157(4) 0.8121(2) 0.1104(4) 0.0742(13) Uani 1 d . . H22A H 0.5952(4) 0.8038(2) 0.1729(4) 0.089 Uiso 1 calc R . C23 C 0.5226(6) 0.8291(2) -0.0033(5) 0.087(2) Uani 1 d . . H23A H 0.6062(6) 0.8326(2) -0.0171(5) 0.104 Uiso 1 calc R . C24 C 0.4064(6) 0.8409(2) -0.0947(4) 0.0798(14) Uani 1 d . . H24A H 0.4107(6) 0.8528(2) -0.1712(4) 0.096 Uiso 1 calc R . C25 C 0.2829(5) 0.8353(2) -0.0752(4) 0.0679(12) Uani 1 d . . H25A H 0.2037(5) 0.8423(2) -0.1392(4) 0.081 Uiso 1 calc R . C26 C 0.2760(4) 0.81925(14) 0.0388(3) 0.0509(9) Uani 1 d . . H26A H 0.1921(4) 0.81663(14) 0.0525(3) 0.061 Uiso 1 calc R . C31 C 0.2603(4) 0.94165(13) 0.4996(3) 0.0454(8) Uani 1 d . . C32 C 0.2535(5) 0.9196(2) 0.6079(4) 0.0743(14) Uani 1 d . . H32A H 0.2757(5) 0.8838(2) 0.6243(4) 0.089 Uiso 1 calc R . C33 C 0.2138(6) 0.9498(2) 0.6943(4) 0.0765(14) Uani 1 d . . H33A H 0.2135(6) 0.9346(2) 0.7691(4) 0.092 Uiso 1 calc R . C34 C 0.1757(4) 1.0014(2) 0.6687(4) 0.0587(10) Uani 1 d . . H34A H 0.1473(4) 1.0215(2) 0.7252(4) 0.070 Uiso 1 calc R . C35 C 0.1791(4) 1.0236(2) 0.5602(4) 0.0616(10) Uani 1 d . . H35A H 0.1531(4) 1.0590(2) 0.5427(4) 0.074 Uiso 1 calc R . C36 C 0.2207(4) 0.99403(14) 0.4760(3) 0.0528(9) Uani 1 d . . H36A H 0.2220(4) 1.00972(14) 0.4020(3) 0.063 Uiso 1 calc R . C41 C 0.3158(4) 0.94337(14) 0.2631(3) 0.0470(8) Uani 1 d . . C41 C 0.4220(5) 0.9775(2) 0.2644(4) 0.0690(12) Uani 1 d . . H41A H 0.4971(5) 0.9799(2) 0.3349(4) 0.083 Uiso 1 calc R . C43 C 0.4161(6) 1.0079(2) 0.1610(6) 0.090(2) Uani 1 d . . H43A H 0.4881(6) 1.0303(2) 0.1622(6) 0.107 Uiso 1 calc R . C44 C 0.3064(6) 1.0053(2) 0.0575(5) 0.0831(15) Uani 1 d . . H44A H 0.3041(6) 1.0256(2) -0.0118(5) 0.100 Uiso 1 calc R . C45 C 0.2002(6) 0.9731(2) 0.0554(4) 0.0808(15) Uani 1 d . . H45A H 0.1241(6) 0.9718(2) -0.0144(4) 0.097 Uiso 1 calc R . C46 C 0.2064(4) 0.9420(2) 0.1590(4) 0.0624(11) Uani 1 d . . H46A H 0.1339(4) 0.9197(2) 0.1570(4) 0.075 Uiso 1 calc R . C02' C -0.1295(11) 0.8365(5) 0.2296(16) 0.060(4) Uani 0.30 d P . 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 Pd 0.0333(2) 0.0378(2) 0.0454(2) -0.00526(10) 0.01530(11) -0.00018(10) S1 0.0484(5) 0.0570(6) 0.0710(6) -0.0183(5) 0.0264(5) -0.0157(4) S2 0.0498(6) 0.0804(8) 0.1151(10) -0.0339(7) 0.0393(6) 0.0023(5) P1 0.0318(4) 0.0380(4) 0.0440(5) -0.0012(3) 0.0119(3) 0.0021(3) P2 0.0421(5) 0.0375(5) 0.0449(5) -0.0050(4) 0.0095(4) 0.0006(4) C01 0.039(2) 0.089(4) 0.137(5) -0.015(3) 0.020(3) -0.004(2) C02 0.048(4) 0.128(7) 0.101(6) -0.034(5) 0.039(4) -0.015(4) C1 0.033(2) 0.049(2) 0.053(2) 0.002(2) 0.0030(15) 0.0063(15) C2 0.031(2) 0.050(2) 0.072(2) -0.008(2) 0.001(2) -0.003(2) C3 0.047(2) 0.049(2) 0.055(2) -0.010(2) -0.002(2) -0.002(2) C11 0.039(2) 0.039(2) 0.059(2) -0.003(2) 0.012(2) 0.0032(14) C12 0.088(3) 0.056(3) 0.054(2) -0.011(2) 0.009(2) 0.015(2) C13 0.122(5) 0.056(3) 0.071(3) -0.021(2) -0.005(3) 0.022(3) C14 0.103(4) 0.043(2) 0.100(4) -0.008(3) -0.004(3) 0.002(3) C15 0.118(5) 0.047(3) 0.125(5) 0.016(3) 0.056(4) 0.000(3) C16 0.109(4) 0.048(2) 0.102(4) 0.005(2) 0.062(3) 0.009(2) C21 0.038(2) 0.042(2) 0.048(2) -0.0016(14) 0.0141(15) 0.0012(14) C22 0.042(2) 0.125(4) 0.058(3) 0.004(3) 0.018(2) 0.004(2) C23 0.066(3) 0.134(5) 0.073(3) 0.006(3) 0.039(3) -0.007(3) C24 0.101(4) 0.088(3) 0.059(3) 0.016(2) 0.038(3) 0.009(3) C25 0.078(3) 0.065(3) 0.057(3) 0.013(2) 0.014(2) 0.014(2) C26 0.046(2) 0.053(2) 0.053(2) 0.003(2) 0.014(2) 0.007(2) C31 0.052(2) 0.037(2) 0.046(2) -0.0079(14) 0.013(2) -0.0038(15) C32 0.130(4) 0.041(2) 0.061(3) 0.006(2) 0.043(3) 0.013(2) C33 0.123(4) 0.063(3) 0.054(2) 0.003(2) 0.043(3) 0.007(3) C34 0.069(3) 0.051(2) 0.059(2) -0.009(2) 0.023(2) 0.004(2) C35 0.072(3) 0.049(2) 0.065(3) -0.001(2) 0.022(2) 0.017(2) C36 0.065(2) 0.044(2) 0.049(2) 0.004(2) 0.016(2) 0.011(2) C41 0.051(2) 0.041(2) 0.050(2) -0.003(2) 0.017(2) 0.001(2) C41 0.062(3) 0.069(3) 0.074(3) 0.005(2) 0.018(2) -0.010(2) C43 0.087(4) 0.078(3) 0.111(4) 0.025(3) 0.042(3) -0.008(3) C44 0.111(4) 0.077(3) 0.068(3) 0.015(3) 0.037(3) 0.010(3) C45 0.109(4) 0.069(3) 0.053(3) 0.005(2) 0.007(3) 0.003(3) C46 0.067(3) 0.058(2) 0.054(2) 0.001(2) 0.006(2) -0.009(2) C02' 0.018(5) 0.051(7) 0.101(11) -0.021(7) 0.004(6) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are 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 Pd P1 2.2797(9) . ? Pd P2 2.2810(10) . ? Pd S2 2.3096(11) . ? Pd S1 2.3184(11) . ? S1 C01 1.834(5) . ? S2 C02' 1.827(13) . ? S2 C02 1.868(8) . ? P1 C11 1.820(4) . ? P1 C21 1.821(4) . ? P1 C1 1.830(3) . ? P2 C41 1.825(4) . ? P2 C31 1.828(3) . ? P2 C3 1.828(4) . ? C01 C02 1.417(9) . ? C01 C02' 1.533(14) . ? C02 C02' 1.33(2) . ? C1 C2 1.529(5) . ? C2 C3 1.535(5) . ? C11 C16 1.358(6) . ? C11 C12 1.384(5) . ? C12 C13 1.389(6) . ? C13 C14 1.347(8) . ? C14 C15 1.369(7) . ? C15 C16 1.388(6) . ? C21 C26 1.374(5) . ? C21 C22 1.382(5) . ? C22 C23 1.379(6) . ? C23 C24 1.357(7) . ? C24 C25 1.369(7) . ? C25 C26 1.376(5) . ? C31 C32 1.367(5) . ? C31 C36 1.376(5) . ? C32 C33 1.394(6) . ? C33 C34 1.356(6) . ? C34 C35 1.360(6) . ? C35 C36 1.377(5) . ? C41 C46 1.363(5) . ? C41 C41 1.388(6) . ? C41 C43 1.383(7) . ? C43 C44 1.361(7) . ? C44 C45 1.359(7) . ? C45 C46 1.393(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd P2 91.60(3) . . ? P1 Pd S2 178.12(4) . . ? P2 Pd S2 88.84(4) . . ? P1 Pd S1 90.14(4) . . ? P2 Pd S1 173.48(4) . . ? S2 Pd S1 89.22(4) . . ? C01 S1 Pd 102.4(2) . . ? C02' S2 C02 42.3(5) . . ? C02' S2 Pd 102.1(4) . . ? C02 S2 Pd 99.8(2) . . ? C11 P1 C21 105.6(2) . . ? C11 P1 C1 100.5(2) . . ? C21 P1 C1 105.9(2) . . ? C11 P1 Pd 117.35(12) . . ? C21 P1 Pd 111.25(11) . . ? C1 P1 Pd 115.03(12) . . ? C41 P2 C31 105.5(2) . . ? C41 P2 C3 106.8(2) . . ? C31 P2 C3 101.3(2) . . ? C41 P2 Pd 109.68(12) . . ? C31 P2 Pd 116.85(12) . . ? C3 P2 Pd 115.75(12) . . ? C02 C01 C02' 53.6(7) . . ? C02 C01 S1 111.6(4) . . ? C02' C01 S1 117.2(5) . . ? C02' C02 C01 67.7(7) . . ? C02' C02 S2 67.2(7) . . ? C01 C02 S2 112.5(5) . . ? C2 C1 P1 115.6(2) . . ? C1 C2 C3 114.0(3) . . ? C2 C3 P2 115.3(2) . . ? C16 C11 C12 118.3(4) . . ? C16 C11 P1 118.9(3) . . ? C12 C11 P1 122.7(3) . . ? C11 C12 C13 119.7(5) . . ? C14 C13 C12 121.2(5) . . ? C13 C14 C15 119.7(5) . . ? C14 C15 C16 119.4(5) . . ? C11 C16 C15 121.7(5) . . ? C26 C21 C22 118.6(4) . . ? C26 C21 P1 118.9(3) . . ? C22 C21 P1 122.5(3) . . ? C23 C22 C21 120.9(4) . . ? C24 C23 C22 119.5(5) . . ? C23 C24 C25 120.5(4) . . ? C24 C25 C26 120.1(4) . . ? C21 C26 C25 120.4(4) . . ? C32 C31 C36 117.7(3) . . ? C32 C31 P2 118.6(3) . . ? C36 C31 P2 123.6(3) . . ? C31 C32 C33 121.2(4) . . ? C34 C33 C32 119.7(4) . . ? C33 C34 C35 119.8(4) . . ? C34 C35 C36 120.5(4) . . ? C31 C36 C35 121.0(4) . . ? C46 C41 C41 118.0(4) . . ? C46 C41 P2 119.1(3) . . ? C41 C41 P2 122.9(3) . . ? C43 C41 C41 120.1(5) . . ? C44 C43 C41 120.8(5) . . ? C45 C44 C43 120.0(5) . . ? C44 C45 C46 119.3(5) . . ? C41 C46 C45 121.8(4) . . ? C02 C02' C01 58.7(7) . . ? C02 C02' S2 70.5(7) . . ? C01 C02' S2 109.1(8) . . ? _refine_diff_density_max 0.823 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.078 data_pd3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C31 H35 Cl0 O4.50 P2 Pd2 S4' _chemical_formula_weight 882.57 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, z+1/2' '-x+1/2, y+1, z+1/2' _cell_length_a 15.905(3) _cell_length_b 22.848(5) _cell_length_c 18.904(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6869.7(25) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method ? _exptl_crystal_F_000 3544 _exptl_absorpt_coefficient_mu 1.420 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13643 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5790 _reflns_number_observed 5029 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0005P)^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 ? _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 0.98(3) _refine_ls_number_reflns 5790 _refine_ls_number_parameters 393 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_obs 0.0469 _refine_ls_wR_factor_all 0.0827 _refine_ls_wR_factor_obs 0.0795 _refine_ls_goodness_of_fit_all 1.362 _refine_ls_goodness_of_fit_obs 1.414 _refine_ls_restrained_S_all 1.362 _refine_ls_restrained_S_obs 1.414 _refine_ls_shift/esd_max -0.010 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.22735(3) 0.19622(2) 0.14704(3) 0.03026(13) Uani 1 d . . Pd2 Pd 0.40276(3) 0.18199(2) 0.20711(3) 0.03332(13) Uani 1 d . . S1 S 0.34485(10) 0.26012(7) 0.14148(11) 0.0392(4) Uani 1 d . . S2 S 0.27289(13) 0.19450(8) 0.26701(9) 0.0345(4) Uani 1 d . . S3 S 0.51800(12) 0.16889(8) 0.13766(12) 0.0446(5) Uani 1 d . . S4 S 0.44996(12) 0.10684(8) 0.27447(10) 0.0406(5) Uani 1 d . . P1 P 0.11637(11) 0.13367(8) 0.16027(10) 0.0332(5) Uani 1 d . . P2 P 0.20663(13) 0.19641(8) 0.02745(10) 0.0347(5) Uani 1 d . . O1 O 0.5894(3) 0.2034(2) 0.1599(4) 0.066(2) Uani 1 d . . O2 O 0.5023(4) 0.1700(3) 0.0621(3) 0.066(2) Uani 1 d . . O3 O 0.4688(4) 0.1227(3) 0.3478(3) 0.065(2) Uani 1 d . . O4 O 0.3979(4) 0.0547(2) 0.2664(4) 0.063(2) Uani 1 d . . C1 C 0.3119(6) 0.3063(3) 0.2151(5) 0.058(2) Uani 1 d . . H1A H 0.2684(6) 0.3321(3) 0.1990(5) 0.080 Uiso 1 d R . H1B H 0.3589(6) 0.3299(3) 0.2292(5) 0.080 Uiso 1 d R . C2 C 0.2794(5) 0.2731(4) 0.2789(5) 0.057(2) Uani 1 d . . H2A H 0.3162(5) 0.2808(4) 0.3180(5) 0.080 Uiso 1 d R . H2B H 0.2248(5) 0.2879(4) 0.2912(5) 0.080 Uiso 1 d R . C3 C 0.5461(5) 0.0945(3) 0.1573(5) 0.060(2) Uani 1 d . . H3A H 0.5989(5) 0.0850(3) 0.1356(5) 0.080 Uiso 1 d R . H3B H 0.5040(5) 0.0685(3) 0.1390(5) 0.080 Uiso 1 d R . C4 C 0.5512(5) 0.0870(4) 0.2360(5) 0.057(2) Uani 1 d . . H4A H 0.5653(5) 0.0474(4) 0.2481(5) 0.080 Uiso 1 d R . H4B H 0.5942(5) 0.1123(4) 0.2542(5) 0.080 Uiso 1 d R . C5 C 0.0272(4) 0.1465(3) 0.1015(4) 0.042(2) Uani 1 d . . H5A H 0.0019(4) 0.1831(3) 0.1149(4) 0.080 Uiso 1 d R . H5B H -0.0135(4) 0.1164(3) 0.1103(4) 0.080 Uiso 1 d R . C6 C 0.0437(5) 0.1482(3) 0.0226(4) 0.047(2) Uani 1 d . . H6A H -0.0092(5) 0.1502(3) -0.0018(4) 0.080 Uiso 1 d R . H6B H 0.0707(5) 0.1125(3) 0.0088(4) 0.080 Uiso 1 d R . C7 C 0.0978(5) 0.1998(3) -0.0029(4) 0.040(2) Uani 1 d . . H7A H 0.0971(5) 0.2017(3) -0.0536(4) 0.080 Uiso 1 d R . H7B H 0.0733(5) 0.2354(3) 0.0147(4) 0.080 Uiso 1 d R . C11 C 0.1494(4) 0.0592(3) 0.1474(5) 0.036(2) Uani 1 d . . C12 C 0.2174(5) 0.0390(4) 0.1860(4) 0.054(2) Uani 1 d . . H12A H 0.2458(5) 0.0651(4) 0.2177(4) 0.080 Uiso 1 d R . C13 C 0.2467(6) -0.0175(4) 0.1763(5) 0.066(3) Uani 1 d . . H13A H 0.2909(6) -0.0319(4) 0.2062(5) 0.080 Uiso 1 d R . C14 C 0.2120(7) -0.0529(4) 0.1253(5) 0.075(3) Uani 1 d . . H14A H 0.2323(7) -0.0922(4) 0.1193(5) 0.080 Uiso 1 d R . C15 C 0.1467(6) -0.0330(4) 0.0851(5) 0.062(2) Uani 1 d . . H15A H 0.1252(6) -0.0563(4) 0.0470(5) 0.080 Uiso 1 d R . C16 C 0.1141(5) 0.0221(3) 0.0971(4) 0.047(2) Uani 1 d . . H16A H 0.0654(5) 0.0350(3) 0.0714(4) 0.080 Uiso 1 d R . C21 C 0.0656(5) 0.1354(3) 0.2454(4) 0.039(2) Uani 1 d . . C22 C 0.0462(5) 0.1884(4) 0.2770(4) 0.054(2) Uani 1 d . . H22A H 0.0660(5) 0.2234(4) 0.2544(4) 0.080 Uiso 1 d R . C23 C 0.0023(6) 0.1916(5) 0.3396(5) 0.072(3) Uani 1 d . . H23A H -0.0106(6) 0.2295(5) 0.3587(5) 0.080 Uiso 1 d R . C24 C -0.0224(7) 0.1424(7) 0.3720(5) 0.093(4) Uani 1 d . . H24A H -0.0542(7) 0.1458(7) 0.4150(5) 0.080 Uiso 1 d R . C25 C -0.0041(9) 0.0898(6) 0.3426(7) 0.120(6) Uani 1 d . . H25A H -0.0180(9) 0.0561(6) 0.3706(7) 0.080 Uiso 1 d R . C26 C 0.0385(6) 0.0861(4) 0.2794(6) 0.082(3) Uani 1 d . . H26A H 0.0463(6) 0.0482(4) 0.2583(6) 0.080 Uiso 1 d R . C31 C 0.2522(5) 0.1307(3) -0.0110(4) 0.040(2) Uani 1 d . . C32 C 0.3187(6) 0.1037(4) 0.0235(5) 0.066(3) Uani 1 d . . H32A H 0.3401(6) 0.1209(4) 0.0662(5) 0.080 Uiso 1 d R . C33 C 0.3519(7) 0.0523(4) -0.0018(6) 0.085(4) Uani 1 d . . H33A H 0.3968(7) 0.0333(4) 0.0231(6) 0.080 Uiso 1 d R . C34 C 0.3206(7) 0.0289(4) -0.0632(6) 0.077(3) Uani 1 d . . H34A H 0.3463(7) -0.0056(4) -0.0825(6) 0.080 Uiso 1 d R . C35 C 0.2559(7) 0.0540(4) -0.0978(6) 0.067(2) Uani 1 d . . H35A H 0.2335(7) 0.0368(4) -0.1401(6) 0.080 Uiso 1 d R . C36 C 0.2213(6) 0.1050(3) -0.0716(4) 0.056(2) Uani 1 d . . H36A H 0.1748(6) 0.1234(3) -0.0953(4) 0.080 Uiso 1 d R . C41 C 0.2537(5) 0.2590(3) -0.0169(4) 0.037(2) Uani 1 d . . C42 C 0.3273(5) 0.2546(3) -0.0544(4) 0.049(2) Uani 1 d . . H42A H 0.3541(5) 0.2172(3) -0.0601(4) 0.080 Uiso 1 d R . C43 C 0.3631(6) 0.3053(4) -0.0835(4) 0.053(2) Uani 1 d . . H43A H 0.4150(6) 0.3030(4) -0.1092(4) 0.080 Uiso 1 d R . C44 C 0.3245(6) 0.3590(4) -0.0754(5) 0.060(3) Uani 1 d . . H44A H 0.3484(6) 0.3938(4) -0.0954(5) 0.080 Uiso 1 d R . C45 C 0.2506(6) 0.3630(3) -0.0380(5) 0.062(2) Uani 1 d . . H45A H 0.2217(6) 0.3998(3) -0.0341(5) 0.080 Uiso 1 d R . C46 C 0.2157(6) 0.3134(3) -0.0082(4) 0.053(2) Uani 1 d . . H46A H 0.1653(6) 0.3167(3) 0.0194(4) 0.080 Uiso 1 d R . O1N O 0.5000 0.0000 0.4324(6) 0.153(6) Uani 1 d S . 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 0.0239(3) 0.0343(3) 0.0326(3) 0.0028(3) -0.0005(3) -0.0016(2) Pd2 0.0260(3) 0.0379(3) 0.0361(3) 0.0007(3) 0.0009(3) 0.0003(3) S1 0.0331(10) 0.0407(10) 0.0437(10) 0.0085(10) -0.0036(11) -0.0089(8) S2 0.0283(11) 0.0433(11) 0.0320(9) 0.0019(8) 0.0021(10) 0.0026(9) S3 0.0338(12) 0.0498(10) 0.0501(12) -0.0004(10) 0.0088(11) -0.0019(9) S4 0.0319(12) 0.0446(11) 0.0453(11) 0.0050(9) 0.0016(10) 0.0046(9) P1 0.0266(10) 0.0335(10) 0.0396(11) 0.0013(9) 0.0012(9) -0.0006(8) P2 0.0336(12) 0.0377(11) 0.0328(10) 0.0036(8) -0.0002(9) 0.0017(9) O1 0.035(3) 0.072(4) 0.092(5) -0.007(3) 0.019(4) -0.016(3) O2 0.065(5) 0.088(4) 0.047(3) 0.000(3) 0.009(3) -0.004(4) O3 0.055(4) 0.100(5) 0.039(3) 0.001(3) -0.006(3) 0.007(4) O4 0.051(4) 0.039(3) 0.100(5) 0.015(3) 0.005(4) 0.000(3) C1 0.065(6) 0.036(4) 0.074(6) -0.002(5) 0.002(6) 0.004(4) C2 0.047(6) 0.055(5) 0.070(6) -0.013(5) 0.004(5) 0.000(4) C3 0.051(5) 0.053(5) 0.077(7) -0.011(5) 0.018(5) 0.015(4) C4 0.041(5) 0.064(6) 0.066(6) -0.004(4) -0.001(5) 0.021(4) C5 0.025(4) 0.050(5) 0.051(5) 0.000(4) -0.002(4) 0.000(4) C6 0.036(5) 0.053(5) 0.051(5) 0.003(4) -0.009(4) -0.006(4) C7 0.031(5) 0.050(4) 0.040(4) 0.005(3) -0.010(4) 0.006(4) C11 0.022(4) 0.034(4) 0.051(4) -0.001(4) 0.003(4) -0.003(3) C12 0.046(5) 0.057(5) 0.058(6) -0.005(4) -0.009(4) 0.000(4) C13 0.068(6) 0.051(5) 0.080(7) -0.004(5) -0.010(5) 0.031(5) C14 0.094(8) 0.032(5) 0.098(8) 0.001(5) 0.012(7) 0.013(5) C15 0.066(7) 0.051(5) 0.069(6) -0.006(5) 0.011(6) -0.014(5) C16 0.051(5) 0.035(4) 0.056(5) -0.002(4) 0.000(4) -0.003(4) C21 0.032(5) 0.033(4) 0.051(5) 0.012(4) 0.000(4) 0.002(3) C22 0.025(5) 0.083(7) 0.054(5) -0.011(5) 0.002(4) -0.001(4) C23 0.052(7) 0.112(9) 0.053(6) -0.032(6) 0.005(5) -0.003(6) C24 0.074(8) 0.162(13) 0.043(6) 0.020(7) 0.024(6) 0.012(9) C25 0.141(13) 0.098(10) 0.122(11) 0.043(8) 0.092(10) 0.017(9) C26 0.093(9) 0.068(7) 0.086(8) 0.005(6) 0.045(7) -0.002(6) C31 0.039(5) 0.040(4) 0.040(4) -0.001(4) 0.006(4) -0.002(4) C32 0.052(6) 0.079(7) 0.068(6) -0.032(5) -0.011(5) 0.014(5) C33 0.082(8) 0.081(7) 0.093(8) -0.024(6) -0.026(7) 0.043(6) C34 0.088(9) 0.057(6) 0.085(8) -0.017(5) 0.018(7) 0.021(6) C35 0.089(7) 0.059(5) 0.053(5) -0.020(5) 0.007(5) -0.006(7) C36 0.076(7) 0.050(5) 0.042(5) 0.003(4) -0.005(5) 0.013(5) C41 0.039(5) 0.044(4) 0.030(4) 0.003(3) 0.002(4) -0.004(4) C42 0.046(5) 0.050(5) 0.050(5) 0.003(4) 0.003(5) -0.008(4) C43 0.050(6) 0.057(5) 0.051(5) -0.003(4) 0.007(5) -0.013(5) C44 0.075(8) 0.058(6) 0.048(5) 0.010(4) -0.013(5) -0.026(5) C45 0.071(6) 0.047(4) 0.067(6) 0.007(5) -0.006(5) 0.001(5) C46 0.057(6) 0.040(5) 0.061(5) 0.014(4) 0.009(5) 0.004(4) O1N 0.227(15) 0.170(12) 0.061(7) 0.000 0.000 0.082(12) _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 P2 2.285(2) . ? Pd1 P1 2.285(2) . ? Pd1 S1 2.374(2) . ? Pd1 S2 2.381(2) . ? Pd1 Pd2 3.0297(9) . ? Pd2 S4 2.266(2) . ? Pd2 S3 2.274(2) . ? Pd2 S1 2.361(2) . ? Pd2 S2 2.373(2) . ? S1 C1 1.823(9) . ? S2 C2 1.813(8) . ? S3 O1 1.445(6) . ? S3 O2 1.451(6) . ? S3 C3 1.796(8) . ? S4 O4 1.458(6) . ? S4 O3 1.464(6) . ? S4 C4 1.825(8) . ? P1 C11 1.798(7) . ? P1 C21 1.800(8) . ? P1 C5 1.826(7) . ? P2 C31 1.818(7) . ? P2 C41 1.818(7) . ? P2 C7 1.825(7) . ? C1 C2 1.515(12) . ? C3 C4 1.500(12) . ? C5 C6 1.515(11) . ? C6 C7 1.536(10) . ? C11 C12 1.383(10) . ? C11 C16 1.392(11) . ? C12 C13 1.384(11) . ? C13 C14 1.374(12) . ? C14 C15 1.365(12) . ? C15 C16 1.380(11) . ? C21 C26 1.367(11) . ? C21 C22 1.386(10) . ? C22 C23 1.376(12) . ? C23 C24 1.339(14) . ? C24 C25 1.36(2) . ? C25 C26 1.377(14) . ? C31 C32 1.387(11) . ? C31 C36 1.379(10) . ? C32 C33 1.373(11) . ? C33 C34 1.372(14) . ? C34 C35 1.347(13) . ? C35 C36 1.381(12) . ? C41 C42 1.373(10) . ? C41 C46 1.391(10) . ? C42 C43 1.402(10) . ? C43 C44 1.380(11) . ? C44 C45 1.374(13) . ? C45 C46 1.382(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pd1 P1 89.89(7) . . ? P2 Pd1 S1 93.93(7) . . ? P1 Pd1 S1 176.13(8) . . ? P2 Pd1 S2 170.55(7) . . ? P1 Pd1 S2 96.92(7) . . ? S1 Pd1 S2 79.21(7) . . ? P2 Pd1 Pd2 120.26(6) . . ? P1 Pd1 Pd2 127.11(5) . . ? S1 Pd1 Pd2 50.03(5) . . ? S2 Pd1 Pd2 50.29(5) . . ? S4 Pd2 S3 87.57(7) . . ? S4 Pd2 S1 176.03(7) . . ? S3 Pd2 S1 96.35(7) . . ? S4 Pd2 S2 96.41(7) . . ? S3 Pd2 S2 173.14(8) . . ? S1 Pd2 S2 79.63(7) . . ? S4 Pd2 Pd1 126.66(6) . . ? S3 Pd2 Pd1 122.67(6) . . ? S1 Pd2 Pd1 50.41(4) . . ? S2 Pd2 Pd1 50.53(5) . . ? C1 S1 Pd2 98.5(3) . . ? C1 S1 Pd1 95.5(3) . . ? Pd2 S1 Pd1 79.56(6) . . ? C2 S2 Pd2 97.4(3) . . ? C2 S2 Pd1 96.8(3) . . ? Pd2 S2 Pd1 79.18(6) . . ? O1 S3 O2 114.3(4) . . ? O1 S3 C3 105.1(4) . . ? O2 S3 C3 105.3(4) . . ? O1 S3 Pd2 113.2(3) . . ? O2 S3 Pd2 115.3(3) . . ? C3 S3 Pd2 101.9(3) . . ? O4 S4 O3 114.7(4) . . ? O4 S4 C4 104.9(4) . . ? O3 S4 C4 105.0(4) . . ? O4 S4 Pd2 111.8(3) . . ? O3 S4 Pd2 114.3(3) . . ? C4 S4 Pd2 104.9(3) . . ? C11 P1 C21 105.9(4) . . ? C11 P1 C5 107.3(4) . . ? C21 P1 C5 101.0(4) . . ? C11 P1 Pd1 110.6(2) . . ? C21 P1 Pd1 115.5(3) . . ? C5 P1 Pd1 115.7(3) . . ? C31 P2 C41 107.5(3) . . ? C31 P2 C7 106.7(4) . . ? C41 P2 C7 102.3(3) . . ? C31 P2 Pd1 109.6(3) . . ? C41 P2 Pd1 113.5(2) . . ? C7 P2 Pd1 116.6(3) . . ? C2 C1 S1 114.6(5) . . ? C1 C2 S2 114.6(6) . . ? C4 C3 S3 109.1(6) . . ? C3 C4 S4 108.6(6) . . ? C6 C5 P1 117.9(6) . . ? C5 C6 C7 115.1(7) . . ? C6 C7 P2 113.6(5) . . ? C12 C11 C16 118.2(7) . . ? C12 C11 P1 118.2(6) . . ? C16 C11 P1 123.4(6) . . ? C11 C12 C13 120.3(8) . . ? C14 C13 C12 120.4(9) . . ? C15 C14 C13 119.9(8) . . ? C14 C15 C16 120.0(9) . . ? C15 C16 C11 121.0(8) . . ? C26 C21 C22 116.5(8) . . ? C26 C21 P1 122.9(7) . . ? C22 C21 P1 120.3(6) . . ? C21 C22 C23 122.0(9) . . ? C24 C23 C22 119.9(10) . . ? C23 C24 C25 119.6(11) . . ? C24 C25 C26 121.1(11) . . ? C21 C26 C25 120.9(10) . . ? C32 C31 C36 118.3(8) . . ? C32 C31 P2 118.9(6) . . ? C36 C31 P2 122.8(6) . . ? C33 C32 C31 120.6(9) . . ? C32 C33 C34 119.3(10) . . ? C35 C34 C33 121.4(9) . . ? C34 C35 C36 119.4(10) . . ? C35 C36 C31 120.9(9) . . ? C42 C41 C46 119.7(7) . . ? C42 C41 P2 122.2(6) . . ? C46 C41 P2 118.0(6) . . ? C41 C42 C43 119.2(7) . . ? C44 C43 C42 120.7(8) . . ? C45 C44 C43 119.8(8) . . ? C46 C45 C44 119.9(8) . . ? C45 C46 C41 120.7(8) . . ? _refine_diff_density_max 0.693 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.095 data_pd4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H38 O Pd6 S12' _chemical_formula_weight 1293.60 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 10.506(2) _cell_length_b 16.789(3) _cell_length_c 10.837(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.83(3) _cell_angle_gamma 90.00 _cell_volume 1883.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.281 _exptl_crystal_density_method ? _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 3.484 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8794 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0722 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3269 _reflns_number_observed 2352 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+9.6231P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3269 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_obs 0.0643 _refine_ls_wR_factor_all 0.1687 _refine_ls_wR_factor_obs 0.1512 _refine_ls_goodness_of_fit_all 1.134 _refine_ls_goodness_of_fit_obs 1.205 _refine_ls_restrained_S_all 1.134 _refine_ls_restrained_S_obs 1.205 _refine_ls_shift/esd_max 0.018 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.40600(9) 0.35153(6) -0.16182(9) 0.0352(3) Uani 1 d . . Pd2 Pd 0.25272(10) 0.42158(6) 0.03948(10) 0.0368(3) Uani 1 d . . Pd3 Pd 0.34357(9) 0.56856(5) 0.20259(9) 0.0348(3) Uani 1 d . . S1 S 0.3518(3) 0.2991(2) 0.0216(3) 0.0424(8) Uani 1 d . . S2 S 0.2016(3) 0.4086(2) -0.1773(3) 0.0426(8) Uani 1 d . . S3 S 0.6173(3) 0.3026(2) -0.1437(4) 0.0452(9) Uani 1 d . . S4 S 0.1549(3) 0.5442(2) 0.0644(4) 0.0437(9) Uani 1 d . . S5 S 0.3099(4) 0.4374(2) 0.2552(3) 0.0437(9) Uani 1 d . . S6 S 0.4663(3) 0.4076(2) -0.3401(3) 0.0423(8) Uani 1 d . . C1 C 0.2157(16) 0.2339(8) -0.0327(14) 0.055(4) Uani 1 d . . H1A H 0.2453(16) 0.1792(8) -0.0231(14) 0.067 Uiso 1 calc R . H1B H 0.1517(16) 0.2414(8) 0.0211(14) 0.067 Uiso 1 calc R . C2 C 0.1504(18) 0.2462(10) -0.1676(17) 0.075(5) Uani 1 d . . H2A H 0.2143(18) 0.2372(10) -0.2210(17) 0.090 Uiso 1 calc R . H2B H 0.0845(18) 0.2056(10) -0.1878(17) 0.090 Uiso 1 calc R . C3 C 0.0901(14) 0.3239(8) -0.2003(14) 0.052(4) Uani 1 d . . H3A H 0.0232(14) 0.3323(8) -0.1501(14) 0.062 Uiso 1 calc R . H3B H 0.0488(14) 0.3227(8) -0.2874(14) 0.062 Uiso 1 calc R . C4 C 0.6860(16) 0.2870(10) 0.0180(16) 0.068(5) Uani 1 d . . H4A H 0.6328(16) 0.3154(10) 0.0682(16) 0.081 Uiso 1 calc R . H4B H 0.6780(16) 0.2307(10) 0.0357(16) 0.081 Uiso 1 calc R . C5 C 0.8210(20) 0.3099(11) 0.0631(21) 0.098(7) Uani 1 d . . H5A H 0.8732(20) 0.2861(11) 0.0071(21) 0.118 Uiso 1 calc R . H5B H 0.8473(20) 0.2855(11) 0.1446(21) 0.118 Uiso 1 calc R . C6 C 0.8555(15) 0.3958(8) 0.0754(14) 0.057(4) Uani 1 d . . H6A H 0.9436(15) 0.3993(8) 0.1202(14) 0.069 Uiso 1 calc R . H6B H 0.8005(15) 0.4201(8) 0.1282(14) 0.069 Uiso 1 calc R . C7 C 0.4630(14) 0.3883(7) 0.3100(13) 0.044(3) Uani 1 d . . H7A H 0.4690(14) 0.3782(7) 0.3989(13) 0.053 Uiso 1 calc R . H7B H 0.4614(14) 0.3370(7) 0.2687(13) 0.053 Uiso 1 calc R . C8 C 0.5840(15) 0.4310(8) 0.2908(14) 0.053(4) Uani 1 d . . H8A H 0.5721(15) 0.4502(8) 0.2051(14) 0.063 Uiso 1 calc R . H8B H 0.6545(15) 0.3929(8) 0.3011(14) 0.063 Uiso 1 calc R . C9 C 0.3770(14) 0.4992(8) -0.3781(13) 0.053(4) Uani 1 d . . H9A H 0.3865(14) 0.5150(8) -0.4621(13) 0.064 Uiso 1 calc R . H9B H 0.2861(14) 0.4883(8) -0.3792(13) 0.064 Uiso 1 calc R . O O 0.0000 0.5000 -0.5000 0.150(10) Uiso 1 d S . 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 0.0412(6) 0.0309(5) 0.0326(6) 0.0000(4) 0.0039(4) -0.0015(4) Pd2 0.0436(6) 0.0284(5) 0.0384(6) -0.0027(4) 0.0067(5) -0.0009(4) Pd3 0.0390(6) 0.0295(5) 0.0364(6) -0.0045(4) 0.0075(4) -0.0017(4) S1 0.057(2) 0.030(2) 0.040(2) 0.0034(15) 0.010(2) 0.003(2) S2 0.047(2) 0.041(2) 0.038(2) 0.001(2) 0.001(2) 0.005(2) S3 0.048(2) 0.027(2) 0.059(2) -0.003(2) 0.007(2) 0.0005(15) S4 0.037(2) 0.036(2) 0.058(2) -0.010(2) 0.009(2) -0.0021(15) S5 0.061(2) 0.033(2) 0.040(2) -0.0027(15) 0.018(2) -0.006(2) S6 0.051(2) 0.041(2) 0.032(2) -0.0039(15) 0.002(2) -0.007(2) C1 0.086(12) 0.040(8) 0.046(9) -0.006(7) 0.030(9) -0.018(8) C2 0.083(13) 0.073(12) 0.068(12) -0.007(10) 0.010(10) -0.024(10) C3 0.050(9) 0.058(10) 0.044(9) 0.000(7) -0.001(7) -0.011(7) C4 0.062(10) 0.053(10) 0.080(13) 0.026(9) -0.010(9) -0.009(8) C5 0.106(16) 0.076(13) 0.100(17) 0.027(12) -0.023(13) -0.028(12) C6 0.060(10) 0.043(8) 0.059(10) 0.009(7) -0.018(8) 0.002(7) C7 0.068(10) 0.027(7) 0.035(8) 0.011(6) 0.003(7) 0.000(7) C8 0.069(10) 0.041(8) 0.049(9) 0.008(7) 0.010(8) 0.020(7) C9 0.052(9) 0.064(10) 0.040(8) 0.016(8) -0.003(7) -0.015(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S1 2.332(4) . ? Pd1 S2 2.331(4) . ? Pd1 S6 2.332(4) . ? Pd1 S3 2.344(4) . ? Pd1 Pd3 3.0519(15) 3_665 ? Pd1 Pd2 3.152(2) . ? Pd2 S1 2.327(3) . ? Pd2 S5 2.327(4) . ? Pd2 S2 2.329(4) . ? Pd2 S4 2.338(3) . ? Pd2 Pd3 3.0902(14) . ? Pd3 S4 2.307(4) . ? Pd3 S3 2.312(3) 3_665 ? Pd3 S6 2.315(4) 3_665 ? Pd3 S5 2.316(3) . ? Pd3 Pd1 3.0519(15) 3_665 ? S1 C1 1.817(15) . ? S2 C3 1.831(14) . ? S3 C4 1.80(2) . ? S3 Pd3 2.312(3) 3_665 ? S4 C6 1.808(15) 3_665 ? S5 C7 1.815(14) . ? S6 C9 1.812(15) . ? S6 Pd3 2.315(4) 3_665 ? C1 C2 1.52(2) . ? C2 C3 1.47(2) . ? C4 C5 1.47(2) . ? C5 C6 1.49(2) . ? C6 S4 1.808(15) 3_665 ? C7 C8 1.50(2) . ? C8 C9 1.52(2) 3_665 ? C9 C8 1.52(2) 3_665 ? 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 S1 Pd1 S2 81.98(13) . . ? S1 Pd1 S6 177.59(13) . . ? S2 Pd1 S6 98.73(13) . . ? S1 Pd1 S3 99.33(13) . . ? S2 Pd1 S3 176.24(13) . . ? S6 Pd1 S3 79.83(13) . . ? S1 Pd1 Pd3 129.15(10) . 3_665 ? S2 Pd1 Pd3 127.98(10) . 3_665 ? S6 Pd1 Pd3 48.70(9) . 3_665 ? S3 Pd1 Pd3 48.59(9) . 3_665 ? S1 Pd1 Pd2 47.37(9) . . ? S2 Pd1 Pd2 47.42(9) . . ? S6 Pd1 Pd2 131.77(10) . . ? S3 Pd1 Pd2 131.42(10) . . ? Pd3 Pd1 Pd2 119.42(4) 3_665 . ? S1 Pd2 S5 98.18(13) . . ? S1 Pd2 S2 82.11(12) . . ? S5 Pd2 S2 177.97(13) . . ? S1 Pd2 S4 178.16(14) . . ? S5 Pd2 S4 79.99(13) . . ? S2 Pd2 S4 99.73(13) . . ? S1 Pd2 Pd3 130.86(10) . . ? S5 Pd2 Pd3 48.12(8) . . ? S2 Pd2 Pd3 130.34(9) . . ? S4 Pd2 Pd3 47.88(9) . . ? S1 Pd2 Pd1 47.48(9) . . ? S5 Pd2 Pd1 131.53(10) . . ? S2 Pd2 Pd1 47.47(9) . . ? S4 Pd2 Pd1 134.05(10) . . ? Pd3 Pd2 Pd1 123.33(4) . . ? S4 Pd3 S3 99.22(13) . 3_665 ? S4 Pd3 S6 179.55(12) . 3_665 ? S3 Pd3 S6 80.85(13) 3_665 3_665 ? S4 Pd3 S5 80.86(13) . . ? S3 Pd3 S5 177.43(13) 3_665 . ? S6 Pd3 S5 99.05(13) 3_665 . ? S4 Pd3 Pd1 130.55(10) . 3_665 ? S3 Pd3 Pd1 49.49(9) 3_665 3_665 ? S6 Pd3 Pd1 49.19(9) 3_665 3_665 ? S5 Pd3 Pd1 128.67(10) . 3_665 ? S4 Pd3 Pd2 48.72(9) . . ? S3 Pd3 Pd2 129.91(10) 3_665 . ? S6 Pd3 Pd2 130.92(9) 3_665 . ? S5 Pd3 Pd2 48.43(9) . . ? Pd1 Pd3 Pd2 117.25(4) 3_665 . ? C1 S1 Pd2 102.7(5) . . ? C1 S1 Pd1 104.1(5) . . ? Pd2 S1 Pd1 85.14(11) . . ? C3 S2 Pd2 104.0(5) . . ? C3 S2 Pd1 104.5(5) . . ? Pd2 S2 Pd1 85.11(12) . . ? C4 S3 Pd3 110.2(5) . 3_665 ? C4 S3 Pd1 110.5(6) . . ? Pd3 S3 Pd1 81.92(11) 3_665 . ? C6 S4 Pd3 111.6(5) 3_665 . ? C6 S4 Pd2 111.0(5) 3_665 . ? Pd3 S4 Pd2 83.40(12) . . ? C7 S5 Pd3 110.4(4) . . ? C7 S5 Pd2 109.8(5) . . ? Pd3 S5 Pd2 83.45(12) . . ? C9 S6 Pd3 110.8(5) . 3_665 ? C9 S6 Pd1 109.1(5) . . ? Pd3 S6 Pd1 82.11(12) 3_665 . ? C2 C1 S1 115.5(10) . . ? C3 C2 C1 117.3(15) . . ? C2 C3 S2 114.7(11) . . ? C5 C4 S3 119.3(13) . . ? C4 C5 C6 119.4(17) . . ? C5 C6 S4 119.1(13) . 3_665 ? C8 C7 S5 117.4(9) . . ? C7 C8 C9 115.2(12) . 3_665 ? C8 C9 S6 116.1(10) 3_665 . ? _refine_diff_density_max 2.310 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.232 data_swp _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C57 H58 Cl2 P4 Pd2 S2' _chemical_formula_weight 1214.73 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 ? _symmetry_space_group_name_H-M ? 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 22.5683(7) _cell_length_b 11.6585(4) _cell_length_c 20.5798(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.9050(10) _cell_angle_gamma 90.00 _cell_volume 5363.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method ? _exptl_crystal_F_000 2472 _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10133 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0745 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.06 _reflns_number_total 4613 _reflns_number_observed 3276 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0005P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4613 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_obs 0.0478 _refine_ls_wR_factor_all 0.0759 _refine_ls_wR_factor_obs 0.0695 _refine_ls_goodness_of_fit_all 1.187 _refine_ls_goodness_of_fit_obs 1.306 _refine_ls_restrained_S_all 1.187 _refine_ls_restrained_S_obs 1.306 _refine_ls_shift/esd_max 0.035 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd Pd 0.930397(14) 0.21147(3) 0.76050(2) 0.03273(11) Uani 1 d . . S S 0.98074(5) 0.14623(11) 0.67484(5) 0.0396(3) Uani 1 d . . P1 P 0.84670(5) 0.25987(11) 0.68990(6) 0.0384(3) Uani 1 d . . P2 P 0.89222(5) 0.29952(10) 0.84509(6) 0.0359(3) Uani 1 d . . C1 C 0.9848(2) -0.0076(5) 0.6881(3) 0.082(2) Uani 1 d . . H1A H 1.0232(2) -0.0305(5) 0.6776(3) 0.080 Uiso 1 d R . H1B H 0.9555(2) -0.0418(5) 0.6556(3) 0.080 Uiso 1 d R . C2 C 0.9772(7) -0.0551(9) 0.7434(11) 0.089(8) Uani 0.50 d P . H2A H 0.9816(7) -0.1366(9) 0.7395(11) 0.080 Uiso 0.50 d PR . H2B H 1.0073(7) -0.0265(9) 0.7770(11) 0.080 Uiso 0.50 d PR . C01 C 0.7764(2) 0.2534(4) 0.7239(2) 0.0446(13) Uani 1 d . . H01A H 0.7684(2) 0.1743(4) 0.7321(2) 0.080 Uiso 1 d R . H01B H 0.7452(2) 0.2804(4) 0.6911(2) 0.080 Uiso 1 d R . C02 C 0.7725(2) 0.3182(4) 0.7883(2) 0.0468(13) Uani 1 d . . H02A H 0.7319(2) 0.3195(4) 0.7973(2) 0.080 Uiso 1 d R . H02B H 0.7846(2) 0.3959(4) 0.7821(2) 0.080 Uiso 1 d R . C03 C 0.8130(2) 0.2705(4) 0.8473(2) 0.0431(12) Uani 1 d . . H03A H 0.8017(2) 0.3023(4) 0.8869(2) 0.080 Uiso 1 d R . H03B H 0.8070(2) 0.1890(4) 0.8484(2) 0.080 Uiso 1 d R . C11 C 0.8318(2) 0.1587(5) 0.6221(2) 0.0447(12) Uani 1 d . . C12 C 0.8248(2) 0.0444(5) 0.6359(3) 0.060(2) Uani 1 d . . H12A H 0.8301(2) 0.0197(5) 0.6809(3) 0.080 Uiso 1 d R . C13 C 0.8119(2) -0.0337(5) 0.5854(3) 0.075(2) Uani 1 d . . H13A H 0.8051(2) -0.1125(5) 0.5956(3) 0.080 Uiso 1 d R . C14 C 0.8074(3) 0.0012(7) 0.5219(3) 0.088(2) Uani 1 d . . H14A H 0.7986(3) -0.0538(7) 0.4872(3) 0.080 Uiso 1 d R . C15 C 0.8150(3) 0.1116(7) 0.5075(3) 0.108(3) Uani 1 d . . H15A H 0.8129(3) 0.1349(7) 0.4625(3) 0.080 Uiso 1 d R . C16 C 0.8271(3) 0.1920(5) 0.5575(3) 0.082(2) Uani 1 d . . H16A H 0.8324(3) 0.2714(5) 0.5474(3) 0.080 Uiso 1 d R . C21 C 0.8525(2) 0.3981(4) 0.6527(2) 0.0413(12) Uani 1 d . . C22 C 0.9060(2) 0.4279(5) 0.6316(3) 0.079(2) Uani 1 d . . H22A H 0.9372(2) 0.3714(5) 0.6349(3) 0.080 Uiso 1 d R . C23 C 0.9140(3) 0.5331(5) 0.6041(3) 0.095(2) Uani 1 d . . H23A H 0.9525(3) 0.5533(5) 0.5926(3) 0.080 Uiso 1 d R . C24 C 0.8682(3) 0.6118(5) 0.5953(3) 0.082(2) Uani 1 d . . H24A H 0.8723(3) 0.6827(5) 0.5726(3) 0.080 Uiso 1 d R . C25 C 0.8162(3) 0.5863(5) 0.6169(3) 0.076(2) Uani 1 d . . H25A H 0.7849(3) 0.6425(5) 0.6135(3) 0.080 Uiso 1 d R . C26 C 0.8071(2) 0.4804(5) 0.6457(3) 0.0557(14) Uani 1 d . . H26A H 0.7697(2) 0.4629(5) 0.6605(3) 0.080 Uiso 1 d R . C31 C 0.8947(2) 0.4547(4) 0.8417(2) 0.0465(13) Uani 1 d . . C32 C 0.9252(2) 0.5088(5) 0.7969(3) 0.063(2) Uani 1 d . . H32A H 0.9485(2) 0.4644(5) 0.7704(3) 0.080 Uiso 1 d R . C33 C 0.9219(3) 0.6267(7) 0.7903(4) 0.099(2) Uani 1 d . . H33A H 0.9440(3) 0.6651(7) 0.7600(4) 0.080 Uiso 1 d R . C34 C 0.8892(4) 0.6914(6) 0.8262(4) 0.111(3) Uani 1 d . . H34A H 0.8843(4) 0.7725(6) 0.8192(4) 0.080 Uiso 1 d R . C35 C 0.8605(3) 0.6388(6) 0.8718(4) 0.097(3) Uani 1 d . . H35A H 0.8397(3) 0.6848(6) 0.9001(4) 0.080 Uiso 1 d R . C36 C 0.8620(2) 0.5220(5) 0.8801(3) 0.068(2) Uani 1 d . . H36A H 0.8405(2) 0.4856(5) 0.9116(3) 0.080 Uiso 1 d R . C41 C 0.9311(2) 0.2607(4) 0.9252(2) 0.0370(11) Uani 1 d . . C42 C 0.9740(2) 0.3331(4) 0.9575(2) 0.0485(13) Uani 1 d . . H42A H 0.9793(2) 0.4084(4) 0.9402(2) 0.080 Uiso 1 d R . C43 C 1.0086(2) 0.2968(5) 1.0142(2) 0.064(2) Uani 1 d . . H43A H 1.0390(2) 0.3464(5) 1.0359(2) 0.080 Uiso 1 d R . C44 C 0.9997(2) 0.1916(5) 1.0394(3) 0.068(2) Uani 1 d . . H44A H 1.0240(2) 0.1678(5) 1.0791(3) 0.080 Uiso 1 d R . C45 C 0.9565(2) 0.1196(5) 1.0087(3) 0.066(2) Uani 1 d . . H45A H 0.9503(2) 0.0460(5) 1.0276(3) 0.080 Uiso 1 d R . C46 C 0.9227(2) 0.1533(5) 0.9510(2) 0.0540(14) Uani 1 d . . H46A H 0.8933(2) 0.1028(5) 0.9283(2) 0.080 Uiso 1 d R . Cl Cl 0.84500(5) -0.01510(12) 0.81517(7) 0.0665(4) Uani 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 Pd 0.0260(2) 0.0389(2) 0.0332(2) -0.0007(2) 0.00361(13) 0.0006(2) S 0.0300(7) 0.0520(9) 0.0363(7) -0.0066(6) 0.0029(5) 0.0018(6) P1 0.0267(7) 0.0505(9) 0.0374(7) 0.0012(6) 0.0021(5) 0.0014(5) P2 0.0308(7) 0.0393(8) 0.0379(7) -0.0040(6) 0.0056(5) 0.0009(6) C1 0.070(4) 0.059(4) 0.104(6) -0.032(4) -0.030(4) 0.007(3) C2 0.187(25) 0.030(6) 0.049(10) 0.000(7) 0.010(17) -0.014(7) C01 0.028(3) 0.056(3) 0.050(3) -0.002(2) 0.007(2) -0.004(2) C02 0.031(3) 0.056(4) 0.053(3) -0.003(3) 0.006(2) 0.008(2) C03 0.031(3) 0.057(3) 0.043(3) -0.006(2) 0.013(2) -0.003(2) C11 0.032(3) 0.059(4) 0.042(3) -0.006(3) 0.000(2) 0.001(2) C12 0.052(3) 0.072(5) 0.058(4) -0.014(3) 0.013(3) -0.011(3) C13 0.073(4) 0.072(5) 0.083(5) -0.026(4) 0.017(4) -0.020(3) C14 0.085(5) 0.108(7) 0.066(5) -0.038(5) -0.002(4) 0.003(4) C15 0.170(7) 0.108(7) 0.038(4) -0.007(5) -0.009(4) 0.014(6) C16 0.125(5) 0.069(5) 0.047(4) 0.002(4) -0.006(4) -0.001(4) C21 0.030(3) 0.046(3) 0.048(3) 0.007(2) 0.006(2) 0.004(2) C22 0.051(4) 0.076(5) 0.116(5) 0.045(4) 0.036(4) 0.025(3) C23 0.074(4) 0.077(5) 0.147(7) 0.054(5) 0.057(4) 0.025(4) C24 0.080(5) 0.063(5) 0.108(5) 0.043(4) 0.035(4) 0.020(4) C25 0.063(4) 0.064(5) 0.102(5) 0.018(4) 0.019(4) 0.028(3) C26 0.032(3) 0.064(4) 0.071(4) 0.003(3) 0.006(3) 0.009(3) C31 0.036(3) 0.045(3) 0.055(3) -0.004(3) -0.007(2) 0.004(2) C32 0.066(4) 0.043(4) 0.077(4) 0.001(3) -0.002(3) -0.007(3) C33 0.108(6) 0.061(5) 0.120(7) 0.026(5) -0.018(5) -0.019(4) C34 0.107(7) 0.042(5) 0.156(9) 0.006(5) -0.078(6) 0.003(4) C35 0.077(5) 0.060(6) 0.136(7) -0.047(5) -0.046(5) 0.032(4) C36 0.057(4) 0.059(4) 0.084(5) -0.024(3) -0.007(3) 0.014(3) C41 0.034(3) 0.045(3) 0.033(3) -0.007(2) 0.009(2) 0.001(2) C42 0.048(3) 0.059(4) 0.038(3) 0.001(3) 0.004(2) -0.001(3) C43 0.059(4) 0.080(5) 0.051(4) -0.003(3) -0.001(3) -0.005(3) C44 0.065(4) 0.094(6) 0.042(3) 0.011(4) -0.008(3) 0.005(4) C45 0.074(4) 0.067(4) 0.053(4) 0.019(3) -0.003(3) -0.005(3) C46 0.053(3) 0.061(4) 0.048(3) -0.004(3) 0.007(3) -0.010(3) Cl 0.0499(8) 0.0561(9) 0.0926(11) -0.0176(8) 0.0059(7) -0.0009(7) _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 Pd P2 2.2889(11) . ? Pd P1 2.2897(12) . ? Pd S 2.3512(11) . ? Pd S 2.3741(12) 2_756 ? Pd Pd 3.2296(6) 2_756 ? S C1 1.814(6) . ? S Pd 2.3741(12) 2_756 ? P1 C21 1.797(5) . ? P1 C01 1.821(4) . ? P1 C11 1.823(5) . ? P2 C31 1.812(5) . ? P2 C41 1.815(5) . ? P2 C03 1.826(4) . ? C1 C2 1.30(2) . ? C1 C2 1.64(2) 2_756 ? C2 C2 1.03(3) 2_756 ? C2 C1 1.64(2) 2_756 ? C01 C02 1.539(6) . ? C02 C03 1.521(6) . ? C11 C16 1.375(6) . ? C11 C12 1.377(6) . ? C12 C13 1.382(7) . ? C13 C14 1.361(8) . ? C14 C15 1.336(8) . ? C15 C16 1.391(8) . ? C21 C22 1.382(6) . ? C21 C26 1.395(6) . ? C22 C23 1.374(7) . ? C23 C24 1.376(7) . ? C24 C25 1.343(6) . ? C25 C26 1.396(7) . ? C31 C32 1.377(6) . ? C31 C36 1.393(6) . ? C32 C33 1.383(8) . ? C33 C34 1.346(9) . ? C34 C35 1.357(9) . ? C35 C36 1.373(8) . ? C41 C46 1.383(6) . ? C41 C42 1.385(6) . ? C42 C43 1.378(6) . ? C43 C44 1.357(7) . ? C44 C45 1.373(7) . ? C45 C46 1.377(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pd P1 90.47(4) . . ? P2 Pd S 170.60(4) . . ? P1 Pd S 92.61(4) . . ? P2 Pd S 95.44(4) . 2_756 ? P1 Pd S 173.79(4) . 2_756 ? S Pd S 81.87(5) . 2_756 ? P2 Pd Pd 125.22(3) . 2_756 ? P1 Pd Pd 130.38(3) . 2_756 ? S Pd Pd 47.18(3) . 2_756 ? S Pd Pd 46.59(3) 2_756 2_756 ? C1 S Pd 103.1(2) . . ? C1 S Pd 102.2(2) . 2_756 ? Pd S Pd 86.23(4) . 2_756 ? C21 P1 C01 108.6(2) . . ? C21 P1 C11 105.7(2) . . ? C01 P1 C11 100.9(2) . . ? C21 P1 Pd 112.95(15) . . ? C01 P1 Pd 115.6(2) . . ? C11 P1 Pd 112.1(2) . . ? C31 P2 C41 105.7(2) . . ? C31 P2 C03 102.8(2) . . ? C41 P2 C03 106.4(2) . . ? C31 P2 Pd 113.7(2) . . ? C41 P2 Pd 113.16(13) . . ? C03 P2 Pd 114.11(15) . . ? C2 C1 C2 38.7(13) . 2_756 ? C2 C1 S 123.0(8) . . ? C2 C1 S 118.2(5) 2_756 . ? C2 C2 C1 89.1(27) 2_756 . ? C2 C2 C1 52.1(19) 2_756 2_756 ? C1 C2 C1 119.5(10) . 2_756 ? C02 C01 P1 117.8(3) . . ? C03 C02 C01 114.2(4) . . ? C02 C03 P2 113.2(3) . . ? C16 C11 C12 118.6(5) . . ? C16 C11 P1 122.6(4) . . ? C12 C11 P1 118.8(4) . . ? C11 C12 C13 120.0(6) . . ? C14 C13 C12 120.5(6) . . ? C15 C14 C13 120.4(7) . . ? C14 C15 C16 120.2(7) . . ? C11 C16 C15 120.4(6) . . ? C22 C21 C26 117.1(5) . . ? C22 C21 P1 118.4(4) . . ? C26 C21 P1 124.4(4) . . ? C23 C22 C21 121.6(5) . . ? C22 C23 C24 120.7(5) . . ? C25 C24 C23 118.9(6) . . ? C24 C25 C26 121.5(5) . . ? C21 C26 C25 120.2(5) . . ? C32 C31 C36 118.3(5) . . ? C32 C31 P2 120.2(4) . . ? C36 C31 P2 121.2(4) . . ? C31 C32 C33 119.8(6) . . ? C34 C33 C32 121.9(7) . . ? C33 C34 C35 118.5(8) . . ? C34 C35 C36 121.9(7) . . ? C35 C36 C31 119.6(6) . . ? C46 C41 C42 119.4(5) . . ? C46 C41 P2 120.0(4) . . ? C42 C41 P2 120.2(4) . . ? C43 C42 C41 119.8(5) . . ? C44 C43 C42 120.4(5) . . ? C43 C44 C45 120.6(5) . . ? C44 C45 C46 119.8(5) . . ? C45 C46 C41 120.0(5) . . ? _refine_diff_density_max 0.530 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.095 data_swp0413 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C63 H74 Cl2 N O3 P4 Pd3 S4' _chemical_formula_weight 1535.45 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 ? _symmetry_space_group_name_H-M ? 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 27.118(5) _cell_length_b 14.987(3) _cell_length_c 20.477(4) _cell_angle_alpha 90.00 _cell_angle_beta 126.65(3) _cell_angle_gamma 90.00 _cell_volume 6676.9(22) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method ? _exptl_crystal_F_000 3116 _exptl_absorpt_coefficient_mu 1.144 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11457 _diffrn_reflns_av_R_equivalents 0.0855 _diffrn_reflns_av_sigmaI/netI 0.1636 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.27 _reflns_number_total 5962 _reflns_number_observed 3225 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 12 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5950 _refine_ls_number_parameters 386 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1466 _refine_ls_R_factor_obs 0.0678 _refine_ls_wR_factor_all 0.1634 _refine_ls_wR_factor_obs 0.1277 _refine_ls_goodness_of_fit_all 1.044 _refine_ls_goodness_of_fit_obs 1.152 _refine_ls_restrained_S_all 1.059 _refine_ls_restrained_S_obs 1.152 _refine_ls_shift/esd_max -2.103 _refine_ls_shift/esd_mean 0.014 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.30787(3) 0.36037(5) 0.43391(4) 0.0318(2) Uani 1 d . . Pd2 Pd 0.2500 0.2500 0.5000 0.0294(3) Uani 1 d S . P1 P 0.39786(11) 0.4381(2) 0.51571(14) 0.0369(6) Uani 1 d . . S1 S 0.21484(10) 0.2800(2) 0.36719(13) 0.0344(6) Uani 1 d . . P2 P 0.26114(11) 0.4770(2) 0.34601(14) 0.0385(7) Uani 1 d . . S2 S 0.34614(10) 0.2393(2) 0.52660(13) 0.0362(6) Uani 1 d . . C02 C 0.2765(5) 0.1151(7) 0.3974(6) 0.052(3) Uani 1 d . . H02A H 0.2583(5) 0.0971(7) 0.4236(6) 0.080 Uiso 1 d R . H02B H 0.2796(5) 0.0630(7) 0.3727(6) 0.080 Uiso 1 d R . C03 C 0.3398(5) 0.1502(7) 0.4616(6) 0.054(3) Uani 1 d . . H03A H 0.3649(5) 0.1013(7) 0.4958(6) 0.080 Uiso 1 d R . H03B H 0.3569(5) 0.1715(7) 0.4347(6) 0.080 Uiso 1 d R . C11 C 0.4647(4) 0.3664(7) 0.5761(5) 0.044(3) Uani 1 d . . C1 C 0.4173(4) 0.5115(8) 0.4635(6) 0.060(3) Uani 1 d . . H1A H 0.4234(4) 0.4755(8) 0.4301(6) 0.080 Uiso 1 d R . H1B H 0.4555(4) 0.5408(8) 0.5034(6) 0.080 Uiso 1 d R . C2 C 0.3104(5) 0.5417(8) 0.3312(6) 0.059(3) Uani 1 d . . H2A H 0.2864(5) 0.5894(8) 0.2942(6) 0.080 Uiso 1 d R . H2B H 0.3231(5) 0.5042(8) 0.3058(6) 0.080 Uiso 1 d R . C41 C 0.2312(4) 0.5563(7) 0.3813(6) 0.045(3) Uani 1 d . . C21 C 0.3975(4) 0.5068(8) 0.5876(5) 0.044(3) Uani 1 d . . C36 C 0.1456(5) 0.5040(9) 0.1958(6) 0.068(4) Uani 1 d . . H36A H 0.1392(5) 0.5496(9) 0.2229(6) 0.080 Uiso 1 d R . C32 C 0.2069(5) 0.3878(8) 0.2007(6) 0.062(3) Uani 1 d . . H32A H 0.2439(5) 0.3530(8) 0.2314(6) 0.080 Uiso 1 d R . C15 C 0.5243(5) 0.2445(8) 0.5795(7) 0.072(4) Uani 1 d . . H15A H 0.5314(5) 0.2011(8) 0.5514(7) 0.080 Uiso 1 d R . C26 C 0.4260(5) 0.5865(8) 0.6144(7) 0.063(3) Uani 1 d . . H26A H 0.4486(5) 0.6077(8) 0.5950(7) 0.080 Uiso 1 d R . C25 C 0.4246(6) 0.6372(10) 0.6697(8) 0.085(4) Uani 1 d . . H25A H 0.4412(6) 0.6965(10) 0.6843(8) 0.080 Uiso 1 d R . C43 C 0.1975(7) 0.6990(8) 0.3846(10) 0.092(5) Uani 1 d . . H43A H 0.1892(7) 0.7601(8) 0.3669(10) 0.080 Uiso 1 d R . C42 C 0.2211(6) 0.6465(10) 0.3577(7) 0.078(4) Uani 1 d . . H42A H 0.2318(6) 0.6688(10) 0.3237(7) 0.080 Uiso 1 d R . C31 C 0.1981(5) 0.4523(7) 0.2392(6) 0.045(3) Uani 1 d . . C44 C 0.1837(7) 0.6715(11) 0.4357(9) 0.104(5) Uani 1 d . . H44A H 0.1675(7) 0.7119(11) 0.4550(9) 0.080 Uiso 1 d R . C16 C 0.4761(4) 0.3038(7) 0.5367(6) 0.050(3) Uani 1 d . . H16A H 0.4497(4) 0.3021(7) 0.4783(6) 0.080 Uiso 1 d R . C13 C 0.5518(5) 0.3086(8) 0.7022(6) 0.062(3) Uani 1 d . . H13A H 0.5792(5) 0.3097(8) 0.7606(6) 0.080 Uiso 1 d R . C34 C 0.1106(7) 0.4239(11) 0.0746(7) 0.078(5) Uani 1 d . . H34A H 0.0808(7) 0.4153(11) 0.0170(7) 0.080 Uiso 1 d R . C23 C 0.3683(6) 0.5247(11) 0.6771(7) 0.082(4) Uani 1 d . . H23A H 0.3476(6) 0.5033(11) 0.6990(7) 0.080 Uiso 1 d R . C35 C 0.1021(6) 0.4877(11) 0.1134(7) 0.086(5) Uani 1 d . . H35A H 0.0652(6) 0.5228(11) 0.0828(7) 0.080 Uiso 1 d R . C14 C 0.5618(5) 0.2481(9) 0.6619(7) 0.071(4) Uani 1 d . . H14A H 0.5949(5) 0.2060(9) 0.6921(7) 0.080 Uiso 1 d R . C01 C 0.2343(5) 0.1820(7) 0.3328(5) 0.045(3) Uani 1 d . . H01A H 0.2533(5) 0.2019(7) 0.3081(5) 0.080 Uiso 1 d R . H01B H 0.1967(5) 0.1524(7) 0.2916(5) 0.080 Uiso 1 d R . C24 C 0.3975(6) 0.6011(10) 0.7041(7) 0.076(4) Uani 1 d . . H24A H 0.4001(6) 0.6310(10) 0.7475(7) 0.080 Uiso 1 d R . C33 C 0.1628(7) 0.3728(11) 0.1183(7) 0.083(4) Uani 1 d . . H33A H 0.1685(7) 0.3256(11) 0.0916(7) 0.080 Uiso 1 d R . C22 C 0.3674(5) 0.4741(8) 0.6191(6) 0.059(3) Uani 1 d . . H22A H 0.3842(5) 0.4164(8) 0.6420(6) 0.080 Uiso 1 d R . H22B H 0.3251(5) 0.4659(8) 0.5739(6) 0.080 Uiso 1 d R . C12 C 0.5039(5) 0.3700(9) 0.6601(6) 0.067(4) Uani 1 d . . H12A H 0.4980(5) 0.4140(9) 0.6889(6) 0.080 Uiso 1 d R . C46 C 0.2175(6) 0.5295(8) 0.4323(7) 0.073(4) Uani 1 d . . H46A H 0.2274(6) 0.4691(8) 0.4516(7) 0.080 Uiso 1 d R . C3 C 0.3688(5) 0.5799(8) 0.4072(6) 0.059(3) Uani 1 d . . H3A H 0.3859(5) 0.6243(8) 0.3922(6) 0.080 Uiso 1 d R . H3B H 0.3573(5) 0.6088(8) 0.4381(6) 0.080 Uiso 1 d R . C45 C 0.1931(8) 0.5834(10) 0.4580(9) 0.117(6) Uani 1 d . . H45A H 0.1819(8) 0.5602(10) 0.4912(9) 0.080 Uiso 1 d R . Cl Cl 0.14561(14) 0.7935(2) 0.1728(2) 0.0746(9) Uani 1 d . . O O 0.0000 0.6334(22) 0.2500 0.222(11) Uani 1 d S . OW O 0.4818(6) 0.2050(10) 0.3763(7) 0.176(6) Uani 1 d . . N N 0.0000 0.4911(26) 0.2500 0.153(11) Uani 1 d S . C2'' C -0.0341(65) 0.5648(43) 0.2517(159) 0.367(147) Uani 0.25 d P . C2' C 0.0404(34) 0.4114(28) 0.2795(54) 0.229(32) Uani 0.50 d P . C2 C -0.0301(73) 0.4471(44) 0.1694(47) 0.277(96) Uani 0.25 d P . C1 C 0.0327(52) 0.5078(86) 0.3139(75) 0.638(171) Uani 0.50 d P . 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 0.0360(4) 0.0333(5) 0.0282(4) 0.0031(4) 0.0203(3) -0.0001(4) Pd2 0.0364(6) 0.0300(7) 0.0252(5) 0.0015(5) 0.0203(5) 0.0001(5) P1 0.0358(14) 0.038(2) 0.0381(14) 0.0019(12) 0.0229(13) -0.0006(13) S1 0.0388(13) 0.038(2) 0.0258(12) -0.0006(11) 0.0189(11) -0.0031(12) P2 0.0428(15) 0.042(2) 0.0305(13) 0.0083(12) 0.0219(12) -0.0010(13) S2 0.0362(13) 0.043(2) 0.0310(12) 0.0056(12) 0.0207(11) 0.0057(12) C02 0.070(7) 0.052(8) 0.058(7) -0.007(6) 0.051(7) 0.001(6) C03 0.080(8) 0.046(8) 0.065(7) 0.004(6) 0.059(7) 0.014(6) C11 0.030(5) 0.061(8) 0.041(6) 0.004(6) 0.021(5) -0.003(5) C1 0.034(6) 0.079(10) 0.055(7) 0.004(7) 0.021(6) -0.015(6) C2 0.067(7) 0.056(8) 0.048(7) 0.018(6) 0.032(6) 0.002(6) C41 0.056(7) 0.026(7) 0.041(6) 0.003(5) 0.022(5) 0.002(5) C21 0.034(6) 0.056(8) 0.036(6) -0.011(5) 0.017(5) -0.008(5) C36 0.047(7) 0.100(11) 0.043(7) 0.010(7) 0.018(6) 0.013(7) C32 0.078(8) 0.066(9) 0.047(7) -0.002(6) 0.041(7) -0.012(7) C15 0.045(7) 0.090(11) 0.068(8) -0.015(7) 0.027(7) 0.026(7) C26 0.058(7) 0.059(9) 0.061(8) -0.018(7) 0.030(7) -0.008(7) C25 0.064(8) 0.083(11) 0.079(9) -0.024(9) 0.026(8) -0.006(8) C43 0.126(13) 0.021(8) 0.126(13) 0.020(8) 0.075(12) 0.025(8) C42 0.086(9) 0.073(11) 0.069(8) 0.023(8) 0.044(8) 0.024(8) C31 0.060(7) 0.036(7) 0.032(6) 0.011(5) 0.025(6) -0.010(6) C44 0.149(14) 0.062(12) 0.110(12) 0.006(9) 0.083(12) 0.042(10) C16 0.044(6) 0.054(8) 0.049(6) -0.008(6) 0.026(6) 0.010(6) C13 0.064(7) 0.064(9) 0.044(6) 0.010(6) 0.024(6) 0.025(7) C34 0.083(10) 0.096(12) 0.039(7) 0.000(8) 0.028(8) -0.050(9) C23 0.090(10) 0.110(13) 0.067(9) -0.034(9) 0.058(8) -0.013(9) C35 0.054(8) 0.126(15) 0.047(8) 0.024(9) 0.014(7) -0.001(9) C14 0.042(7) 0.095(11) 0.070(8) 0.012(8) 0.030(7) 0.022(7) C01 0.070(7) 0.037(7) 0.035(6) -0.011(5) 0.035(6) -0.008(6) C24 0.075(9) 0.084(11) 0.051(8) -0.032(7) 0.027(7) 0.019(8) C33 0.104(11) 0.103(12) 0.045(8) -0.014(8) 0.046(8) -0.032(10) C22 0.060(7) 0.062(9) 0.049(7) -0.009(6) 0.029(6) -0.001(7) C12 0.051(7) 0.098(11) 0.045(7) -0.008(7) 0.025(6) 0.015(7) C46 0.119(11) 0.055(9) 0.084(9) 0.030(7) 0.082(9) 0.030(8) C3 0.059(7) 0.054(8) 0.064(7) 0.012(6) 0.036(7) -0.016(6) C45 0.215(18) 0.067(12) 0.152(14) 0.042(10) 0.155(15) 0.069(12) Cl 0.078(2) 0.098(3) 0.052(2) 0.000(2) 0.041(2) 0.003(2) O 0.207(24) 0.285(36) 0.194(23) 0.000 0.131(21) 0.000 OW 0.185(12) 0.219(15) 0.142(10) 0.019(10) 0.107(10) 0.077(11) N 0.165(26) 0.178(39) 0.111(22) 0.000 0.079(22) 0.000 C2'' 0.293(135) 0.000(35) 0.986(454) -0.063(102) 0.479(241) -0.010(60) C2' 0.251(64) 0.050(30) 0.346(98) -0.038(47) 0.157(81) 0.027(35) C2 0.463(202) 0.000(35) 0.098(58) 0.033(35) 0.022(81) 0.132(74) C1 0.313(117) 0.425(176) 0.395(146) 0.202(152) -0.211(103) -0.225(143) _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 P2 2.275(3) . ? Pd1 P1 2.289(3) . ? Pd1 S1 2.360(3) . ? Pd1 S2 2.371(2) . ? Pd1 Pd2 3.0930(8) . ? Pd2 S1 2.326(2) 7_556 ? Pd2 S1 2.326(2) . ? Pd2 S2 2.329(2) 7_556 ? Pd2 S2 2.329(2) . ? Pd2 Pd1 3.0930(8) 7_556 ? P1 C21 1.801(10) . ? P1 C11 1.814(10) . ? P1 C1 1.818(10) . ? S1 C01 1.837(9) . ? P2 C41 1.814(10) . ? P2 C2 1.815(10) . ? P2 C31 1.838(10) . ? S2 C03 1.820(10) . ? C02 C01 1.502(13) . ? C02 C03 1.503(14) . ? C11 C12 1.382(12) . ? C11 C16 1.387(13) . ? C1 C3 1.516(14) . ? C2 C3 1.522(13) . ? C41 C46 1.361(13) . ? C41 C42 1.407(15) . ? C21 C26 1.348(14) . ? C21 C22 1.397(12) . ? C36 C31 1.380(14) . ? C36 C35 1.386(15) . ? C32 C31 1.356(14) . ? C32 C33 1.385(15) . ? C15 C14 1.355(14) . ? C15 C16 1.379(14) . ? C26 C25 1.38(2) . ? C25 C24 1.40(2) . ? C43 C42 1.32(2) . ? C43 C44 1.37(2) . ? C44 C45 1.37(2) . ? C13 C14 1.358(15) . ? C13 C12 1.393(14) . ? C34 C35 1.35(2) . ? C34 C33 1.37(2) . ? C23 C24 1.31(2) . ? C23 C22 1.396(14) . ? C46 C45 1.335(14) . ? O C2'' 1.40(8) . ? O C2'' 1.40(8) 2 ? N C1 1.08(12) . ? N C1 1.08(12) 2 ? N C2'' 1.45(7) . ? N C2'' 1.45(7) 2 ? N C2 1.49(8) . ? N C2 1.49(8) 2 ? N C2' 1.48(5) 2 ? N C2' 1.48(5) . ? C2'' C1 1.61(20) 2 ? C2'' C1 1.70(15) . ? C2'' C2'' 1.89(19) 2 ? C2' C2 1.34(15) 2 ? C2' C1 1.67(19) . ? C2' C2' 1.76(15) 2 ? C2' C2 1.97(10) . ? C2 C1 0.99(11) 2 ? C2 C2' 1.34(15) 2 ? C1 C2 0.99(11) 2 ? C1 C2'' 1.61(20) 2 ? C1 C1 2.11(22) 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 P2 Pd1 P1 92.01(10) . . ? P2 Pd1 S1 92.06(9) . . ? P1 Pd1 S1 171.13(8) . . ? P2 Pd1 S2 172.82(9) . . ? P1 Pd1 S2 92.16(9) . . ? S1 Pd1 S2 83.02(9) . . ? P2 Pd1 Pd2 124.64(7) . . ? P1 Pd1 Pd2 123.35(7) . . ? S1 Pd1 Pd2 48.23(5) . . ? S2 Pd1 Pd2 48.27(6) . . ? S1 Pd2 S1 180.0 7_556 . ? S1 Pd2 S2 84.68(8) 7_556 7_556 ? S1 Pd2 S2 95.32(8) . 7_556 ? S1 Pd2 S2 95.32(8) 7_556 . ? S1 Pd2 S2 84.67(8) . . ? S2 Pd2 S2 180.0 7_556 . ? S1 Pd2 Pd1 130.84(6) 7_556 . ? S1 Pd2 Pd1 49.16(6) . . ? S2 Pd2 Pd1 130.56(6) 7_556 . ? S2 Pd2 Pd1 49.44(6) . . ? S1 Pd2 Pd1 49.16(6) 7_556 7_556 ? S1 Pd2 Pd1 130.84(6) . 7_556 ? S2 Pd2 Pd1 49.44(6) 7_556 7_556 ? S2 Pd2 Pd1 130.56(6) . 7_556 ? Pd1 Pd2 Pd1 180.0 . 7_556 ? C21 P1 C11 105.8(4) . . ? C21 P1 C1 106.2(5) . . ? C11 P1 C1 103.7(4) . . ? C21 P1 Pd1 111.5(3) . . ? C11 P1 Pd1 113.1(4) . . ? C1 P1 Pd1 115.8(3) . . ? C01 S1 Pd2 106.4(3) . . ? C01 S1 Pd1 100.3(3) . . ? Pd2 S1 Pd1 82.61(8) . . ? C41 P2 C2 105.3(5) . . ? C41 P2 C31 106.6(5) . . ? C2 P2 C31 99.4(4) . . ? C41 P2 Pd1 111.0(3) . . ? C2 P2 Pd1 115.1(4) . . ? C31 P2 Pd1 118.0(3) . . ? C03 S2 Pd2 106.0(4) . . ? C03 S2 Pd1 99.8(3) . . ? Pd2 S2 Pd1 82.29(8) . . ? C01 C02 C03 114.2(9) . . ? C02 C03 S2 117.1(7) . . ? C12 C11 C16 118.5(9) . . ? C12 C11 P1 122.6(8) . . ? C16 C11 P1 118.9(7) . . ? C3 C1 P1 115.6(7) . . ? C3 C2 P2 116.8(7) . . ? C46 C41 C42 117.4(11) . . ? C46 C41 P2 120.3(8) . . ? C42 C41 P2 122.3(9) . . ? C26 C21 C22 118.3(10) . . ? C26 C21 P1 123.9(8) . . ? C22 C21 P1 117.8(8) . . ? C31 C36 C35 119.1(12) . . ? C31 C32 C33 120.1(12) . . ? C14 C15 C16 119.2(11) . . ? C21 C26 C25 122.0(12) . . ? C26 C25 C24 118.7(13) . . ? C42 C43 C44 124.0(13) . . ? C43 C42 C41 118.2(12) . . ? C32 C31 C36 119.8(10) . . ? C32 C31 P2 118.3(9) . . ? C36 C31 P2 121.5(9) . . ? C43 C44 C45 117.6(13) . . ? C15 C16 C11 121.5(10) . . ? C14 C13 C12 121.1(10) . . ? C35 C34 C33 119.0(12) . . ? C24 C23 C22 122.1(12) . . ? C34 C35 C36 121.4(13) . . ? C15 C14 C13 120.6(11) . . ? C02 C01 S1 116.0(6) . . ? C23 C24 C25 119.6(12) . . ? C34 C33 C32 120.6(14) . . ? C23 C22 C21 119.0(11) . . ? C11 C12 C13 119.0(10) . . ? C45 C46 C41 123.4(12) . . ? C1 C3 C2 115.1(10) . . ? C46 C45 C44 119.3(13) . . ? C2'' O C2'' 85.2(66) . 2 ? C1 N C1 153.2(100) . 2 ? C1 N C2'' 82.5(100) . . ? C1 N C2'' 77.2(100) 2 . ? C1 N C2'' 77.2(100) . 2 ? C1 N C2'' 82.5(100) 2 2 ? C2'' N C2'' 81.1(76) . 2 ? C1 N C2 162.3(100) . . ? C1 N C2 41.6(60) 2 . ? C2'' N C2 115.3(100) . . ? C2'' N C2 104.3(100) 2 . ? C1 N C2 41.6(60) . 2 ? C1 N C2 162.3(100) 2 2 ? C2'' N C2 104.3(100) . 2 ? C2'' N C2 115.3(100) 2 2 ? C2 N C2 127.4(60) . 2 ? C1 N C2' 123.4(83) . 2 ? C1 N C2' 79.7(96) 2 2 ? C2'' N C2' 107.3(45) . 2 ? C2'' N C2' 158.0(100) 2 2 ? C2 N C2' 53.7(61) . 2 ? C2 N C2' 83.0(43) 2 2 ? C1 N C2' 79.7(96) . . ? C1 N C2' 123.4(83) 2 . ? C2'' N C2' 158.0(100) . . ? C2'' N C2' 107.3(44) 2 . ? C2 N C2' 83.0(43) . . ? C2 N C2' 53.7(61) 2 . ? C2' N C2' 72.7(57) 2 . ? O C2'' N 96.9(62) . . ? O C2'' C1 91.4(98) . 2 ? N C2'' C1 41.0(55) . 2 ? O C2'' C1 87.9(67) . . ? N C2'' C1 39.3(58) . . ? C1 C2'' C1 79.2(89) 2 . ? O C2'' C2'' 47.4(33) . 2 ? N C2'' C2'' 49.5(38) . 2 ? C1 C2'' C2'' 57.3(90) 2 2 ? C1 C2'' C2'' 53.0(76) . 2 ? C2 C2' N 63.3(48) 2 . ? C2 C2' C1 36.2(63) 2 . ? N C2' C1 39.6(30) . . ? C2 C2' C2' 77.6(73) 2 2 ? N C2' C2' 53.6(29) . 2 ? C1 C2' C2' 82.7(51) . 2 ? C2 C2' C2 105.8(62) 2 . ? N C2' C2 48.6(34) . . ? C1 C2' C2 88.1(54) . . ? C2' C2' C2 41.7(54) 2 . ? C1 C2 C2' 90.4(100) 2 2 ? C1 C2 N 46.7(82) 2 . ? C2' C2 N 62.9(52) 2 . ? C1 C2 C2' 94.3(84) 2 . ? C2' C2 C2' 60.7(53) 2 . ? N C2 C2' 48.4(27) . . ? N C1 C2 91.7(100) . 2 ? N C1 C2'' 61.7(87) . 2 ? C2 C1 C2'' 144.9(100) 2 2 ? N C1 C2' 60.7(97) . . ? C2 C1 C2' 53.4(100) 2 . ? C2'' C1 C2' 92.1(100) 2 . ? N C1 C2'' 58.2(73) . . ? C2 C1 C2'' 117.4(100) 2 . ? C2'' C1 C2'' 69.7(73) 2 . ? C2' C1 C2'' 117.6(100) . . ? N C1 C1 13.4(74) . 2 ? C2 C1 C1 104.4(68) 2 2 ? C2'' C1 C1 52.2(82) 2 2 ? C2' C1 C1 72.7(77) . 2 ? C2'' C1 C1 48.6(72) . 2 ? _refine_diff_density_max 0.737 _refine_diff_density_min -1.363 _refine_diff_density_rms 0.171