# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2289 data_kf1a _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C31 H38 Cl N2 O4 P Pd S' _chemical_formula_weight 707.51 _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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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' _cell_length_a 10.7346(2) _cell_length_b 14.3998(3) _cell_length_c 20.3434(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3144.60(9) _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 'Plate-like crystal fragment' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method ? _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.831 _exptl_absorpt_correction_type 'Sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.793 _exptl_absorpt_correction_T_max 0.942 _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18439 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 26.41 _reflns_number_total 6426 _reflns_number_observed 5694 _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 2 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^)+(0.0552P)^2^+0.9022P] 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 0.00(3) _refine_ls_number_reflns 6424 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_obs 0.0379 _refine_ls_wR_factor_all 0.1025 _refine_ls_wR_factor_obs 0.0891 _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_obs 1.052 _refine_ls_restrained_S_all 1.136 _refine_ls_restrained_S_obs 1.052 _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 0.67096(3) 0.18256(2) 0.155821(14) 0.03115(9) Uani 1 d . . C1 C 0.4958(4) 0.1364(3) 0.1410(2) 0.0320(9) Uani 1 d . . C2 C 0.3864(4) 0.1608(3) 0.1758(2) 0.0360(10) Uani 1 d . . H2A H 0.3932(4) 0.1960(3) 0.2140(2) 0.043 Uiso 1 calc R . C3 C 0.2720(4) 0.1341(3) 0.1548(3) 0.0428(9) Uani 1 d . . H3A H 0.2016(4) 0.1536(3) 0.1777(3) 0.051 Uiso 1 calc R . C4 C 0.2580(4) 0.0773(3) 0.0987(2) 0.0383(10) Uani 1 d . . C5 C 0.1397(4) 0.0439(4) 0.0788(2) 0.0518(12) Uani 1 d . . H5A H 0.0688(4) 0.0639(4) 0.1009(2) 0.062 Uiso 1 calc R . C6 C 0.1276(5) -0.0168(4) 0.0278(3) 0.0630(15) Uani 1 d . . H6A H 0.0494(5) -0.0385(4) 0.0155(3) 0.076 Uiso 1 calc R . C7 C 0.2345(5) -0.0462(4) -0.0058(3) 0.0587(14) Uani 1 d . . H7A H 0.2266(5) -0.0891(4) -0.0397(3) 0.070 Uiso 1 calc R . C8 C 0.3494(5) -0.0137(3) 0.0098(2) 0.0471(11) Uani 1 d . . H8A H 0.4180(5) -0.0324(3) -0.0147(2) 0.056 Uiso 1 calc R . C9 C 0.3661(4) 0.0493(3) 0.0637(2) 0.0365(9) Uani 1 d . . C10 C 0.4844(4) 0.0840(3) 0.0841(2) 0.0351(9) Uani 1 d . . C11 C 0.6033(4) 0.0636(3) 0.0472(2) 0.0413(10) Uani 1 d . . H11A H 0.5837(4) 0.0508(3) 0.0010(2) 0.050 Uiso 1 calc R . N12 N 0.6824(4) 0.1508(3) 0.0516(2) 0.0414(8) Uani 1 d . . C13 C 0.6711(6) -0.0201(4) 0.0768(3) 0.0640(14) Uani 1 d . . H13A H 0.7462(6) -0.0317(4) 0.0526(3) 0.096 Uiso 1 calc R . H13B H 0.6181(6) -0.0737(4) 0.0746(3) 0.096 Uiso 1 calc R . H13C H 0.6914(6) -0.0074(4) 0.1219(3) 0.096 Uiso 1 calc R . C14 C 0.6236(6) 0.2264(4) 0.0133(3) 0.065(2) Uani 1 d . . H14A H 0.5411(6) 0.2376(4) 0.0298(3) 0.098 Uiso 1 calc R . H14B H 0.6190(6) 0.2087(4) -0.0321(3) 0.098 Uiso 1 calc R . H14C H 0.6725(6) 0.2819(4) 0.0175(3) 0.098 Uiso 1 calc R . C15 C 0.8079(5) 0.1353(5) 0.0254(3) 0.078(2) Uani 1 d . . H15A H 0.8477(5) 0.0864(5) 0.0497(3) 0.117 Uiso 1 calc R . H15B H 0.8559(5) 0.1913(5) 0.0295(3) 0.117 Uiso 1 calc R . H15C H 0.8024(5) 0.1181(5) -0.0201(3) 0.117 Uiso 1 calc R . P16 P 0.65238(8) 0.18013(7) 0.26366(4) 0.0288(2) Uani 1 d . . C17 C 0.5983(4) 0.0702(3) 0.2972(2) 0.0356(9) Uani 1 d . . C18 C 0.4874(5) 0.0617(3) 0.3317(2) 0.0485(11) Uani 1 d . . H18A H 0.4357(5) 0.1128(3) 0.3378(2) 0.058 Uiso 1 calc R . C19 C 0.4551(5) -0.0246(4) 0.3567(2) 0.0602(15) Uani 1 d . . H19A H 0.3811(5) -0.0313(4) 0.3800(2) 0.072 Uiso 1 calc R . C20 C 0.5309(6) -0.1002(3) 0.3476(3) 0.0641(14) Uani 1 d . . H20A H 0.5086(6) -0.1574(3) 0.3653(3) 0.077 Uiso 1 calc R . C21 C 0.6399(5) -0.0920(3) 0.3124(3) 0.0617(15) Uani 1 d . . H21A H 0.6914(5) -0.1432(3) 0.3062(3) 0.074 Uiso 1 calc R . C22 C 0.6719(5) -0.0063(3) 0.2864(3) 0.0516(11) Uani 1 d . . H22A H 0.7440(5) -0.0005(3) 0.2614(3) 0.062 Uiso 1 calc R . C23 C 0.5932(4) 0.2764(3) 0.3155(2) 0.0322(9) Uani 1 d . . H23A H 0.5037(4) 0.2890(3) 0.3118(2) 0.039 Uiso 1 calc R . C24 C 0.6374(4) 0.2436(3) 0.3830(2) 0.0317(9) Uani 1 d . . C25 C 0.7515(4) 0.2077(3) 0.3784(2) 0.0354(10) Uani 1 d . . C26 C 0.7976(4) 0.2089(3) 0.3072(2) 0.0313(9) Uani 1 d . . H26A H 0.8688(4) 0.1685(3) 0.2977(2) 0.038 Uiso 1 calc R . C27 C 0.8139(3) 0.3125(3) 0.2879(2) 0.0317(8) Uani 1 d . . H27A H 0.8656(3) 0.3422(3) 0.3215(2) 0.038 Uiso 1 calc R . C28 C 0.6794(4) 0.3551(3) 0.2926(2) 0.0353(9) Uani 1 d . . H28A H 0.6780(4) 0.4060(3) 0.3238(2) 0.042 Uiso 1 calc R . H28B H 0.6530(4) 0.3783(3) 0.2500(2) 0.042 Uiso 1 calc R . C29 C 0.5572(5) 0.2523(4) 0.4423(2) 0.0486(12) Uani 1 d . . H29A H 0.4798(5) 0.2811(4) 0.4304(2) 0.073 Uiso 1 calc R . H29B H 0.5988(5) 0.2896(4) 0.4746(2) 0.073 Uiso 1 calc R . H29C H 0.5412(5) 0.1917(4) 0.4601(2) 0.073 Uiso 1 calc R . C30 C 0.8329(5) 0.1705(4) 0.4320(2) 0.0590(13) Uani 1 d . . H30A H 0.9101(5) 0.1493(4) 0.4136(2) 0.088 Uiso 1 calc R . H30B H 0.7915(5) 0.1196(4) 0.4534(2) 0.088 Uiso 1 calc R . H30C H 0.8491(5) 0.2186(4) 0.4635(2) 0.088 Uiso 1 calc R . C31 C 0.8750(4) 0.3291(3) 0.2216(2) 0.0360(9) Uani 1 d . . N32 N 0.9324(4) 0.4083(3) 0.2125(2) 0.0462(9) Uani 1 d . . C33 C 0.9438(6) 0.4800(4) 0.2645(3) 0.065(2) Uani 1 d . . H33A H 0.9890(6) 0.5323(4) 0.2476(3) 0.098 Uiso 1 calc R . H33B H 0.9875(6) 0.4545(4) 0.3015(3) 0.098 Uiso 1 calc R . H33C H 0.8622(6) 0.4995(4) 0.2780(3) 0.098 Uiso 1 calc R . C34 C 0.9943(6) 0.4311(4) 0.1502(3) 0.072(2) Uani 1 d . . H34A H 1.0308(6) 0.4919(4) 0.1532(3) 0.108 Uiso 1 calc R . H34B H 0.9344(6) 0.4302(4) 0.1152(3) 0.108 Uiso 1 calc R . H34C H 1.0584(6) 0.3863(4) 0.1414(3) 0.108 Uiso 1 calc R . S35 S 0.87429(11) 0.24856(9) 0.15984(6) 0.0523(3) Uani 1 d . . Cl1 Cl 1.16246(11) 0.25443(9) 0.33983(7) 0.0542(3) Uani 1 d . . O1 O 1.0938(5) 0.3139(5) 0.3808(3) 0.111(2) Uani 1 d . . O2 O 1.2869(4) 0.2582(5) 0.3495(4) 0.144(3) Uani 1 d . . O3 O 1.1196(7) 0.1638(4) 0.3461(5) 0.164(3) Uani 1 d . . O4 O 1.1327(8) 0.2746(8) 0.2766(3) 0.190(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 0.03276(14) 0.03298(14) 0.02772(13) -0.00338(13) -0.00002(13) -0.00330(13) C1 0.034(2) 0.027(2) 0.035(2) 0.001(2) -0.003(2) -0.004(2) C2 0.039(2) 0.035(2) 0.034(2) -0.002(2) 0.000(2) 0.001(2) C3 0.038(2) 0.044(2) 0.047(2) 0.003(2) 0.004(2) 0.000(2) C4 0.041(2) 0.038(2) 0.036(2) 0.006(2) -0.005(2) -0.003(2) C5 0.044(3) 0.060(3) 0.051(3) 0.009(2) -0.007(2) -0.007(2) C6 0.052(3) 0.072(4) 0.065(3) 0.001(3) -0.021(3) -0.022(3) C7 0.068(4) 0.051(3) 0.057(3) -0.007(2) -0.021(3) -0.010(3) C8 0.055(3) 0.045(2) 0.042(2) -0.007(2) -0.013(2) -0.001(2) C9 0.042(2) 0.032(2) 0.035(2) 0.006(2) -0.007(2) -0.001(2) C10 0.039(2) 0.030(2) 0.036(2) -0.001(2) -0.003(2) 0.002(2) C11 0.040(2) 0.048(3) 0.036(2) -0.011(2) -0.007(2) -0.001(2) N12 0.037(2) 0.057(2) 0.031(2) -0.0078(15) 0.005(2) -0.009(2) C13 0.067(3) 0.054(3) 0.071(3) -0.023(3) -0.014(3) 0.026(3) C14 0.081(4) 0.072(4) 0.043(3) 0.016(3) -0.008(3) -0.014(3) C15 0.044(3) 0.135(6) 0.054(3) -0.037(3) 0.014(3) -0.018(3) P16 0.0297(5) 0.0277(4) 0.0290(4) -0.0015(4) -0.0002(4) -0.0011(5) C17 0.042(2) 0.034(2) 0.032(2) 0.003(2) -0.004(2) -0.009(2) C18 0.058(3) 0.039(2) 0.049(3) -0.007(2) 0.013(2) -0.009(2) C19 0.077(4) 0.059(3) 0.046(3) -0.005(2) 0.016(3) -0.032(3) C20 0.098(4) 0.036(3) 0.058(3) 0.003(3) -0.004(4) -0.021(3) C21 0.063(4) 0.031(2) 0.092(4) 0.004(2) -0.010(3) -0.003(2) C22 0.049(3) 0.039(2) 0.067(3) 0.000(2) 0.000(3) -0.002(2) C23 0.026(2) 0.034(2) 0.036(2) -0.003(2) 0.002(2) 0.000(2) C24 0.037(2) 0.027(2) 0.032(2) -0.004(2) 0.000(2) -0.005(2) C25 0.038(2) 0.037(2) 0.032(2) 0.001(2) -0.004(2) -0.005(2) C26 0.033(2) 0.030(2) 0.031(2) -0.0007(15) -0.003(2) 0.0007(15) C27 0.031(2) 0.035(2) 0.029(2) 0.001(2) -0.0022(15) -0.006(2) C28 0.039(2) 0.028(2) 0.039(2) -0.002(2) 0.003(2) 0.001(2) C29 0.055(3) 0.055(3) 0.036(2) -0.006(2) 0.011(2) -0.009(2) C30 0.048(3) 0.092(4) 0.037(2) 0.016(2) -0.009(2) 0.000(3) C31 0.029(2) 0.044(2) 0.035(2) -0.001(2) 0.0001(15) 0.000(2) N32 0.050(2) 0.044(2) 0.045(2) 0.003(2) 0.010(2) -0.010(2) C33 0.085(4) 0.039(3) 0.073(4) -0.007(2) 0.019(3) -0.016(3) C34 0.092(4) 0.072(4) 0.052(3) 0.008(3) 0.022(3) -0.034(3) S35 0.0457(6) 0.0709(8) 0.0404(6) -0.0165(6) 0.0110(5) -0.0226(5) Cl1 0.0368(5) 0.0672(7) 0.0588(6) -0.0033(6) 0.0002(6) 0.0011(5) O1 0.091(3) 0.118(4) 0.123(4) -0.047(4) 0.028(3) 0.004(4) O2 0.047(2) 0.137(5) 0.249(8) -0.051(6) -0.028(4) 0.006(3) O3 0.129(5) 0.086(4) 0.278(10) -0.022(5) 0.043(6) -0.034(3) O4 0.171(7) 0.310(12) 0.089(5) 0.009(6) -0.013(4) 0.091(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 Pd C1 2.017(4) . ? Pd N12 2.172(3) . ? Pd P16 2.2031(9) . ? Pd S35 2.3820(11) . ? C1 C10 1.386(5) . ? C1 C2 1.417(6) . ? C2 C3 1.357(6) . ? C3 C4 1.412(7) . ? C4 C5 1.417(6) . ? C4 C9 1.421(6) . ? C5 C6 1.363(8) . ? C6 C7 1.401(8) . ? C7 C8 1.356(7) . ? C8 C9 1.434(6) . ? C9 C10 1.427(6) . ? C10 C11 1.510(6) . ? C11 N12 1.518(6) . ? C11 C13 1.531(7) . ? N12 C15 1.466(6) . ? N12 C14 1.480(7) . ? P16 C17 1.818(4) . ? P16 C26 1.840(4) . ? P16 C23 1.854(4) . ? C17 C22 1.374(7) . ? C17 C18 1.387(6) . ? C18 C19 1.387(7) . ? C19 C20 1.372(8) . ? C20 C21 1.377(8) . ? C21 C22 1.386(7) . ? C23 C24 1.527(6) . ? C23 C28 1.536(6) . ? C24 C25 1.333(6) . ? C24 C29 1.488(6) . ? C25 C30 1.496(6) . ? C25 C26 1.531(6) . ? C26 C27 1.552(5) . ? C27 C31 1.517(5) . ? C27 C28 1.571(6) . ? C31 N32 1.309(6) . ? C31 S35 1.711(4) . ? N32 C34 1.469(6) . ? N32 C33 1.484(6) . ? Cl1 O2 1.351(5) . ? Cl1 O4 1.356(7) . ? Cl1 O3 1.389(6) . ? Cl1 O1 1.404(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd N12 80.61(15) . . ? C1 Pd P16 93.41(11) . . ? N12 Pd P16 166.80(10) . . ? C1 Pd S35 172.24(11) . . ? N12 Pd S35 93.78(10) . . ? P16 Pd S35 93.16(4) . . ? C10 C1 C2 118.7(4) . . ? C10 C1 Pd 112.8(3) . . ? C2 C1 Pd 128.0(3) . . ? C3 C2 C1 121.5(4) . . ? C2 C3 C4 121.1(4) . . ? C3 C4 C5 121.6(4) . . ? C3 C4 C9 118.9(4) . . ? C5 C4 C9 119.5(4) . . ? C6 C5 C4 121.4(5) . . ? C5 C6 C7 119.1(5) . . ? C8 C7 C6 121.8(5) . . ? C7 C8 C9 120.7(5) . . ? C4 C9 C10 118.8(4) . . ? C4 C9 C8 117.4(4) . . ? C10 C9 C8 123.8(4) . . ? C1 C10 C9 120.8(4) . . ? C1 C10 C11 116.5(4) . . ? C9 C10 C11 122.6(4) . . ? C10 C11 N12 106.4(3) . . ? C10 C11 C13 111.1(4) . . ? N12 C11 C13 111.3(4) . . ? C15 N12 C14 108.2(5) . . ? C15 N12 C11 111.5(4) . . ? C14 N12 C11 109.8(4) . . ? C15 N12 Pd 116.0(3) . . ? C14 N12 Pd 109.6(3) . . ? C11 N12 Pd 101.6(2) . . ? C17 P16 C26 106.6(2) . . ? C17 P16 C23 109.1(2) . . ? C26 P16 C23 81.3(2) . . ? C17 P16 Pd 114.60(14) . . ? C26 P16 Pd 113.53(13) . . ? C23 P16 Pd 125.83(14) . . ? C22 C17 C18 120.2(4) . . ? C22 C17 P16 117.0(4) . . ? C18 C17 P16 122.8(3) . . ? C17 C18 C19 118.7(5) . . ? C20 C19 C18 120.9(5) . . ? C19 C20 C21 120.4(5) . . ? C20 C21 C22 119.1(5) . . ? C17 C22 C21 120.7(5) . . ? C24 C23 C28 108.3(3) . . ? C24 C23 P16 100.0(3) . . ? C28 C23 P16 99.9(3) . . ? C25 C24 C29 128.4(4) . . ? C25 C24 C23 110.1(4) . . ? C29 C24 C23 121.5(4) . . ? C24 C25 C30 128.7(4) . . ? C24 C25 C26 111.0(4) . . ? C30 C25 C26 120.3(4) . . ? C25 C26 C27 106.7(3) . . ? C25 C26 P16 100.3(3) . . ? C27 C26 P16 101.0(2) . . ? C31 C27 C26 115.2(3) . . ? C31 C27 C28 112.9(3) . . ? C26 C27 C28 104.8(3) . . ? C23 C28 C27 106.5(3) . . ? N32 C31 C27 117.9(4) . . ? N32 C31 S35 119.2(3) . . ? C27 C31 S35 122.9(3) . . ? C31 N32 C34 122.1(4) . . ? C31 N32 C33 122.9(4) . . ? C34 N32 C33 115.0(4) . . ? C31 S35 Pd 107.44(14) . . ? O2 Cl1 O4 111.2(6) . . ? O2 Cl1 O3 110.6(4) . . ? O4 Cl1 O3 102.1(6) . . ? O2 Cl1 O1 114.1(4) . . ? O4 Cl1 O1 108.0(5) . . ? O3 Cl1 O1 110.2(4) . . ? _refine_diff_density_max 1.401 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.075 data_kf31 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H43 Cl N2 O0.50 P Pd S' _chemical_formula_weight 680.57 _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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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' _cell_length_a 12.5862(4) _cell_length_b 22.6849(7) _cell_length_c 23.3035(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6653.5(4) _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 'Prismatic crystal fragment' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method ? _exptl_crystal_F_000 2824 _exptl_absorpt_coefficient_mu 0.775 _exptl_absorpt_correction_type 'Sababs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 0.915 _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40678 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.08 _reflns_number_total 14416 _reflns_number_observed 11838 _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 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^)+(0.0313P)^2^+2.4097P] 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 -0.03(2) _refine_ls_number_reflns 14416 _refine_ls_number_parameters 712 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_obs 0.0362 _refine_ls_wR_factor_all 0.0805 _refine_ls_wR_factor_obs 0.0716 _refine_ls_goodness_of_fit_all 1.060 _refine_ls_goodness_of_fit_obs 1.044 _refine_ls_restrained_S_all 1.060 _refine_ls_restrained_S_obs 1.044 _refine_ls_shift/esd_max 0.003 _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 Pd1 Pd 1.31051(2) 0.414142(12) 0.970591(10) 0.03364(7) Uani 1 d . . Cl1 Cl 1.24338(10) 0.31586(4) 0.95845(4) 0.0581(3) Uani 1 d . . P1 P 1.30265(8) 0.40550(4) 1.06555(3) 0.0332(2) Uani 1 d . . S1 S 0.94231(11) 0.40146(6) 1.16249(6) 0.0746(4) Uani 1 d . . N1 N 1.3257(2) 0.43251(12) 0.88034(12) 0.0371(7) Uani 1 d . . N3 N 0.9779(3) 0.3058(2) 1.10183(15) 0.0495(9) Uani 1 d . . C1 C 1.3632(3) 0.49784(15) 0.97531(15) 0.0349(8) Uani 1 d . . C2 C 1.4138(3) 0.5271(2) 1.0218(2) 0.0414(9) Uani 1 d . . H2A H 1.4275(3) 0.5061(2) 1.0553(2) 0.050 Uiso 1 calc R . C3 C 1.4427(3) 0.5849(2) 1.0189(2) 0.0478(9) Uani 1 d . . H3A H 1.4740(3) 0.6028(2) 1.0506(2) 0.057 Uiso 1 calc R . C4 C 1.4260(3) 0.6181(2) 0.9684(2) 0.0443(9) Uani 1 d . . C5 C 1.4531(4) 0.6787(2) 0.9643(2) 0.0571(11) Uani 1 d . . H5A H 1.4846(4) 0.6973(2) 0.9955(2) 0.069 Uiso 1 calc R . C6 C 1.4342(4) 0.7098(2) 0.9160(2) 0.0658(14) Uani 1 d . . H6A H 1.4502(4) 0.7498(2) 0.9149(2) 0.079 Uiso 1 calc R . C7 C 1.3908(4) 0.6823(2) 0.8679(2) 0.0654(13) Uani 1 d . . H7A H 1.3802(4) 0.7039(2) 0.8344(2) 0.078 Uiso 1 calc R . C8 C 1.3636(4) 0.6239(2) 0.8695(2) 0.0572(11) Uani 1 d . . H8A H 1.3345(4) 0.6063(2) 0.8371(2) 0.069 Uiso 1 calc R . C9 C 1.3793(3) 0.5896(2) 0.91993(15) 0.0419(8) Uani 1 d . . C10 C 1.3494(3) 0.5285(2) 0.92462(15) 0.0361(8) Uani 1 d . . C11 C 1.2970(3) 0.4966(2) 0.87523(15) 0.0394(9) Uani 1 d . . H11A H 1.3247(3) 0.5121(2) 0.83893(15) 0.047 Uiso 1 calc R . C12 C 1.1774(4) 0.5055(2) 0.8772(2) 0.0607(12) Uani 1 d . . H12A H 1.1450(4) 0.4850(2) 0.8456(2) 0.091 Uiso 1 calc R . H12B H 1.1616(4) 0.5468(2) 0.8745(2) 0.091 Uiso 1 calc R . H12C H 1.1500(4) 0.4902(2) 0.9126(2) 0.091 Uiso 1 calc R . C13 C 1.2625(4) 0.3949(2) 0.8408(2) 0.0527(11) Uani 1 d . . H13A H 1.2833(4) 0.3544(2) 0.8455(2) 0.079 Uiso 1 calc R . H13B H 1.2751(4) 0.4069(2) 0.8019(2) 0.079 Uiso 1 calc R . H13C H 1.1883(4) 0.3989(2) 0.8496(2) 0.079 Uiso 1 calc R . C14 C 1.4401(3) 0.4250(2) 0.8634(2) 0.0541(11) Uani 1 d . . H14A H 1.4841(3) 0.4486(2) 0.8880(2) 0.081 Uiso 1 calc R . H14B H 1.4494(3) 0.4372(2) 0.8243(2) 0.081 Uiso 1 calc R . H14C H 1.4598(3) 0.3843(2) 0.8672(2) 0.081 Uiso 1 calc R . C15 C 1.2041(3) 0.35625(15) 1.09902(14) 0.0334(8) Uani 1 d . . H15A H 1.2115(3) 0.31428(15) 1.08988(14) 0.040 Uiso 1 calc R . C16 C 1.2168(3) 0.3723(2) 1.16195(15) 0.0384(9) Uani 1 d . . C17 C 1.2316(3) 0.43011(15) 1.16780(14) 0.0407(9) Uani 1 d . . C18 C 1.2317(3) 0.4606(2) 1.10946(14) 0.0389(9) Uani 1 d . . H18A H 1.2609(3) 0.5006(2) 1.10871(14) 0.047 Uiso 1 calc R . C19 C 1.1186(3) 0.4531(2) 1.0829(2) 0.0440(10) Uani 1 d . . H19A H 1.0656(3) 0.4711(2) 1.1075(2) 0.053 Uiso 1 calc R . H19B H 1.1154(3) 0.4717(2) 1.0455(2) 0.053 Uiso 1 calc R . C20 C 1.0982(3) 0.3865(2) 1.0776(2) 0.0380(9) Uani 1 d . . H20A H 1.0881(3) 0.3769(2) 1.0370(2) 0.046 Uiso 1 calc R . C21 C 1.0048(3) 0.3614(2) 1.1117(2) 0.0451(10) Uani 1 d . . C22 C 1.0166(4) 0.2700(2) 1.0530(2) 0.0609(13) Uani 1 d . . H22A H 0.9862(4) 0.2313(2) 1.0551(2) 0.091 Uiso 1 calc R . H22B H 1.0926(4) 0.2672(2) 1.0547(2) 0.091 Uiso 1 calc R . H22C H 0.9961(4) 0.2885(2) 1.0176(2) 0.091 Uiso 1 calc R . C23 C 0.9043(4) 0.2731(2) 1.1388(2) 0.0716(14) Uani 1 d . . H23A H 0.8957(4) 0.2338(2) 1.1242(2) 0.107 Uiso 1 calc R . H23B H 0.8367(4) 0.2926(2) 1.1393(2) 0.107 Uiso 1 calc R . H23C H 0.9324(4) 0.2714(2) 1.1771(2) 0.107 Uiso 1 calc R . C24 C 1.2077(4) 0.3266(2) 1.2082(2) 0.0596(13) Uani 1 d . . H24A H 1.1973(4) 0.2885(2) 1.1911(2) 0.089 Uiso 1 calc R . H24B H 1.1484(4) 0.3357(2) 1.2325(2) 0.089 Uiso 1 calc R . H24C H 1.2717(4) 0.3262(2) 1.2307(2) 0.089 Uiso 1 calc R . C25 C 1.2354(4) 0.4653(2) 1.2218(2) 0.0608(13) Uani 1 d . . H25A H 1.2472(4) 0.5060(2) 1.2127(2) 0.091 Uiso 1 calc R . H25B H 1.2921(4) 0.4511(2) 1.2457(2) 0.091 Uiso 1 calc R . H25C H 1.1691(4) 0.4613(2) 1.2419(2) 0.091 Uiso 1 calc R . C26 C 1.4323(3) 0.3869(2) 1.09581(15) 0.0373(8) Uani 1 d . . C27 C 1.4855(4) 0.3398(2) 1.0706(2) 0.0479(10) Uani 1 d . . H27A H 1.4533(4) 0.3185(2) 1.0412(2) 0.058 Uiso 1 calc R . C28 C 1.5869(4) 0.3244(2) 1.0893(2) 0.0651(14) Uani 1 d . . H28A H 1.6227(4) 0.2931(2) 1.0724(2) 0.078 Uiso 1 calc R . C29 C 1.6339(4) 0.3559(2) 1.1331(2) 0.0683(14) Uani 1 d . . H29A H 1.7021(4) 0.3463(2) 1.1453(2) 0.082 Uiso 1 calc R . C30 C 1.5801(4) 0.4014(2) 1.1588(2) 0.0679(14) Uani 1 d . . H30A H 1.6116(4) 0.4217(2) 1.1890(2) 0.081 Uiso 1 calc R . C31 C 1.4801(3) 0.4176(2) 1.1404(2) 0.0532(10) Uani 1 d . . H31A H 1.4449(3) 0.4489(2) 1.1578(2) 0.064 Uiso 1 calc R . Pd2 Pd 0.72627(2) 0.417115(12) 0.864091(10) 0.03526(7) Uani 1 d . . Cl2 Cl 0.73764(12) 0.31218(4) 0.87341(5) 0.0674(3) Uani 1 d . . P2 P 0.72501(8) 0.40723(4) 0.76900(3) 0.0341(2) Uani 1 d . . S2 S 1.09486(10) 0.39264(6) 0.68315(5) 0.0665(3) Uani 1 d . . N2 N 0.7473(2) 0.43511(13) 0.95390(12) 0.0412(8) Uani 1 d . . N4 N 1.0626(3) 0.3128(2) 0.7634(2) 0.0596(10) Uani 1 d . . C41 C 0.7105(3) 0.5052(2) 0.8623(2) 0.0382(8) Uani 1 d . . C42 C 0.6587(3) 0.5400(2) 0.8202(2) 0.0471(10) Uani 1 d . . H42A H 0.6285(3) 0.5219(2) 0.7884(2) 0.056 Uiso 1 calc R . C43 C 0.6526(4) 0.5998(2) 0.8256(2) 0.0582(12) Uani 1 d . . H43A H 0.6166(4) 0.6214(2) 0.7979(2) 0.070 Uiso 1 calc R . C44 C 0.6993(4) 0.6294(2) 0.8722(2) 0.0547(11) Uani 1 d . . C45 C 0.6990(5) 0.6920(2) 0.8766(3) 0.078(2) Uani 1 d . . H45A H 0.6682(5) 0.7144(2) 0.8476(3) 0.093 Uiso 1 calc R . C46 C 0.7426(5) 0.7194(2) 0.9224(3) 0.088(2) Uani 1 d . . H46A H 0.7425(5) 0.7603(2) 0.9242(3) 0.106 Uiso 1 calc R . C47 C 0.7878(5) 0.6869(2) 0.9668(3) 0.084(2) Uani 1 d . . H47A H 0.8159(5) 0.7062(2) 0.9986(3) 0.101 Uiso 1 calc R . C48 C 0.7908(4) 0.6265(2) 0.9639(2) 0.0611(12) Uani 1 d . . H48A H 0.8224(4) 0.6054(2) 0.9936(2) 0.073 Uiso 1 calc R . C49 C 0.7469(3) 0.5956(2) 0.9167(2) 0.0471(10) Uani 1 d . . C50 C 0.7513(3) 0.5332(2) 0.91086(15) 0.0401(9) Uani 1 d . . C51 C 0.8042(3) 0.4939(2) 0.9551(2) 0.0451(10) Uani 1 d . . H51A H 0.7955(3) 0.5117(2) 0.9932(2) 0.054 Uiso 1 calc R . C52 C 0.9220(4) 0.4883(2) 0.9420(2) 0.0617(12) Uani 1 d . . H52A H 0.9550(4) 0.4634(2) 0.9701(2) 0.093 Uiso 1 calc R . H52B H 0.9544(4) 0.5266(2) 0.9429(2) 0.093 Uiso 1 calc R . H52C H 0.9311(4) 0.4714(2) 0.9046(2) 0.093 Uiso 1 calc R . C53 C 0.6410(3) 0.4422(2) 0.9810(2) 0.0529(11) Uani 1 d . . H53A H 0.6014(3) 0.4717(2) 0.9606(2) 0.079 Uiso 1 calc R . H53B H 0.6496(3) 0.4541(2) 1.0202(2) 0.079 Uiso 1 calc R . H53C H 0.6035(3) 0.4054(2) 0.9795(2) 0.079 Uiso 1 calc R . C54 C 0.8055(4) 0.3893(2) 0.9866(2) 0.0646(13) Uani 1 d . . H54A H 0.8746(4) 0.3838(2) 0.9700(2) 0.097 Uiso 1 calc R . H54B H 0.7667(4) 0.3529(2) 0.9851(2) 0.097 Uiso 1 calc R . H54C H 0.8129(4) 0.4016(2) 1.0258(2) 0.097 Uiso 1 calc R . C55 C 0.8288(3) 0.3577(2) 0.73986(15) 0.0347(8) Uani 1 d . . H55A H 0.8229(3) 0.3163(2) 0.75156(15) 0.042 Uiso 1 calc R . C56 C 0.8188(3) 0.3687(2) 0.67606(14) 0.0382(8) Uani 1 d . . C57 C 0.7997(3) 0.4255(2) 0.66624(14) 0.0410(9) Uani 1 d . . C58 C 0.7955(3) 0.46021(15) 0.72196(14) 0.0373(9) Uani 1 d . . H58A H 0.7644(3) 0.49973(15) 0.71946(14) 0.045 Uiso 1 calc R . C59 C 0.9089(3) 0.4567(2) 0.7487(2) 0.0448(10) Uani 1 d . . H59A H 0.9615(3) 0.4710(2) 0.7217(2) 0.054 Uiso 1 calc R . H59B H 0.9126(3) 0.4804(2) 0.7833(2) 0.054 Uiso 1 calc R . C60 C 0.9294(3) 0.3908(2) 0.7630(2) 0.0391(9) Uani 1 d . . H60A H 0.9311(3) 0.3865(2) 0.8048(2) 0.047 Uiso 1 calc R . C61 C 1.0297(3) 0.3631(2) 0.7386(2) 0.0462(10) Uani 1 d . . C62 C 1.0150(4) 0.2857(2) 0.8145(2) 0.077(2) Uani 1 d . . H62A H 1.0525(4) 0.2502(2) 0.8238(2) 0.116 Uiso 1 calc R . H62B H 0.9418(4) 0.2767(2) 0.8070(2) 0.116 Uiso 1 calc R . H62C H 1.0195(4) 0.3127(2) 0.8462(2) 0.116 Uiso 1 calc R . C63 C 1.1545(5) 0.2813(2) 0.7405(3) 0.090(2) Uani 1 d . . H63A H 1.1671(5) 0.2465(2) 0.7630(3) 0.134 Uiso 1 calc R . H63B H 1.2159(5) 0.3063(2) 0.7420(3) 0.134 Uiso 1 calc R . H63C H 1.1409(5) 0.2702(2) 0.7014(3) 0.134 Uiso 1 calc R . C64 C 0.8342(4) 0.3200(2) 0.6333(2) 0.0648(13) Uani 1 d . . H64A H 0.8467(4) 0.2836(2) 0.6532(2) 0.097 Uiso 1 calc R . H64B H 0.8942(4) 0.3289(2) 0.6093(2) 0.097 Uiso 1 calc R . H64C H 0.7717(4) 0.3163(2) 0.6100(2) 0.097 Uiso 1 calc R . C65 C 0.7933(4) 0.4579(2) 0.6100(2) 0.0632(13) Uani 1 d . . H65A H 0.7783(4) 0.4988(2) 0.6171(2) 0.095 Uiso 1 calc R . H65B H 0.7377(4) 0.4412(2) 0.5870(2) 0.095 Uiso 1 calc R . H65C H 0.8598(4) 0.4544(2) 0.5901(2) 0.095 Uiso 1 calc R . C66 C 0.6017(3) 0.3862(2) 0.73473(15) 0.0371(8) Uani 1 d . . C67 C 0.5608(4) 0.3305(2) 0.7452(2) 0.0488(10) Uani 1 d . . H67A H 0.5967(4) 0.3051(2) 0.7699(2) 0.059 Uiso 1 calc R . C68 C 0.4673(4) 0.3120(2) 0.7196(2) 0.0601(12) Uani 1 d . . H68A H 0.4412(4) 0.2744(2) 0.7267(2) 0.072 Uiso 1 calc R . C69 C 0.4130(4) 0.3494(2) 0.6835(2) 0.0609(12) Uani 1 d . . H69A H 0.3505(4) 0.3369(2) 0.6661(2) 0.073 Uiso 1 calc R . C70 C 0.4505(4) 0.4050(2) 0.6732(2) 0.0619(12) Uani 1 d . . H70A H 0.4129(4) 0.4305(2) 0.6495(2) 0.074 Uiso 1 calc R . C71 C 0.5453(3) 0.4234(2) 0.6984(2) 0.0523(10) Uani 1 d . . H71A H 0.5712(3) 0.4610(2) 0.6908(2) 0.063 Uiso 1 calc R . O1 O 1.0564(4) 0.6321(2) 0.9134(2) 0.0934(12) Uani 1 d . . C72 C 0.9913(7) 0.6276(4) 0.8177(3) 0.129(3) Uani 1 d . . H72A H 0.9769(7) 0.6517(4) 0.7848(3) 0.193 Uiso 1 calc R . H72B H 0.9269(7) 0.6090(4) 0.8303(3) 0.193 Uiso 1 calc R . H72C H 1.0426(7) 0.5980(4) 0.8078(3) 0.193 Uiso 1 calc R . C73 C 1.0342(7) 0.6649(3) 0.8647(4) 0.125(3) Uani 1 d . . H73A H 1.0986(7) 0.6842(3) 0.8517(4) 0.150 Uiso 1 calc R . H73B H 0.9828(7) 0.6953(3) 0.8742(4) 0.150 Uiso 1 calc R . C74 C 1.1029(6) 0.6637(3) 0.9584(4) 0.123(3) Uani 1 d . . H74A H 1.0569(6) 0.6961(3) 0.9694(4) 0.148 Uiso 1 calc R . H74B H 1.1702(6) 0.6801(3) 0.9459(4) 0.148 Uiso 1 calc R . C75 C 1.1205(7) 0.6246(4) 1.0085(3) 0.133(3) Uani 1 d . . H75A H 1.1524(7) 0.6467(4) 1.0391(3) 0.199 Uiso 1 calc R . H75B H 1.1668(7) 0.5928(4) 0.9977(3) 0.199 Uiso 1 calc R . H75C H 1.0537(7) 0.6088(4) 1.0212(3) 0.199 Uiso 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 0.04147(15) 0.03460(14) 0.02487(12) -0.00290(12) 0.00060(11) -0.00274(13) Cl1 0.0862(9) 0.0426(5) 0.0454(6) -0.0124(4) 0.0122(6) -0.0168(5) P1 0.0423(5) 0.0316(5) 0.0258(4) -0.0033(4) 0.0011(4) -0.0016(4) S1 0.0695(8) 0.0685(9) 0.0857(9) -0.0314(7) 0.0323(7) -0.0127(6) N1 0.045(2) 0.039(2) 0.0279(14) -0.0026(12) 0.0010(13) 0.0000(13) N3 0.049(2) 0.048(2) 0.051(2) -0.008(2) 0.003(2) -0.006(2) C1 0.037(2) 0.037(2) 0.031(2) -0.002(2) 0.003(2) -0.002(2) C2 0.052(2) 0.042(2) 0.031(2) 0.003(2) -0.004(2) -0.008(2) C3 0.052(2) 0.054(2) 0.038(2) -0.010(2) -0.005(2) -0.011(2) C4 0.047(2) 0.041(2) 0.045(2) -0.005(2) 0.003(2) -0.008(2) C5 0.067(3) 0.042(2) 0.062(3) -0.009(2) 0.000(2) -0.012(2) C6 0.086(4) 0.035(2) 0.076(3) 0.002(2) 0.010(3) -0.008(2) C7 0.089(4) 0.047(3) 0.060(3) 0.011(2) 0.004(3) -0.005(2) C8 0.079(3) 0.048(3) 0.044(2) 0.002(2) -0.008(2) -0.003(2) C9 0.045(2) 0.041(2) 0.039(2) 0.000(2) 0.001(2) 0.002(2) C10 0.038(2) 0.039(2) 0.032(2) -0.001(2) 0.003(2) 0.000(2) C11 0.046(2) 0.041(2) 0.031(2) 0.003(2) -0.001(2) -0.001(2) C12 0.055(3) 0.070(3) 0.057(3) -0.012(2) -0.016(2) 0.015(2) C13 0.074(3) 0.050(2) 0.034(2) -0.007(2) -0.015(2) -0.008(2) C14 0.055(2) 0.066(3) 0.041(2) -0.003(2) 0.010(2) 0.012(2) C15 0.043(2) 0.028(2) 0.029(2) -0.0020(13) 0.006(2) 0.000(2) C16 0.045(2) 0.037(2) 0.033(2) -0.0004(15) 0.000(2) 0.001(2) C17 0.058(2) 0.035(2) 0.029(2) -0.0064(14) 0.003(2) -0.003(2) C18 0.052(2) 0.030(2) 0.035(2) -0.0008(15) 0.006(2) -0.004(2) C19 0.048(3) 0.036(2) 0.049(2) -0.001(2) 0.004(2) 0.005(2) C20 0.043(2) 0.038(2) 0.033(2) -0.005(2) -0.002(2) 0.001(2) C21 0.040(2) 0.049(3) 0.046(2) -0.008(2) -0.002(2) -0.003(2) C22 0.063(3) 0.052(3) 0.068(3) -0.023(2) 0.000(2) -0.008(2) C23 0.064(3) 0.066(3) 0.084(4) -0.004(3) 0.017(3) -0.020(2) C24 0.095(4) 0.047(2) 0.037(2) 0.009(2) 0.007(2) -0.011(2) C25 0.094(4) 0.056(3) 0.033(2) -0.013(2) 0.007(2) -0.011(3) C26 0.041(2) 0.039(2) 0.032(2) -0.001(2) 0.001(2) -0.005(2) C27 0.056(3) 0.047(2) 0.040(2) 0.003(2) 0.002(2) 0.006(2) C28 0.065(3) 0.051(3) 0.080(3) 0.016(3) 0.011(3) 0.014(2) C29 0.049(3) 0.065(3) 0.091(4) 0.024(3) -0.015(3) 0.002(2) C30 0.065(3) 0.061(3) 0.078(3) 0.002(3) -0.029(3) -0.014(2) C31 0.057(3) 0.044(2) 0.058(2) -0.005(2) -0.014(2) -0.002(2) Pd2 0.0430(2) 0.03535(14) 0.02737(12) 0.00089(12) 0.00263(11) -0.00369(13) Cl2 0.1170(11) 0.0367(5) 0.0484(6) 0.0066(4) 0.0103(7) -0.0086(6) P2 0.0425(5) 0.0310(5) 0.0288(4) 0.0008(4) 0.0021(4) -0.0044(4) S2 0.0552(7) 0.0857(9) 0.0586(7) 0.0083(6) 0.0159(6) -0.0032(6) N2 0.044(2) 0.050(2) 0.0291(15) 0.0017(13) -0.0002(13) -0.0005(14) N4 0.046(2) 0.058(2) 0.075(3) 0.005(2) 0.000(2) 0.003(2) C41 0.041(2) 0.039(2) 0.034(2) 0.000(2) 0.002(2) 0.004(2) C42 0.052(3) 0.042(2) 0.047(2) -0.003(2) -0.004(2) 0.010(2) C43 0.060(3) 0.056(3) 0.059(3) 0.006(2) -0.002(2) 0.018(2) C44 0.055(3) 0.042(2) 0.068(3) -0.005(2) 0.013(2) 0.008(2) C45 0.088(4) 0.046(3) 0.099(4) -0.001(3) 0.011(4) 0.011(3) C46 0.110(5) 0.044(3) 0.110(5) -0.019(3) 0.016(4) -0.005(3) C47 0.102(5) 0.066(3) 0.084(4) -0.032(3) 0.017(4) -0.027(3) C48 0.071(3) 0.053(3) 0.059(3) -0.012(2) 0.008(3) -0.007(2) C49 0.048(3) 0.044(2) 0.049(2) -0.008(2) 0.010(2) -0.002(2) C50 0.044(2) 0.041(2) 0.036(2) -0.005(2) 0.003(2) 0.001(2) C51 0.054(3) 0.050(2) 0.032(2) -0.002(2) -0.004(2) -0.011(2) C52 0.048(3) 0.070(3) 0.066(3) 0.007(2) -0.014(2) -0.006(2) C53 0.053(3) 0.068(3) 0.038(2) -0.003(2) 0.011(2) -0.012(2) C54 0.080(3) 0.069(3) 0.045(2) 0.013(2) -0.014(2) -0.002(3) C55 0.038(2) 0.033(2) 0.033(2) 0.0028(15) 0.004(2) -0.004(2) C56 0.041(2) 0.044(2) 0.030(2) -0.005(2) 0.002(2) -0.005(2) C57 0.049(2) 0.047(2) 0.027(2) 0.002(2) 0.003(2) -0.007(2) C58 0.049(2) 0.028(2) 0.035(2) 0.0053(14) 0.000(2) -0.003(2) C59 0.051(3) 0.038(2) 0.045(2) 0.000(2) 0.003(2) -0.013(2) C60 0.045(2) 0.043(2) 0.029(2) 0.005(2) -0.001(2) -0.005(2) C61 0.042(2) 0.051(3) 0.045(2) -0.001(2) -0.003(2) -0.005(2) C62 0.073(4) 0.067(3) 0.092(4) 0.031(3) -0.002(3) 0.009(3) C63 0.066(4) 0.077(4) 0.125(5) -0.004(4) 0.002(4) 0.016(3) C64 0.082(4) 0.061(3) 0.052(3) -0.017(2) 0.001(3) 0.002(2) C65 0.094(4) 0.064(3) 0.031(2) 0.010(2) 0.000(2) 0.001(3) C66 0.038(2) 0.040(2) 0.033(2) -0.003(2) 0.002(2) 0.000(2) C67 0.056(3) 0.038(2) 0.052(2) 0.005(2) -0.007(2) -0.005(2) C68 0.060(3) 0.052(3) 0.069(3) 0.004(2) -0.010(2) -0.020(2) C69 0.048(3) 0.073(3) 0.061(3) 0.002(2) -0.010(2) -0.012(2) C70 0.056(3) 0.060(3) 0.069(3) 0.008(2) -0.024(2) 0.004(2) C71 0.055(2) 0.041(2) 0.061(3) 0.008(2) -0.006(2) 0.000(2) O1 0.100(3) 0.068(3) 0.113(3) -0.012(3) 0.010(3) -0.001(2) C72 0.139(7) 0.134(7) 0.115(6) 0.026(5) -0.011(5) 0.030(6) C73 0.163(8) 0.059(4) 0.152(7) 0.032(5) 0.033(7) 0.016(4) C74 0.121(6) 0.095(5) 0.153(7) -0.049(5) 0.033(6) -0.015(5) C75 0.132(7) 0.165(8) 0.101(6) -0.048(5) 0.008(5) -0.034(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.014(3) . ? Pd1 N1 2.152(3) . ? Pd1 P1 2.2238(9) . ? Pd1 Cl1 2.4010(10) . ? P1 C26 1.827(4) . ? P1 C15 1.842(4) . ? P1 C18 1.845(4) . ? S1 C21 1.687(4) . ? N1 C13 1.487(5) . ? N1 C11 1.502(4) . ? N1 C14 1.503(5) . ? N3 C21 1.326(5) . ? N3 C23 1.467(5) . ? N3 C22 1.479(5) . ? C1 C10 1.381(5) . ? C1 C2 1.421(5) . ? C2 C3 1.363(5) . ? C3 C4 1.412(5) . ? C4 C5 1.420(5) . ? C4 C9 1.428(5) . ? C5 C6 1.348(6) . ? C6 C7 1.394(7) . ? C7 C8 1.370(6) . ? C8 C9 1.424(5) . ? C9 C10 1.440(5) . ? C10 C11 1.512(5) . ? C11 C12 1.520(6) . ? C15 C16 1.520(5) . ? C15 C20 1.580(5) . ? C16 C17 1.331(5) . ? C16 C24 1.502(5) . ? C17 C25 1.491(5) . ? C17 C18 1.525(5) . ? C18 C19 1.561(6) . ? C19 C20 1.537(5) . ? C20 C21 1.528(6) . ? C26 C31 1.389(5) . ? C26 C27 1.391(5) . ? C27 C28 1.393(6) . ? C28 C29 1.379(7) . ? C29 C30 1.371(7) . ? C30 C31 1.380(6) . ? Pd2 C41 2.008(4) . ? Pd2 N2 2.149(3) . ? Pd2 P2 2.2272(8) . ? Pd2 Cl2 2.3946(10) . ? P2 C66 1.810(4) . ? P2 C55 1.853(4) . ? P2 C58 1.853(3) . ? S2 C61 1.671(4) . ? N2 C54 1.481(5) . ? N2 C53 1.488(5) . ? N2 C51 1.515(5) . ? N4 C61 1.344(5) . ? N4 C63 1.461(6) . ? N4 C62 1.469(6) . ? C41 C50 1.397(5) . ? C41 C42 1.419(5) . ? C42 C43 1.363(6) . ? C43 C44 1.405(6) . ? C44 C49 1.423(6) . ? C44 C45 1.425(6) . ? C45 C46 1.350(8) . ? C46 C47 1.392(8) . ? C47 C48 1.372(6) . ? C48 C49 1.418(6) . ? C49 C50 1.423(5) . ? C50 C51 1.517(5) . ? C51 C52 1.519(6) . ? C55 C56 1.513(5) . ? C55 C60 1.567(5) . ? C56 C57 1.332(5) . ? C56 C64 1.500(5) . ? C57 C65 1.504(5) . ? C57 C58 1.519(5) . ? C58 C59 1.559(6) . ? C59 C60 1.552(5) . ? C60 C61 1.520(6) . ? C66 C67 1.386(5) . ? C66 C71 1.391(5) . ? C67 C68 1.385(6) . ? C68 C69 1.375(6) . ? C69 C70 1.368(6) . ? C70 C71 1.393(6) . ? O1 C73 1.385(8) . ? O1 C74 1.400(8) . ? C72 C73 1.486(9) . ? C74 C75 1.483(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N1 80.88(13) . . ? C1 Pd1 P1 92.49(10) . . ? N1 Pd1 P1 173.36(8) . . ? C1 Pd1 Cl1 176.07(11) . . ? N1 Pd1 Cl1 95.51(8) . . ? P1 Pd1 Cl1 91.13(3) . . ? C26 P1 C15 107.3(2) . . ? C26 P1 C18 112.0(2) . . ? C15 P1 C18 81.4(2) . . ? C26 P1 Pd1 111.39(12) . . ? C15 P1 Pd1 120.31(11) . . ? C18 P1 Pd1 120.91(12) . . ? C13 N1 C11 112.2(3) . . ? C13 N1 C14 106.5(3) . . ? C11 N1 C14 108.7(3) . . ? C13 N1 Pd1 116.5(2) . . ? C11 N1 Pd1 104.1(2) . . ? C14 N1 Pd1 108.6(2) . . ? C21 N3 C23 122.7(4) . . ? C21 N3 C22 124.8(4) . . ? C23 N3 C22 112.4(4) . . ? C10 C1 C2 118.3(3) . . ? C10 C1 Pd1 112.7(3) . . ? C2 C1 Pd1 129.0(3) . . ? C3 C2 C1 122.1(3) . . ? C2 C3 C4 121.0(3) . . ? C3 C4 C5 122.5(4) . . ? C3 C4 C9 118.6(3) . . ? C5 C4 C9 118.9(4) . . ? C6 C5 C4 121.4(4) . . ? C5 C6 C7 120.4(4) . . ? C8 C7 C6 120.5(4) . . ? C7 C8 C9 121.1(4) . . ? C8 C9 C4 117.5(4) . . ? C8 C9 C10 123.6(4) . . ? C4 C9 C10 118.9(3) . . ? C1 C10 C9 121.1(3) . . ? C1 C10 C11 117.7(3) . . ? C9 C10 C11 121.1(3) . . ? N1 C11 C10 107.3(3) . . ? N1 C11 C12 111.4(3) . . ? C10 C11 C12 110.3(3) . . ? C16 C15 C20 106.8(3) . . ? C16 C15 P1 101.1(2) . . ? C20 C15 P1 99.8(2) . . ? C17 C16 C24 128.2(3) . . ? C17 C16 C15 110.5(3) . . ? C24 C16 C15 121.3(3) . . ? C16 C17 C25 128.1(3) . . ? C16 C17 C18 110.8(3) . . ? C25 C17 C18 120.7(3) . . ? C17 C18 C19 107.6(3) . . ? C17 C18 P1 100.8(2) . . ? C19 C18 P1 98.5(2) . . ? C20 C19 C18 106.9(3) . . ? C21 C20 C19 116.9(3) . . ? C21 C20 C15 108.9(3) . . ? C19 C20 C15 105.1(3) . . ? N3 C21 C20 117.4(4) . . ? N3 C21 S1 121.0(3) . . ? C20 C21 S1 121.5(3) . . ? C31 C26 C27 119.6(4) . . ? C31 C26 P1 124.0(3) . . ? C27 C26 P1 116.4(3) . . ? C26 C27 C28 120.1(4) . . ? C29 C28 C27 119.7(5) . . ? C30 C29 C28 120.1(4) . . ? C29 C30 C31 121.0(4) . . ? C30 C31 C26 119.6(4) . . ? C41 Pd2 N2 81.01(13) . . ? C41 Pd2 P2 94.50(10) . . ? N2 Pd2 P2 171.51(9) . . ? C41 Pd2 Cl2 175.42(10) . . ? N2 Pd2 Cl2 95.35(9) . . ? P2 Pd2 Cl2 89.46(4) . . ? C66 P2 C55 106.4(2) . . ? C66 P2 C58 108.7(2) . . ? C55 P2 C58 80.7(2) . . ? C66 P2 Pd2 118.15(12) . . ? C55 P2 Pd2 114.88(12) . . ? C58 P2 Pd2 121.32(12) . . ? C54 N2 C53 107.6(3) . . ? C54 N2 C51 112.0(3) . . ? C53 N2 C51 108.7(3) . . ? C54 N2 Pd2 115.3(2) . . ? C53 N2 Pd2 108.8(2) . . ? C51 N2 Pd2 104.1(2) . . ? C61 N4 C63 120.2(4) . . ? C61 N4 C62 125.3(4) . . ? C63 N4 C62 114.4(4) . . ? C50 C41 C42 118.4(3) . . ? C50 C41 Pd2 113.6(3) . . ? C42 C41 Pd2 128.0(3) . . ? C43 C42 C41 121.1(4) . . ? C42 C43 C44 121.6(4) . . ? C43 C44 C49 118.7(4) . . ? C43 C44 C45 122.2(4) . . ? C49 C44 C45 119.1(4) . . ? C46 C45 C44 121.0(5) . . ? C45 C46 C47 120.7(5) . . ? C48 C47 C46 120.2(5) . . ? C47 C48 C49 121.4(5) . . ? C48 C49 C44 117.6(4) . . ? C48 C49 C50 123.5(4) . . ? C44 C49 C50 118.9(4) . . ? C41 C50 C49 121.1(3) . . ? C41 C50 C51 116.5(3) . . ? C49 C50 C51 122.4(3) . . ? N2 C51 C50 107.3(3) . . ? N2 C51 C52 112.5(4) . . ? C50 C51 C52 109.9(3) . . ? C56 C55 C60 109.0(3) . . ? C56 C55 P2 101.6(2) . . ? C60 C55 P2 98.8(2) . . ? C57 C56 C64 128.5(3) . . ? C57 C56 C55 110.1(3) . . ? C64 C56 C55 121.4(3) . . ? C56 C57 C65 129.2(3) . . ? C56 C57 C58 111.2(3) . . ? C65 C57 C58 119.3(3) . . ? C57 C58 C59 106.5(3) . . ? C57 C58 P2 100.7(2) . . ? C59 C58 P2 99.7(2) . . ? C60 C59 C58 106.7(3) . . ? C61 C60 C59 117.1(3) . . ? C61 C60 C55 110.2(3) . . ? C59 C60 C55 104.7(3) . . ? N4 C61 C60 116.5(4) . . ? N4 C61 S2 121.4(3) . . ? C60 C61 S2 122.1(3) . . ? C67 C66 C71 118.1(4) . . ? C67 C66 P2 118.8(3) . . ? C71 C66 P2 123.1(3) . . ? C68 C67 C66 121.0(4) . . ? C69 C68 C67 120.0(4) . . ? C70 C69 C68 120.3(4) . . ? C69 C70 C71 119.9(4) . . ? C66 C71 C70 120.7(4) . . ? C73 O1 C74 115.0(6) . . ? O1 C73 C72 111.7(6) . . ? O1 C74 C75 110.3(6) . . ? _refine_diff_density_max 0.359 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.059 data_089 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H16 Cl2 N P Pd S' _chemical_formula_weight 450.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 10.1583(2) _cell_length_b 12.3121(2) _cell_length_c 14.4431(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.122(1) _cell_angle_gamma 90.00 _cell_volume 1788.28(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6753 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'rectangular shape, cut' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 1.534 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.7236 _exptl_absorpt_correction_T_max 0.8918 _exptl_absorpt_process_details 'sadabs (Sheldrick, 1996)' _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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11162 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 29.34 _reflns_number_total 4415 _reflns_number_gt 3531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, 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^)+(0.0319P)^2^+0.0295P] 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 SHELXL _refine_ls_extinction_coef 0.0018(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4415 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.385198(17) 0.324938(14) 0.494347(13) 0.03210(7) Uani 1 1 d . . . Cl1 Cl 0.18529(6) 0.27196(6) 0.40677(5) 0.05271(18) Uani 1 1 d . . . Cl2 Cl 0.28757(7) 0.38781(6) 0.62452(5) 0.05584(19) Uani 1 1 d . . . S1 S 0.59891(7) 0.36426(6) 0.55882(5) 0.04948(18) Uani 1 1 d . . . C1 C 0.6596(2) 0.32460(18) 0.45996(17) 0.0349(5) Uani 1 1 d . . . N1 N 0.7815(2) 0.33482(17) 0.44382(16) 0.0423(5) Uani 1 1 d . . . C2 C 0.8798(3) 0.3909(3) 0.5113(2) 0.0614(8) Uani 1 1 d . . . H2A H 0.9674 0.3773 0.4963 0.092 Uiso 1 1 calc R . . H2B H 0.8738 0.3646 0.5732 0.092 Uiso 1 1 calc R . . H2C H 0.8624 0.4676 0.5087 0.092 Uiso 1 1 calc R . . C3 C 0.8240(3) 0.2994(3) 0.3554(2) 0.0719(10) Uani 1 1 d . . . H3A H 0.9121 0.2697 0.3676 0.108 Uiso 1 1 calc R . . H3B H 0.8237 0.3605 0.3140 0.108 Uiso 1 1 calc R . . H3C H 0.7638 0.2450 0.3268 0.108 Uiso 1 1 calc R . . P1 P 0.50886(6) 0.27235(5) 0.38849(4) 0.02987(13) Uani 1 1 d . . . C4 C 0.4843(2) 0.33874(18) 0.27591(17) 0.0331(5) Uani 1 1 d . . . C5 C 0.5393(3) 0.3012(2) 0.19867(18) 0.0448(6) Uani 1 1 d . . . H5 H 0.5889 0.2374 0.2027 0.054 Uiso 1 1 calc R . . C6 C 0.5196(3) 0.3593(3) 0.1161(2) 0.0578(8) Uani 1 1 d . . . H6 H 0.5552 0.3345 0.0641 0.069 Uiso 1 1 calc R . . C7 C 0.4471(3) 0.4543(3) 0.1110(2) 0.0709(10) Uani 1 1 d . . . H7 H 0.4342 0.4932 0.0553 0.085 Uiso 1 1 calc R . . C8 C 0.3939(4) 0.4921(3) 0.1868(2) 0.0728(10) Uani 1 1 d . . . H8 H 0.3463 0.5569 0.1828 0.087 Uiso 1 1 calc R . . C9 C 0.4110(3) 0.4338(2) 0.2691(2) 0.0486(7) Uani 1 1 d . . . H9 H 0.3732 0.4585 0.3202 0.058 Uiso 1 1 calc R . . C10 C 0.5320(2) 0.12915(19) 0.37217(17) 0.0350(5) Uani 1 1 d . . . C11 C 0.6245(3) 0.0701(2) 0.4323(2) 0.0479(6) Uani 1 1 d . . . H11 H 0.6789 0.1052 0.4803 0.058 Uiso 1 1 calc R . . C12 C 0.6358(3) -0.0409(2) 0.4205(2) 0.0600(8) Uani 1 1 d . . . H12 H 0.6978 -0.0803 0.4607 0.072 Uiso 1 1 calc R . . C13 C 0.5556(3) -0.0929(2) 0.3498(2) 0.0605(8) Uani 1 1 d . . . H13 H 0.5649 -0.1672 0.3414 0.073 Uiso 1 1 calc R . . C14 C 0.4622(3) -0.0364(2) 0.2917(2) 0.0604(8) Uani 1 1 d . . . H14 H 0.4070 -0.0726 0.2447 0.073 Uiso 1 1 calc R . . C15 C 0.4496(3) 0.0754(2) 0.3026(2) 0.0492(7) Uani 1 1 d . . . H15 H 0.3857 0.1138 0.2632 0.059 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 0.03068(10) 0.03169(11) 0.03577(11) 0.00126(8) 0.01109(7) 0.00180(7) Cl1 0.0310(3) 0.0645(5) 0.0616(4) 0.0027(4) 0.0028(3) -0.0018(3) Cl2 0.0647(5) 0.0563(4) 0.0535(4) -0.0026(3) 0.0326(4) 0.0049(3) S1 0.0415(4) 0.0627(4) 0.0444(4) -0.0177(3) 0.0065(3) -0.0064(3) C1 0.0329(12) 0.0321(12) 0.0394(13) 0.0026(10) 0.0046(10) 0.0006(10) N1 0.0294(10) 0.0474(12) 0.0500(13) 0.0035(10) 0.0057(9) -0.0039(9) C2 0.0336(14) 0.064(2) 0.082(2) 0.0034(17) -0.0067(14) -0.0134(13) C3 0.0348(16) 0.122(3) 0.062(2) 0.000(2) 0.0186(14) -0.0025(17) P1 0.0263(3) 0.0312(3) 0.0327(3) -0.0008(2) 0.0063(2) 0.0012(2) C4 0.0332(12) 0.0336(13) 0.0333(12) 0.0004(10) 0.0067(9) -0.0006(9) C5 0.0456(15) 0.0462(15) 0.0445(15) -0.0038(12) 0.0133(12) 0.0033(11) C6 0.0598(19) 0.075(2) 0.0419(16) 0.0058(15) 0.0198(14) -0.0011(16) C7 0.069(2) 0.092(3) 0.056(2) 0.0355(18) 0.0224(17) 0.0084(19) C8 0.084(2) 0.067(2) 0.075(2) 0.0337(18) 0.0331(19) 0.0313(18) C9 0.0570(17) 0.0422(15) 0.0500(16) 0.0063(12) 0.0189(13) 0.0137(12) C10 0.0357(12) 0.0310(12) 0.0399(14) -0.0010(11) 0.0114(10) 0.0031(10) C11 0.0484(16) 0.0393(14) 0.0553(17) 0.0037(13) 0.0049(13) 0.0053(12) C12 0.0621(19) 0.0459(17) 0.075(2) 0.0144(16) 0.0203(17) 0.0186(15) C13 0.085(2) 0.0334(15) 0.070(2) 0.0022(15) 0.0357(19) 0.0080(15) C14 0.081(2) 0.0404(16) 0.061(2) -0.0127(15) 0.0148(17) -0.0097(15) C15 0.0534(17) 0.0419(15) 0.0512(17) -0.0035(13) 0.0037(13) 0.0008(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 P1 2.2086(6) . ? Pd1 S1 2.2899(7) . ? Pd1 Cl1 2.3288(7) . ? Pd1 Cl2 2.3758(7) . ? S1 C1 1.705(3) . ? C1 N1 1.298(3) . ? C1 P1 1.838(2) . ? N1 C2 1.466(3) . ? N1 C3 1.471(4) . ? P1 C10 1.799(2) . ? P1 C4 1.805(2) . ? C4 C9 1.384(3) . ? C4 C5 1.395(3) . ? C5 C6 1.381(4) . ? C6 C7 1.378(4) . ? C7 C8 1.369(5) . ? C8 C9 1.379(4) . ? C10 C15 1.383(4) . ? C10 C11 1.391(4) . ? C11 C12 1.383(4) . ? C12 C13 1.372(5) . ? C13 C14 1.365(5) . ? C14 C15 1.393(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 S1 75.18(2) . . ? P1 Pd1 Cl1 94.56(2) . . ? S1 Pd1 Cl1 169.73(3) . . ? P1 Pd1 Cl2 170.14(3) . . ? S1 Pd1 Cl2 95.00(3) . . ? Cl1 Pd1 Cl2 95.25(3) . . ? C1 S1 Pd1 91.89(9) . . ? N1 C1 S1 126.1(2) . . ? N1 C1 P1 132.3(2) . . ? S1 C1 P1 101.52(12) . . ? C1 N1 C2 120.2(2) . . ? C1 N1 C3 122.1(2) . . ? C2 N1 C3 117.5(2) . . ? C10 P1 C4 109.26(11) . . ? C10 P1 C1 107.62(11) . . ? C4 P1 C1 110.22(11) . . ? C10 P1 Pd1 118.42(8) . . ? C4 P1 Pd1 118.10(8) . . ? C1 P1 Pd1 91.07(8) . . ? C9 C4 C5 119.8(2) . . ? C9 C4 P1 116.83(18) . . ? C5 C4 P1 123.35(19) . . ? C6 C5 C4 119.5(3) . . ? C7 C6 C5 119.8(3) . . ? C8 C7 C6 121.0(3) . . ? C7 C8 C9 119.7(3) . . ? C8 C9 C4 120.2(3) . . ? C15 C10 C11 119.3(2) . . ? C15 C10 P1 119.2(2) . . ? C11 C10 P1 121.3(2) . . ? C12 C11 C10 120.0(3) . . ? C13 C12 C11 120.1(3) . . ? C14 C13 C12 120.5(3) . . ? C13 C14 C15 120.0(3) . . ? C10 C15 C14 120.0(3) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 29.34 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 0.461 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.071