# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1655 # Note this CIF contains data for compound 2,3,4 and 7 only (5 available only as hard copy) data_ab347 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H63 O6 P3 Pd3 S3' _chemical_formula_weight 1424.42 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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 24.985(2) _cell_length_b 24.985(2) _cell_length_c 16.219(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8768.0(19) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 4.88 _cell_measurement_theta_max 12.46 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4320 _exptl_absorpt_coefficient_mu 1.154 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.325522 _exptl_absorpt_correction_T_max 0.755360 _exptl_absorpt_process_details - _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method 'Theta/2 theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 4121 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3354 _reflns_number_gt 2219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+74.1161P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3354 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1400 _refine_ls_wR_factor_gt 0.1105 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd -0.00044(2) 0.06269(2) 0.64348(4) 0.02795(19) Uani 1 1 d . . . S1 S 0.10356(8) 0.10506(8) 0.63932(12) 0.0326(4) Uani 1 1 d . . . P1 P 0.00235(9) 0.15745(8) 0.65086(12) 0.0286(4) Uani 1 1 d . . . O1 O 0.1347(2) 0.1401(3) 0.7117(4) 0.0522(16) Uani 1 1 d . . . O2 O 0.1310(2) 0.1328(3) 0.5613(4) 0.0498(16) Uani 1 1 d . . . C11A C -0.0710(3) 0.1497(3) 0.6126(5) 0.0332(17) Uani 1 1 d . . . H11A H -0.0828 0.1246 0.5624 0.040 Uiso 1 1 calc R . . H11B H -0.1031 0.1268 0.6539 0.040 Uiso 1 1 calc R . . C12A C -0.0711(3) 0.2083(3) 0.5937(5) 0.0351(18) Uani 1 1 d . . . C13A C -0.0883(3) 0.2382(3) 0.6509(5) 0.0377(18) Uani 1 1 d . . . H13A H -0.1008 0.2212 0.7040 0.045 Uiso 1 1 calc R . . C14A C -0.0872(4) 0.2922(4) 0.6311(6) 0.050(2) Uani 1 1 d . . . H14A H -0.0997 0.3116 0.6700 0.060 Uiso 1 1 calc R . . C15A C -0.0679(4) 0.3174(4) 0.5555(6) 0.052(2) Uani 1 1 d . . . H15A H -0.0655 0.3554 0.5435 0.062 Uiso 1 1 calc R . . C16A C -0.0520(4) 0.2893(4) 0.4961(6) 0.051(2) Uani 1 1 d . . . H16A H -0.0403 0.3066 0.4432 0.061 Uiso 1 1 calc R . . C17A C -0.0536(4) 0.2343(4) 0.5158(5) 0.042(2) Uani 1 1 d . . . H17A H -0.0425 0.2144 0.4757 0.051 Uiso 1 1 calc R . . C11B C 0.0658(3) 0.2230(3) 0.5943(4) 0.0322(17) Uani 1 1 d . . . H11C H 0.0949 0.2101 0.5755 0.039 Uiso 1 1 calc R . . H11D H 0.0481 0.2309 0.5450 0.039 Uiso 1 1 calc R . . C12B C 0.1017(3) 0.2831(3) 0.6408(5) 0.0337(17) Uani 1 1 d . . . C13B C 0.0848(3) 0.3275(3) 0.6409(5) 0.041(2) Uani 1 1 d . . . H13B H 0.0503 0.3211 0.6099 0.049 Uiso 1 1 calc R . . C14B C 0.1173(4) 0.3814(4) 0.6855(6) 0.052(2) Uani 1 1 d . . . H14B H 0.1040 0.4107 0.6855 0.063 Uiso 1 1 calc R . . C15B C 0.1689(5) 0.3929(4) 0.7298(6) 0.055(2) Uani 1 1 d . . . H15B H 0.1913 0.4298 0.7598 0.066 Uiso 1 1 calc R . . C16B C 0.1872(4) 0.3493(4) 0.7294(6) 0.054(2) Uani 1 1 d . . . H16B H 0.2228 0.3567 0.7586 0.065 Uiso 1 1 calc R . . C17B C 0.1531(4) 0.2941(4) 0.6858(5) 0.044(2) Uani 1 1 d . . . H17B H 0.1653 0.2641 0.6871 0.053 Uiso 1 1 calc R . . C11C C 0.0100(3) 0.1854(3) 0.7566(4) 0.0321(17) Uani 1 1 d . . . H11E H 0.0529 0.2022 0.7745 0.039 Uiso 1 1 calc R . . H11F H 0.0007 0.2192 0.7579 0.039 Uiso 1 1 calc R . . C12C C -0.0319(3) 0.1362(3) 0.8162(4) 0.0322(17) Uani 1 1 d . . . C13C C -0.0883(4) 0.1289(4) 0.8382(5) 0.045(2) Uani 1 1 d . . . H13C H -0.1012 0.1553 0.8157 0.054 Uiso 1 1 calc R . . C14C C -0.1261(4) 0.0834(4) 0.8928(5) 0.050(2) Uani 1 1 d . . . H14C H -0.1638 0.0802 0.9083 0.060 Uiso 1 1 calc R . . C15C C -0.1101(4) 0.0432(4) 0.9247(5) 0.050(2) Uani 1 1 d . . . H15C H -0.1368 0.0116 0.9608 0.060 Uiso 1 1 calc R . . C16C C -0.0536(4) 0.0497(4) 0.9029(5) 0.048(2) Uani 1 1 d . . . H16C H -0.0412 0.0228 0.9254 0.057 Uiso 1 1 calc R . . C17C C -0.0151(4) 0.0954(4) 0.8485(5) 0.0386(19) Uani 1 1 d . . . H17C H 0.0228 0.0988 0.8332 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0283(3) 0.0274(3) 0.0285(3) -0.0007(2) -0.0012(2) 0.0142(2) S1 0.0305(9) 0.0293(9) 0.0403(12) 0.0050(8) 0.0022(8) 0.0166(8) P1 0.0369(10) 0.0276(9) 0.0253(11) -0.0011(8) -0.0003(8) 0.0190(8) O1 0.041(3) 0.044(3) 0.069(4) -0.019(3) -0.027(3) 0.019(3) O2 0.047(3) 0.053(3) 0.060(4) 0.032(3) 0.028(3) 0.033(3) C11A 0.034(4) 0.043(4) 0.032(4) -0.006(3) -0.002(3) 0.026(3) C12A 0.041(4) 0.038(4) 0.035(5) -0.004(4) -0.005(4) 0.025(4) C13A 0.043(4) 0.040(4) 0.036(5) 0.002(4) -0.002(4) 0.025(4) C14A 0.062(6) 0.065(6) 0.043(6) -0.015(5) -0.003(5) 0.047(5) C15A 0.072(6) 0.040(5) 0.059(7) -0.005(4) -0.016(5) 0.040(5) C16A 0.076(6) 0.052(5) 0.043(6) 0.005(4) -0.006(5) 0.045(5) C17A 0.050(5) 0.050(5) 0.034(5) -0.007(4) -0.006(4) 0.030(4) C11B 0.036(4) 0.039(4) 0.021(4) 0.002(3) 0.006(3) 0.019(3) C12B 0.037(4) 0.036(4) 0.028(4) 0.007(3) 0.011(3) 0.018(3) C13B 0.033(4) 0.039(4) 0.051(6) -0.003(4) 0.005(4) 0.018(4) C14B 0.073(6) 0.031(4) 0.056(6) 0.010(4) 0.034(5) 0.029(4) C15B 0.067(6) 0.028(4) 0.053(6) -0.006(4) 0.011(5) 0.011(4) C16B 0.055(5) 0.053(5) 0.038(5) 0.003(4) -0.005(4) 0.015(5) C17B 0.056(5) 0.049(5) 0.032(5) 0.006(4) 0.004(4) 0.029(4) C11C 0.032(4) 0.038(4) 0.026(4) -0.003(3) -0.001(3) 0.017(3) C12C 0.039(4) 0.037(4) 0.015(4) -0.010(3) -0.003(3) 0.015(3) C13C 0.055(5) 0.069(6) 0.023(4) 0.005(4) 0.007(4) 0.039(5) C14C 0.040(5) 0.076(6) 0.034(5) -0.003(5) 0.003(4) 0.029(5) C15C 0.051(5) 0.054(5) 0.036(5) -0.003(4) 0.001(4) 0.020(4) C16C 0.066(6) 0.047(5) 0.034(5) 0.009(4) -0.002(4) 0.030(4) C17C 0.048(5) 0.047(5) 0.028(5) 0.004(4) 0.001(4) 0.030(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S1 2.2641(19) . ? Pd1 S1 2.2841(18) 2 ? Pd1 P1 2.3367(18) . ? Pd1 Pd1 2.7225(9) 2 ? Pd1 Pd1 2.7225(9) 3 ? S1 O1 1.438(6) . ? S1 O2 1.440(6) . ? S1 Pd1 2.2841(18) 3 ? P1 C11C 1.826(7) . ? P1 C11A 1.851(7) . ? P1 C11B 1.854(7) . ? C11A C12A 1.497(10) . ? C12A C13A 1.386(10) . ? C12A C17A 1.386(11) . ? C13A C14A 1.374(11) . ? C14A C15A 1.353(12) . ? C15A C16A 1.363(12) . ? C16A C17A 1.393(11) . ? C11B C12B 1.511(10) . ? C12B C13B 1.372(10) . ? C12B C17B 1.379(11) . ? C13B C14B 1.380(11) . ? C14B C15B 1.377(13) . ? C15B C16B 1.374(13) . ? C16B C17B 1.399(12) . ? C11C C12C 1.503(10) . ? C12C C13C 1.375(10) . ? C12C C17C 1.385(10) . ? C13C C14C 1.376(11) . ? C14C C15C 1.357(12) . ? C15C C16C 1.385(12) . ? C16C C17C 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 S1 Pd1 S1 166.01(6) . 2 ? S1 Pd1 P1 94.70(7) . . ? S1 Pd1 P1 99.02(7) 2 . ? S1 Pd1 Pd1 113.54(5) . 2 ? S1 Pd1 Pd1 52.90(5) 2 2 ? P1 Pd1 Pd1 151.68(6) . 2 ? S1 Pd1 Pd1 53.57(5) . 3 ? S1 Pd1 Pd1 112.87(5) 2 3 ? P1 Pd1 Pd1 148.06(6) . 3 ? Pd1 Pd1 Pd1 60.0 2 3 ? O1 S1 O2 116.2(4) . . ? O1 S1 Pd1 113.9(3) . . ? O2 S1 Pd1 114.2(2) . . ? O1 S1 Pd1 117.9(3) . 3 ? O2 S1 Pd1 114.1(3) . 3 ? Pd1 S1 Pd1 73.53(6) . 3 ? C11C P1 C11A 105.3(3) . . ? C11C P1 C11B 104.3(3) . . ? C11A P1 C11B 106.9(3) . . ? C11C P1 Pd1 112.4(2) . . ? C11A P1 Pd1 110.5(2) . . ? C11B P1 Pd1 116.7(2) . . ? C12A C11A P1 117.0(5) . . ? C13A C12A C17A 118.0(7) . . ? C13A C12A C11A 122.7(7) . . ? C17A C12A C11A 119.3(7) . . ? C14A C13A C12A 120.8(8) . . ? C15A C14A C13A 119.8(8) . . ? C14A C15A C16A 121.9(8) . . ? C15A C16A C17A 118.3(9) . . ? C12A C17A C16A 121.1(8) . . ? C12B C11B P1 116.8(5) . . ? C13B C12B C17B 118.1(7) . . ? C13B C12B C11B 122.3(7) . . ? C17B C12B C11B 119.6(7) . . ? C12B C13B C14B 121.5(8) . . ? C15B C14B C13B 120.6(8) . . ? C16B C15B C14B 118.8(8) . . ? C15B C16B C17B 120.3(9) . . ? C12B C17B C16B 120.7(8) . . ? C12C C11C P1 113.2(5) . . ? C13C C12C C17C 118.4(7) . . ? C13C C12C C11C 121.5(7) . . ? C17C C12C C11C 120.2(7) . . ? C12C C13C C14C 120.6(8) . . ? C15C C14C C13C 121.6(8) . . ? C14C C15C C16C 118.4(8) . . ? C17C C16C C15C 120.5(8) . . ? C16C C17C C12C 120.4(8) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.366 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.140 data_ss159 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H64 O6 P4 Pd2 S' _chemical_formula_weight 1417.99 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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.498(7) _cell_length_b 14.064(3) _cell_length_c 23.376(13) _cell_angle_alpha 90.00 _cell_angle_beta 112.47(3) _cell_angle_gamma 90.00 _cell_volume 6835(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 12.52 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type Semi-Empirical _exptl_absorpt_correction_T_min 0.79593 _exptl_absorpt_correction_T_max 0.98317 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method 'Theta/2 theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 9.69 _diffrn_reflns_number 11348 _diffrn_reflns_av_R_equivalents 0.1248 _diffrn_reflns_av_sigmaI/netI 0.1506 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 23.00 _reflns_number_total 9505 _reflns_number_gt 5296 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0923P)^2^+12.5960P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9505 _refine_ls_number_parameters 764 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1604 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.1977 _refine_ls_wR_factor_gt 0.1679 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 2.607 _refine_ls_shift/su_mean 0.023 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd -0.29112(4) 1.18448(6) 0.12157(4) 0.0233(2) Uani 1 1 d D . . Pd2 Pd -0.21658(4) 1.06645(6) 0.20910(4) 0.0238(2) Uani 1 1 d D . . P1 P -0.36006(13) 1.2247(2) 0.02172(10) 0.0256(7) Uani 1 1 d D . . P2 P -0.15332(13) 0.93338(18) 0.25041(12) 0.0280(7) Uani 1 1 d D . . P3 P -0.30763(13) 1.28217(18) 0.19422(11) 0.0219(7) Uani 1 1 d D . . P4 P -0.24297(13) 1.1309(2) 0.28788(11) 0.0235(7) Uani 1 1 d D . . S1 S -0.23176(12) 1.06490(17) 0.10864(10) 0.0307(7) Uani 1 1 d D . . O1 O -0.2644(4) 0.9803(6) 0.0710(3) 0.045(2) Uani 1 1 d . . . O2 O -0.1781(4) 1.0968(6) 0.0903(4) 0.040(2) Uani 1 1 d . . . C1 C -0.3138(5) 1.2111(8) 0.2574(5) 0.027(3) Uani 1 1 d . . . H1A H -0.3539 1.1731 0.2420 0.032 Uiso 1 1 calc R . . H1B H -0.3151 1.2534 0.2908 0.032 Uiso 1 1 calc R . . C11A C -0.4224(4) 1.1315(6) -0.0084(5) 0.032(3) Uani 1 1 d D . . H11P H -0.4531 1.1505 -0.0499 0.039 Uiso 1 1 calc R . . H11Q H -0.4016 1.0715 -0.0130 0.039 Uiso 1 1 calc R . . C11B C -0.4092(5) 1.3343(5) 0.0082(5) 0.032(3) Uani 1 1 d D . . H11R H -0.4353 1.3387 -0.0367 0.038 Uiso 1 1 calc R . . H11S H -0.4396 1.3267 0.0293 0.038 Uiso 1 1 calc R . . C11C C -0.3257(5) 1.2303(8) -0.0386(4) 0.031(3) Uani 1 1 d D . . H11T H -0.2950 1.2841 -0.0290 0.037 Uiso 1 1 calc R . . H11U H -0.3010 1.1713 -0.0365 0.037 Uiso 1 1 calc R . . C12B C -0.3750(6) 1.4265(9) 0.0284(5) 0.035(3) Uani 1 1 d U . . C12A C -0.4588(5) 1.1141(8) 0.0329(5) 0.027(3) Uani 1 1 d . . . C12C C -0.3744(5) 1.2421(8) -0.1041(5) 0.026(3) Uani 1 1 d . . . C13A C -0.4310(6) 1.0598(8) 0.0870(5) 0.039(3) Uani 1 1 d . . . H13A H -0.3889 1.0348 0.0982 0.047 Uiso 1 1 calc R . . C13B C -0.3096(6) 1.4363(8) 0.0651(5) 0.038(3) Uani 1 1 d . . . H13B H -0.2833 1.3811 0.0748 0.046 Uiso 1 1 calc R . . C13C C -0.4016(6) 1.1627(8) -0.1407(5) 0.034(3) Uani 1 1 d . . . H13C H -0.3887 1.1007 -0.1246 0.041 Uiso 1 1 calc R . . C14A C -0.4654(6) 1.0428(8) 0.1239(6) 0.040(3) Uani 1 1 d . . . H14A H -0.4463 1.0064 0.1606 0.048 Uiso 1 1 calc R . . C14B C -0.2819(7) 1.5230(10) 0.0876(6) 0.055(4) Uani 1 1 d . . . H14B H -0.2376 1.5266 0.1137 0.066 Uiso 1 1 calc R . . C14C C -0.4475(6) 1.1738(9) -0.2006(5) 0.040(3) Uani 1 1 d . . . H14C H -0.4651 1.1195 -0.2255 0.048 Uiso 1 1 calc R . . C15A C -0.5269(6) 1.0776(9) 0.1085(6) 0.043(3) Uani 1 1 d . . . H15A H -0.5499 1.0658 0.1344 0.052 Uiso 1 1 calc R . . C15B C -0.3186(9) 1.6041(11) 0.0722(6) 0.068(5) Uani 1 1 d . . . H15B H -0.3002 1.6645 0.0867 0.082 Uiso 1 1 calc R . . C15C C -0.4667(5) 1.2614(10) -0.2230(5) 0.040(3) Uani 1 1 d . . . H15C H -0.4991 1.2681 -0.2633 0.047 Uiso 1 1 calc R . . C16B C -0.3831(9) 1.5958(11) 0.0349(7) 0.088(6) Uani 1 1 d . . . H16B H -0.4086 1.6517 0.0235 0.105 Uiso 1 1 calc R . . C16A C -0.5545(6) 1.1301(9) 0.0545(6) 0.045(3) Uani 1 1 d . . . H16B H -0.5971 1.1537 0.0427 0.054 Uiso 1 1 calc R . . C16C C -0.4401(5) 1.3430(8) -0.1882(5) 0.032(3) Uani 1 1 d . . . H16C H -0.4536 1.4046 -0.2047 0.039 Uiso 1 1 calc R . . C17A C -0.5203(6) 1.1478(8) 0.0181(6) 0.036(3) Uani 1 1 d . . . H17A H -0.5396 1.1846 -0.0184 0.043 Uiso 1 1 calc R . . C17B C -0.4112(7) 1.5103(10) 0.0141(6) 0.066(5) Uani 1 1 d . . . H17B H -0.4559 1.5075 -0.0105 0.079 Uiso 1 1 calc R . . C17C C -0.3936(5) 1.3315(8) -0.1293(5) 0.030(3) Uani 1 1 d . . . H17C H -0.3745 1.3863 -0.1056 0.036 Uiso 1 1 calc R . . C21A C -0.1851(5) 0.8170(5) 0.2148(5) 0.034(3) Uani 1 1 d D . . H21P H -0.1845 0.8155 0.1727 0.040 Uiso 1 1 calc R . . H21Q H -0.1558 0.7665 0.2394 0.040 Uiso 1 1 calc R . . C21B C -0.0765(3) 0.9355(8) 0.2386(5) 0.031(3) Uani 1 1 d D . . H21R H -0.0514 0.8779 0.2577 0.037 Uiso 1 1 calc R . . H21S H -0.0859 0.9332 0.1937 0.037 Uiso 1 1 calc R . . C21C C -0.1296(6) 0.9175(8) 0.3349(2) 0.034(3) Uani 1 1 d D . . H21T H -0.0943 0.9628 0.3558 0.041 Uiso 1 1 calc R . . H21U H -0.1666 0.9371 0.3451 0.041 Uiso 1 1 calc R . . C22A C -0.2508(6) 0.7943(7) 0.2101(5) 0.035(3) Uani 1 1 d . . . C22B C -0.0365(5) 1.0217(9) 0.2656(5) 0.036(3) Uani 1 1 d . . . C22C C -0.1079(5) 0.8202(8) 0.3639(5) 0.029(3) Uani 1 1 d . . . C23A C -0.2631(7) 0.7251(9) 0.2457(6) 0.053(4) Uani 1 1 d . . . H23A H -0.2278 0.6917 0.2748 0.063 Uiso 1 1 calc R . . C23B C 0.0135(6) 1.0231(9) 0.3239(6) 0.042(3) Uani 1 1 d . . . H23B H 0.0227 0.9668 0.3482 0.050 Uiso 1 1 calc R . . C23C C -0.0479(6) 0.7824(8) 0.3688(5) 0.034(3) Uani 1 1 d . . . H23C H -0.0212 0.8169 0.3529 0.041 Uiso 1 1 calc R . . C24A C -0.3237(8) 0.7023(11) 0.2411(7) 0.067(5) Uani 1 1 d . . . H24A H -0.3297 0.6533 0.2663 0.081 Uiso 1 1 calc R . . C24B C 0.0500(6) 1.1030(11) 0.3475(6) 0.052(4) Uani 1 1 d . . . H24B H 0.0846 1.1002 0.3867 0.062 Uiso 1 1 calc R . . C24C C -0.0279(6) 0.6941(10) 0.3971(6) 0.050(4) Uani 1 1 d . . . H24C H 0.0107 0.6662 0.3976 0.060 Uiso 1 1 calc R . . C25A C -0.3754(8) 0.7491(11) 0.2008(7) 0.061(4) Uani 1 1 d . . . H25A H -0.4175 0.7343 0.1983 0.073 Uiso 1 1 calc R . . C25B C 0.0367(6) 1.1879(10) 0.3145(7) 0.053(4) Uani 1 1 d . . . H25B H 0.0618 1.2429 0.3313 0.064 Uiso 1 1 calc R . . C25C C -0.0634(7) 0.6483(9) 0.4238(6) 0.052(4) Uani 1 1 d . . . H25C H -0.0480 0.5904 0.4453 0.062 Uiso 1 1 calc R . . C26A C -0.3663(6) 0.8178(9) 0.1638(6) 0.045(3) Uani 1 1 d . . . H26A H -0.4023 0.8511 0.1355 0.054 Uiso 1 1 calc R . . C26B C -0.0123(6) 1.1917(9) 0.2580(7) 0.055(4) Uani 1 1 d . . . H26B H -0.0224 1.2495 0.2353 0.066 Uiso 1 1 calc R . . C26C C -0.1216(7) 0.6841(10) 0.4204(6) 0.051(4) Uani 1 1 d . . . H26C H -0.1471 0.6501 0.4378 0.061 Uiso 1 1 calc R . . C27A C -0.3053(6) 0.8392(8) 0.1671(5) 0.041(3) Uani 1 1 d . . . H27A H -0.3000 0.8853 0.1397 0.049 Uiso 1 1 calc R . . C27B C -0.0486(5) 1.1070(9) 0.2333(5) 0.038(3) Uani 1 1 d . . . H27B H -0.0822 1.1094 0.1934 0.046 Uiso 1 1 calc R . . C27C C -0.1427(6) 0.7717(10) 0.3906(5) 0.042(3) Uani 1 1 d . . . H27C H -0.1822 0.7975 0.3892 0.051 Uiso 1 1 calc R . . C31A C -0.3815(4) 1.3531(7) 0.1729(4) 0.023(3) Uani 1 1 d D . . C31B C -0.2405(4) 1.3642(7) 0.2308(4) 0.026(3) Uani 1 1 d D . . C32A C -0.3830(5) 1.4530(8) 0.1766(5) 0.033(3) Uani 1 1 d . . . H32A H -0.3439 1.4880 0.1914 0.039 Uiso 1 1 calc R . . C32B C -0.2366(5) 1.4233(7) 0.2794(5) 0.027(3) Uani 1 1 d . . . H32B H -0.2700 1.4217 0.2949 0.033 Uiso 1 1 calc R . . C33A C -0.4407(5) 1.4999(9) 0.1589(5) 0.038(3) Uani 1 1 d . . . H33A H -0.4413 1.5673 0.1615 0.046 Uiso 1 1 calc R . . C33B C -0.1860(6) 1.4839(8) 0.3056(6) 0.045(3) Uani 1 1 d . . . H33B H -0.1835 1.5225 0.3398 0.054 Uiso 1 1 calc R . . C34A C -0.4978(6) 1.4505(8) 0.1375(5) 0.036(3) Uani 1 1 d . . . H34A H -0.5375 1.4832 0.1270 0.043 Uiso 1 1 calc R . . C34B C -0.1377(6) 1.4884(9) 0.2814(7) 0.055(4) Uani 1 1 d . . . H34B H -0.1032 1.5322 0.2977 0.066 Uiso 1 1 calc R . . C35A C -0.4970(5) 1.3527(8) 0.1314(5) 0.032(3) Uani 1 1 d . . . H35A H -0.5362 1.3183 0.1147 0.039 Uiso 1 1 calc R . . C35B C -0.1415(5) 1.4283(9) 0.2338(6) 0.039(3) Uani 1 1 d . . . H35B H -0.1085 1.4301 0.2179 0.046 Uiso 1 1 calc R . . C36A C -0.4405(5) 1.3067(8) 0.1493(4) 0.030(3) Uani 1 1 d . . . H36A H -0.4409 1.2394 0.1456 0.036 Uiso 1 1 calc R . . C36B C -0.1912(5) 1.3661(9) 0.2087(5) 0.036(3) Uani 1 1 d . . . H36B H -0.1921 1.3243 0.1765 0.043 Uiso 1 1 calc R . . C41A C -0.2696(5) 1.0457(6) 0.3326(4) 0.026(3) Uani 1 1 d D . . C41B C -0.1835(4) 1.2053(6) 0.3467(4) 0.025(3) Uani 1 1 d D . . C42A C -0.3183(5) 0.9828(8) 0.2991(5) 0.032(3) Uani 1 1 d . . . H42A H -0.3356 0.9849 0.2551 0.039 Uiso 1 1 calc R . . C42B C -0.1228(5) 1.2157(8) 0.3441(5) 0.032(3) Uani 1 1 d . . . H42B H -0.1119 1.1814 0.3145 0.038 Uiso 1 1 calc R . . C43A C -0.3419(6) 0.9166(9) 0.3297(6) 0.049(4) Uani 1 1 d . . . H43A H -0.3762 0.8754 0.3066 0.059 Uiso 1 1 calc R . . C43B C -0.0791(6) 1.2765(9) 0.3851(6) 0.046(3) Uani 1 1 d . . . H43B H -0.0385 1.2865 0.3825 0.055 Uiso 1 1 calc R . . C44C C -0.3151(6) 0.9110(9) 0.3948(6) 0.040(3) Uani 1 1 d . . . H44C H -0.3302 0.8650 0.4158 0.047 Uiso 1 1 calc R . . C44B C -0.0940(6) 1.3228(9) 0.4296(5) 0.040(3) Uani 1 1 d . . . H44B H -0.0628 1.3633 0.4581 0.048 Uiso 1 1 calc R . . C45B C -0.1526(6) 1.3123(8) 0.4341(5) 0.036(3) Uani 1 1 d . . . H45B H -0.1622 1.3449 0.4651 0.044 Uiso 1 1 calc R . . C45C C -0.2671(6) 0.9722(9) 0.4271(5) 0.037(3) Uani 1 1 d . . . H45C H -0.2495 0.9694 0.4711 0.044 Uiso 1 1 calc R . . C46B C -0.1968(5) 1.2540(7) 0.3930(5) 0.027(3) Uani 1 1 d . . . H46B H -0.2376 1.2461 0.3956 0.032 Uiso 1 1 calc R . . C46A C -0.2438(5) 1.0378(8) 0.3977(5) 0.035(3) Uani 1 1 d . . . H46A H -0.2097 1.0787 0.4216 0.042 Uiso 1 1 calc R . . O1M O -0.3131(5) 0.9707(8) -0.0580(5) 0.078(3) Uani 1 1 d . . . C1M C -0.2702(8) 0.9655(14) -0.0851(8) 0.087(6) Uani 1 1 d . . . O2M O -0.0572(8) 0.9551(15) 0.0775(8) 0.168(8) Uani 1 1 d . . . C2M C -0.0967(11) 1.0173(17) 0.0374(7) 0.014(7) Uiso 0.61(7) 1 d P A 1 C2M' C -0.122(2) 0.983(3) 0.0334(15) 0.035(13) Uiso 0.39(7) 1 d P A 2 C4M C -0.2060(11) 0.7521(18) 0.0284(11) 0.081(9) Uiso 0.77(3) 1 d P B 1 C4M' C -0.262(3) 0.803(4) 0.017(2) 0.04(2) Uiso 0.23(3) 1 d P B 2 O4 O -0.1812(11) 0.8153(18) 0.0700(9) 0.227(10) Uani 1 1 d . . . C1B C 0.0486(6) 0.9316(10) 0.5198(6) 0.051(4) Uiso 1 1 d . . . C2B C 0.0647(7) 1.0235(11) 0.5069(6) 0.056(4) Uiso 1 1 d . . . C3B C -0.0155(7) 0.9067(10) 0.5115(6) 0.054(4) Uiso 1 1 d . . . O3M O -0.1396(9) 1.3324(12) 0.0717(8) 0.157(6) Uiso 1 1 d . . . C3M C -0.1154(6) 1.2809(10) 0.1208(6) 0.026(4) Uiso 0.77(2) 1 d P C 1 C3M' C -0.1925(17) 1.289(2) 0.0593(15) 0.000(11) Uiso 0.23(2) 1 d P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0278(5) 0.0196(5) 0.0205(4) -0.0005(4) 0.0071(4) 0.0028(4) Pd2 0.0276(5) 0.0209(5) 0.0215(4) 0.0011(4) 0.0077(4) 0.0046(4) P1 0.0332(17) 0.0231(16) 0.0191(15) 0.0003(13) 0.0084(13) 0.0039(14) P2 0.0311(17) 0.0230(16) 0.0291(16) 0.0013(14) 0.0104(13) 0.0058(15) P3 0.0240(15) 0.0189(15) 0.0193(14) 0.0002(13) 0.0044(12) 0.0029(13) P4 0.0238(16) 0.0239(16) 0.0210(15) -0.0020(13) 0.0067(13) -0.0001(13) S1 0.0449(18) 0.0232(15) 0.0265(15) 0.0007(14) 0.0165(14) 0.0087(15) O1 0.071(6) 0.034(5) 0.028(4) -0.002(4) 0.018(4) 0.001(5) O2 0.045(5) 0.042(5) 0.044(5) 0.013(4) 0.029(4) 0.015(4) C1 0.017(6) 0.034(7) 0.030(6) -0.001(5) 0.010(5) 0.002(5) C11A 0.030(7) 0.032(7) 0.027(6) -0.010(6) 0.002(5) -0.002(6) C11B 0.047(7) 0.030(7) 0.028(6) -0.001(6) 0.024(6) 0.004(6) C11C 0.033(7) 0.030(7) 0.031(7) 0.000(6) 0.016(6) -0.004(6) C12B 0.043(5) 0.037(5) 0.022(4) 0.006(4) 0.010(4) 0.007(4) C12A 0.027(7) 0.019(6) 0.033(7) -0.009(5) 0.011(5) -0.007(5) C12C 0.025(6) 0.027(7) 0.025(6) -0.004(5) 0.008(5) 0.008(5) C13A 0.053(8) 0.027(7) 0.045(8) 0.002(6) 0.026(7) -0.002(7) C13B 0.067(9) 0.015(6) 0.033(7) 0.003(6) 0.019(7) 0.004(6) C13C 0.053(8) 0.025(7) 0.034(7) -0.005(6) 0.027(6) -0.006(6) C14A 0.046(8) 0.028(7) 0.042(8) 0.002(6) 0.012(7) -0.007(6) C14B 0.069(10) 0.048(9) 0.040(8) -0.008(8) 0.012(7) -0.009(8) C14C 0.059(9) 0.034(8) 0.030(7) -0.012(6) 0.022(7) -0.016(7) C15A 0.046(8) 0.034(8) 0.058(9) -0.009(7) 0.030(7) -0.017(7) C15B 0.111(14) 0.036(9) 0.039(9) -0.011(7) 0.008(9) -0.015(10) C15C 0.030(7) 0.061(10) 0.025(7) -0.005(7) 0.008(6) -0.010(7) C16B 0.127(17) 0.035(10) 0.064(11) -0.010(9) -0.004(11) 0.039(10) C16A 0.048(8) 0.035(8) 0.052(9) -0.013(7) 0.018(7) -0.023(7) C16C 0.032(7) 0.032(7) 0.029(6) 0.002(6) 0.008(6) 0.013(6) C17A 0.040(8) 0.021(7) 0.045(7) -0.003(6) 0.014(6) -0.016(6) C17B 0.071(11) 0.045(10) 0.055(10) -0.008(8) -0.006(8) 0.035(9) C17C 0.020(6) 0.035(7) 0.033(7) -0.006(6) 0.008(5) -0.003(6) C21A 0.033(7) 0.021(6) 0.036(7) -0.007(6) 0.001(6) 0.008(6) C21B 0.036(7) 0.028(6) 0.024(6) 0.002(6) 0.006(5) 0.009(6) C21C 0.039(7) 0.039(8) 0.022(6) 0.002(6) 0.009(5) 0.007(6) C22A 0.054(8) 0.006(6) 0.030(7) -0.008(5) 0.000(6) 0.005(6) C22B 0.034(7) 0.054(8) 0.025(6) 0.010(6) 0.018(6) 0.008(7) C22C 0.033(7) 0.026(6) 0.022(6) -0.001(5) 0.004(5) 0.000(6) C23A 0.047(9) 0.029(8) 0.062(10) -0.005(7) -0.002(7) -0.005(7) C23B 0.039(8) 0.034(7) 0.043(8) 0.008(6) 0.004(6) 0.007(7) C23C 0.049(8) 0.015(6) 0.035(7) -0.001(5) 0.013(6) 0.007(6) C24A 0.087(13) 0.043(10) 0.056(10) 0.006(8) 0.011(9) -0.018(9) C24B 0.035(8) 0.072(11) 0.042(8) 0.012(8) 0.007(6) -0.008(8) C24C 0.042(8) 0.046(9) 0.048(8) 0.012(7) 0.002(7) 0.016(7) C25A 0.069(11) 0.051(10) 0.067(11) -0.028(9) 0.031(9) -0.037(9) C25B 0.044(8) 0.053(9) 0.067(10) 0.014(8) 0.028(8) -0.011(8) C25C 0.064(10) 0.030(8) 0.042(8) 0.008(7) -0.001(8) -0.004(8) C26A 0.032(7) 0.036(8) 0.055(8) -0.015(7) 0.003(6) -0.010(7) C26B 0.037(8) 0.031(8) 0.094(11) 0.019(8) 0.022(8) -0.017(7) C26C 0.053(9) 0.050(9) 0.039(8) 0.012(7) 0.005(7) -0.011(8) C27A 0.065(9) 0.019(7) 0.037(7) 0.004(6) 0.018(7) 0.005(7) C27B 0.031(7) 0.047(8) 0.034(7) 0.002(7) 0.010(6) -0.012(6) C27C 0.030(7) 0.063(9) 0.036(7) 0.014(7) 0.015(6) -0.001(7) C31A 0.030(7) 0.023(6) 0.013(5) -0.003(5) 0.007(5) 0.010(5) C31B 0.030(7) 0.021(6) 0.018(6) 0.001(5) 0.000(5) 0.000(5) C32A 0.029(7) 0.021(7) 0.036(7) 0.010(5) 0.000(5) 0.012(5) C32B 0.033(7) 0.022(6) 0.020(6) 0.000(5) 0.004(5) -0.004(5) C33A 0.035(7) 0.026(7) 0.042(7) 0.001(6) 0.003(6) 0.010(6) C33B 0.059(9) 0.015(6) 0.043(8) -0.014(6) -0.001(7) -0.008(7) C34A 0.032(7) 0.035(8) 0.030(7) -0.004(6) 0.000(6) 0.013(6) C34B 0.032(8) 0.032(8) 0.071(10) 0.018(8) -0.014(7) -0.016(7) C35A 0.022(6) 0.038(8) 0.030(7) 0.003(6) 0.004(5) 0.013(6) C35B 0.029(7) 0.037(8) 0.050(8) 0.006(7) 0.016(6) -0.007(6) C36A 0.046(8) 0.024(6) 0.019(6) 0.000(5) 0.011(5) 0.005(6) C36B 0.031(7) 0.051(8) 0.024(6) -0.002(6) 0.008(6) 0.005(7) C41A 0.023(6) 0.019(6) 0.035(7) -0.005(5) 0.011(5) 0.006(5) C41B 0.033(7) 0.018(6) 0.022(6) 0.011(5) 0.009(5) 0.008(5) C42A 0.046(8) 0.022(6) 0.028(6) 0.003(6) 0.013(6) 0.000(6) C42B 0.038(7) 0.021(6) 0.038(7) 0.001(6) 0.015(6) 0.004(6) C43A 0.051(9) 0.027(8) 0.067(10) 0.000(7) 0.021(8) -0.001(7) C43B 0.032(8) 0.048(9) 0.051(8) -0.001(7) 0.008(7) -0.009(7) C44C 0.032(7) 0.038(8) 0.050(8) 0.016(7) 0.017(6) 0.005(6) C44B 0.042(8) 0.033(7) 0.037(7) 0.003(6) 0.006(6) -0.011(7) C45B 0.058(9) 0.022(7) 0.019(6) -0.017(6) 0.003(6) -0.008(7) C45C 0.039(7) 0.043(8) 0.033(7) 0.027(6) 0.018(6) 0.013(7) C46B 0.039(7) 0.017(6) 0.027(6) 0.005(5) 0.016(6) 0.004(5) C46A 0.033(7) 0.038(8) 0.027(6) 0.006(6) 0.006(6) 0.002(6) O1M 0.051(6) 0.109(9) 0.068(7) 0.002(7) 0.017(6) 0.012(6) C1M 0.086(12) 0.120(16) 0.080(12) 0.018(11) 0.057(11) 0.041(12) O2M 0.142(14) 0.23(2) 0.171(16) -0.061(16) 0.103(13) -0.010(15) O4 0.25(3) 0.26(3) 0.129(16) -0.033(18) 0.031(16) 0.04(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S1 2.239(2) . ? Pd1 P3 2.322(2) . ? Pd1 P1 2.325(2) . ? Pd1 Pd2 2.6704(14) . ? Pd2 S1 2.240(3) . ? Pd2 P2 2.326(2) . ? Pd2 P4 2.324(2) . ? P1 C11B 1.851(4) . ? P1 C11A 1.851(4) . ? P1 C11C 1.851(4) . ? P2 C21B 1.851(4) . ? P2 C21A 1.851(4) . ? P2 C21C 1.851(5) . ? P3 C31B 1.833(6) . ? P3 C1 1.832(10) . ? P3 C31A 1.836(6) . ? P4 C41A 1.835(6) . ? P4 C1 1.858(10) . ? P4 C41B 1.836(6) . ? S1 O1 1.495(8) . ? S1 O2 1.497(8) . ? C11A C12A 1.505(14) . ? C11B C12B 1.490(15) . ? C11C C12C 1.513(14) . ? C12B C13B 1.398(16) . ? C12B C17B 1.398(16) . ? C12A C17A 1.376(15) . ? C12A C13A 1.403(16) . ? C12C C17C 1.387(15) . ? C12C C13C 1.397(15) . ? C13A C14A 1.381(16) . ? C13B C14B 1.380(17) . ? C13C C14C 1.396(16) . ? C14A C15A 1.379(16) . ? C14B C15B 1.374(19) . ? C14C C15C 1.344(17) . ? C15A C16A 1.388(17) . ? C15B C16B 1.38(2) . ? C15C C16C 1.402(16) . ? C16B C17B 1.36(2) . ? C16A C17A 1.371(16) . ? C16C C17C 1.384(15) . ? C21A C22A 1.474(15) . ? C21B C22B 1.498(16) . ? C21C C22C 1.522(15) . ? C22A C23A 1.376(17) . ? C22A C27A 1.403(16) . ? C22B C27B 1.389(16) . ? C22B C23B 1.396(16) . ? C22C C27C 1.357(15) . ? C22C C23C 1.416(15) . ? C23A C24A 1.365(19) . ? C23B C24B 1.376(17) . ? C23C C24C 1.398(16) . ? C24A C25A 1.35(2) . ? C24B C25B 1.390(18) . ? C24C C25C 1.349(17) . ? C25A C26A 1.363(18) . ? C25B C26B 1.360(18) . ? C25C C26C 1.376(18) . ? C26A C27A 1.378(16) . ? C26B C27B 1.435(17) . ? C26C C27C 1.404(17) . ? C31A C36A 1.390(14) . ? C31A C32A 1.409(14) . ? C31B C32B 1.383(14) . ? C31B C36B 1.390(14) . ? C32A C33A 1.372(15) . ? C32B C33B 1.365(15) . ? C33A C34A 1.376(15) . ? C33B C34B 1.405(18) . ? C34A C35A 1.383(16) . ? C34B C35B 1.375(18) . ? C35A C36A 1.343(14) . ? C35B C36B 1.363(16) . ? C41A C46A 1.410(14) . ? C41A C42A 1.394(14) . ? C41B C42B 1.398(14) . ? C41B C46B 1.404(13) . ? C42A C43A 1.397(16) . ? C42B C43B 1.377(16) . ? C43A C44C 1.407(17) . ? C43B C44B 1.374(17) . ? C44C C45C 1.362(16) . ? C44B C45B 1.368(16) . ? C45B C46B 1.362(15) . ? C45C C46A 1.370(15) . ? O1M C1M 1.343(16) . ? O2M C2M 1.34(2) . ? O2M C2M' 1.49(4) . ? C4M O4 1.28(3) . ? C4M' O4 1.78(6) . ? C1B C2B 1.405(18) . ? C1B C3B 1.425(17) . ? C2B C3B 1.418(18) 3_576 ? C3B C2B 1.418(18) 3_576 ? O3M C3M' 1.27(3) . ? O3M C3M 1.289(19) . ? 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 P3 144.46(9) . . ? S1 Pd1 P1 104.53(10) . . ? P3 Pd1 P1 110.99(10) . . ? S1 Pd1 Pd2 53.43(5) . . ? P3 Pd1 Pd2 92.09(8) . . ? P1 Pd1 Pd2 154.57(8) . . ? S1 Pd2 P2 104.56(9) . . ? S1 Pd2 P4 148.40(9) . . ? P2 Pd2 P4 106.61(11) . . ? S1 Pd2 Pd1 53.37(5) . . ? P2 Pd2 Pd1 157.47(8) . . ? P4 Pd2 Pd1 95.10(8) . . ? C11B P1 C11A 102.0(5) . . ? C11B P1 C11C 103.4(5) . . ? C11A P1 C11C 102.5(5) . . ? C11B P1 Pd1 120.0(4) . . ? C11A P1 Pd1 109.1(4) . . ? C11C P1 Pd1 117.5(4) . . ? C21B P2 C21A 99.8(5) . . ? C21B P2 C21C 104.8(5) . . ? C21A P2 C21C 106.1(5) . . ? C21B P2 Pd2 112.5(4) . . ? C21A P2 Pd2 117.0(4) . . ? C21C P2 Pd2 114.9(4) . . ? C31B P3 C1 105.7(5) . . ? C31B P3 C31A 106.5(5) . . ? C1 P3 C31A 100.1(5) . . ? C31B P3 Pd1 112.3(4) . . ? C1 P3 Pd1 110.4(4) . . ? C31A P3 Pd1 120.3(3) . . ? C41A P4 C1 101.3(5) . . ? C41A P4 C41B 104.3(5) . . ? C1 P4 C41B 102.4(5) . . ? C41A P4 Pd2 115.8(3) . . ? C1 P4 Pd2 112.0(3) . . ? C41B P4 Pd2 118.8(3) . . ? O1 S1 O2 109.8(5) . . ? O1 S1 Pd1 119.6(4) . . ? O2 S1 Pd1 113.7(3) . . ? O1 S1 Pd2 117.9(3) . . ? O2 S1 Pd2 118.7(3) . . ? Pd1 S1 Pd2 73.19(9) . . ? P3 C1 P4 108.8(5) . . ? C12A C11A P1 113.0(7) . . ? C12B C11B P1 117.9(7) . . ? C12C C11C P1 115.1(7) . . ? C13B C12B C17B 116.4(12) . . ? C13B C12B C11B 125.1(10) . . ? C17B C12B C11B 118.4(11) . . ? C17A C12A C13A 118.2(11) . . ? C17A C12A C11A 121.6(10) . . ? C13A C12A C11A 120.2(10) . . ? C17C C12C C13C 118.2(10) . . ? C17C C12C C11C 121.2(10) . . ? C13C C12C C11C 120.7(10) . . ? C14A C13A C12A 119.6(12) . . ? C14B C13B C12B 122.5(12) . . ? C12C C13C C14C 120.5(11) . . ? C15A C14A C13A 121.4(12) . . ? C13B C14B C15B 119.6(13) . . ? C15C C14C C13C 119.9(11) . . ? C14A C15A C16A 118.8(12) . . ? C16B C15B C14B 118.5(14) . . ? C14C C15C C16C 121.5(11) . . ? C17B C16B C15B 122.2(14) . . ? C17A C16A C15A 119.9(13) . . ? C17C C16C C15C 118.3(11) . . ? C12A C17A C16A 122.1(12) . . ? C16B C17B C12B 120.7(14) . . ? C16C C17C C12C 121.6(11) . . ? C22A C21A P2 115.5(7) . . ? C22B C21B P2 113.3(7) . . ? C22C C21C P2 119.8(7) . . ? C23A C22A C27A 115.4(12) . . ? C23A C22A C21A 122.3(11) . . ? C27A C22A C21A 122.2(11) . . ? C27B C22B C23B 115.8(12) . . ? C27B C22B C21B 120.6(10) . . ? C23B C22B C21B 123.6(11) . . ? C27C C22C C23C 118.3(11) . . ? C27C C22C C21C 121.0(11) . . ? C23C C22C C21C 120.4(10) . . ? C24A C23A C22A 123.0(13) . . ? C24B C23B C22B 122.5(12) . . ? C22C C23C C24C 119.7(12) . . ? C23A C24A C25A 120.4(14) . . ? C23B C24B C25B 120.7(12) . . ? C25C C24C C23C 120.2(13) . . ? C26A C25A C24A 119.3(14) . . ? C26B C25B C24B 119.7(13) . . ? C24C C25C C26C 121.1(13) . . ? C25A C26A C27A 120.4(13) . . ? C25B C26B C27B 118.9(13) . . ? C27C C26C C25C 118.9(12) . . ? C26A C27A C22A 121.4(12) . . ? C22B C27B C26B 122.3(12) . . ? C22C C27C C26C 121.6(12) . . ? C36A C31A C32A 116.8(8) . . ? C36A C31A P3 118.7(8) . . ? C32A C31A P3 124.5(8) . . ? C32B C31B C36B 119.0(8) . . ? C32B C31B P3 122.9(8) . . ? C36B C31B P3 118.1(8) . . ? C33A C32A C31A 120.2(11) . . ? C33B C32B C31B 121.6(11) . . ? C34A C33A C32A 120.8(11) . . ? C32B C33B C34B 119.2(12) . . ? C33A C34A C35A 119.5(11) . . ? C35B C34B C33B 118.7(11) . . ? C36A C35A C34A 119.7(12) . . ? C36B C35B C34B 121.9(11) . . ? C35A C36A C31A 123.0(11) . . ? C35B C36B C31B 119.5(11) . . ? C46A C41A C42A 117.9(8) . . ? C46A C41A P4 125.3(8) . . ? C42A C41A P4 116.9(7) . . ? C42B C41B C46B 118.7(8) . . ? C42B C41B P4 118.1(8) . . ? C46B C41B P4 123.1(8) . . ? C43A C42A C41A 120.4(10) . . ? C43B C42B C41B 118.9(11) . . ? C42A C43A C44C 120.1(12) . . ? C42B C43B C44B 120.4(12) . . ? C45C C44C C43A 119.1(11) . . ? C45B C44B C43B 121.8(12) . . ? C44B C45B C46B 118.4(11) . . ? C44C C45C C46A 121.4(11) . . ? C45B C46B C41B 121.7(10) . . ? C45C C46A C41A 121.1(11) . . ? C2M O2M C2M' 29.2(15) . . ? C4M O4 C4M' 51(2) . . ? C2B C1B C3B 121.9(13) . . ? C1B C2B C3B 117.8(12) . 3_576 ? C2B C3B C1B 120.2(13) 3_576 . ? C3M' O3M C3M 89(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.236 _refine_diff_density_min -1.244 _refine_diff_density_rms 0.163 data_sy173 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H44 Cl2 O2 P2 Pd S' _chemical_formula_weight 864.08 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.931(3) _cell_length_b 11.331(2) _cell_length_c 19.275(4) _cell_angle_alpha 84.427(12) _cell_angle_beta 87.305(16) _cell_angle_gamma 64.216(14) _cell_volume 1943.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 39 _cell_measurement_theta_min 4.64 _cell_measurement_theta_max 12.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.788 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.388193 _exptl_absorpt_correction_T_max 0.789350 _exptl_absorpt_process_details ? _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_type ? _diffrn_measurement_method 'Theta/2 theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 83.13 _diffrn_reflns_number 5108 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 21.00 _reflns_number_total 4178 _reflns_number_gt 3452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+39.1163P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4178 _refine_ls_number_parameters 460 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1098 _refine_ls_R_factor_gt 0.0870 _refine_ls_wR_factor_ref 0.2344 _refine_ls_wR_factor_gt 0.2234 _refine_ls_goodness_of_fit_ref 1.249 _refine_ls_restrained_S_all 1.246 _refine_ls_shift/su_max 0.110 _refine_ls_shift/su_mean 0.012 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd -0.14084(12) -0.27366(11) 0.25415(6) 0.0259(4) Uani 1 1 d D . . P1 P 0.0302(4) -0.3109(3) 0.16371(18) 0.0261(9) Uani 1 1 d D . . P2 P -0.3462(4) -0.2563(3) 0.32324(18) 0.0250(9) Uani 1 1 d D . . S1 S -0.1127(4) -0.1021(4) 0.2933(2) 0.0357(10) Uani 1 1 d . . . O1 O -0.1778(18) 0.0034(11) 0.2404(7) 0.081(5) Uani 1 1 d . . . O2 O 0.0485(15) -0.1444(13) 0.3005(7) 0.068(4) Uani 1 1 d . . . C11A C 0.2288(12) -0.3633(12) 0.1838(7) 0.031(4) Uani 1 1 d D . . H11C H 0.2856 -0.3718 0.1407 0.037 Uiso 1 1 calc R . . H11D H 0.2385 -0.2969 0.2086 0.037 Uiso 1 1 calc R . . C12A C 0.2911(15) -0.4922(12) 0.2274(7) 0.032(4) Uani 1 1 d D . . C13A C 0.3782(17) -0.6106(15) 0.1992(9) 0.039(4) Uani 1 1 d . . . H13A H 0.4023 -0.6111 0.1520 0.047 Uiso 1 1 calc R . . C14A C 0.4287(19) -0.7269(16) 0.2407(11) 0.053(5) Uani 1 1 d . . . H14A H 0.4897 -0.8054 0.2217 0.064 Uiso 1 1 calc R . . C15A C 0.3902(16) -0.7282(15) 0.3094(10) 0.039(4) Uani 1 1 d . . . H15A H 0.4226 -0.8079 0.3366 0.046 Uiso 1 1 calc R . . C16A C 0.3053(18) -0.6147(17) 0.3385(9) 0.047(5) Uani 1 1 d . . . H16A H 0.2814 -0.6168 0.3857 0.057 Uiso 1 1 calc R . . C17A C 0.2530(16) -0.4939(15) 0.2979(8) 0.036(4) Uani 1 1 d . . . H17A H 0.1938 -0.4160 0.3178 0.043 Uiso 1 1 calc R . . C11B C 0.0414(12) -0.4408(13) 0.1107(8) 0.033(4) Uani 1 1 d D . . H11E H 0.0865 -0.4313 0.0660 0.039 Uiso 1 1 calc R . . H11F H 0.1062 -0.5256 0.1337 0.039 Uiso 1 1 calc R . . C12B C -0.1077(11) -0.4383(13) 0.0986(8) 0.024(4) Uani 1 1 d D . . C13B C -0.1836(17) -0.3856(14) 0.0362(8) 0.036(4) Uani 1 1 d . . . H13B H -0.1413 -0.3490 0.0016 0.043 Uiso 1 1 calc R . . C14B C -0.3197(16) -0.3852(16) 0.0237(9) 0.039(4) Uani 1 1 d . . . H14B H -0.3668 -0.3505 -0.0190 0.046 Uiso 1 1 calc R . . C15B C -0.3845(17) -0.4364(16) 0.0748(9) 0.043(4) Uani 1 1 d . . . H15B H -0.4761 -0.4366 0.0671 0.052 Uiso 1 1 calc R . . C16B C -0.3137(19) -0.4870(15) 0.1369(8) 0.040(4) Uani 1 1 d . . . H16B H -0.3584 -0.5204 0.1719 0.048 Uiso 1 1 calc R . . C17B C -0.1772(19) -0.4894(14) 0.1487(8) 0.039(4) Uani 1 1 d . . . H17B H -0.1303 -0.5263 0.1912 0.046 Uiso 1 1 calc R . . C11C C -0.0196(15) -0.1639(12) 0.1020(7) 0.036(4) Uani 1 1 d D . . H11A H -0.1173 -0.1421 0.0832 0.044 Uiso 1 1 calc R . . H11B H -0.0300 -0.0917 0.1283 0.044 Uiso 1 1 calc R . . C12C C 0.0832(14) -0.1688(13) 0.0417(7) 0.027(4) Uani 1 1 d D . . C13C C 0.0504(18) -0.1918(15) -0.0241(8) 0.038(4) Uani 1 1 d . . . H13C H -0.0335 -0.2059 -0.0304 0.046 Uiso 1 1 calc R . . C14C C 0.145(2) -0.1933(16) -0.0800(9) 0.052(5) Uani 1 1 d . . . H14C H 0.1241 -0.2074 -0.1241 0.062 Uiso 1 1 calc R . . C15C C 0.2715(17) -0.1737(15) -0.0699(9) 0.041(4) Uani 1 1 d . . . H15C H 0.3353 -0.1759 -0.1072 0.049 Uiso 1 1 calc R . . C16C C 0.3018(18) -0.1514(16) -0.0064(9) 0.044(4) Uani 1 1 d . . . H16C H 0.3857 -0.1372 -0.0002 0.052 Uiso 1 1 calc R . . C17C C 0.2112(17) -0.1497(15) 0.0483(8) 0.037(4) Uani 1 1 d . . . H17C H 0.2350 -0.1352 0.0918 0.045 Uiso 1 1 calc R . . C21A C -0.4189(16) -0.1138(12) 0.3755(7) 0.036(4) Uani 1 1 d D . . H21C H -0.3359 -0.1177 0.4018 0.043 Uiso 1 1 calc R . . H21D H -0.4506 -0.0354 0.3433 0.043 Uiso 1 1 calc R . . C22A C -0.5450(14) -0.0946(13) 0.4257(7) 0.030(4) Uani 1 1 d D . . C23A C -0.6890(16) -0.0084(16) 0.4048(9) 0.039(4) Uani 1 1 d . . . H23A H -0.7069 0.0334 0.3600 0.047 Uiso 1 1 calc R . . C24A C -0.8055(19) 0.0142(17) 0.4516(10) 0.054(5) Uani 1 1 d . . . H24A H -0.9023 0.0707 0.4375 0.065 Uiso 1 1 calc R . . C25A C -0.782(2) -0.0452(18) 0.5192(9) 0.051(5) Uani 1 1 d . . . H25A H -0.8604 -0.0262 0.5510 0.061 Uiso 1 1 calc R . . C26A C -0.638(2) -0.1334(17) 0.5375(9) 0.048(5) Uani 1 1 d . . . H26A H -0.6198 -0.1785 0.5816 0.058 Uiso 1 1 calc R . . C27A C -0.5220(17) -0.1555(15) 0.4926(8) 0.034(4) Uani 1 1 d . . . H27A H -0.4255 -0.2126 0.5070 0.041 Uiso 1 1 calc R . . C21B C -0.3162(16) -0.3979(10) 0.3861(6) 0.027(4) Uani 1 1 d D . . H21E H -0.2594 -0.3959 0.4252 0.033 Uiso 1 1 calc R . . H21F H -0.4123 -0.3908 0.4037 0.033 Uiso 1 1 calc R . . C22B C -0.2345(15) -0.5267(11) 0.3548(6) 0.024(3) Uani 1 1 d D . . C23B C -0.0802(16) -0.5791(13) 0.3446(7) 0.030(4) Uani 1 1 d . . . H23B H -0.0259 -0.5353 0.3573 0.036 Uiso 1 1 calc R . . C24B C -0.0104(17) -0.6968(14) 0.3155(8) 0.035(4) Uani 1 1 d . . . H24B H 0.0928 -0.7323 0.3093 0.042 Uiso 1 1 calc R . . C25B C -0.0838(17) -0.7637(14) 0.2955(8) 0.033(4) Uani 1 1 d . . . H25B H -0.0322 -0.8430 0.2757 0.040 Uiso 1 1 calc R . . C26B C -0.2350(16) -0.7131(14) 0.3048(8) 0.031(4) Uani 1 1 d . . . H26B H -0.2873 -0.7582 0.2915 0.037 Uiso 1 1 calc R . . C27B C -0.3099(16) -0.5952(14) 0.3340(7) 0.030(4) Uani 1 1 d . . . H27B H -0.4130 -0.5609 0.3399 0.036 Uiso 1 1 calc R . . C21C C -0.5061(14) -0.2406(12) 0.2732(7) 0.029(4) Uani 1 1 d DU . . H21A H -0.4794 -0.3216 0.2515 0.035 Uiso 1 1 calc R . . H21B H -0.5887 -0.2292 0.3050 0.035 Uiso 1 1 calc R . . C22C C -0.5568(18) -0.1280(13) 0.2178(7) 0.041(4) Uani 1 1 d D . . C23C C -0.4613(15) -0.1312(15) 0.1628(7) 0.032(4) Uani 1 1 d . . . H23C H -0.3678 -0.2022 0.1604 0.039 Uiso 1 1 calc R . . C24C C -0.505(2) -0.0280(18) 0.1112(9) 0.049(5) Uani 1 1 d . . . H24C H -0.4407 -0.0287 0.0747 0.059 Uiso 1 1 calc R . . C25C C -0.646(2) 0.0765(18) 0.1140(10) 0.054(5) Uani 1 1 d . . . H25C H -0.6753 0.1468 0.0800 0.065 Uiso 1 1 calc R . . C26C C -0.741(2) 0.0753(17) 0.1669(10) 0.055(5) Uani 1 1 d . . . H26C H -0.8356 0.1458 0.1678 0.066 Uiso 1 1 calc R . . C27C C -0.7049(15) -0.0259(14) 0.2196(8) 0.035(4) Uani 1 1 d . . . H27C H -0.7732 -0.0270 0.2541 0.042 Uiso 1 1 calc R . . C1S C 0.1385(19) -0.2874(18) 0.4679(11) 0.060(5) Uani 1 1 d . . . H1S1 H 0.1158 -0.2173 0.4309 0.072 Uiso 1 1 calc R . . H1S2 H 0.1240 -0.2488 0.5120 0.072 Uiso 1 1 calc R . . Cl1 Cl 0.0141(6) -0.3585(5) 0.4633(3) 0.0703(15) Uani 1 1 d . . . Cl2 Cl 0.3243(6) -0.4001(5) 0.4605(3) 0.0647(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0242(7) 0.0236(7) 0.0281(7) -0.0034(5) 0.0029(5) -0.0087(5) P1 0.021(2) 0.022(2) 0.028(2) 0.0009(17) -0.0044(17) -0.0026(17) P2 0.025(2) 0.019(2) 0.026(2) 0.0017(17) 0.0001(17) -0.0053(17) S1 0.038(3) 0.035(2) 0.041(3) -0.011(2) 0.0053(19) -0.020(2) O1 0.140(14) 0.033(7) 0.074(10) -0.001(7) -0.035(9) -0.038(8) O2 0.071(10) 0.071(9) 0.082(10) -0.026(8) -0.005(8) -0.045(8) C11A 0.022(8) 0.032(9) 0.037(10) -0.005(7) 0.003(7) -0.009(7) C12A 0.024(8) 0.034(10) 0.032(10) 0.011(8) -0.011(7) -0.010(8) C13A 0.039(10) 0.033(10) 0.039(10) 0.001(8) -0.009(8) -0.009(8) C14A 0.035(10) 0.033(11) 0.084(16) -0.007(11) -0.028(11) -0.005(8) C15A 0.019(9) 0.024(10) 0.058(13) 0.024(9) -0.024(8) 0.001(8) C16A 0.032(10) 0.049(12) 0.051(11) 0.020(10) -0.026(9) -0.010(9) C17A 0.024(9) 0.042(10) 0.039(11) 0.001(8) -0.003(7) -0.012(8) C11B 0.015(8) 0.033(9) 0.039(10) -0.007(7) -0.005(7) 0.001(7) C12B 0.003(7) 0.024(8) 0.035(9) -0.014(7) -0.007(7) 0.006(6) C13B 0.037(10) 0.036(9) 0.028(10) -0.004(7) 0.002(8) -0.011(8) C14B 0.014(9) 0.052(11) 0.045(11) -0.005(9) -0.012(8) -0.010(8) C15B 0.015(8) 0.058(11) 0.057(12) -0.018(9) -0.009(9) -0.012(8) C16B 0.049(11) 0.044(10) 0.032(10) -0.015(8) 0.006(9) -0.024(9) C17B 0.058(12) 0.027(9) 0.027(9) 0.002(7) -0.012(9) -0.013(8) C11C 0.036(10) 0.024(8) 0.032(9) 0.006(7) 0.003(8) 0.001(7) C12C 0.013(8) 0.015(7) 0.039(10) 0.008(7) -0.004(7) 0.005(6) C13C 0.046(11) 0.038(10) 0.031(10) 0.005(8) -0.007(8) -0.020(8) C14C 0.079(15) 0.037(10) 0.030(10) -0.006(8) -0.009(10) -0.013(10) C15C 0.027(10) 0.039(10) 0.051(13) 0.008(8) 0.009(8) -0.012(8) C16C 0.035(10) 0.046(10) 0.045(12) 0.025(9) -0.016(9) -0.017(8) C17C 0.043(10) 0.048(10) 0.024(9) 0.011(7) -0.014(8) -0.024(9) C21A 0.048(10) 0.024(8) 0.029(9) 0.000(7) 0.007(8) -0.010(8) C22A 0.025(9) 0.020(8) 0.037(10) -0.012(7) 0.002(7) -0.002(7) C23A 0.019(9) 0.050(10) 0.044(11) -0.008(8) -0.004(8) -0.010(8) C24A 0.035(11) 0.050(11) 0.053(13) -0.005(10) 0.006(9) 0.003(9) C25A 0.044(12) 0.065(12) 0.046(12) -0.018(10) 0.013(9) -0.026(11) C26A 0.066(14) 0.057(12) 0.026(10) -0.003(8) 0.000(10) -0.031(11) C27A 0.035(10) 0.038(9) 0.026(10) 0.001(8) 0.000(8) -0.014(8) C21B 0.036(9) 0.027(8) 0.020(8) 0.007(7) -0.001(7) -0.016(7) C22B 0.033(10) 0.024(8) 0.014(8) 0.009(6) -0.002(6) -0.012(7) C23B 0.034(10) 0.023(9) 0.030(9) 0.009(7) -0.007(7) -0.011(7) C24B 0.020(8) 0.027(9) 0.049(11) 0.004(8) -0.002(8) -0.004(8) C25B 0.042(11) 0.015(8) 0.037(10) -0.005(7) -0.003(8) -0.005(8) C26B 0.020(9) 0.025(9) 0.039(10) -0.001(7) -0.005(7) -0.002(7) C27B 0.024(8) 0.033(9) 0.027(9) 0.005(7) -0.001(7) -0.009(8) C21C 0.023(5) 0.028(5) 0.033(5) -0.004(4) -0.007(4) -0.008(4) C22C 0.059(12) 0.038(10) 0.048(11) 0.002(8) -0.008(9) -0.041(10) C23C 0.015(8) 0.040(9) 0.023(9) 0.013(7) -0.005(7) 0.003(7) C24C 0.050(12) 0.063(12) 0.042(11) 0.013(10) -0.013(9) -0.035(11) C25C 0.065(14) 0.047(12) 0.049(12) 0.012(9) -0.013(11) -0.025(11) C26C 0.038(11) 0.042(11) 0.066(14) -0.013(10) -0.016(10) 0.003(9) C27C 0.014(8) 0.034(9) 0.037(10) 0.010(8) -0.017(7) 0.007(7) C1S 0.039(11) 0.052(12) 0.085(15) -0.003(11) -0.002(10) -0.017(9) Cl1 0.067(3) 0.085(4) 0.073(4) -0.012(3) -0.004(3) -0.045(3) Cl2 0.057(3) 0.080(3) 0.060(3) -0.006(3) -0.003(2) -0.031(3) _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 2.282(4) . ? Pd1 P1 2.312(3) . ? Pd1 P2 2.328(3) . ? P1 C11B 1.833(11) . ? P1 C11C 1.840(11) . ? P1 C11A 1.845(11) . ? P2 C21B 1.836(10) . ? P2 C21A 1.837(11) . ? P2 C21C 1.830(11) . ? S1 O1 1.428(13) . ? S1 O2 1.467(13) . ? C11A C12A 1.499(9) . ? C12A C13A 1.39(2) . ? C12A C17A 1.39(2) . ? C13A C14A 1.37(2) . ? C14A C15A 1.36(2) . ? C15A C16A 1.35(2) . ? C16A C17A 1.40(2) . ? C11B C12B 1.498(9) . ? C12B C13B 1.39(2) . ? C12B C17B 1.39(2) . ? C13B C14B 1.38(2) . ? C14B C15B 1.37(2) . ? C15B C16B 1.36(2) . ? C16B C17B 1.37(2) . ? C11C C12C 1.499(9) . ? C12C C13C 1.40(2) . ? C12C C17C 1.39(2) . ? C13C C14C 1.39(2) . ? C14C C15C 1.39(2) . ? C15C C16C 1.35(2) . ? C16C C17C 1.35(2) . ? C21A C22A 1.499(9) . ? C22A C27A 1.38(2) . ? C22A C23A 1.39(2) . ? C23A C24A 1.38(2) . ? C24A C25A 1.39(2) . ? C25A C26A 1.38(2) . ? C26A C27A 1.35(2) . ? C21B C22B 1.499(9) . ? C22B C27B 1.384(19) . ? C22B C23B 1.39(2) . ? C23B C24B 1.37(2) . ? C24B C25B 1.35(2) . ? C25B C26B 1.36(2) . ? C26B C27B 1.38(2) . ? C21C C22C 1.499(9) . ? C22C C23C 1.38(2) . ? C22C C27C 1.42(2) . ? C23C C24C 1.38(2) . ? C24C C25C 1.39(2) . ? C25C C26C 1.36(2) . ? C26C C27C 1.39(2) . ? C1S Cl2 1.737(18) . ? C1S Cl1 1.753(18) . ? 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 P1 96.52(14) . . ? S1 Pd1 P2 97.27(14) . . ? P1 Pd1 P2 163.67(14) . . ? C11B P1 C11C 105.0(7) . . ? C11B P1 C11A 101.6(6) . . ? C11C P1 C11A 104.6(6) . . ? C11B P1 Pd1 113.4(5) . . ? C11C P1 Pd1 111.6(4) . . ? C11A P1 Pd1 119.2(5) . . ? C21B P2 C21A 104.9(6) . . ? C21B P2 C21C 102.5(6) . . ? C21A P2 C21C 105.3(7) . . ? C21B P2 Pd1 115.7(4) . . ? C21A P2 Pd1 113.7(4) . . ? C21C P2 Pd1 113.4(5) . . ? O1 S1 O2 112.4(9) . . ? O1 S1 Pd1 104.8(5) . . ? O2 S1 Pd1 106.8(5) . . ? C12A C11A P1 110.9(9) . . ? C13A C12A C17A 118.9(12) . . ? C13A C12A C11A 122.4(13) . . ? C17A C12A C11A 118.6(13) . . ? C14A C13A C12A 120.4(16) . . ? C15A C14A C13A 120.4(16) . . ? C14A C15A C16A 120.7(15) . . ? C15A C16A C17A 120.4(17) . . ? C12A C17A C16A 119.1(15) . . ? C12B C11B P1 113.2(8) . . ? C13B C12B C17B 116.1(12) . . ? C13B C12B C11B 121.8(13) . . ? C17B C12B C11B 122.1(13) . . ? C12B C13B C14B 122.5(15) . . ? C15B C14B C13B 119.4(15) . . ? C16B C15B C14B 119.4(14) . . ? C15B C16B C17B 121.0(16) . . ? C16B C17B C12B 121.6(14) . . ? C12C C11C P1 118.7(9) . . ? C13C C12C C17C 118.0(12) . . ? C13C C12C C11C 119.7(13) . . ? C17C C12C C11C 122.3(14) . . ? C14C C13C C12C 119.1(15) . . ? C13C C14C C15C 120.1(16) . . ? C16C C15C C14C 120.3(16) . . ? C17C C16C C15C 120.5(16) . . ? C16C C17C C12C 122.1(15) . . ? C22A C21A P2 119.6(9) . . ? C27A C22A C23A 119.2(12) . . ? C27A C22A C21A 122.4(13) . . ? C23A C22A C21A 118.4(13) . . ? C24A C23A C22A 118.9(15) . . ? C23A C24A C25A 121.8(16) . . ? C26A C25A C24A 117.6(16) . . ? C27A C26A C25A 121.3(16) . . ? C26A C27A C22A 121.1(15) . . ? C22B C21B P2 112.6(8) . . ? C27B C22B C23B 118.4(11) . . ? C27B C22B C21B 121.2(12) . . ? C23B C22B C21B 120.4(13) . . ? C24B C23B C22B 118.3(14) . . ? C25B C24B C23B 123.3(14) . . ? C24B C25B C26B 119.0(14) . . ? C25B C26B C27B 119.8(14) . . ? C22B C27B C26B 121.3(13) . . ? C22C C21C P2 113.7(9) . . ? C23C C22C C27C 121.1(12) . . ? C23C C22C C21C 118.6(14) . . ? C27C C22C C21C 120.1(14) . . ? C22C C23C C24C 119.6(14) . . ? C25C C24C C23C 120.1(16) . . ? C26C C25C C24C 119.5(17) . . ? C25C C26C C27C 123.2(16) . . ? C26C C27C C22C 116.1(15) . . ? Cl2 C1S Cl1 112.7(10) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.374 _refine_diff_density_min -1.113 _refine_diff_density_rms 0.162 data_ab257 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C73 H82 N2 O4.50 P3 Pd3 S2' _chemical_formula_weight 1535.64 _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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 22.985(9) _cell_length_b 24.213(10) _cell_length_c 26.926(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14985.0(126) _cell_formula_units_Z 8 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 55 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 9.46 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method ? _exptl_crystal_F_000 6280 _exptl_absorpt_coefficient_mu 0.878 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.432 _exptl_absorpt_correction_T_max 0.454 _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(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 'Siemens P4' _diffrn_measurement_method 'Theta/2 theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15236 _diffrn_reflns_av_R_equivalents 0.1146 _diffrn_reflns_av_sigmaI/netI 0.2816 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13177 _reflns_number_observed 3071 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 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^)+(0.0908P)^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 13173 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2803 _refine_ls_R_factor_obs 0.0821 _refine_ls_wR_factor_all 0.2949 _refine_ls_wR_factor_obs 0.1798 _refine_ls_goodness_of_fit_all 0.921 _refine_ls_goodness_of_fit_obs 1.240 _refine_ls_restrained_S_all 0.922 _refine_ls_restrained_S_obs 1.240 _refine_ls_shift/esd_max 0.012 _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 -0.52133(7) -0.26108(6) 0.34965(5) 0.0598(5) Uani 1 d . . Pd2 Pd -0.47166(6) -0.27523(6) 0.25708(5) 0.0547(4) Uani 1 d . . Pd3 Pd -0.45246(7) -0.35092(6) 0.33397(6) 0.0619(5) Uani 1 d . . P1 P -0.5827(3) -0.2097(2) 0.3984(2) 0.069(2) Uani 1 d . . P2 P -0.4756(2) -0.2336(2) 0.1797(2) 0.0626(14) Uani 1 d . . P3 P -0.4078(3) -0.4252(2) 0.3716(2) 0.069(2) Uani 1 d . . S1 S -0.5637(2) -0.2523(3) 0.2739(2) 0.070(2) Uani 1 d . . S2 S -0.4443(3) -0.2895(2) 0.3963(2) 0.068(2) Uani 1 d . . O1 O -0.5800(6) -0.1954(6) 0.2607(5) 0.084(4) Uani 1 d . . O2 O -0.6065(6) -0.2928(7) 0.2574(5) 0.100(5) Uani 1 d . . O3 O -0.3930(6) -0.2520(6) 0.3941(6) 0.104(5) Uani 1 d . . O4 O -0.4535(7) -0.3131(6) 0.4468(5) 0.097(5) Uani 1 d . . N1 N -0.3360(7) -0.2882(8) 0.2674(7) 0.077(6) Uani 1 d . . C1 C -0.2738(10) -0.2824(12) 0.2674(11) 0.099(8) Uani 1 d . . C2 C -0.3839(10) -0.2884(9) 0.2669(8) 0.076(7) Uani 1 d . . N2 N -0.5223(8) -0.4143(7) 0.2532(7) 0.073(5) Uani 1 d . . C3 C -0.5581(13) -0.4486(12) 0.2217(9) 0.103(9) Uani 1 d . . C4 C -0.4957(9) -0.3883(9) 0.2808(8) 0.079(7) Uani 1 d . . C11 C -0.2602(12) -0.2559(18) 0.3184(12) 0.215(21) Uani 1 d . . H11A H -0.2711(12) -0.2808(18) 0.3445(12) 0.322 Uiso 1 calc R . H11B H -0.2817(12) -0.2221(18) 0.3218(12) 0.322 Uiso 1 calc R . H11C H -0.2193(12) -0.2482(18) 0.3207(12) 0.322 Uiso 1 calc R . C12 C -0.2468(10) -0.3389(12) 0.2640(13) 0.186(17) Uani 1 d . . H12A H -0.2602(10) -0.3612(12) 0.2912(13) 0.279 Uiso 1 calc R . H12B H -0.2052(10) -0.3356(12) 0.2655(13) 0.279 Uiso 1 calc R . H12C H -0.2579(10) -0.3558(12) 0.2332(13) 0.279 Uiso 1 calc R . C13 C -0.2574(10) -0.2449(11) 0.2287(10) 0.130(11) Uani 1 d . . H13A H -0.2766(10) -0.2102(11) 0.2337(10) 0.195 Uiso 1 calc R . H13B H -0.2687(10) -0.2600(11) 0.1972(10) 0.195 Uiso 1 calc R . H13C H -0.2161(10) -0.2396(11) 0.2293(10) 0.195 Uiso 1 calc R . C21 C -0.5306(14) -0.5010(10) 0.2087(11) 0.167(15) Uani 1 d . . H21A H -0.5221(14) -0.5213(10) 0.2384(11) 0.251 Uiso 1 calc R . H21B H -0.4952(14) -0.4941(10) 0.1909(11) 0.251 Uiso 1 calc R . H21C H -0.5566(14) -0.5222(10) 0.1882(11) 0.251 Uiso 1 calc R . C22 C -0.6150(12) -0.4589(12) 0.2497(12) 0.188(16) Uani 1 d . . H22A H -0.6326(12) -0.4241(12) 0.2582(12) 0.282 Uiso 1 calc R . H22B H -0.6071(12) -0.4793(12) 0.2795(12) 0.282 Uiso 1 calc R . H22C H -0.6411(12) -0.4796(12) 0.2291(12) 0.282 Uiso 1 calc R . C23 C -0.5711(13) -0.4174(12) 0.1767(10) 0.161(13) Uani 1 d . . H23A H -0.5892(13) -0.3830(12) 0.1854(10) 0.242 Uiso 1 calc R . H23B H -0.5971(13) -0.4384(12) 0.1561(10) 0.242 Uiso 1 calc R . H23C H -0.5357(13) -0.4104(12) 0.1589(10) 0.242 Uiso 1 calc R . C11A C -0.6612(9) -0.2179(9) 0.3880(8) 0.095(8) Uani 1 d . . H11D H -0.6815(9) -0.1947(9) 0.4117(8) 0.114 Uiso 1 calc R . H11E H -0.6701(9) -0.2040(9) 0.3551(8) 0.114 Uiso 1 calc R . C12A C -0.6856(9) -0.2755(7) 0.3920(8) 0.087(7) Uani 1 d G . C13A C -0.6702(7) -0.3222(10) 0.3651(6) 0.125(11) Uani 1 d G . H13D H -0.6392(9) -0.3208(16) 0.3430(9) 0.150 Uiso 1 calc R . C14A C -0.7012(10) -0.3711(8) 0.3713(7) 0.157(15) Uani 1 d G . H14A H -0.6909(16) -0.4023(10) 0.3533(11) 0.189 Uiso 1 calc R . C15A C -0.7475(9) -0.3731(9) 0.4044(9) 0.354(46) Uani 1 d G . H15A H -0.7682(13) -0.4058(11) 0.4086(13) 0.424 Uiso 1 calc R . C16A C -0.7629(8) -0.3264(12) 0.4313(7) 0.265(28) Uani 1 d G . H16A H -0.7939(10) -0.3278(18) 0.4535(10) 0.318 Uiso 1 calc R . C17A C -0.7320(11) -0.2776(9) 0.4251(7) 0.175(16) Uani 1 d G . H17A H -0.7423(16) -0.2463(12) 0.4432(11) 0.210 Uiso 1 calc R . C11B C -0.5701(8) -0.2166(9) 0.4643(6) 0.084(7) Uani 1 d . . H11F H -0.5707(8) -0.2558(9) 0.4718(6) 0.101 Uiso 1 calc R . H11G H -0.5308(8) -0.2039(9) 0.4707(6) 0.101 Uiso 1 calc R . C12B C -0.6081(7) -0.1893(8) 0.5007(5) 0.071(6) Uani 1 d G . C13B C -0.6560(8) -0.2157(6) 0.5215(6) 0.126(11) Uani 1 d G . H13E H -0.6645(13) -0.2520(7) 0.5129(10) 0.152 Uiso 1 calc R . C14B C -0.6912(6) -0.1878(10) 0.5551(7) 0.160(14) Uani 1 d G . H14B H -0.7232(8) -0.2055(15) 0.5691(10) 0.192 Uiso 1 calc R . C15B C -0.6785(10) -0.1335(10) 0.5680(6) 0.174(17) Uani 1 d G . H15B H -0.7021(14) -0.1148(14) 0.5905(8) 0.209 Uiso 1 calc R . C16B C -0.6307(12) -0.1071(6) 0.5472(8) 0.222(23) Uani 1 d G . H16B H -0.6222(17) -0.0708(7) 0.5557(11) 0.267 Uiso 1 calc R . C17B C -0.5955(8) -0.1350(8) 0.5135(7) 0.147(13) Uani 1 d G . H17B H -0.5635(10) -0.1174(12) 0.4996(10) 0.177 Uiso 1 calc R . C11C C -0.5798(9) -0.1355(8) 0.3861(8) 0.083(7) Uani 1 d . . H11H H -0.5850(9) -0.1299(8) 0.3507(8) 0.100 Uiso 1 calc R . H11I H -0.6126(9) -0.1183(8) 0.4027(8) 0.100 Uiso 1 calc R . C12C C -0.5246(6) -0.1052(7) 0.4020(6) 0.089(7) Uani 1 d G . C13C C -0.5315(6) -0.0531(7) 0.4228(6) 0.097(8) Uani 1 d G . H13F H -0.5686(7) -0.0388(10) 0.4278(8) 0.117 Uiso 1 calc R . C14C C -0.4830(9) -0.0223(5) 0.4363(5) 0.115(10) Uani 1 d G . H14C H -0.4876(13) 0.0126(6) 0.4502(7) 0.138 Uiso 1 calc R . C15C C -0.4275(7) -0.0436(7) 0.4289(5) 0.095(8) Uani 1 d G . H15C H -0.3950(9) -0.0230(10) 0.4379(8) 0.114 Uiso 1 calc R . C16C C -0.4206(5) -0.0957(7) 0.4080(5) 0.087(7) Uani 1 d G . H16C H -0.3834(6) -0.1099(10) 0.4030(8) 0.104 Uiso 1 calc R . C17C C -0.4691(7) -0.1265(5) 0.3946(5) 0.081(7) Uani 1 d G . H17C H -0.4645(11) -0.1613(6) 0.3806(7) 0.097 Uiso 1 calc R . C21A C -0.4147(8) -0.2430(8) 0.1358(7) 0.066(6) Uani 1 d . . H21D H -0.4166(8) -0.2144(8) 0.1106(7) 0.079 Uiso 1 calc R . H21E H -0.3782(8) -0.2386(8) 0.1535(7) 0.079 Uiso 1 calc R . C22A C -0.4155(6) -0.2995(6) 0.1106(7) 0.078(7) Uani 1 d G . C23A C -0.4197(6) -0.2992(7) 0.0591(7) 0.097(8) Uani 1 d G . H23D H -0.4229(10) -0.2659(9) 0.0421(11) 0.116 Uiso 1 calc R . C24A C -0.4193(6) -0.3487(11) 0.0330(5) 0.140(14) Uani 1 d G . H24A H -0.4221(9) -0.3485(16) -0.0015(5) 0.169 Uiso 1 calc R . C25A C -0.4146(6) -0.3985(7) 0.0584(9) 0.125(13) Uani 1 d G . H25A H -0.4143(10) -0.4316(10) 0.0409(12) 0.151 Uiso 1 calc R . C26A C -0.4104(7) -0.3988(6) 0.1098(9) 0.111(9) Uani 1 d G . H26A H -0.4072(10) -0.4321(8) 0.1268(12) 0.133 Uiso 1 calc R . C27A C -0.4108(6) -0.3493(9) 0.1360(5) 0.098(8) Uani 1 d G . H27A H -0.4080(9) -0.3494(14) 0.1704(5) 0.118 Uiso 1 calc R . C21B C -0.4758(8) -0.1566(7) 0.1853(7) 0.074(6) Uani 1 d . . H21F H -0.4793(8) -0.1402(7) 0.1526(7) 0.088 Uiso 1 calc R . H21G H -0.5089(8) -0.1449(7) 0.2050(7) 0.088 Uiso 1 calc R . C22B C -0.4201(6) -0.1372(6) 0.2096(6) 0.079(7) Uani 1 d G . C23B C -0.3769(9) -0.1154(7) 0.1792(5) 0.114(10) Uani 1 d G . H23E H -0.3831(13) -0.1126(11) 0.1451(5) 0.137 Uiso 1 calc R . C24B C -0.3246(7) -0.0979(6) 0.1996(8) 0.129(11) Uani 1 d G . H24B H -0.2957(10) -0.0833(9) 0.1793(11) 0.155 Uiso 1 calc R . C25B C -0.3154(6) -0.1021(6) 0.2505(9) 0.115(10) Uani 1 d G . H25B H -0.2803(7) -0.0904(9) 0.2642(12) 0.138 Uiso 1 calc R . C26B C -0.3585(8) -0.1239(7) 0.2809(5) 0.095(8) Uani 1 d G . H26B H -0.3523(13) -0.1267(10) 0.3150(5) 0.115 Uiso 1 calc R . C27B C -0.4109(7) -0.1414(6) 0.2605(6) 0.089(7) Uani 1 d G . H27B H -0.4397(9) -0.1559(9) 0.2808(8) 0.106 Uiso 1 calc R . C21C C -0.5382(8) -0.2503(7) 0.1443(7) 0.065(6) Uani 1 d . . H21H H -0.5284(8) -0.2813(7) 0.1230(7) 0.079 Uiso 1 calc R . H21I H -0.5681(8) -0.2629(7) 0.1671(7) 0.079 Uiso 1 calc R . C22C C -0.5656(8) -0.2035(6) 0.1105(6) 0.078(7) Uani 1 d G . C23C C -0.6147(8) -0.1754(8) 0.1270(6) 0.115(10) Uani 1 d G . H23F H -0.6306(12) -0.1836(12) 0.1579(7) 0.138 Uiso 1 calc R . C24C C -0.6401(6) -0.1352(7) 0.0972(9) 0.129(12) Uani 1 d G . H24C H -0.6729(7) -0.1164(10) 0.1082(13) 0.155 Uiso 1 calc R . C25C C -0.6163(9) -0.1229(6) 0.0510(8) 0.118(11) Uani 1 d G . H25C H -0.6333(13) -0.0960(7) 0.0311(11) 0.142 Uiso 1 calc R . C26C C -0.5672(9) -0.1510(7) 0.0346(5) 0.101(8) Uani 1 d G . H26C H -0.5513(13) -0.1428(11) 0.0037(5) 0.122 Uiso 1 calc R . C27C C -0.5418(6) -0.1913(7) 0.0643(6) 0.082(7) Uani 1 d G . H27C H -0.5089(7) -0.2100(10) 0.0533(10) 0.099 Uiso 1 calc R . C31A C -0.3325(8) -0.4117(9) 0.3870(8) 0.086(7) Uani 1 d . . H31A H -0.3134(8) -0.3973(9) 0.3576(8) 0.104 Uiso 1 calc R . H31B H -0.3315(8) -0.3830(9) 0.4121(8) 0.104 Uiso 1 calc R . C32A C -0.2980(7) -0.4596(6) 0.4056(9) 0.090(8) Uani 1 d G . C33A C -0.2657(8) -0.4951(9) 0.3757(5) 0.103(9) Uani 1 d G . H33A H -0.2659(13) -0.4906(15) 0.3414(5) 0.123 Uiso 1 calc R . C34A C -0.2332(7) -0.5372(8) 0.3971(9) 0.142(13) Uani 1 d G . H34A H -0.2116(10) -0.5609(11) 0.3771(13) 0.171 Uiso 1 calc R . C35A C -0.2329(7) -0.5439(7) 0.4484(10) 0.133(13) Uani 1 d G . H35A H -0.2111(11) -0.5721(9) 0.4627(15) 0.159 Uiso 1 calc R . C36A C -0.2651(9) -0.5084(10) 0.4782(6) 0.157(15) Uani 1 d G . H36A H -0.2649(14) -0.5129(16) 0.5125(6) 0.188 Uiso 1 calc R . C37A C -0.2976(8) -0.4663(8) 0.4568(8) 0.125(12) Uani 1 d G . H37A H -0.3192(11) -0.4426(12) 0.4768(12) 0.150 Uiso 1 calc R . C31B C -0.4393(9) -0.4461(9) 0.4322(7) 0.081(7) Uani 1 d . . H31C H -0.4135(9) -0.4729(9) 0.4475(7) 0.097 Uiso 1 calc R . H31D H -0.4406(9) -0.4140(9) 0.4537(7) 0.097 Uiso 1 calc R . C32B C -0.4984(7) -0.4703(9) 0.4293(5) 0.075(6) Uani 1 d G . C33B C -0.5042(9) -0.5270(8) 0.4358(6) 0.109(9) Uani 1 d G . H33B H -0.4714(12) -0.5489(12) 0.4402(9) 0.131 Uiso 1 calc R . C34B C -0.5592(12) -0.5510(6) 0.4358(6) 0.144(13) Uani 1 d G . H34B H -0.5631(18) -0.5889(7) 0.4401(9) 0.172 Uiso 1 calc R . C35B C -0.6083(8) -0.5183(11) 0.4292(6) 0.150(15) Uani 1 d G . H35B H -0.6450(10) -0.5343(17) 0.4291(9) 0.180 Uiso 1 calc R . C36B C -0.6024(8) -0.4616(11) 0.4227(7) 0.171(16) Uani 1 d G . H36B H -0.6353(10) -0.4397(15) 0.4183(10) 0.206 Uiso 1 calc R . C37B C -0.5475(10) -0.4376(6) 0.4228(6) 0.117(10) Uani 1 d G . H37B H -0.5436(16) -0.3997(6) 0.4184(9) 0.140 Uiso 1 calc R . C31C C -0.4111(9) -0.4923(7) 0.3387(8) 0.077(6) Uani 1 d . . H31E H -0.3947(9) -0.5201(7) 0.3606(8) 0.093 Uiso 1 calc R . H31F H -0.4517(9) -0.5015(7) 0.3340(8) 0.093 Uiso 1 calc R . C32C C -0.3813(6) -0.4974(7) 0.2894(4) 0.067(6) Uani 1 d G . C33C C -0.3748(6) -0.5517(6) 0.2736(6) 0.094(8) Uani 1 d G . H33C H -0.3884(9) -0.5806(8) 0.2933(9) 0.112 Uiso 1 calc R . C34C C -0.3481(7) -0.5630(6) 0.2284(7) 0.104(9) Uani 1 d G . H34C H -0.3437(11) -0.5993(7) 0.2179(10) 0.125 Uiso 1 calc R . C35C C -0.3278(6) -0.5199(9) 0.1990(5) 0.115(10) Uani 1 d G . H35C H -0.3099(9) -0.5274(13) 0.1688(6) 0.138 Uiso 1 calc R . C36C C -0.3343(7) -0.4656(7) 0.2148(6) 0.108(9) Uani 1 d G . H36C H -0.3207(10) -0.4367(10) 0.1952(8) 0.129 Uiso 1 calc R . C37C C -0.3610(7) -0.4543(5) 0.2600(6) 0.088(7) Uani 1 d G . H37C H -0.3654(10) -0.4180(6) 0.2706(10) 0.106 Uiso 1 calc R . O1W O -0.3583(14) -0.3323(12) 0.5124(11) 0.113(12) Uani 0.50 d P . H1WB H -0.3450 -0.3127 0.5322 0.170 Uiso 0.50 d P . H1WA H -0.4044 -0.3385 0.5282 0.170 Uiso 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 0.0546(9) 0.0653(10) 0.0596(9) -0.0038(8) 0.0029(8) 0.0074(9) Pd2 0.0476(8) 0.0609(9) 0.0557(9) 0.0024(8) 0.0026(8) -0.0005(8) Pd3 0.0705(10) 0.0539(9) 0.0613(9) -0.0020(8) 0.0003(9) 0.0068(9) P1 0.065(4) 0.080(4) 0.062(3) -0.004(3) -0.002(3) 0.018(3) P2 0.065(3) 0.066(3) 0.057(3) 0.001(3) -0.007(3) -0.005(3) P3 0.074(4) 0.062(4) 0.072(4) 0.002(3) 0.000(3) 0.009(3) S1 0.049(3) 0.089(4) 0.071(4) 0.004(3) -0.002(3) 0.010(3) S2 0.074(4) 0.060(3) 0.070(4) -0.005(3) -0.003(3) 0.015(3) O1 0.070(9) 0.103(11) 0.079(10) 0.011(9) 0.005(8) 0.025(9) O2 0.052(8) 0.162(15) 0.086(11) -0.025(11) 0.000(8) -0.035(10) O3 0.066(10) 0.106(12) 0.141(15) -0.028(11) -0.019(10) -0.012(10) O4 0.111(12) 0.090(11) 0.090(11) -0.012(9) 0.006(10) 0.020(10) N1 0.043(10) 0.103(15) 0.085(13) -0.005(11) -0.002(10) 0.005(11) C1 0.064(16) 0.113(21) 0.120(22) 0.020(19) 0.026(17) 0.026(16) C2 0.074(15) 0.090(17) 0.065(14) 0.023(13) 0.008(13) 0.024(15) N2 0.088(14) 0.054(11) 0.077(13) 0.005(10) 0.021(12) 0.013(10) C3 0.127(24) 0.112(22) 0.071(17) 0.016(17) -0.010(18) -0.038(20) C4 0.072(15) 0.072(15) 0.093(18) -0.035(13) -0.018(13) -0.015(13) C11 0.078(22) 0.385(65) 0.181(35) 0.046(40) -0.006(24) -0.065(32) C12 0.050(15) 0.152(27) 0.356(50) 0.089(34) 0.081(24) 0.030(18) C13 0.080(17) 0.148(25) 0.163(26) 0.090(22) 0.046(18) 0.003(18) C21 0.220(35) 0.069(16) 0.213(34) -0.074(20) -0.090(29) 0.039(22) C22 0.131(26) 0.182(32) 0.251(40) -0.071(31) 0.030(29) -0.103(26) C23 0.181(32) 0.170(31) 0.132(25) -0.008(25) -0.086(25) -0.040(26) C11A 0.092(18) 0.099(19) 0.093(17) -0.023(16) -0.038(15) 0.037(16) C12A 0.062(16) 0.097(20) 0.103(20) 0.005(18) -0.021(15) -0.015(16) C13A 0.149(28) 0.090(20) 0.136(26) 0.018(21) 0.013(22) 0.035(22) C14A 0.199(38) 0.097(23) 0.176(33) 0.031(23) -0.070(31) -0.029(24) C15A 0.035(16) 0.745(115) 0.282(52) 0.395(68) 0.007(26) -0.017(39) C16A 0.165(42) 0.458(82) 0.172(37) 0.036(53) 0.093(32) 0.022(51) C17A 0.145(34) 0.148(32) 0.232(41) 0.036(29) 0.083(30) -0.007(26) C11B 0.075(15) 0.116(18) 0.061(13) -0.010(13) -0.001(12) 0.054(14) C12B 0.069(15) 0.088(16) 0.055(13) 0.005(13) 0.022(12) 0.003(14) C13B 0.103(20) 0.178(28) 0.097(19) -0.067(20) 0.048(17) -0.042(21) C14B 0.101(22) 0.214(39) 0.166(33) 0.012(30) 0.074(22) 0.048(26) C15B 0.302(51) 0.134(30) 0.087(21) -0.015(23) 0.074(27) 0.061(33) C16B 0.410(71) 0.136(31) 0.121(30) 0.050(25) 0.076(35) -0.068(40) C17B 0.212(35) 0.127(26) 0.103(23) -0.017(20) 0.050(23) -0.084(26) C11C 0.098(18) 0.070(15) 0.082(16) -0.006(13) 0.008(14) 0.017(14) C12C 0.062(15) 0.085(17) 0.119(20) -0.017(16) 0.006(16) -0.001(15) C13C 0.108(22) 0.100(19) 0.084(17) -0.017(15) -0.016(16) 0.041(18) C14C 0.089(20) 0.147(26) 0.108(21) -0.008(19) -0.010(19) 0.040(22) C15C 0.141(26) 0.075(17) 0.069(15) -0.006(14) -0.016(17) -0.015(18) C16C 0.071(16) 0.079(17) 0.111(20) 0.031(16) 0.013(15) -0.014(15) C17C 0.087(17) 0.065(14) 0.090(16) -0.025(12) 0.034(15) 0.021(14) C21A 0.060(13) 0.070(13) 0.068(13) 0.003(12) 0.009(11) -0.015(12) C22A 0.058(14) 0.090(18) 0.085(18) -0.021(15) -0.008(13) -0.009(14) C23A 0.079(17) 0.132(24) 0.079(18) -0.018(17) -0.009(15) 0.020(17) C24A 0.076(19) 0.222(38) 0.124(24) -0.088(29) 0.057(18) -0.018(25) C25A 0.092(21) 0.162(32) 0.122(26) -0.085(24) -0.018(21) -0.026(22) C26A 0.112(22) 0.089(20) 0.132(26) -0.018(19) 0.021(21) 0.007(18) C27A 0.110(20) 0.107(20) 0.078(16) -0.001(18) 0.004(15) -0.001(19) C21B 0.093(16) 0.052(12) 0.076(14) 0.006(11) -0.025(13) 0.016(13) C22B 0.085(17) 0.082(16) 0.069(15) -0.001(13) -0.029(14) -0.017(14) C23B 0.085(19) 0.141(25) 0.117(22) 0.040(19) 0.019(18) -0.025(19) C24B 0.152(31) 0.126(25) 0.110(24) 0.024(21) 0.009(22) -0.035(23) C25B 0.072(18) 0.112(22) 0.160(29) -0.011(24) -0.003(21) 0.001(17) C26B 0.109(20) 0.096(19) 0.082(17) -0.032(15) -0.028(18) 0.030(17) C27B 0.069(15) 0.102(18) 0.095(18) -0.022(16) -0.011(14) 0.001(15) C21C 0.063(13) 0.046(11) 0.088(14) -0.006(11) -0.004(12) -0.026(10) C22C 0.066(15) 0.071(15) 0.098(19) -0.021(15) -0.011(14) 0.012(13) C23C 0.101(22) 0.139(26) 0.106(21) -0.055(21) 0.004(19) -0.011(20) C24C 0.109(23) 0.091(22) 0.188(35) -0.021(23) -0.035(26) 0.037(18) C25C 0.137(29) 0.094(21) 0.124(26) -0.020(20) -0.060(22) 0.009(21) C26C 0.145(26) 0.068(16) 0.091(18) -0.003(16) 0.001(19) 0.009(17) C27C 0.110(19) 0.084(16) 0.053(13) 0.000(12) -0.012(14) -0.007(16) C31A 0.063(15) 0.086(17) 0.110(19) 0.030(15) -0.019(14) 0.016(13) C32A 0.084(19) 0.099(21) 0.086(18) 0.003(17) -0.007(16) -0.020(16) C33A 0.066(18) 0.125(23) 0.117(21) -0.011(20) -0.010(16) 0.022(16) C34A 0.056(17) 0.178(34) 0.193(36) -0.067(29) -0.017(21) 0.036(19) C35A 0.125(29) 0.123(27) 0.150(30) 0.053(26) -0.035(26) -0.015(23) C36A 0.158(36) 0.186(39) 0.125(27) -0.018(29) 0.041(26) -0.015(29) C37A 0.132(25) 0.110(23) 0.133(28) 0.009(21) -0.063(22) 0.033(20) C31B 0.092(17) 0.103(18) 0.048(12) 0.031(12) -0.017(13) 0.026(15) C32B 0.085(18) 0.092(18) 0.048(12) -0.009(13) 0.002(13) -0.001(16) C33B 0.123(24) 0.097(21) 0.107(21) 0.020(17) 0.038(19) -0.028(18) C34B 0.165(33) 0.186(34) 0.080(19) -0.021(21) -0.006(25) -0.017(32) C35B 0.170(37) 0.146(31) 0.135(28) 0.011(27) 0.028(27) -0.084(30) C36B 0.056(20) 0.263(51) 0.195(36) 0.001(37) -0.001(23) 0.018(25) C37B 0.118(23) 0.109(20) 0.123(22) -0.027(18) -0.009(21) 0.054(22) C31C 0.084(16) 0.056(13) 0.093(17) -0.001(13) 0.003(14) 0.006(12) C32C 0.071(15) 0.056(13) 0.072(15) -0.011(13) -0.006(13) 0.016(12) C33C 0.082(18) 0.126(24) 0.073(17) 0.002(17) -0.006(14) -0.008(17) C34C 0.100(21) 0.080(18) 0.132(25) 0.029(19) -0.044(20) -0.004(16) C35C 0.140(25) 0.147(26) 0.057(15) -0.026(19) 0.007(16) 0.043(24) C36C 0.110(21) 0.131(25) 0.083(19) 0.005(18) 0.028(17) -0.007(19) C37C 0.097(18) 0.072(15) 0.096(18) 0.016(15) 0.019(16) 0.017(14) O1W 0.142(29) 0.088(21) 0.109(24) -0.039(20) -0.050(22) 0.045(22) _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 2.270(6) . ? Pd1 S2 2.278(6) . ? Pd1 P1 2.294(6) . ? Pd1 Pd3 2.723(2) . ? Pd1 Pd2 2.763(2) . ? Pd2 C2 2.06(2) . ? Pd2 S1 2.234(5) . ? Pd2 P2 2.315(5) . ? Pd2 Pd3 2.800(2) . ? Pd3 C4 1.96(2) . ? Pd3 S2 2.249(6) . ? Pd3 P3 2.305(6) . ? P1 C11B 1.81(2) . ? P1 C11C 1.83(2) . ? P1 C11A 1.84(2) . ? P2 C21C 1.77(2) . ? P2 C21A 1.85(2) . ? P2 C21B 1.87(2) . ? P3 C31A 1.81(2) . ? P3 C31C 1.85(2) . ? P3 C31B 1.86(2) . ? S1 O2 1.458(14) . ? S1 O1 1.471(14) . ? S2 O3 1.488(14) . ? S2 O4 1.490(15) . ? N1 C2 1.10(2) . ? N1 C1 1.44(3) . ? C1 C13 1.43(3) . ? C1 C12 1.50(3) . ? C1 C11 1.55(4) . ? N2 C4 1.15(2) . ? N2 C3 1.44(3) . ? C3 C21 1.46(3) . ? C3 C23 1.46(3) . ? C3 C22 1.53(3) . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C12 H12C 0.96 . ? C13 H13A 0.96 . ? C13 H13B 0.96 . ? C13 H13C 0.96 . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C22 H22A 0.96 . ? C22 H22B 0.96 . ? C22 H22C 0.96 . ? C23 H23A 0.96 . ? C23 H23B 0.96 . ? C23 H23C 0.96 . ? C11A C12A 1.51(2) . ? C11A H11D 0.97 . ? C11A H11E 0.97 . ? C12A C13A 1.39 . ? C12A C17A 1.39 . ? C13A C14A 1.39 . ? C13A H13D 0.93 . ? C14A C15A 1.39 . ? C14A H14A 0.93 . ? C15A C16A 1.39 . ? C15A H15A 0.93 . ? C16A C17A 1.39 . ? C16A H16A 0.93 . ? C17A H17A 0.93 . ? C11B C12B 1.47(2) . ? C11B H11F 0.97 . ? C11B H11G 0.97 . ? C12B C13B 1.39 . ? C12B C17B 1.39 . ? C13B C14B 1.39 . ? C13B H13E 0.93 . ? C14B C15B 1.39 . ? C14B H14B 0.93 . ? C15B C16B 1.39 . ? C15B H15B 0.93 . ? C16B C17B 1.39 . ? C16B H16B 0.93 . ? C17B H17B 0.93 . ? C11C C12C 1.53(2) . ? C11C H11H 0.97 . ? C11C H11I 0.97 . ? C12C C13C 1.39 . ? C12C C17C 1.39 . ? C13C C14C 1.39 . ? C13C H13F 0.93 . ? C14C C15C 1.39 . ? C14C H14C 0.93 . ? C15C C16C 1.39 . ? C15C H15C 0.93 . ? C16C C17C 1.39 . ? C16C H16C 0.93 . ? C17C H17C 0.93 . ? C21A C22A 1.53(2) . ? C21A H21D 0.97 . ? C21A H21E 0.97 . ? C22A C23A 1.39 . ? C22A C27A 1.39 . ? C23A C24A 1.39 . ? C23A H23D 0.93 . ? C24A C25A 1.39 . ? C24A H24A 0.93 . ? C25A C26A 1.39 . ? C25A H25A 0.93 . ? C26A C27A 1.39 . ? C26A H26A 0.93 . ? C27A H27A 0.93 . ? C21B C22B 1.51(2) . ? C21B H21F 0.97 . ? C21B H21G 0.97 . ? C22B C23B 1.39 . ? C22B C27B 1.39 . ? C23B C24B 1.39 . ? C23B H23E 0.93 . ? C24B C25B 1.39 . ? C24B H24B 0.93 . ? C25B C26B 1.39 . ? C25B H25B 0.93 . ? C26B C27B 1.39 . ? C26B H26B 0.93 . ? C27B H27B 0.93 . ? C21C C22C 1.58(2) . ? C21C H21H 0.97 . ? C21C H21I 0.97 . ? C22C C23C 1.39 . ? C22C C27C 1.39 . ? C23C C24C 1.39 . ? C23C H23F 0.93 . ? C24C C25C 1.39 . ? C24C H24C 0.93 . ? C25C C26C 1.39 . ? C25C H25C 0.93 . ? C26C C27C 1.39 . ? C26C H26C 0.93 . ? C27C H27C 0.93 . ? C31A C32A 1.49(2) . ? C31A H31A 0.97 . ? C31A H31B 0.97 . ? C32A C33A 1.39 . ? C32A C37A 1.39 . ? C33A C34A 1.39 . ? C33A H33A 0.93 . ? C34A C35A 1.39 . ? C34A H34A 0.93 . ? C35A C36A 1.39 . ? C35A H35A 0.93 . ? C36A C37A 1.39 . ? C36A H36A 0.93 . ? C37A H37A 0.93 . ? C31B C32B 1.48(2) . ? C31B H31C 0.97 . ? C31B H31D 0.97 . ? C32B C33B 1.39 . ? C32B C37B 1.39 . ? C33B C34B 1.39 . ? C33B H33B 0.93 . ? C34B C35B 1.39 . ? C34B H34B 0.93 . ? C35B C36B 1.39 . ? C35B H35B 0.93 . ? C36B C37B 1.39 . ? C36B H36B 0.93 . ? C37B H37B 0.93 . ? C31C C32C 1.50(2) . ? C31C H31E 0.97 . ? C31C H31F 0.97 . ? C32C C33C 1.39 . ? C32C C37C 1.39 . ? C33C C34C 1.39 . ? C33C H33C 0.93 . ? C34C C35C 1.39 . ? C34C H34C 0.93 . ? C35C C36C 1.39 . ? C35C H35C 0.93 . ? C36C C37C 1.39 . ? C36C H36C 0.93 . ? C37C H37C 0.93 . ? O1W H1WB 0.78(3) . ? O1W H1WA 1.15(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 S1 Pd1 S2 149.0(2) . . ? S1 Pd1 P1 101.5(2) . . ? S2 Pd1 P1 109.1(2) . . ? S1 Pd1 Pd3 100.7(2) . . ? S2 Pd1 Pd3 52.55(14) . . ? P1 Pd1 Pd3 151.6(2) . . ? S1 Pd1 Pd2 51.57(14) . . ? S2 Pd1 Pd2 98.0(2) . . ? P1 Pd1 Pd2 146.9(2) . . ? Pd3 Pd1 Pd2 61.37(5) . . ? C2 Pd2 S1 160.1(6) . . ? C2 Pd2 P2 102.8(6) . . ? S1 Pd2 P2 92.1(2) . . ? C2 Pd2 Pd1 108.0(6) . . ? S1 Pd2 Pd1 52.76(14) . . ? P2 Pd2 Pd1 137.8(2) . . ? C2 Pd2 Pd3 69.5(6) . . ? S1 Pd2 Pd3 99.3(2) . . ? P2 Pd2 Pd3 162.97(15) . . ? Pd1 Pd2 Pd3 58.61(6) . . ? C4 Pd3 S2 153.0(6) . . ? C4 Pd3 P3 100.7(7) . . ? S2 Pd3 P3 98.7(2) . . ? C4 Pd3 Pd1 100.8(6) . . ? S2 Pd3 Pd1 53.51(14) . . ? P3 Pd3 Pd1 144.5(2) . . ? C4 Pd3 Pd2 71.5(7) . . ? S2 Pd3 Pd2 97.6(2) . . ? P3 Pd3 Pd2 154.9(2) . . ? Pd1 Pd3 Pd2 60.01(6) . . ? C11B P1 C11C 105.3(10) . . ? C11B P1 C11A 107.3(10) . . ? C11C P1 C11A 96.6(10) . . ? C11B P1 Pd1 114.4(6) . . ? C11C P1 Pd1 114.0(7) . . ? C11A P1 Pd1 117.2(7) . . ? C21C P2 C21A 104.0(9) . . ? C21C P2 C21B 105.6(8) . . ? C21A P2 C21B 100.1(9) . . ? C21C P2 Pd2 114.6(6) . . ? C21A P2 Pd2 119.6(7) . . ? C21B P2 Pd2 111.3(6) . . ? C31A P3 C31C 107.8(10) . . ? C31A P3 C31B 102.7(10) . . ? C31C P3 C31B 99.5(10) . . ? C31A P3 Pd3 112.6(7) . . ? C31C P3 Pd3 117.2(7) . . ? C31B P3 Pd3 115.2(7) . . ? O2 S1 O1 112.6(9) . . ? O2 S1 Pd2 114.2(7) . . ? O1 S1 Pd2 115.1(6) . . ? O2 S1 Pd1 119.9(7) . . ? O1 S1 Pd1 114.5(6) . . ? Pd2 S1 Pd1 75.7(2) . . ? O3 S2 O4 112.5(9) . . ? O3 S2 Pd3 116.1(7) . . ? O4 S2 Pd3 114.6(6) . . ? O3 S2 Pd1 114.1(7) . . ? O4 S2 Pd1 120.5(7) . . ? Pd3 S2 Pd1 73.9(2) . . ? C2 N1 C1 174.6(26) . . ? C13 C1 N1 108.8(22) . . ? C13 C1 C12 115.0(23) . . ? N1 C1 C12 108.7(22) . . ? C13 C1 C11 109.2(27) . . ? N1 C1 C11 104.1(21) . . ? C12 C1 C11 110.4(27) . . ? N1 C2 Pd2 168.6(21) . . ? C4 N2 C3 175.6(22) . . ? N2 C3 C21 113.3(24) . . ? N2 C3 C23 107.9(22) . . ? C21 C3 C23 109.8(25) . . ? N2 C3 C22 106.9(21) . . ? C21 C3 C22 110.3(25) . . ? C23 C3 C22 108.5(27) . . ? N2 C4 Pd3 173.1(21) . . ? C1 C11 H11A 109.5(18) . . ? C1 C11 H11B 109.5(18) . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5(14) . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C12 H12A 109.5(15) . . ? C1 C12 H12B 109.5(14) . . ? H12A C12 H12B 109.5 . . ? C1 C12 H12C 109.5(19) . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 C13 H13A 109.5(15) . . ? C1 C13 H13B 109.5(17) . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5(14) . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C21 H21A 109.5(16) . . ? C3 C21 H21B 109.5(17) . . ? H21A C21 H21B 109.5 . . ? C3 C21 H21C 109.5(16) . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C3 C22 H22A 109.5(17) . . ? C3 C22 H22B 109.5(17) . . ? H22A C22 H22B 109.5 . . ? C3 C22 H22C 109.5(15) . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C23 H23A 109.5(17) . . ? C3 C23 H23B 109.5(15) . . ? H23A C23 H23B 109.5 . . ? C3 C23 H23C 109.5(18) . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C12A C11A P1 117.1(14) . . ? C12A C11A H11D 108.0(13) . . ? P1 C11A H11D 108.0(7) . . ? C12A C11A H11E 108.0(11) . . ? P1 C11A H11E 108.0(8) . . ? H11D C11A H11E 107.3 . . ? C13A C12A C17A 120.0 . . ? C13A C12A C11A 128.4(20) . . ? C17A C12A C11A 111.5(20) . . ? C14A C13A C12A 120.0 . . ? C14A C13A H13D 120.0 . . ? C12A C13A H13D 120.0 . . ? C13A C14A C15A 120.0 . . ? C13A C14A H14A 120.0 . . ? C15A C14A H14A 120.0 . . ? C14A C15A C16A 120.0 . . ? C14A C15A H15A 120.0 . . ? C16A C15A H15A 120.0 . . ? C17A C16A C15A 120.0 . . ? C17A C16A H16A 120.0 . . ? C15A C16A H16A 120.0 . . ? C16A C17A C12A 120.0 . . ? C16A C17A H17A 120.0 . . ? C12A C17A H17A 120.0 . . ? C12B C11B P1 121.2(13) . . ? C12B C11B H11F 107.0(11) . . ? P1 C11B H11F 107.0(7) . . ? C12B C11B H11G 107.0(11) . . ? P1 C11B H11G 107.0(7) . . ? H11F C11B H11G 106.8 . . ? C13B C12B C17B 120.0 . . ? C13B C12B C11B 122.2(17) . . ? C17B C12B C11B 117.8(17) . . ? C14B C13B C12B 120.0 . . ? C14B C13B H13E 120.0 . . ? C12B C13B H13E 120.0 . . ? C13B C14B C15B 120.0 . . ? C13B C14B H14B 120.0 . . ? C15B C14B H14B 120.0 . . ? C14B C15B C16B 120.0 . . ? C14B C15B H15B 120.0 . . ? C16B C15B H15B 120.0 . . ? C17B C16B C15B 120.0 . . ? C17B C16B H16B 120.0 . . ? C15B C16B H16B 120.0 . . ? C16B C17B C12B 120.0 . . ? C16B C17B H17B 120.0 . . ? C12B C17B H17B 120.0 . . ? C12C C11C P1 116.9(14) . . ? C12C C11C H11H 108.1(10) . . ? P1 C11C H11H 108.1(7) . . ? C12C C11C H11I 108.1(10) . . ? P1 C11C H11I 108.1(7) . . ? H11H C11C H11I 107.3 . . ? C13C C12C C17C 120.0 . . ? C13C C12C C11C 117.0(14) . . ? C17C C12C C11C 123.0(14) . . ? C12C C13C C14C 120.0 . . ? C12C C13C H13F 120.0 . . ? C14C C13C H13F 120.0 . . ? C15C C14C C13C 120.0 . . ? C15C C14C H14C 120.0 . . ? C13C C14C H14C 120.0 . . ? C16C C15C C14C 120.0 . . ? C16C C15C H15C 120.0 . . ? C14C C15C H15C 120.0 . . ? C15C C16C C17C 120.0 . . ? C15C C16C H16C 120.0 . . ? C17C C16C H16C 120.0 . . ? C16C C17C C12C 120.0 . . ? C16C C17C H17C 120.0 . . ? C12C C17C H17C 120.0 . . ? C22A C21A P2 112.7(12) . . ? C22A C21A H21D 109.1(10) . . ? P2 C21A H21D 109.1(6) . . ? C22A C21A H21E 109.1(10) . . ? P2 C21A H21E 109.1(6) . . ? H21D C21A H21E 107.8 . . ? C23A C22A C27A 120.0 . . ? C23A C22A C21A 116.1(16) . . ? C27A C22A C21A 123.9(16) . . ? C24A C23A C22A 120.0 . . ? C24A C23A H23D 120.0 . . ? C22A C23A H23D 120.0 . . ? C23A C24A C25A 120.0 . . ? C23A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C26A C25A C24A 120.0 . . ? C26A C25A H25A 120.0 . . ? C24A C25A H25A 120.0 . . ? C27A C26A C25A 120.0 . . ? C27A C26A H26A 120.0 . . ? C25A C26A H26A 120.0 . . ? C26A C27A C22A 120.0 . . ? C26A C27A H27A 120.0 . . ? C22A C27A H27A 120.0 . . ? C22B C21B P2 110.0(12) . . ? C22B C21B H21F 109.7(10) . . ? P2 C21B H21F 109.7(6) . . ? C22B C21B H21G 109.7(10) . . ? P2 C21B H21G 109.7(7) . . ? H21F C21B H21G 108.2 . . ? C23B C22B C27B 120.0 . . ? C23B C22B C21B 117.8(15) . . ? C27B C22B C21B 122.2(15) . . ? C24B C23B C22B 120.0 . . ? C24B C23B H23E 120.0 . . ? C22B C23B H23E 120.0 . . ? C25B C24B C23B 120.0 . . ? C25B C24B H24B 120.0 . . ? C23B C24B H24B 120.0 . . ? C24B C25B C26B 120.0 . . ? C24B C25B H25B 120.0 . . ? C26B C25B H25B 120.0 . . ? C25B C26B C27B 120.0 . . ? C25B C26B H26B 120.0 . . ? C27B C26B H26B 120.0 . . ? C26B C27B C22B 120.0 . . ? C26B C27B H27B 120.0 . . ? C22B C27B H27B 120.0 . . ? C22C C21C P2 117.9(11) . . ? C22C C21C H21H 107.8(9) . . ? P2 C21C H21H 107.8(6) . . ? C22C C21C H21I 107.8(9) . . ? P2 C21C H21I 107.8(6) . . ? H21H C21C H21I 107.2 . . ? C23C C22C C27C 120.0 . . ? C23C C22C C21C 119.3(15) . . ? C27C C22C C21C 120.7(15) . . ? C22C C23C C24C 120.0 . . ? C22C C23C H23F 120.0 . . ? C24C C23C H23F 120.0 . . ? C23C C24C C25C 120.0 . . ? C23C C24C H24C 120.0 . . ? C25C C24C H24C 120.0 . . ? C26C C25C C24C 120.0 . . ? C26C C25C H25C 120.0 . . ? C24C C25C H25C 120.0 . . ? C25C C26C C27C 120.0 . . ? C25C C26C H26C 120.0 . . ? C27C C26C H26C 120.0 . . ? C26C C27C C22C 120.0 . . ? C26C C27C H27C 120.0 . . ? C22C C27C H27C 120.0 . . ? C32A C31A P3 116.4(14) . . ? C32A C31A H31A 108.2(12) . . ? P3 C31A H31A 108.2(7) . . ? C32A C31A H31B 108.2(12) . . ? P3 C31A H31B 108.2(7) . . ? H31A C31A H31B 107.3 . . ? C33A C32A C37A 120.0 . . ? C33A C32A C31A 124.7(20) . . ? C37A C32A C31A 115.2(20) . . ? C32A C33A C34A 120.0 . . ? C32A C33A H33A 120.0 . . ? C34A C33A H33A 120.0 . . ? C33A C34A C35A 120.0 . . ? C33A C34A H34A 120.0 . . ? C35A C34A H34A 120.0 . . ? C36A C35A C34A 120.0 . . ? C36A C35A H35A 120.0 . . ? C34A C35A H35A 120.0 . . ? C37A C36A C35A 120.0 . . ? C37A C36A H36A 120.0 . . ? C35A C36A H36A 120.0 . . ? C36A C37A C32A 120.0 . . ? C36A C37A H37A 120.0 . . ? C32A C37A H37A 120.0 . . ? C32B C31B P3 114.8(13) . . ? C32B C31B H31C 108.6(11) . . ? P3 C31B H31C 108.6(6) . . ? C32B C31B H31D 108.6(11) . . ? P3 C31B H31D 108.6(7) . . ? H31C C31B H31D 107.5 . . ? C33B C32B C37B 120.0 . . ? C33B C32B C31B 118.2(18) . . ? C37B C32B C31B 121.8(18) . . ? C32B C33B C34B 120.0 . . ? C32B C33B H33B 120.0 . . ? C34B C33B H33B 120.0 . . ? C35B C34B C33B 120.0 . . ? C35B C34B H34B 120.0 . . ? C33B C34B H34B 120.0 . . ? C34B C35B C36B 120.0 . . ? C34B C35B H35B 120.0 . . ? C36B C35B H35B 120.0 . . ? C37B C36B C35B 120.0 . . ? C37B C36B H36B 120.0 . . ? C35B C36B H36B 120.0 . . ? C36B C37B C32B 120.0 . . ? C36B C37B H37B 120.0 . . ? C32B C37B H37B 120.0 . . ? C32C C31C P3 118.6(13) . . ? C32C C31C H31E 107.7(10) . . ? P3 C31C H31E 107.7(7) . . ? C32C C31C H31F 107.7(10) . . ? P3 C31C H31F 107.7(7) . . ? H31E C31C H31F 107.1 . . ? C33C C32C C37C 120.0 . . ? C33C C32C C31C 113.5(15) . . ? C37C C32C C31C 126.5(15) . . ? C34C C33C C32C 120.0 . . ? C34C C33C H33C 120.0 . . ? C32C C33C H33C 120.0 . . ? C35C C34C C33C 120.0 . . ? C35C C34C H34C 120.0 . . ? C33C C34C H34C 120.0 . . ? C34C C35C C36C 120.0 . . ? C34C C35C H35C 120.0 . . ? C36C C35C H35C 120.0 . . ? C37C C36C C35C 120.0 . . ? C37C C36C H36C 120.0 . . ? C35C C36C H36C 120.0 . . ? C36C C37C C32C 120.0 . . ? C36C C37C H37C 120.0 . . ? C32C C37C H37C 120.0 . . ? H1WB O1W H1WA 100.9(30) . . ? _refine_diff_density_max 0.963 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.127