# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #============================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Original Palladium Pincer Complexes Deriving from Bis(thiophosphinoyle)indene Proligands: Csp3-H versus Csp2-H Activation ; _publ_contact_author_email dbouriss@chimie.ups-tlse.fr _publ_contact_author_name 'Bourissou, Didier' loop_ _publ_author_name 'Noel Nebra' 'Jerome Lisena' 'Nathalie Saffon' 'Laurent Maron' 'Blanca Martin-Vaca' 'Didier Bourissou' data_2 _database_code_depnum_ccdc_archive 'CCDC 800695' #TrackingRef '- RX_Bourissou-DT-pincer.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H27 Cl3 P2 Pd S2' _chemical_formula_weight 774.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 10.4520(2) _cell_length_b 14.1161(3) _cell_length_c 21.7006(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.020(2) _cell_angle_gamma 90.00 _cell_volume 3199.75(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3283 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 24.27 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 1.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8541 _exptl_absorpt_correction_T_max 0.9182 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34209 _diffrn_reflns_av_R_equivalents 0.1088 _diffrn_reflns_av_sigmaI/netI 0.0837 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6487 _reflns_number_gt 4142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Restraints have been used in order to refine disorders. The similar-ADP (Anisotropic Displacement Parameter) restraint and the rigid-bond restraint have been used in disorders to make the ADP values of the disordered atoms more reasonable. ; _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^)+(0.0284P)^2^+0.3048P] 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 6487 _refine_ls_number_parameters 410 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.43606(3) 0.19396(2) 0.107922(14) 0.02256(10) Uani 1 1 d . . . Cl1 Cl 0.64373(9) 0.18814(9) 0.15650(5) 0.0354(3) Uani 1 1 d . . . P1 P 0.17690(9) 0.09498(8) 0.15904(5) 0.0209(2) Uani 1 1 d . . . P2 P 0.30802(10) 0.36535(8) 0.02584(5) 0.0247(3) Uani 1 1 d . . . S1 S 0.36619(9) 0.08213(8) 0.17859(5) 0.0266(3) Uani 1 1 d . . . S2 S 0.48815(9) 0.31584(8) 0.03969(5) 0.0312(3) Uani 1 1 d . . . C1 C 0.2640(3) 0.1941(3) 0.06867(17) 0.0223(9) Uani 1 1 d . . . C2 C 0.1663(4) 0.1165(3) 0.07590(19) 0.0245(10) Uani 1 1 d . . . H2 H 0.193(4) 0.062(3) 0.0580(17) 0.029 Uiso 1 1 d . . . C3 C 0.2063(3) 0.2679(3) 0.03921(18) 0.0241(9) Uani 1 1 d . . . C4 C 0.0694(4) 0.2477(3) 0.02526(17) 0.0224(9) Uani 1 1 d . . . C5 C -0.0289(4) 0.3005(3) -0.00233(18) 0.0295(10) Uani 1 1 d . . . H5 H -0.0129 0.3618 -0.0184 0.035 Uiso 1 1 calc R . . C6 C -0.1508(4) 0.2618(3) -0.00596(18) 0.0339(11) Uani 1 1 d . . . H6 H -0.2187 0.2972 -0.0249 0.041 Uiso 1 1 calc R . . C7 C -0.1757(4) 0.1729(3) 0.01734(19) 0.0354(12) Uani 1 1 d . . . H7 H -0.2607 0.1489 0.0151 0.042 Uiso 1 1 calc R . . C8 C -0.0777(4) 0.1179(3) 0.04407(18) 0.0292(10) Uani 1 1 d . . . H8 H -0.0942 0.0559 0.0588 0.035 Uiso 1 1 calc R . . C9 C 0.0445(3) 0.1564(3) 0.04858(17) 0.0220(9) Uani 1 1 d . . . C10 C 0.1060(3) 0.1949(3) 0.19624(16) 0.0208(8) Uani 1 1 d . . . C11 C 0.1850(4) 0.2663(3) 0.22053(18) 0.0276(10) Uani 1 1 d . . . H11 H 0.2753 0.2608 0.2183 0.033 Uiso 1 1 calc R . . C12 C 0.1325(4) 0.3446(3) 0.2477(2) 0.0350(11) Uani 1 1 d . . . H12 H 0.1869 0.3926 0.2646 0.042 Uiso 1 1 calc R . . C13 C 0.0011(4) 0.3538(3) 0.25044(19) 0.0337(11) Uani 1 1 d . . . H13 H -0.0347 0.4076 0.2697 0.040 Uiso 1 1 calc R . . C14 C -0.0783(4) 0.2844(3) 0.22508(18) 0.0293(10) Uani 1 1 d . . . H14 H -0.1686 0.2912 0.2262 0.035 Uiso 1 1 calc R . . C15 C -0.0262(4) 0.2052(3) 0.19811(18) 0.0262(9) Uani 1 1 d . . . H15 H -0.0808 0.1577 0.1808 0.031 Uiso 1 1 calc R . . C16 C 0.0912(3) -0.0104(3) 0.17917(18) 0.0200(9) Uani 1 1 d . . . C17 C 0.0482(4) -0.0218(3) 0.23900(18) 0.0264(10) Uani 1 1 d . . . H17 H 0.0549 0.0293 0.2675 0.032 Uiso 1 1 calc R . . C18 C -0.0041(4) -0.1073(3) 0.2569(2) 0.0317(11) Uani 1 1 d . . . H18 H -0.0319 -0.1151 0.2978 0.038 Uiso 1 1 calc R . . C19 C -0.0157(4) -0.1811(3) 0.2153(2) 0.0313(10) Uani 1 1 d . . . H19 H -0.0525 -0.2395 0.2274 0.038 Uiso 1 1 calc R . . C20 C 0.0260(4) -0.1701(3) 0.1566(2) 0.0355(11) Uani 1 1 d . . . H20 H 0.0175 -0.2210 0.1281 0.043 Uiso 1 1 calc R . . C21 C 0.0801(4) -0.0859(3) 0.13815(19) 0.0288(10) Uani 1 1 d . . . H21 H 0.1098 -0.0796 0.0975 0.035 Uiso 1 1 calc R . . C22 C 0.2734(4) 0.4618(3) 0.07741(18) 0.0264(10) Uani 1 1 d . . . C23 C 0.3666(4) 0.5298(3) 0.08945(19) 0.0308(10) Uani 1 1 d . . . H23 H 0.4485 0.5238 0.0722 0.037 Uiso 1 1 calc R . . C24 C 0.3401(5) 0.6068(3) 0.1267(2) 0.0373(11) Uani 1 1 d . . . H24 H 0.4033 0.6540 0.1347 0.045 Uiso 1 1 calc R . . C25 C 0.2213(5) 0.6145(3) 0.1520(2) 0.0403(12) Uani 1 1 d . . . H25 H 0.2029 0.6672 0.1774 0.048 Uiso 1 1 calc R . . C26 C 0.1292(5) 0.5464(3) 0.1408(2) 0.0421(12) Uani 1 1 d . . . H26 H 0.0481 0.5521 0.1589 0.050 Uiso 1 1 calc R . . C27 C 0.1536(4) 0.4695(3) 0.10329(19) 0.0349(11) Uani 1 1 d . . . H27 H 0.0898 0.4227 0.0953 0.042 Uiso 1 1 calc R . . C28 C 0.2802(4) 0.4106(3) -0.05141(18) 0.0251(9) Uani 1 1 d . . . C29 C 0.2540(4) 0.5041(3) -0.0632(2) 0.0337(11) Uani 1 1 d . . . H29 H 0.2481 0.5473 -0.0298 0.040 Uiso 1 1 calc R . . C30 C 0.2359(4) 0.5362(4) -0.1235(2) 0.0450(13) Uani 1 1 d . . . H30 H 0.2200 0.6014 -0.1313 0.054 Uiso 1 1 calc R . . C31 C 0.2413(4) 0.4733(4) -0.1714(2) 0.0427(12) Uani 1 1 d . . . H31 H 0.2276 0.4950 -0.2126 0.051 Uiso 1 1 calc R . . C32 C 0.2661(5) 0.3792(4) -0.1605(2) 0.0474(13) Uani 1 1 d . . . H32 H 0.2696 0.3359 -0.1939 0.057 Uiso 1 1 calc R . . C33 C 0.2862(4) 0.3472(3) -0.1001(2) 0.0404(12) Uani 1 1 d . . . H33 H 0.3040 0.2822 -0.0923 0.049 Uiso 1 1 calc R . . C34 C 0.613(4) 0.972(3) 0.1088(18) 0.073(5) Uani 0.162(4) 1 d PDU A 1 H34A H 0.6263 1.0396 0.0997 0.088 Uiso 0.162(4) 1 calc PR A 1 H34B H 0.5401 0.9667 0.1368 0.088 Uiso 0.162(4) 1 calc PR A 1 Cl2 Cl 0.5764(15) 0.9109(11) 0.0408(6) 0.105(5) Uani 0.162(4) 1 d PDU A 1 Cl3 Cl 0.7471(14) 0.9256(14) 0.1438(7) 0.071(4) Uani 0.162(4) 1 d PDU A 1 C34' C 0.5980(8) 0.9582(6) 0.0734(5) 0.075(2) Uani 0.838(4) 1 d PDU A 2 H34C H 0.6145 0.9702 0.0295 0.091 Uiso 0.838(4) 1 calc PR A 2 H34D H 0.5760 1.0195 0.0926 0.091 Uiso 0.838(4) 1 calc PR A 2 Cl2' Cl 0.46682(19) 0.88075(14) 0.07815(10) 0.0761(8) Uani 0.838(4) 1 d PDU A 2 Cl3' Cl 0.7343(3) 0.9147(2) 0.10905(19) 0.0883(11) Uani 0.838(4) 1 d PDU A 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 0.01898(14) 0.02045(18) 0.02842(18) 0.00101(16) 0.00324(11) 0.00019(15) Cl1 0.0202(5) 0.0438(7) 0.0422(7) -0.0074(6) 0.0000(4) -0.0006(5) P1 0.0203(5) 0.0183(6) 0.0239(6) 0.0031(5) -0.0002(4) -0.0014(4) P2 0.0277(5) 0.0175(6) 0.0292(6) 0.0040(5) 0.0068(5) 0.0000(5) S1 0.0209(5) 0.0277(6) 0.0310(6) 0.0085(5) -0.0001(4) 0.0020(5) S2 0.0244(5) 0.0265(6) 0.0434(7) 0.0070(6) 0.0097(4) -0.0015(5) C1 0.0247(19) 0.017(2) 0.025(2) 0.000(2) 0.0031(16) 0.0005(19) C2 0.029(2) 0.020(2) 0.025(2) 0.0012(19) 0.0009(17) 0.0004(19) C3 0.025(2) 0.021(2) 0.026(2) 0.0051(19) 0.0038(17) 0.0030(18) C4 0.025(2) 0.024(2) 0.018(2) 0.0009(18) 0.0031(16) 0.0002(18) C5 0.033(2) 0.028(3) 0.028(2) 0.005(2) 0.0009(18) 0.009(2) C6 0.032(2) 0.046(3) 0.024(2) -0.002(2) -0.0021(19) 0.012(2) C7 0.026(2) 0.054(4) 0.026(2) -0.005(2) 0.0002(18) -0.008(2) C8 0.029(2) 0.033(3) 0.026(2) -0.001(2) -0.0010(18) -0.004(2) C9 0.023(2) 0.026(2) 0.018(2) 0.0008(18) 0.0007(16) -0.0015(18) C10 0.0226(18) 0.017(2) 0.022(2) 0.0013(19) -0.0028(15) -0.0007(18) C11 0.024(2) 0.027(2) 0.031(3) -0.002(2) 0.0001(17) -0.0026(19) C12 0.041(3) 0.023(3) 0.041(3) -0.010(2) -0.005(2) -0.008(2) C13 0.037(2) 0.029(3) 0.035(3) -0.009(2) -0.001(2) 0.008(2) C14 0.024(2) 0.028(3) 0.036(3) 0.000(2) 0.0000(18) 0.0058(19) C15 0.026(2) 0.022(2) 0.030(2) -0.001(2) -0.0033(17) -0.0043(19) C16 0.0217(19) 0.012(2) 0.026(2) 0.0056(18) -0.0042(16) 0.0014(16) C17 0.033(2) 0.026(3) 0.021(2) -0.0019(19) 0.0008(17) -0.0037(19) C18 0.032(2) 0.031(3) 0.032(3) 0.009(2) 0.0059(19) 0.000(2) C19 0.033(2) 0.019(2) 0.042(3) 0.004(2) -0.0001(19) -0.006(2) C20 0.045(3) 0.022(3) 0.040(3) -0.006(2) -0.001(2) -0.010(2) C21 0.036(2) 0.026(3) 0.025(2) 0.000(2) 0.0045(18) -0.001(2) C22 0.029(2) 0.026(3) 0.024(2) 0.0076(19) 0.0025(17) 0.0070(19) C23 0.034(2) 0.030(3) 0.029(2) 0.006(2) 0.0012(19) 0.005(2) C24 0.053(3) 0.028(3) 0.031(3) 0.000(2) -0.013(2) -0.001(2) C25 0.060(3) 0.036(3) 0.025(3) -0.005(2) -0.010(2) 0.017(3) C26 0.043(3) 0.046(3) 0.038(3) -0.006(2) 0.008(2) 0.014(2) C27 0.039(3) 0.032(3) 0.034(3) 0.003(2) 0.005(2) 0.003(2) C28 0.029(2) 0.019(2) 0.027(2) -0.001(2) 0.0049(17) -0.0018(19) C29 0.043(3) 0.028(3) 0.030(3) 0.001(2) 0.003(2) 0.004(2) C30 0.059(3) 0.031(3) 0.045(3) 0.008(3) 0.000(2) 0.002(2) C31 0.041(3) 0.058(4) 0.029(3) 0.011(3) 0.003(2) -0.002(3) C32 0.058(3) 0.054(4) 0.030(3) -0.014(3) 0.007(2) -0.001(3) C33 0.056(3) 0.023(3) 0.043(3) 0.001(2) 0.008(2) 0.004(2) C34 0.063(8) 0.043(9) 0.113(11) -0.006(9) 0.000(9) 0.007(8) Cl2 0.119(9) 0.095(9) 0.099(9) -0.019(7) -0.029(7) 0.041(8) Cl3 0.036(5) 0.073(8) 0.103(10) -0.006(8) 0.007(6) 0.004(5) C34' 0.073(5) 0.049(5) 0.105(8) -0.002(5) 0.010(6) 0.012(4) Cl2' 0.0658(13) 0.0716(15) 0.0890(16) -0.0346(11) -0.0235(11) 0.0029(10) Cl3' 0.0577(13) 0.0393(14) 0.167(4) 0.008(2) -0.006(2) -0.0045(10) _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 1.962(4) . ? Pd1 S1 2.3358(11) . ? Pd1 S2 2.3465(11) . ? Pd1 Cl1 2.3807(10) . ? P1 C16 1.798(4) . ? P1 C10 1.798(4) . ? P1 C2 1.829(4) . ? P1 S1 2.0169(13) . ? P2 C3 1.769(4) . ? P2 C22 1.807(4) . ? P2 C28 1.808(4) . ? P2 S2 2.0208(14) . ? C1 C3 1.353(5) . ? C1 C2 1.510(5) . ? C2 C9 1.495(5) . ? C3 C4 1.480(5) . ? C4 C5 1.388(5) . ? C4 C9 1.412(5) . ? C5 C6 1.386(5) . ? C6 C7 1.381(6) . ? C7 C8 1.395(6) . ? C8 C9 1.388(5) . ? C10 C15 1.391(5) . ? C10 C11 1.394(5) . ? C11 C12 1.375(5) . ? C12 C13 1.384(6) . ? C13 C14 1.385(6) . ? C14 C15 1.382(5) . ? C16 C21 1.391(5) . ? C16 C17 1.398(5) . ? C17 C18 1.387(6) . ? C18 C19 1.381(6) . ? C19 C20 1.370(6) . ? C20 C21 1.381(6) . ? C22 C23 1.386(6) . ? C22 C27 1.394(5) . ? C23 C24 1.389(6) . ? C24 C25 1.380(6) . ? C25 C26 1.376(6) . ? C26 C27 1.387(6) . ? C28 C29 1.369(6) . ? C28 C33 1.387(6) . ? C29 C30 1.392(6) . ? C30 C31 1.371(6) . ? C31 C32 1.373(7) . ? C32 C33 1.395(6) . ? C34 Cl3 1.703(19) . ? C34 Cl2 1.74(2) . ? C34' Cl3' 1.711(8) . ? C34' Cl2' 1.759(9) . ? 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 S1 89.02(12) . . ? C1 Pd1 S2 87.40(12) . . ? S1 Pd1 S2 174.10(4) . . ? C1 Pd1 Cl1 178.01(13) . . ? S1 Pd1 Cl1 89.27(4) . . ? S2 Pd1 Cl1 94.39(4) . . ? C16 P1 C10 108.85(17) . . ? C16 P1 C2 111.32(18) . . ? C10 P1 C2 107.51(18) . . ? C16 P1 S1 111.59(12) . . ? C10 P1 S1 113.14(12) . . ? C2 P1 S1 104.32(13) . . ? C3 P2 C22 110.48(19) . . ? C3 P2 C28 110.42(18) . . ? C22 P2 C28 106.18(19) . . ? C3 P2 S2 105.60(14) . . ? C22 P2 S2 111.99(14) . . ? C28 P2 S2 112.25(14) . . ? P1 S1 Pd1 97.37(5) . . ? P2 S2 Pd1 96.41(5) . . ? C3 C1 C2 108.4(3) . . ? C3 C1 Pd1 126.4(3) . . ? C2 C1 Pd1 124.6(3) . . ? C9 C2 C1 104.8(3) . . ? C9 C2 P1 118.3(3) . . ? C1 C2 P1 101.8(3) . . ? C1 C3 C4 111.1(3) . . ? C1 C3 P2 114.5(3) . . ? C4 C3 P2 134.3(3) . . ? C5 C4 C9 120.1(4) . . ? C5 C4 C3 132.9(4) . . ? C9 C4 C3 107.0(3) . . ? C6 C5 C4 118.5(4) . . ? C7 C6 C5 121.5(4) . . ? C6 C7 C8 120.8(4) . . ? C9 C8 C7 118.2(4) . . ? C8 C9 C4 120.8(4) . . ? C8 C9 C2 130.5(4) . . ? C4 C9 C2 108.7(3) . . ? C15 C10 C11 119.3(4) . . ? C15 C10 P1 121.4(3) . . ? C11 C10 P1 119.2(3) . . ? C12 C11 C10 120.2(4) . . ? C11 C12 C13 120.4(4) . . ? C12 C13 C14 119.9(4) . . ? C15 C14 C13 120.0(4) . . ? C14 C15 C10 120.2(4) . . ? C21 C16 C17 119.0(4) . . ? C21 C16 P1 120.6(3) . . ? C17 C16 P1 120.0(3) . . ? C18 C17 C16 120.2(4) . . ? C19 C18 C17 120.0(4) . . ? C20 C19 C18 119.9(4) . . ? C19 C20 C21 120.9(4) . . ? C20 C21 C16 120.0(4) . . ? C23 C22 C27 120.4(4) . . ? C23 C22 P2 118.9(3) . . ? C27 C22 P2 120.7(3) . . ? C22 C23 C24 119.9(4) . . ? C25 C24 C23 119.6(4) . . ? C26 C25 C24 120.6(4) . . ? C25 C26 C27 120.6(4) . . ? C26 C27 C22 118.9(4) . . ? C29 C28 C33 119.6(4) . . ? C29 C28 P2 122.5(3) . . ? C33 C28 P2 117.9(3) . . ? C28 C29 C30 120.6(4) . . ? C31 C30 C29 119.7(5) . . ? C30 C31 C32 120.5(4) . . ? C31 C32 C33 119.8(4) . . ? C28 C33 C32 119.8(4) . . ? Cl3 C34 Cl2 110.0(16) . . ? Cl3' C34' Cl2' 112.9(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.479 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.100 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 800696' #TrackingRef '- RX_Bourissou-DT-pincer.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H52 Cl N O P2 Pd S2' _chemical_formula_weight 890.79 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 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 11.5761(5) _cell_length_b 24.9932(10) _cell_length_c 14.8809(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.803(3) _cell_angle_gamma 90.00 _cell_volume 4290.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2437 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 22.00 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5405 _exptl_absorpt_correction_T_max 0.9793 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41879 _diffrn_reflns_av_R_equivalents 0.1867 _diffrn_reflns_av_sigmaI/netI 0.1379 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 5.15 _diffrn_reflns_theta_max 24.71 _reflns_number_total 7258 _reflns_number_gt 3841 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Restraints have been used in order to refine disorders. The similar-ADP (Anisotropic Displacement Parameter) restraint and the rigid-bond restraint have been used in disorders to make the ADP values of the disordered atoms more reasonable. ; _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^)+(0.0433P)^2^+10.5272P] 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 7258 _refine_ls_number_parameters 532 _refine_ls_number_restraints 147 _refine_ls_R_factor_all 0.1448 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1372 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.980 _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 0.28406(5) 0.22789(2) 0.29927(3) 0.02453(16) Uani 1 1 d . . . Cl1 Cl 0.47395(16) 0.26826(8) 0.28849(11) 0.0346(4) Uani 1 1 d . . . P1 P 0.22086(18) 0.09687(7) 0.28296(12) 0.0282(5) Uani 1 1 d . . . P2 P 0.03115(17) 0.29201(7) 0.30376(11) 0.0259(5) Uani 1 1 d . . . S1 S 0.36312(17) 0.14322(7) 0.27937(12) 0.0324(5) Uani 1 1 d . . . S2 S 0.20067(17) 0.31098(7) 0.32774(12) 0.0317(5) Uani 1 1 d . . . C1 C 0.1300(6) 0.1953(3) 0.3002(4) 0.0224(16) Uani 1 1 d . . . C2 C 0.1054(6) 0.1391(2) 0.2922(4) 0.0212(15) Uani 1 1 d . . . C3 C 0.0232(6) 0.2224(3) 0.2999(4) 0.0244(16) Uani 1 1 d . . . C4 C -0.0696(6) 0.1843(3) 0.2917(4) 0.0238(16) Uani 1 1 d . . . C5 C -0.1911(6) 0.1880(3) 0.2888(4) 0.0346(19) Uani 1 1 d . . . H5 H -0.2272 0.2218 0.2943 0.042 Uiso 1 1 calc R . . C6 C -0.2583(7) 0.1418(3) 0.2777(5) 0.039(2) Uani 1 1 d . . . H6 H -0.3403 0.1447 0.2746 0.047 Uiso 1 1 calc R . . C7 C -0.2082(7) 0.0920(3) 0.2712(4) 0.0358(19) Uani 1 1 d . . . H7 H -0.2561 0.0612 0.2636 0.043 Uiso 1 1 calc R . . C8 C -0.0887(7) 0.0865(3) 0.2757(4) 0.0305(18) Uani 1 1 d . . . H8 H -0.0549 0.0520 0.2717 0.037 Uiso 1 1 calc R . . C9 C -0.0180(6) 0.1318(3) 0.2862(4) 0.0261(17) Uani 1 1 d . . . C10 C 0.1990(6) 0.0565(3) 0.1817(4) 0.0297(18) Uani 1 1 d . . . C11 C 0.2132(8) 0.0802(3) 0.0987(5) 0.050(2) Uani 1 1 d . . . H11 H 0.2390 0.1162 0.0966 0.060 Uiso 1 1 calc R . . C12 C 0.1899(8) 0.0518(4) 0.0185(5) 0.056(3) Uani 1 1 d . . . H12 H 0.1993 0.0684 -0.0378 0.067 Uiso 1 1 calc R . . C13 C 0.1536(7) -0.0003(3) 0.0216(6) 0.049(2) Uani 1 1 d . . . H13 H 0.1387 -0.0199 -0.0328 0.059 Uiso 1 1 calc R . . C14 C 0.1386(8) -0.0240(3) 0.1022(6) 0.050(2) Uani 1 1 d . . . H14 H 0.1123 -0.0600 0.1033 0.060 Uiso 1 1 calc R . . C15 C 0.1612(7) 0.0036(3) 0.1823(5) 0.041(2) Uani 1 1 d . . . H15 H 0.1508 -0.0136 0.2380 0.050 Uiso 1 1 calc R . . C16 C 0.2404(7) 0.0503(3) 0.3757(4) 0.0306(18) Uani 1 1 d . . . C17 C 0.1644(7) 0.0506(3) 0.4435(5) 0.039(2) Uani 1 1 d . . . H17 H 0.0987 0.0735 0.4391 0.047 Uiso 1 1 calc R . . C18 C 0.1855(9) 0.0168(3) 0.5181(5) 0.048(2) Uani 1 1 d . . . H18 H 0.1336 0.0164 0.5643 0.057 Uiso 1 1 calc R . . C19 C 0.2818(9) -0.0159(3) 0.5246(6) 0.050(2) Uani 1 1 d . . . H19 H 0.2967 -0.0381 0.5761 0.060 Uiso 1 1 calc R . . C20 C 0.3565(8) -0.0168(3) 0.4574(6) 0.057(3) Uani 1 1 d . . . H20 H 0.4217 -0.0401 0.4618 0.068 Uiso 1 1 calc R . . C21 C 0.3357(7) 0.0167(3) 0.3826(6) 0.046(2) Uani 1 1 d . . . H21 H 0.3873 0.0163 0.3362 0.055 Uiso 1 1 calc R . . C22 C -0.0233(6) 0.3221(3) 0.1982(4) 0.0261(16) Uani 1 1 d . . . C23 C -0.0441(7) 0.3766(3) 0.1915(5) 0.038(2) Uani 1 1 d . . . H23 H -0.0378 0.3982 0.2441 0.046 Uiso 1 1 calc R . . C24 C -0.0744(7) 0.3996(3) 0.1077(5) 0.046(2) Uani 1 1 d . . . H24 H -0.0887 0.4370 0.1034 0.055 Uiso 1 1 calc R . . C25 C -0.0837(7) 0.3687(3) 0.0310(5) 0.039(2) Uani 1 1 d . . . H25 H -0.1052 0.3845 -0.0260 0.047 Uiso 1 1 calc R . . C26 C -0.0615(7) 0.3147(3) 0.0377(5) 0.043(2) Uani 1 1 d . . . H26 H -0.0669 0.2931 -0.0151 0.051 Uiso 1 1 calc R . . C27 C -0.0313(7) 0.2919(3) 0.1206(4) 0.039(2) Uani 1 1 d . . . H27 H -0.0157 0.2546 0.1243 0.046 Uiso 1 1 calc R . . C28 C -0.0550(7) 0.3197(3) 0.3882(4) 0.0280(17) Uani 1 1 d . . . C29 C -0.1731(7) 0.3246(3) 0.3722(5) 0.036(2) Uani 1 1 d . . . H29 H -0.2084 0.3172 0.3135 0.044 Uiso 1 1 calc R . . C30 C -0.2430(8) 0.3402(3) 0.4402(6) 0.050(2) Uani 1 1 d . . . H30 H -0.3249 0.3420 0.4290 0.060 Uiso 1 1 calc R . . C31 C -0.1893(10) 0.3531(3) 0.5245(6) 0.051(3) Uani 1 1 d . . . H31 H -0.2346 0.3647 0.5712 0.061 Uiso 1 1 calc R . . C32 C -0.0722(10) 0.3491(3) 0.5402(5) 0.053(3) Uani 1 1 d . . . H32 H -0.0372 0.3576 0.5984 0.063 Uiso 1 1 calc R . . C33 C -0.0019(7) 0.3330(3) 0.4734(4) 0.0348(19) Uani 1 1 d . . . H33 H 0.0799 0.3310 0.4855 0.042 Uiso 1 1 calc R . . N1 N 0.4624(6) 0.2797(3) 0.0731(4) 0.0504(19) Uani 1 1 d D . . H1 H 0.464(7) 0.271(3) 0.1302(15) 0.061 Uiso 1 1 d D . . C34 C 0.4921(9) 0.2271(4) 0.0217(6) 0.065(3) Uani 1 1 d . . . H34A H 0.4309 0.2208 -0.0277 0.078 Uiso 1 1 calc R . . H34B H 0.5661 0.2324 -0.0059 0.078 Uiso 1 1 calc R . . C35 C 0.5023(10) 0.1794(4) 0.0788(6) 0.078(3) Uani 1 1 d . . . H35A H 0.5656 0.1843 0.1261 0.118 Uiso 1 1 calc R . . H35B H 0.5187 0.1482 0.0420 0.118 Uiso 1 1 calc R . . H35C H 0.4295 0.1736 0.1066 0.118 Uiso 1 1 calc R . . C36 C 0.3449(8) 0.2975(5) 0.0392(6) 0.069(3) Uani 1 1 d . . . H36 H 0.3445 0.3046 -0.0269 0.083 Uiso 1 1 calc R . . C37 C 0.3163(10) 0.3507(4) 0.0872(8) 0.095(4) Uani 1 1 d . . . H37A H 0.3180 0.3446 0.1524 0.143 Uiso 1 1 calc R . . H37B H 0.2389 0.3630 0.0645 0.143 Uiso 1 1 calc R . . H37C H 0.3738 0.3779 0.0750 0.143 Uiso 1 1 calc R . . C38 C 0.2544(7) 0.2552(4) 0.0536(6) 0.064(3) Uani 1 1 d . . . H38A H 0.2768 0.2214 0.0265 0.095 Uiso 1 1 calc R . . H38B H 0.1791 0.2668 0.0252 0.095 Uiso 1 1 calc R . . H38C H 0.2488 0.2500 0.1184 0.095 Uiso 1 1 calc R . . C39 C 0.5610(7) 0.3184(3) 0.0747(5) 0.044(2) Uani 1 1 d . . . H39 H 0.5390 0.3497 0.1117 0.053 Uiso 1 1 calc R . . C40 C 0.5786(8) 0.3400(4) -0.0189(5) 0.062(3) Uani 1 1 d . . . H40A H 0.6443 0.3648 -0.0150 0.093 Uiso 1 1 calc R . . H40B H 0.5084 0.3588 -0.0430 0.093 Uiso 1 1 calc R . . H40C H 0.5944 0.3102 -0.0589 0.093 Uiso 1 1 calc R . . C41 C 0.6677(9) 0.2962(5) 0.1201(7) 0.100(4) Uani 1 1 d . . . H41A H 0.6492 0.2769 0.1745 0.150 Uiso 1 1 calc R . . H41B H 0.7220 0.3253 0.1369 0.150 Uiso 1 1 calc R . . H41C H 0.7030 0.2714 0.0793 0.150 Uiso 1 1 calc R . . O1 O 0.5557(14) 1.0079(6) 0.2351(11) 0.099(3) Uani 0.574(10) 1 d PU A 1 C42 C 0.524(2) 1.0157(8) 0.1502(16) 0.102(4) Uani 0.574(10) 1 d PU A 1 H42A H 0.5917 1.0278 0.1186 0.122 Uiso 0.574(10) 1 calc PR A 1 H42B H 0.4640 1.0439 0.1436 0.122 Uiso 0.574(10) 1 calc PR A 1 C43 C 0.478(3) 0.9651(8) 0.110(2) 0.108(4) Uani 0.574(10) 1 d PU A 1 H43A H 0.3942 0.9618 0.1167 0.130 Uiso 0.574(10) 1 calc PR A 1 H43B H 0.4914 0.9631 0.0454 0.130 Uiso 0.574(10) 1 calc PR A 1 C44 C 0.541(3) 0.9244(8) 0.1599(18) 0.112(4) Uani 0.574(10) 1 d PU A 1 H44A H 0.5954 0.9070 0.1208 0.134 Uiso 0.574(10) 1 calc PR A 1 H44B H 0.4867 0.8968 0.1785 0.134 Uiso 0.574(10) 1 calc PR A 1 C45 C 0.605(3) 0.9454(9) 0.2381(18) 0.106(4) Uani 0.574(10) 1 d PU A 1 H45A H 0.6901 0.9441 0.2327 0.127 Uiso 0.574(10) 1 calc PR A 1 H45B H 0.5872 0.9266 0.2936 0.127 Uiso 0.574(10) 1 calc PR A 1 O1' O 0.585(2) 0.9740(10) 0.2472(16) 0.110(4) Uani 0.426(10) 1 d PU A 2 C42' C 0.566(3) 0.9831(12) 0.151(2) 0.109(3) Uani 0.426(10) 1 d PU A 2 H42C H 0.6419 0.9820 0.1243 0.131 Uiso 0.426(10) 1 calc PR A 2 H42D H 0.5329 1.0192 0.1398 0.131 Uiso 0.426(10) 1 calc PR A 2 C43' C 0.487(4) 0.9428(12) 0.104(3) 0.109(4) Uani 0.426(10) 1 d PU A 2 H43C H 0.5289 0.9154 0.0714 0.130 Uiso 0.426(10) 1 calc PR A 2 H43D H 0.4242 0.9590 0.0645 0.130 Uiso 0.426(10) 1 calc PR A 2 C44' C 0.443(3) 0.9202(11) 0.202(2) 0.104(4) Uani 0.426(10) 1 d PU A 2 H44C H 0.3629 0.9328 0.2068 0.124 Uiso 0.426(10) 1 calc PR A 2 H44D H 0.4412 0.8806 0.1996 0.124 Uiso 0.426(10) 1 calc PR A 2 C45' C 0.507(3) 0.9348(10) 0.275(2) 0.099(4) Uani 0.426(10) 1 d PU A 2 H45C H 0.5499 0.9038 0.3018 0.119 Uiso 0.426(10) 1 calc PR A 2 H45D H 0.4575 0.9499 0.3196 0.119 Uiso 0.426(10) 1 calc PR A 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 0.0332(3) 0.0214(3) 0.0187(3) 0.0014(3) 0.0007(2) -0.0018(3) Cl1 0.0400(11) 0.0409(11) 0.0226(9) 0.0026(9) 0.0010(7) -0.0098(10) P1 0.0396(13) 0.0194(10) 0.0253(10) 0.0004(8) 0.0009(9) 0.0021(9) P2 0.0387(12) 0.0207(10) 0.0181(9) 0.0001(8) 0.0013(8) 0.0040(9) S1 0.0345(12) 0.0260(10) 0.0367(11) -0.0005(8) 0.0037(9) 0.0009(9) S2 0.0386(12) 0.0229(10) 0.0332(11) -0.0012(8) -0.0001(9) -0.0008(9) C1 0.030(4) 0.020(4) 0.018(4) 0.001(3) 0.004(3) -0.003(3) C2 0.024(4) 0.019(4) 0.019(4) -0.001(3) -0.001(3) 0.002(3) C3 0.036(4) 0.018(4) 0.020(3) 0.001(3) 0.004(3) -0.001(4) C4 0.029(4) 0.028(4) 0.013(3) 0.005(3) -0.002(3) 0.000(3) C5 0.035(5) 0.040(5) 0.029(4) 0.001(4) 0.000(3) 0.002(4) C6 0.033(5) 0.052(5) 0.031(4) 0.001(4) 0.004(3) -0.013(4) C7 0.046(6) 0.034(5) 0.028(4) -0.001(3) 0.003(4) -0.019(4) C8 0.042(5) 0.027(4) 0.022(4) 0.000(3) 0.003(3) -0.010(4) C9 0.035(5) 0.022(4) 0.021(4) -0.002(3) 0.007(3) -0.005(3) C10 0.035(5) 0.029(4) 0.025(4) 0.001(3) 0.003(3) -0.001(4) C11 0.079(7) 0.033(5) 0.036(5) -0.001(4) -0.004(5) -0.001(5) C12 0.085(8) 0.051(6) 0.029(5) 0.002(4) -0.009(5) 0.010(5) C13 0.062(6) 0.042(5) 0.043(5) -0.020(4) -0.005(4) 0.004(5) C14 0.075(7) 0.029(5) 0.045(5) -0.008(4) 0.001(5) 0.000(4) C15 0.067(6) 0.027(4) 0.030(4) 0.002(4) 0.005(4) -0.003(4) C16 0.038(5) 0.027(4) 0.027(4) 0.004(3) 0.000(3) 0.000(4) C17 0.061(6) 0.023(4) 0.034(5) 0.003(3) 0.000(4) -0.004(4) C18 0.086(7) 0.030(5) 0.026(5) -0.003(4) -0.004(4) -0.014(5) C19 0.080(7) 0.034(5) 0.033(5) 0.010(4) -0.013(5) -0.012(5) C20 0.049(6) 0.042(6) 0.077(7) 0.026(5) -0.015(5) 0.006(5) C21 0.042(6) 0.042(5) 0.053(5) 0.023(4) -0.002(4) 0.002(4) C22 0.028(4) 0.035(4) 0.015(3) -0.003(3) 0.002(3) 0.000(4) C23 0.060(6) 0.025(4) 0.027(4) 0.002(3) -0.001(4) 0.008(4) C24 0.071(7) 0.031(5) 0.035(5) 0.008(4) -0.004(4) 0.001(4) C25 0.050(6) 0.041(5) 0.028(4) 0.018(4) 0.009(4) 0.003(4) C26 0.056(6) 0.060(6) 0.013(4) -0.005(4) 0.003(4) 0.001(5) C27 0.064(6) 0.028(4) 0.024(4) -0.002(3) 0.004(4) 0.005(4) C28 0.043(5) 0.017(4) 0.026(4) 0.002(3) 0.012(3) 0.008(4) C29 0.054(6) 0.032(5) 0.025(4) 0.005(3) 0.011(4) 0.006(4) C30 0.068(7) 0.036(5) 0.049(6) 0.002(4) 0.025(5) -0.002(4) C31 0.082(8) 0.035(5) 0.041(5) 0.001(4) 0.038(5) 0.007(5) C32 0.106(9) 0.031(5) 0.024(5) -0.001(4) 0.019(5) 0.012(5) C33 0.060(6) 0.025(4) 0.021(4) 0.000(3) 0.004(4) 0.009(4) N1 0.035(4) 0.091(6) 0.026(4) 0.020(4) 0.003(3) -0.001(4) C34 0.084(7) 0.070(6) 0.042(5) -0.007(5) 0.009(5) -0.011(6) C35 0.115(10) 0.065(7) 0.060(6) -0.001(6) 0.037(6) -0.014(7) C36 0.062(7) 0.115(9) 0.028(5) 0.015(5) -0.016(5) -0.020(6) C37 0.109(10) 0.063(8) 0.105(9) 0.017(7) -0.042(7) 0.026(7) C38 0.049(6) 0.099(8) 0.043(5) 0.006(5) 0.001(4) -0.023(6) C39 0.052(6) 0.057(6) 0.022(4) -0.004(4) -0.006(4) -0.019(5) C40 0.075(7) 0.081(7) 0.032(5) 0.011(5) 0.004(4) -0.033(6) C41 0.056(7) 0.180(13) 0.064(7) 0.040(8) 0.005(5) -0.022(8) O1 0.135(8) 0.049(7) 0.109(7) -0.007(6) -0.019(6) 0.009(7) C42 0.131(9) 0.054(7) 0.113(7) -0.004(7) -0.033(7) 0.014(8) C43 0.138(9) 0.062(8) 0.116(7) -0.010(7) -0.042(7) 0.014(8) C44 0.145(9) 0.062(7) 0.119(7) -0.008(7) -0.040(7) 0.017(8) C45 0.141(9) 0.052(7) 0.116(7) -0.011(7) -0.037(6) 0.018(7) O1' 0.141(9) 0.068(8) 0.115(7) -0.013(8) -0.029(7) 0.012(8) C42' 0.143(8) 0.062(7) 0.115(7) -0.009(7) -0.035(6) 0.010(7) C43' 0.140(9) 0.062(8) 0.114(7) -0.006(8) -0.042(7) 0.015(8) C44' 0.135(10) 0.057(8) 0.111(8) -0.009(8) -0.036(7) 0.020(8) C45' 0.131(10) 0.050(8) 0.108(8) -0.016(8) -0.029(7) 0.019(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.962(7) . ? Pd1 S1 2.3341(19) . ? Pd1 S2 2.3438(19) . ? Pd1 Cl1 2.4362(18) . ? P1 C2 1.719(7) . ? P1 C16 1.805(7) . ? P1 C10 1.813(7) . ? P1 S1 2.018(3) . ? P2 C3 1.742(7) . ? P2 C22 1.806(7) . ? P2 C28 1.806(7) . ? P2 S2 2.021(3) . ? C1 C3 1.410(9) . ? C1 C2 1.435(8) . ? C2 C9 1.435(9) . ? C3 C4 1.433(9) . ? C4 C5 1.407(9) . ? C4 C9 1.446(9) . ? C5 C6 1.393(10) . ? C6 C7 1.381(10) . ? C7 C8 1.387(10) . ? C8 C9 1.398(9) . ? C10 C11 1.392(9) . ? C10 C15 1.394(9) . ? C11 C12 1.396(11) . ? C12 C13 1.369(11) . ? C13 C14 1.362(11) . ? C14 C15 1.384(10) . ? C16 C21 1.384(10) . ? C16 C17 1.393(10) . ? C17 C18 1.400(10) . ? C18 C19 1.379(12) . ? C19 C20 1.376(11) . ? C20 C21 1.397(10) . ? C22 C27 1.376(9) . ? C22 C23 1.385(9) . ? C23 C24 1.392(10) . ? C24 C25 1.375(10) . ? C25 C26 1.376(10) . ? C26 C27 1.378(9) . ? C28 C29 1.374(10) . ? C28 C33 1.402(9) . ? C29 C30 1.403(10) . ? C30 C31 1.389(12) . ? C31 C32 1.360(12) . ? C32 C33 1.395(10) . ? N1 C36 1.479(11) . ? N1 C39 1.496(10) . ? N1 C34 1.572(11) . ? C34 C35 1.463(12) . ? C36 C38 1.517(11) . ? C36 C37 1.557(13) . ? C39 C41 1.467(12) . ? C39 C40 1.524(10) . ? O1 C42 1.30(2) . ? O1 C45 1.66(2) . ? C42 C43 1.48(3) . ? C43 C44 1.42(3) . ? C44 C45 1.43(3) . ? O1' C45' 1.41(4) . ? O1' C42' 1.45(4) . ? C42' C43' 1.49(5) . ? C43' C44' 1.67(5) . ? C44' C45' 1.31(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 S1 89.48(19) . . ? C1 Pd1 S2 88.7(2) . . ? S1 Pd1 S2 176.43(7) . . ? C1 Pd1 Cl1 176.62(18) . . ? S1 Pd1 Cl1 90.09(7) . . ? S2 Pd1 Cl1 91.86(7) . . ? C2 P1 C16 112.6(3) . . ? C2 P1 C10 110.7(3) . . ? C16 P1 C10 106.1(3) . . ? C2 P1 S1 106.9(2) . . ? C16 P1 S1 109.9(3) . . ? C10 P1 S1 110.8(2) . . ? C3 P2 C22 111.9(3) . . ? C3 P2 C28 112.0(3) . . ? C22 P2 C28 105.8(3) . . ? C3 P2 S2 106.7(3) . . ? C22 P2 S2 108.6(2) . . ? C28 P2 S2 111.8(3) . . ? P1 S1 Pd1 100.82(10) . . ? P2 S2 Pd1 99.71(9) . . ? C3 C1 C2 107.6(6) . . ? C3 C1 Pd1 126.7(5) . . ? C2 C1 Pd1 125.4(5) . . ? C9 C2 C1 108.6(6) . . ? C9 C2 P1 133.9(5) . . ? C1 C2 P1 117.2(5) . . ? C1 C3 C4 109.3(6) . . ? C1 C3 P2 115.8(5) . . ? C4 C3 P2 134.8(5) . . ? C5 C4 C3 134.3(7) . . ? C5 C4 C9 118.3(6) . . ? C3 C4 C9 107.4(6) . . ? C6 C5 C4 119.7(7) . . ? C7 C6 C5 121.5(7) . . ? C6 C7 C8 120.6(7) . . ? C7 C8 C9 119.8(7) . . ? C8 C9 C2 132.8(7) . . ? C8 C9 C4 120.1(7) . . ? C2 C9 C4 107.1(6) . . ? C11 C10 C15 118.1(7) . . ? C11 C10 P1 118.8(6) . . ? C15 C10 P1 123.0(5) . . ? C10 C11 C12 120.9(8) . . ? C13 C12 C11 119.6(8) . . ? C14 C13 C12 120.4(8) . . ? C13 C14 C15 120.8(8) . . ? C14 C15 C10 120.3(7) . . ? C21 C16 C17 119.8(7) . . ? C21 C16 P1 119.8(6) . . ? C17 C16 P1 120.3(6) . . ? C16 C17 C18 119.5(8) . . ? C19 C18 C17 120.0(8) . . ? C20 C19 C18 120.8(8) . . ? C19 C20 C21 119.5(8) . . ? C16 C21 C20 120.5(8) . . ? C27 C22 C23 118.6(6) . . ? C27 C22 P2 119.7(5) . . ? C23 C22 P2 121.2(5) . . ? C22 C23 C24 120.1(7) . . ? C25 C24 C23 120.5(7) . . ? C24 C25 C26 119.4(7) . . ? C25 C26 C27 120.1(7) . . ? C22 C27 C26 121.3(7) . . ? C29 C28 C33 119.4(6) . . ? C29 C28 P2 120.9(5) . . ? C33 C28 P2 119.6(6) . . ? C28 C29 C30 121.6(8) . . ? C31 C30 C29 118.3(9) . . ? C32 C31 C30 120.1(8) . . ? C31 C32 C33 122.1(8) . . ? C32 C33 C28 118.3(8) . . ? C36 N1 C39 119.3(7) . . ? C36 N1 C34 108.6(7) . . ? C39 N1 C34 110.6(6) . . ? C35 C34 N1 114.2(7) . . ? N1 C36 C38 111.6(8) . . ? N1 C36 C37 109.0(8) . . ? C38 C36 C37 110.8(9) . . ? C41 C39 N1 112.0(8) . . ? C41 C39 C40 112.5(8) . . ? N1 C39 C40 112.0(6) . . ? C42 O1 C45 103.6(16) . . ? O1 C42 C43 108.9(19) . . ? C44 C43 C42 104(2) . . ? C43 C44 C45 111.7(19) . . ? C44 C45 O1 99.7(17) . . ? C45' O1' C42' 110(2) . . ? O1' C42' C43' 113(3) . . ? C42' C43' C44' 93(3) . . ? C45' C44' C43' 116(3) . . ? C44' C45' O1' 106(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.653 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.114 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 800697' #TrackingRef '- RX_Bourissou-DT-pincer.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H42 Cl3 P3 Pd S2' _chemical_formula_weight 1036.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4556(3) _cell_length_b 12.5154(3) _cell_length_c 18.2257(6) _cell_angle_alpha 102.868(2) _cell_angle_beta 96.921(2) _cell_angle_gamma 108.763(2) _cell_volume 2359.21(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2889 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 23.55 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.789 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9252 _exptl_absorpt_correction_T_max 0.9542 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19928 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.1019 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 24.71 _reflns_number_total 7970 _reflns_number_gt 5316 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7970 _refine_ls_number_parameters 553 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1146 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.41624(4) 0.50254(4) 0.24627(2) 0.02278(14) Uani 1 1 d . . . Cl1 Cl 0.62867(13) 0.56710(12) 0.30199(8) 0.0340(3) Uani 1 1 d . . . S1 S 0.20458(13) 0.41815(12) 0.18262(8) 0.0306(3) Uani 1 1 d . . . S2 S 0.62917(14) 0.02067(12) 0.13097(8) 0.0347(4) Uani 1 1 d . . . P1 P 0.27138(12) 0.30094(12) 0.12541(8) 0.0232(3) Uani 1 1 d . . . P2 P 0.68902(12) 0.19268(12) 0.16182(8) 0.0238(3) Uani 1 1 d . . . P3 P 0.38797(14) 0.66262(12) 0.32213(8) 0.0266(3) Uani 1 1 d . . . C1 C 0.4155(5) 0.3293(4) 0.1891(3) 0.0206(11) Uani 1 1 d . . . C2 C 0.5200(5) 0.3122(4) 0.1551(3) 0.0212(11) Uani 1 1 d . . . H2 H 0.544(5) 0.335(4) 0.114(3) 0.025 Uiso 1 1 d . . . C3 C 0.5707(5) 0.2476(4) 0.1898(3) 0.0247(12) Uani 1 1 d . . . C4 C 0.5030(5) 0.2179(4) 0.2501(3) 0.0236(12) Uani 1 1 d . . . C5 C 0.5182(5) 0.1530(5) 0.3013(3) 0.0291(13) Uani 1 1 d . . . H5 H 0.5822 0.1201 0.3014 0.035 Uiso 1 1 calc R . . C6 C 0.4369(6) 0.1380(5) 0.3521(3) 0.0339(14) Uani 1 1 d . . . H6 H 0.4468 0.0954 0.3880 0.041 Uiso 1 1 calc R . . C7 C 0.3420(6) 0.1838(5) 0.3514(3) 0.0376(15) Uani 1 1 d . . . H7 H 0.2868 0.1705 0.3860 0.045 Uiso 1 1 calc R . . C8 C 0.3258(5) 0.2491(5) 0.3009(3) 0.0303(13) Uani 1 1 d . . . H8 H 0.2610 0.2812 0.3011 0.036 Uiso 1 1 calc R . . C9 C 0.4069(5) 0.2662(4) 0.2500(3) 0.0235(12) Uani 1 1 d . . . C10 C 0.1669(5) 0.1504(4) 0.1071(3) 0.0235(12) Uani 1 1 d . . . C11 C 0.2156(5) 0.0620(5) 0.0921(3) 0.0304(13) Uani 1 1 d . . . H11 H 0.3027 0.0803 0.0918 0.036 Uiso 1 1 calc R . . C12 C 0.1361(6) -0.0534(5) 0.0776(3) 0.0380(15) Uani 1 1 d . . . H12 H 0.1680 -0.1150 0.0656 0.046 Uiso 1 1 calc R . . C13 C 0.0103(6) -0.0792(5) 0.0805(3) 0.0363(15) Uani 1 1 d . . . H13 H -0.0438 -0.1586 0.0710 0.044 Uiso 1 1 calc R . . C14 C -0.0368(5) 0.0093(5) 0.0970(3) 0.0361(14) Uani 1 1 d . . . H14 H -0.1233 -0.0092 0.0992 0.043 Uiso 1 1 calc R . . C15 C 0.0406(5) 0.1250(5) 0.1104(3) 0.0292(13) Uani 1 1 d . . . H15 H 0.0080 0.1863 0.1217 0.035 Uiso 1 1 calc R . . C16 C 0.3008(5) 0.3269(4) 0.0338(3) 0.0256(12) Uani 1 1 d . . . C17 C 0.2957(7) 0.4286(6) 0.0184(4) 0.0506(18) Uani 1 1 d . . . H17 H 0.2800 0.4856 0.0559 0.061 Uiso 1 1 calc R . . C18 C 0.3137(8) 0.4463(6) -0.0527(4) 0.062(2) Uani 1 1 d . . . H18 H 0.3082 0.5153 -0.0640 0.074 Uiso 1 1 calc R . . C19 C 0.3392(7) 0.3666(6) -0.1063(4) 0.0528(19) Uani 1 1 d . . . H19 H 0.3528 0.3806 -0.1543 0.063 Uiso 1 1 calc R . . C20 C 0.3451(6) 0.2659(5) -0.0905(3) 0.0392(15) Uani 1 1 d . . . H20 H 0.3619 0.2094 -0.1277 0.047 Uiso 1 1 calc R . . C21 C 0.3263(5) 0.2470(5) -0.0199(3) 0.0336(14) Uani 1 1 d . . . H21 H 0.3312 0.1777 -0.0089 0.040 Uiso 1 1 calc R . . C22 C 0.8205(5) 0.2606(5) 0.2436(3) 0.0296(13) Uani 1 1 d . . . C23 C 0.8481(5) 0.3750(5) 0.2877(3) 0.0325(14) Uani 1 1 d . . . H23 H 0.7972 0.4177 0.2751 0.039 Uiso 1 1 calc R . . C24 C 0.9492(5) 0.4273(5) 0.3497(3) 0.0390(15) Uani 1 1 d . . . H24 H 0.9683 0.5060 0.3791 0.047 Uiso 1 1 calc R . . C25 C 1.0216(6) 0.3652(6) 0.3687(4) 0.0471(18) Uani 1 1 d . . . H25 H 1.0913 0.4016 0.4111 0.057 Uiso 1 1 calc R . . C26 C 0.9942(6) 0.2489(6) 0.3265(3) 0.0454(17) Uani 1 1 d . . . H26 H 1.0433 0.2054 0.3405 0.054 Uiso 1 1 calc R . . C27 C 0.8938(5) 0.1985(5) 0.2639(3) 0.0349(14) Uani 1 1 d . . . H27 H 0.8748 0.1199 0.2344 0.042 Uiso 1 1 calc R . . C28 C 0.7392(5) 0.2530(4) 0.0841(3) 0.0249(12) Uani 1 1 d . . . C29 C 0.6564(5) 0.2116(5) 0.0130(3) 0.0344(14) Uani 1 1 d . . . H29 H 0.5750 0.1545 0.0069 0.041 Uiso 1 1 calc R . . C30 C 0.6900(6) 0.2517(5) -0.0488(3) 0.0382(15) Uani 1 1 d . . . H30 H 0.6319 0.2242 -0.0967 0.046 Uiso 1 1 calc R . . C31 C 0.8102(6) 0.3330(5) -0.0399(3) 0.0372(15) Uani 1 1 d . . . H31 H 0.8348 0.3606 -0.0823 0.045 Uiso 1 1 calc R . . C32 C 0.8942(6) 0.3738(5) 0.0297(3) 0.0367(15) Uani 1 1 d . . . H32 H 0.9769 0.4279 0.0349 0.044 Uiso 1 1 calc R . . C33 C 0.8580(5) 0.3358(5) 0.0922(3) 0.0315(13) Uani 1 1 d . . . H33 H 0.9147 0.3667 0.1408 0.038 Uiso 1 1 calc R . . C34 C 0.5252(5) 0.7985(5) 0.3566(3) 0.0320(13) Uani 1 1 d . . . C35 C 0.5935(6) 0.8345(5) 0.3031(3) 0.0379(15) Uani 1 1 d . . . H35 H 0.5713 0.7865 0.2516 0.045 Uiso 1 1 calc R . . C36 C 0.6948(6) 0.9411(6) 0.3249(4) 0.0514(18) Uani 1 1 d . . . H36 H 0.7418 0.9653 0.2882 0.062 Uiso 1 1 calc R . . C37 C 0.7266(7) 1.0108(6) 0.3989(4) 0.0550(19) Uani 1 1 d . . . H37 H 0.7947 1.0842 0.4138 0.066 Uiso 1 1 calc R . . C38 C 0.6597(7) 0.9740(6) 0.4511(4) 0.059(2) Uani 1 1 d . . . H38 H 0.6835 1.0213 0.5029 0.071 Uiso 1 1 calc R . . C39 C 0.5574(6) 0.8690(5) 0.4304(3) 0.0436(16) Uani 1 1 d . . . H39 H 0.5100 0.8463 0.4674 0.052 Uiso 1 1 calc R . . C40 C 0.2626(5) 0.7080(5) 0.2832(3) 0.0297(13) Uani 1 1 d . . . C41 C 0.2872(6) 0.8150(5) 0.2657(3) 0.0389(15) Uani 1 1 d . . . H41 H 0.3717 0.8675 0.2742 0.047 Uiso 1 1 calc R . . C42 C 0.1887(7) 0.8450(6) 0.2358(4) 0.0491(17) Uani 1 1 d . . . H42 H 0.2057 0.9183 0.2244 0.059 Uiso 1 1 calc R . . C43 C 0.0660(7) 0.7682(6) 0.2226(4) 0.0510(18) Uani 1 1 d . . . H43 H -0.0013 0.7886 0.2019 0.061 Uiso 1 1 calc R . . C44 C 0.0410(6) 0.6616(6) 0.2395(3) 0.0436(16) Uani 1 1 d . . . H44 H -0.0434 0.6081 0.2297 0.052 Uiso 1 1 calc R . . C45 C 0.1389(6) 0.6334(5) 0.2705(3) 0.0336(14) Uani 1 1 d . . . H45 H 0.1211 0.5611 0.2835 0.040 Uiso 1 1 calc R . . C46 C 0.3436(5) 0.6262(4) 0.4087(3) 0.0252(12) Uani 1 1 d . . . C47 C 0.2777(6) 0.6822(5) 0.4521(3) 0.0370(15) Uani 1 1 d . . . H47 H 0.2500 0.7382 0.4352 0.044 Uiso 1 1 calc R . . C48 C 0.2521(6) 0.6569(5) 0.5200(3) 0.0388(15) Uani 1 1 d . . . H48 H 0.2105 0.6980 0.5509 0.047 Uiso 1 1 calc R . . C49 C 0.2879(5) 0.5707(5) 0.5426(3) 0.0373(15) Uani 1 1 d . . . H49 H 0.2696 0.5523 0.5888 0.045 Uiso 1 1 calc R . . C50 C 0.3497(5) 0.5124(5) 0.4985(3) 0.0328(14) Uani 1 1 d . . . H50 H 0.3733 0.4534 0.5141 0.039 Uiso 1 1 calc R . . C51 C 0.3774(5) 0.5390(5) 0.4317(3) 0.0317(13) Uani 1 1 d . . . H51 H 0.4197 0.4980 0.4013 0.038 Uiso 1 1 calc R . . C52 C 0.9027(9) 0.8199(8) 0.4060(6) 0.096(3) Uani 1 1 d . . . H52A H 0.8408 0.8483 0.4295 0.115 Uiso 1 1 calc R . . H52B H 0.8590 0.7657 0.3544 0.115 Uiso 1 1 calc R . . Cl2 Cl 0.9572(3) 0.7449(2) 0.46206(17) 0.1259(12) Uani 1 1 d . . . Cl3 Cl 1.0242(3) 0.9390(3) 0.39641(17) 0.1161(10) 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 0.0263(2) 0.0219(2) 0.0216(2) 0.00524(16) 0.00676(17) 0.01037(19) Cl1 0.0296(7) 0.0326(8) 0.0349(8) 0.0064(6) -0.0001(6) 0.0092(7) S1 0.0274(7) 0.0285(8) 0.0352(8) 0.0004(6) 0.0062(6) 0.0150(7) S2 0.0382(8) 0.0237(8) 0.0401(8) 0.0043(6) 0.0048(7) 0.0127(7) P1 0.0229(7) 0.0240(8) 0.0244(7) 0.0050(6) 0.0061(6) 0.0116(6) P2 0.0205(7) 0.0241(8) 0.0267(7) 0.0049(6) 0.0048(6) 0.0093(6) P3 0.0344(8) 0.0228(8) 0.0237(7) 0.0070(6) 0.0084(6) 0.0107(7) C1 0.024(3) 0.018(3) 0.022(3) 0.004(2) 0.004(2) 0.010(2) C2 0.020(3) 0.018(3) 0.024(3) 0.005(2) 0.007(2) 0.004(2) C3 0.025(3) 0.021(3) 0.028(3) 0.004(2) 0.006(2) 0.010(2) C4 0.024(3) 0.023(3) 0.022(3) 0.004(2) 0.004(2) 0.009(2) C5 0.033(3) 0.030(3) 0.027(3) 0.010(2) 0.005(3) 0.014(3) C6 0.047(4) 0.027(3) 0.029(3) 0.012(3) 0.006(3) 0.013(3) C7 0.047(4) 0.038(4) 0.033(3) 0.016(3) 0.017(3) 0.013(3) C8 0.029(3) 0.029(3) 0.034(3) 0.008(3) 0.014(3) 0.010(3) C9 0.021(3) 0.020(3) 0.023(3) 0.002(2) 0.001(2) 0.003(2) C10 0.024(3) 0.025(3) 0.019(3) 0.008(2) 0.001(2) 0.006(2) C11 0.034(3) 0.026(3) 0.033(3) 0.010(3) 0.003(3) 0.014(3) C12 0.045(4) 0.028(3) 0.044(4) 0.013(3) 0.010(3) 0.016(3) C13 0.039(3) 0.029(3) 0.031(3) 0.010(3) 0.004(3) -0.001(3) C14 0.030(3) 0.039(4) 0.033(3) 0.007(3) 0.008(3) 0.006(3) C15 0.030(3) 0.028(3) 0.030(3) 0.008(2) 0.009(3) 0.009(3) C16 0.029(3) 0.023(3) 0.025(3) 0.006(2) 0.006(2) 0.011(3) C17 0.083(5) 0.045(4) 0.049(4) 0.023(3) 0.036(4) 0.041(4) C18 0.109(6) 0.052(4) 0.068(5) 0.044(4) 0.053(5) 0.057(5) C19 0.074(5) 0.066(5) 0.047(4) 0.040(4) 0.032(4) 0.039(4) C20 0.055(4) 0.038(4) 0.039(3) 0.015(3) 0.025(3) 0.027(3) C21 0.045(4) 0.028(3) 0.035(3) 0.017(3) 0.012(3) 0.016(3) C22 0.019(3) 0.042(4) 0.028(3) 0.014(3) 0.008(2) 0.007(3) C23 0.028(3) 0.027(3) 0.035(3) 0.001(3) 0.006(3) 0.005(3) C24 0.030(3) 0.039(4) 0.032(3) -0.001(3) 0.007(3) -0.001(3) C25 0.023(3) 0.066(5) 0.043(4) 0.020(4) 0.001(3) 0.001(3) C26 0.035(4) 0.073(5) 0.043(4) 0.038(4) 0.015(3) 0.021(4) C27 0.030(3) 0.042(4) 0.034(3) 0.017(3) 0.003(3) 0.011(3) C28 0.024(3) 0.023(3) 0.031(3) 0.008(2) 0.007(2) 0.012(2) C29 0.031(3) 0.041(4) 0.030(3) 0.002(3) 0.009(3) 0.014(3) C30 0.045(4) 0.049(4) 0.026(3) 0.005(3) 0.008(3) 0.026(3) C31 0.059(4) 0.035(4) 0.036(3) 0.020(3) 0.025(3) 0.029(3) C32 0.038(3) 0.029(3) 0.049(4) 0.021(3) 0.016(3) 0.010(3) C33 0.037(3) 0.024(3) 0.034(3) 0.010(3) 0.003(3) 0.011(3) C34 0.038(3) 0.026(3) 0.033(3) 0.008(3) 0.005(3) 0.013(3) C35 0.046(4) 0.030(3) 0.037(3) 0.016(3) 0.010(3) 0.007(3) C36 0.051(4) 0.044(4) 0.064(5) 0.030(4) 0.020(4) 0.011(4) C37 0.051(4) 0.023(4) 0.080(5) 0.011(4) 0.008(4) 0.003(3) C38 0.054(4) 0.040(4) 0.057(4) -0.012(3) 0.011(4) 0.001(4) C39 0.044(4) 0.038(4) 0.037(3) 0.000(3) 0.012(3) 0.005(3) C40 0.042(3) 0.031(3) 0.018(3) 0.003(2) 0.008(3) 0.019(3) C41 0.053(4) 0.032(3) 0.034(3) 0.013(3) 0.007(3) 0.016(3) C42 0.068(5) 0.040(4) 0.042(4) 0.014(3) 0.003(4) 0.026(4) C43 0.056(5) 0.058(5) 0.045(4) 0.010(3) 0.002(3) 0.034(4) C44 0.043(4) 0.045(4) 0.045(4) 0.009(3) 0.007(3) 0.021(3) C45 0.044(4) 0.032(3) 0.035(3) 0.014(3) 0.016(3) 0.021(3) C46 0.029(3) 0.022(3) 0.022(3) 0.001(2) 0.006(2) 0.008(3) C47 0.050(4) 0.031(3) 0.033(3) 0.012(3) 0.013(3) 0.016(3) C48 0.045(4) 0.047(4) 0.025(3) 0.006(3) 0.014(3) 0.019(3) C49 0.037(3) 0.049(4) 0.025(3) 0.013(3) 0.012(3) 0.011(3) C50 0.030(3) 0.039(4) 0.031(3) 0.021(3) 0.002(3) 0.010(3) C51 0.028(3) 0.039(4) 0.030(3) 0.009(3) 0.006(3) 0.015(3) C52 0.076(6) 0.075(6) 0.118(8) 0.024(6) -0.012(6) 0.014(5) Cl2 0.148(3) 0.0910(19) 0.121(2) 0.0210(16) -0.034(2) 0.0474(19) Cl3 0.109(2) 0.107(2) 0.114(2) 0.0131(16) 0.0420(18) 0.0211(18) _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 2.183(5) . ? Pd1 P3 2.3069(15) . ? Pd1 Cl1 2.3196(14) . ? Pd1 S1 2.3386(14) . ? Pd1 P1 2.8146(14) . ? S1 P1 2.0144(19) . ? S2 P2 1.959(2) . ? P1 C1 1.782(5) . ? P1 C10 1.807(5) . ? P1 C16 1.821(5) . ? P2 C3 1.782(5) . ? P2 C22 1.812(5) . ? P2 C28 1.818(5) . ? P3 C46 1.822(5) . ? P3 C34 1.824(6) . ? P3 C40 1.830(6) . ? C1 C2 1.465(7) . ? C1 C9 1.495(7) . ? C2 C3 1.353(7) . ? C3 C4 1.466(7) . ? C4 C5 1.397(7) . ? C4 C9 1.415(7) . ? C5 C6 1.389(8) . ? C6 C7 1.382(8) . ? C7 C8 1.394(7) . ? C8 C9 1.392(7) . ? C10 C11 1.382(7) . ? C10 C15 1.390(7) . ? C11 C12 1.382(7) . ? C12 C13 1.382(8) . ? C13 C14 1.372(8) . ? C14 C15 1.381(7) . ? C16 C21 1.365(7) . ? C16 C17 1.379(8) . ? C17 C18 1.391(9) . ? C18 C19 1.363(9) . ? C19 C20 1.374(8) . ? C20 C21 1.388(7) . ? C22 C27 1.385(8) . ? C22 C23 1.389(7) . ? C23 C24 1.384(7) . ? C24 C25 1.370(9) . ? C25 C26 1.399(9) . ? C26 C27 1.385(8) . ? C28 C33 1.387(7) . ? C28 C29 1.391(7) . ? C29 C30 1.379(8) . ? C30 C31 1.389(8) . ? C31 C32 1.378(8) . ? C32 C33 1.387(8) . ? C34 C39 1.368(8) . ? C34 C35 1.383(8) . ? C35 C36 1.393(8) . ? C36 C37 1.367(9) . ? C37 C38 1.359(10) . ? C38 C39 1.387(8) . ? C40 C45 1.381(8) . ? C40 C41 1.394(8) . ? C41 C42 1.388(9) . ? C42 C43 1.379(9) . ? C43 C44 1.384(9) . ? C44 C45 1.377(8) . ? C46 C47 1.387(8) . ? C46 C51 1.398(7) . ? C47 C48 1.386(8) . ? C48 C49 1.394(8) . ? C49 C50 1.374(8) . ? C50 C51 1.378(7) . ? C52 Cl2 1.722(9) . ? C52 Cl3 1.740(9) . ? 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 P3 167.08(13) . . ? C1 Pd1 Cl1 91.67(13) . . ? P3 Pd1 Cl1 93.40(5) . . ? C1 Pd1 S1 81.95(13) . . ? P3 Pd1 S1 92.98(5) . . ? Cl1 Pd1 S1 173.59(5) . . ? C1 Pd1 P1 39.28(13) . . ? P3 Pd1 P1 137.75(5) . . ? Cl1 Pd1 P1 128.81(5) . . ? S1 Pd1 P1 44.85(4) . . ? P1 S1 Pd1 80.19(6) . . ? C1 P1 C10 110.9(2) . . ? C1 P1 C16 110.6(2) . . ? C10 P1 C16 108.3(2) . . ? C1 P1 S1 102.66(17) . . ? C10 P1 S1 113.12(18) . . ? C16 P1 S1 111.22(18) . . ? C1 P1 Pd1 50.87(16) . . ? C10 P1 Pd1 141.90(16) . . ? C16 P1 Pd1 109.64(17) . . ? S1 P1 Pd1 54.96(5) . . ? C3 P2 C22 104.9(2) . . ? C3 P2 C28 106.4(2) . . ? C22 P2 C28 106.9(2) . . ? C3 P2 S2 112.62(18) . . ? C22 P2 S2 113.6(2) . . ? C28 P2 S2 111.78(18) . . ? C46 P3 C34 105.2(2) . . ? C46 P3 C40 104.0(2) . . ? C34 P3 C40 104.0(3) . . ? C46 P3 Pd1 107.94(17) . . ? C34 P3 Pd1 116.67(19) . . ? C40 P3 Pd1 117.69(17) . . ? C2 C1 C9 104.8(4) . . ? C2 C1 P1 117.9(4) . . ? C9 C1 P1 116.4(3) . . ? C2 C1 Pd1 122.8(3) . . ? C9 C1 Pd1 104.7(3) . . ? P1 C1 Pd1 89.8(2) . . ? C3 C2 C1 110.7(5) . . ? C2 C3 C4 108.9(5) . . ? C2 C3 P2 126.7(4) . . ? C4 C3 P2 124.1(4) . . ? C5 C4 C9 120.6(5) . . ? C5 C4 C3 131.3(5) . . ? C9 C4 C3 108.1(4) . . ? C6 C5 C4 118.1(5) . . ? C7 C6 C5 121.4(5) . . ? C6 C7 C8 121.3(5) . . ? C9 C8 C7 118.2(5) . . ? C8 C9 C4 120.4(5) . . ? C8 C9 C1 132.2(5) . . ? C4 C9 C1 107.4(4) . . ? C11 C10 C15 120.8(5) . . ? C11 C10 P1 118.9(4) . . ? C15 C10 P1 120.2(4) . . ? C10 C11 C12 119.2(5) . . ? C11 C12 C13 120.1(6) . . ? C14 C13 C12 120.3(5) . . ? C13 C14 C15 120.4(5) . . ? C14 C15 C10 119.0(5) . . ? C21 C16 C17 119.8(5) . . ? C21 C16 P1 121.1(4) . . ? C17 C16 P1 119.1(4) . . ? C16 C17 C18 119.0(6) . . ? C19 C18 C17 121.2(6) . . ? C18 C19 C20 119.5(6) . . ? C19 C20 C21 119.7(6) . . ? C16 C21 C20 120.7(5) . . ? C27 C22 C23 119.0(5) . . ? C27 C22 P2 120.5(5) . . ? C23 C22 P2 120.5(4) . . ? C24 C23 C22 120.6(6) . . ? C25 C24 C23 119.8(6) . . ? C24 C25 C26 120.8(6) . . ? C27 C26 C25 118.6(6) . . ? C22 C27 C26 121.2(6) . . ? C33 C28 C29 118.9(5) . . ? C33 C28 P2 122.5(4) . . ? C29 C28 P2 118.5(4) . . ? C30 C29 C28 121.3(5) . . ? C29 C30 C31 118.9(5) . . ? C32 C31 C30 120.6(5) . . ? C31 C32 C33 120.0(5) . . ? C28 C33 C32 120.2(5) . . ? C39 C34 C35 119.4(5) . . ? C39 C34 P3 123.1(5) . . ? C35 C34 P3 117.4(4) . . ? C34 C35 C36 120.1(6) . . ? C37 C36 C35 120.2(6) . . ? C38 C37 C36 119.2(6) . . ? C37 C38 C39 121.6(6) . . ? C34 C39 C38 119.5(6) . . ? C45 C40 C41 118.7(6) . . ? C45 C40 P3 118.8(4) . . ? C41 C40 P3 122.5(5) . . ? C42 C41 C40 120.3(6) . . ? C43 C42 C41 119.9(6) . . ? C42 C43 C44 120.1(6) . . ? C45 C44 C43 119.6(6) . . ? C44 C45 C40 121.3(6) . . ? C47 C46 C51 119.4(5) . . ? C47 C46 P3 122.0(4) . . ? C51 C46 P3 118.6(4) . . ? C48 C47 C46 120.3(6) . . ? C47 C48 C49 119.5(6) . . ? C50 C49 C48 120.3(5) . . ? C49 C50 C51 120.3(5) . . ? C50 C51 C46 120.1(5) . . ? Cl2 C52 Cl3 112.0(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.628 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.103 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 800698' #TrackingRef '- RX_Bourissou-DT-pincer.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H41 Cl2 P3 Pd S2' _chemical_formula_weight 1000.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 8.9679(12) _cell_length_b 20.433(3) _cell_length_c 24.908(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.220(12) _cell_angle_gamma 90.00 _cell_volume 4551.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 976 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 23.08 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8330 _exptl_absorpt_correction_T_max 0.9850 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25044 _diffrn_reflns_av_R_equivalents 0.2514 _diffrn_reflns_av_sigmaI/netI 0.2755 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 24.71 _reflns_number_total 7635 _reflns_number_gt 3315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Restraints have been used in order to refine disorders. The similar-ADP (Anisotropic Displacement Parameter) restraint and the rigid-bond restraint have been used in disorders to make the ADP values of the disordered atoms more reasonable. ; _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^)+(0.0224P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7635 _refine_ls_number_parameters 600 _refine_ls_number_restraints 336 _refine_ls_R_factor_all 0.1982 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.1368 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.921 _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 0.25716(7) 0.43174(4) 0.21617(3) 0.0193(2) Uani 1 1 d . . . S1 S 0.1526(3) 0.53076(11) 0.24273(10) 0.0291(7) Uani 1 1 d . . . S2 S 0.3839(3) 0.33726(12) 0.19528(10) 0.0307(7) Uani 1 1 d . A . P2 P 0.1890(3) 0.52635(12) 0.32416(11) 0.0230(6) Uani 1 1 d . . . P3 P 0.1559(2) 0.44958(12) 0.12632(10) 0.0220(7) Uani 1 1 d . . . C1 C 0.3320(8) 0.4189(4) 0.2930(4) 0.022(2) Uani 1 1 d . . . C2 C 0.4211(10) 0.3654(4) 0.3135(4) 0.026(2) Uani 1 1 d . A . C3 C 0.3087(9) 0.4603(4) 0.3372(4) 0.017(2) Uani 1 1 d . . . C4 C 0.3719(9) 0.4302(5) 0.3862(3) 0.023(2) Uani 1 1 d . . . C5 C 0.3744(9) 0.4494(4) 0.4404(4) 0.023(2) Uani 1 1 d . . . H5 H 0.3267 0.4888 0.4501 0.028 Uiso 1 1 calc R . . C6 C 0.4469(10) 0.4104(5) 0.4796(4) 0.034(3) Uani 1 1 d . . . H6 H 0.4464 0.4223 0.5165 0.041 Uiso 1 1 calc R . . C7 C 0.5222(11) 0.3527(5) 0.4647(4) 0.039(3) Uani 1 1 d . . . H7 H 0.5732 0.3266 0.4917 0.046 Uiso 1 1 calc R . . C8 C 0.5219(10) 0.3341(5) 0.4108(4) 0.036(3) Uani 1 1 d . . . H8 H 0.5755 0.2963 0.4012 0.043 Uiso 1 1 calc R . . C9 C 0.4442(9) 0.3704(4) 0.3718(4) 0.023(2) Uani 1 1 d . . . P1 P 0.4650(2) 0.30495(12) 0.26914(11) 0.0233(6) Uani 1 1 d D . . C10 C 0.389(2) 0.2261(6) 0.2848(8) 0.040(3) Uani 0.489(19) 1 d PGDU A 1 C11 C 0.4156(19) 0.1722(7) 0.2529(7) 0.048(3) Uani 0.489(19) 1 d PGDU A 1 H11 H 0.4763 0.1766 0.2234 0.057 Uiso 0.489(19) 1 calc PR A 1 C12 C 0.353(2) 0.1119(6) 0.2641(8) 0.055(3) Uani 0.489(19) 1 d PGDU A 1 H12 H 0.3716 0.0750 0.2422 0.066 Uiso 0.489(19) 1 calc PR A 1 C13 C 0.265(2) 0.1054(6) 0.3072(8) 0.055(3) Uani 0.489(19) 1 d PGDU A 1 H13 H 0.2221 0.0642 0.3148 0.066 Uiso 0.489(19) 1 calc PR A 1 C14 C 0.238(2) 0.1594(9) 0.3391(8) 0.052(3) Uani 0.489(19) 1 d PGDU A 1 H14 H 0.1772 0.1549 0.3686 0.062 Uiso 0.489(19) 1 calc PR A 1 C15 C 0.300(2) 0.2197(7) 0.3280(8) 0.044(3) Uani 0.489(19) 1 d PGDU A 1 H15 H 0.2819 0.2566 0.3498 0.053 Uiso 0.489(19) 1 calc PR A 1 C10' C 0.3733(18) 0.2285(5) 0.2811(7) 0.040(3) Uani 0.511(19) 1 d PGDU A 2 C11' C 0.3545(18) 0.1839(7) 0.2390(7) 0.048(3) Uani 0.511(19) 1 d PGDU A 2 H11' H 0.3949 0.1930 0.2056 0.057 Uiso 0.511(19) 1 calc PR A 2 C12' C 0.276(2) 0.1261(7) 0.2458(8) 0.055(3) Uani 0.511(19) 1 d PGDU A 2 H12' H 0.2635 0.0956 0.2170 0.066 Uiso 0.511(19) 1 calc PR A 2 C13' C 0.2172(17) 0.1128(6) 0.2946(9) 0.055(3) Uani 0.511(19) 1 d PGDU A 2 H13' H 0.1639 0.0733 0.2993 0.066 Uiso 0.511(19) 1 calc PR A 2 C14' C 0.236(2) 0.1574(8) 0.3368(7) 0.052(3) Uani 0.511(19) 1 d PGDU A 2 H14' H 0.1957 0.1484 0.3702 0.063 Uiso 0.511(19) 1 calc PR A 2 C15' C 0.314(2) 0.2153(7) 0.3300(7) 0.044(3) Uani 0.511(19) 1 d PGDU A 2 H15' H 0.3270 0.2457 0.3588 0.053 Uiso 0.511(19) 1 calc PR A 2 C16 C 0.6640(9) 0.2878(4) 0.2684(4) 0.024(2) Uani 1 1 d U A . C17 C 0.7230(13) 0.2288(5) 0.2797(5) 0.056(3) Uani 1 1 d U . . H17 H 0.6605 0.1936 0.2890 0.068 Uiso 1 1 calc R A . C18 C 0.8773(13) 0.2191(6) 0.2779(5) 0.061(4) Uani 1 1 d U A . H18 H 0.9195 0.1775 0.2866 0.074 Uiso 1 1 calc R . . C19 C 0.9667(14) 0.2689(7) 0.2639(5) 0.068(4) Uani 1 1 d U . . H19 H 1.0711 0.2616 0.2629 0.082 Uiso 1 1 calc R A . C20 C 0.9104(13) 0.3279(7) 0.2515(6) 0.078(4) Uani 1 1 d U A . H20 H 0.9727 0.3624 0.2408 0.094 Uiso 1 1 calc R . . C21 C 0.7537(12) 0.3376(5) 0.2548(5) 0.061(4) Uani 1 1 d U . . H21 H 0.7116 0.3796 0.2475 0.073 Uiso 1 1 calc R A . C22 C 0.2688(10) 0.6021(4) 0.3507(4) 0.026(2) Uani 1 1 d . . . C23 C 0.1802(11) 0.6592(5) 0.3508(4) 0.036(3) Uani 1 1 d . . . H23 H 0.0774 0.6573 0.3387 0.043 Uiso 1 1 calc R . . C24 C 0.2428(14) 0.7182(5) 0.3687(5) 0.060(4) Uani 1 1 d . . . H24 H 0.1834 0.7568 0.3684 0.072 Uiso 1 1 calc R . . C25 C 0.3919(15) 0.7205(6) 0.3869(5) 0.051(3) Uani 1 1 d . . . H25 H 0.4345 0.7605 0.4000 0.062 Uiso 1 1 calc R . . C26 C 0.4787(13) 0.6654(6) 0.3863(4) 0.048(3) Uani 1 1 d . . . H26 H 0.5814 0.6678 0.3986 0.058 Uiso 1 1 calc R . . C27 C 0.4194(11) 0.6063(5) 0.3681(4) 0.038(3) Uani 1 1 d . . . H27 H 0.4815 0.5687 0.3674 0.046 Uiso 1 1 calc R . . C28 C 0.0153(9) 0.5174(4) 0.3561(4) 0.023(2) Uani 1 1 d . . . C29 C -0.1044(11) 0.4852(5) 0.3303(5) 0.055(3) Uani 1 1 d . . . H29 H -0.0989 0.4711 0.2941 0.066 Uiso 1 1 calc R . . C30 C -0.2316(11) 0.4733(6) 0.3562(5) 0.059(4) Uani 1 1 d . . . H30 H -0.3128 0.4507 0.3379 0.070 Uiso 1 1 calc R . . C31 C -0.2427(11) 0.4934(5) 0.4081(5) 0.044(3) Uani 1 1 d . . . H31 H -0.3314 0.4852 0.4256 0.053 Uiso 1 1 calc R . . C32 C -0.1263(11) 0.5253(5) 0.4345(5) 0.058(4) Uani 1 1 d . . . H32 H -0.1324 0.5392 0.4706 0.070 Uiso 1 1 calc R . . C33 C 0.0012(10) 0.5371(5) 0.4081(5) 0.048(3) Uani 1 1 d . . . H33 H 0.0820 0.5598 0.4267 0.058 Uiso 1 1 calc R . . C34 C 0.2303(9) 0.4052(5) 0.0710(4) 0.025(2) Uani 1 1 d . . . C35 C 0.2268(10) 0.3363(5) 0.0714(4) 0.036(3) Uani 1 1 d . . . H35 H 0.1850 0.3140 0.1002 0.043 Uiso 1 1 calc R . . C36 C 0.2841(11) 0.3007(5) 0.0301(5) 0.040(3) Uani 1 1 d . . . H36 H 0.2833 0.2543 0.0310 0.048 Uiso 1 1 calc R . . C37 C 0.3423(11) 0.3331(6) -0.0126(5) 0.048(3) Uani 1 1 d . . . H37 H 0.3818 0.3088 -0.0408 0.057 Uiso 1 1 calc R . . C38 C 0.3429(11) 0.3997(6) -0.0141(5) 0.047(3) Uani 1 1 d . . . H38 H 0.3828 0.4214 -0.0436 0.056 Uiso 1 1 calc R . . C39 C 0.2862(9) 0.4363(5) 0.0266(4) 0.029(2) Uani 1 1 d . . . H39 H 0.2853 0.4827 0.0243 0.035 Uiso 1 1 calc R . . C40 C -0.0460(8) 0.4353(4) 0.1149(4) 0.023(2) Uani 1 1 d . . . C41 C -0.1380(10) 0.4477(6) 0.1554(4) 0.058(4) Uani 1 1 d . . . H41 H -0.0961 0.4610 0.1899 0.069 Uiso 1 1 calc R . . C42 C -0.2899(11) 0.4410(7) 0.1465(5) 0.073(4) Uani 1 1 d . . . H42 H -0.3532 0.4540 0.1735 0.087 Uiso 1 1 calc R . . C43 C -0.3504(11) 0.4161(5) 0.0995(5) 0.050(3) Uani 1 1 d . . . H43 H -0.4552 0.4088 0.0947 0.060 Uiso 1 1 calc R . . C44 C -0.2628(12) 0.4017(5) 0.0600(5) 0.054(3) Uani 1 1 d . . . H44 H -0.3055 0.3849 0.0267 0.065 Uiso 1 1 calc R . . C45 C -0.1110(10) 0.4111(5) 0.0676(4) 0.045(3) Uani 1 1 d . . . H45 H -0.0497 0.4005 0.0393 0.055 Uiso 1 1 calc R . . C46 C 0.1769(8) 0.5342(4) 0.1074(3) 0.016(2) Uani 1 1 d . . . C47 C 0.0649(9) 0.5721(5) 0.0812(4) 0.028(2) Uani 1 1 d . . . H47 H -0.0308 0.5535 0.0725 0.033 Uiso 1 1 calc R . . C48 C 0.0913(11) 0.6372(5) 0.0677(4) 0.036(3) Uani 1 1 d . . . H48 H 0.0135 0.6625 0.0501 0.043 Uiso 1 1 calc R . . C49 C 0.2291(12) 0.6646(5) 0.0798(4) 0.043(3) Uani 1 1 d . . . H49 H 0.2471 0.7087 0.0701 0.052 Uiso 1 1 calc R . . C50 C 0.3408(11) 0.6286(5) 0.1059(4) 0.039(3) Uani 1 1 d . . . H50 H 0.4359 0.6481 0.1143 0.047 Uiso 1 1 calc R . . C51 C 0.3172(9) 0.5638(5) 0.1204(4) 0.034(3) Uani 1 1 d . . . H51 H 0.3953 0.5395 0.1390 0.041 Uiso 1 1 calc R . . C52 C -0.064(3) 0.3464(18) 0.4405(12) 0.085(4) Uani 0.344(8) 1 d PDU B 1 H52A H -0.1411 0.3342 0.4119 0.102 Uiso 0.344(8) 1 calc PR B 1 H52B H -0.0688 0.3943 0.4463 0.102 Uiso 0.344(8) 1 calc PR B 1 Cl1 Cl 0.1110(15) 0.3247(7) 0.4221(6) 0.113(4) Uani 0.344(8) 1 d PDU B 1 Cl2 Cl -0.0958(15) 0.3031(6) 0.5028(5) 0.087(4) Uani 0.344(8) 1 d PDU B 1 C52' C 0.049(3) 0.3578(9) 0.4457(7) 0.078(4) Uani 0.656(8) 1 d PDU B 2 H52C H 0.0092 0.4025 0.4396 0.094 Uiso 0.656(8) 1 calc PR B 2 H52D H 0.1590 0.3606 0.4531 0.094 Uiso 0.656(8) 1 calc PR B 2 Cl1' Cl 0.0053(7) 0.3091(3) 0.3901(2) 0.080(2) Uani 0.656(8) 1 d PDU B 2 Cl2' Cl -0.0371(8) 0.3188(3) 0.5028(3) 0.086(2) Uani 0.656(8) 1 d PDU B 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 0.0126(4) 0.0254(4) 0.0197(4) 0.0009(4) -0.0006(3) 0.0000(4) S1 0.0353(15) 0.0252(15) 0.0254(16) -0.0017(13) -0.0067(12) 0.0076(12) S2 0.0260(14) 0.0401(17) 0.0250(16) -0.0082(13) -0.0043(12) 0.0100(13) P2 0.0178(14) 0.0246(15) 0.0261(17) -0.0026(13) -0.0017(12) 0.0007(12) P3 0.0123(13) 0.0308(17) 0.0223(16) 0.0017(12) -0.0024(11) 0.0009(12) C1 0.006(4) 0.022(6) 0.038(7) 0.011(5) 0.005(4) 0.000(4) C2 0.025(6) 0.036(6) 0.018(6) -0.006(5) 0.001(5) 0.002(5) C3 0.015(5) 0.016(5) 0.023(6) -0.005(5) 0.007(4) -0.003(4) C4 0.023(5) 0.030(6) 0.016(5) 0.002(5) -0.006(4) -0.007(5) C5 0.017(5) 0.033(6) 0.020(6) 0.005(5) 0.004(4) -0.003(4) C6 0.042(6) 0.048(8) 0.013(6) 0.001(5) 0.003(5) -0.008(6) C7 0.056(7) 0.038(7) 0.019(7) 0.014(6) -0.017(6) 0.000(6) C8 0.037(6) 0.048(7) 0.023(7) 0.005(6) 0.000(5) 0.012(6) C9 0.016(5) 0.028(6) 0.024(6) -0.002(5) 0.000(4) 0.000(5) P1 0.0148(14) 0.0266(16) 0.0283(17) -0.0012(13) 0.0010(12) -0.0014(12) C10 0.017(5) 0.025(5) 0.077(7) 0.011(5) -0.006(5) 0.000(5) C11 0.026(6) 0.031(5) 0.085(7) 0.008(5) -0.009(5) -0.003(5) C12 0.032(6) 0.035(5) 0.094(7) 0.011(5) -0.013(5) -0.009(5) C13 0.029(6) 0.039(5) 0.094(7) 0.016(5) -0.015(5) -0.015(5) C14 0.025(5) 0.040(5) 0.089(7) 0.020(5) -0.012(5) -0.011(5) C15 0.019(5) 0.032(5) 0.081(7) 0.016(5) -0.009(5) -0.004(5) C10' 0.016(5) 0.024(5) 0.078(7) 0.011(5) -0.006(5) 0.000(4) C11' 0.024(6) 0.031(5) 0.086(7) 0.006(5) -0.009(5) -0.005(5) C12' 0.031(6) 0.037(5) 0.094(7) 0.009(5) -0.015(6) -0.012(5) C13' 0.029(6) 0.038(5) 0.095(7) 0.019(5) -0.017(6) -0.014(5) C14' 0.025(5) 0.040(5) 0.089(7) 0.020(5) -0.013(5) -0.011(5) C15' 0.018(5) 0.030(5) 0.082(6) 0.015(5) -0.009(5) -0.003(4) C16 0.020(5) 0.016(5) 0.036(6) 0.007(4) 0.000(4) 0.007(4) C17 0.052(7) 0.054(7) 0.063(7) -0.003(6) 0.008(6) 0.000(6) C18 0.052(6) 0.062(7) 0.069(7) 0.017(6) 0.000(6) 0.019(6) C19 0.042(6) 0.069(7) 0.092(8) 0.010(7) -0.008(6) 0.002(6) C20 0.047(7) 0.069(7) 0.120(9) 0.018(7) 0.007(6) -0.013(6) C21 0.035(6) 0.041(6) 0.107(8) 0.014(6) 0.001(6) 0.006(5) C22 0.034(6) 0.019(6) 0.023(6) -0.002(5) 0.002(5) -0.005(5) C23 0.031(6) 0.028(6) 0.046(8) -0.012(6) -0.007(5) 0.000(5) C24 0.079(10) 0.022(7) 0.078(11) -0.014(7) -0.004(8) 0.007(7) C25 0.068(9) 0.029(8) 0.056(9) 0.011(6) 0.000(7) -0.023(7) C26 0.054(8) 0.057(8) 0.032(7) -0.008(7) 0.000(6) -0.035(7) C27 0.025(6) 0.058(8) 0.031(7) -0.002(6) 0.004(5) -0.001(6) C28 0.019(5) 0.025(6) 0.024(6) -0.008(5) -0.004(4) 0.004(5) C29 0.039(7) 0.077(9) 0.050(9) -0.021(7) 0.003(6) -0.025(7) C30 0.028(7) 0.095(10) 0.053(9) -0.004(8) -0.001(6) -0.032(7) C31 0.021(6) 0.051(8) 0.061(9) 0.008(7) 0.011(6) -0.006(6) C32 0.026(7) 0.090(10) 0.060(9) -0.024(8) 0.022(6) -0.019(7) C33 0.018(6) 0.072(9) 0.054(9) -0.013(7) -0.003(6) -0.009(6) C34 0.012(5) 0.030(7) 0.030(7) -0.003(5) -0.014(5) 0.004(5) C35 0.026(6) 0.062(8) 0.018(6) 0.004(6) -0.009(5) 0.007(6) C36 0.040(7) 0.033(7) 0.045(8) -0.008(6) -0.012(6) 0.009(6) C37 0.045(7) 0.063(9) 0.037(8) -0.014(7) 0.010(6) 0.023(7) C38 0.040(7) 0.062(9) 0.038(8) -0.013(6) 0.005(6) 0.007(6) C39 0.027(5) 0.031(6) 0.027(6) -0.004(6) -0.004(5) 0.007(5) C40 0.015(5) 0.015(5) 0.036(6) 0.009(5) -0.010(4) -0.003(5) C41 0.021(6) 0.108(11) 0.043(8) -0.031(7) 0.003(5) 0.006(7) C42 0.018(6) 0.134(12) 0.067(10) -0.022(10) 0.004(6) -0.006(8) C43 0.015(6) 0.074(9) 0.060(9) 0.015(7) -0.011(6) -0.021(6) C44 0.032(7) 0.088(10) 0.039(8) -0.007(7) -0.012(6) -0.011(7) C45 0.027(6) 0.081(9) 0.028(7) -0.005(6) -0.007(5) -0.012(6) C46 0.004(4) 0.023(5) 0.020(6) -0.001(4) 0.004(4) 0.001(4) C47 0.021(5) 0.026(6) 0.035(6) -0.007(6) 0.001(4) -0.007(5) C48 0.037(7) 0.032(7) 0.037(7) 0.008(6) -0.013(5) 0.006(5) C49 0.046(7) 0.038(7) 0.045(8) -0.008(6) 0.004(6) -0.012(6) C50 0.032(7) 0.046(8) 0.038(7) -0.010(6) -0.004(6) -0.019(6) C51 0.020(5) 0.037(7) 0.046(7) 0.002(6) 0.002(5) 0.003(6) C52 0.085(4) 0.085(5) 0.085(4) 0.0001(10) 0.0061(11) 0.0000(10) Cl1 0.112(4) 0.114(4) 0.113(4) 0.0009(10) 0.0088(11) -0.0003(10) Cl2 0.088(4) 0.088(4) 0.087(4) -0.0010(10) 0.0069(11) 0.0000(10) C52' 0.078(4) 0.078(4) 0.078(4) -0.0003(10) 0.0053(11) 0.0000(10) Cl1' 0.081(2) 0.080(2) 0.080(2) -0.0015(10) 0.0062(10) -0.0021(10) Cl2' 0.087(2) 0.086(2) 0.085(2) -0.0020(10) 0.0076(10) -0.0008(10) _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 1.997(9) . ? Pd1 S2 2.319(3) . ? Pd1 S1 2.346(2) . ? Pd1 P3 2.381(3) . ? S1 P2 2.033(4) . ? S2 P1 2.038(4) . ? P2 C3 1.740(8) . ? P2 C22 1.809(9) . ? P2 C28 1.810(9) . ? P3 C46 1.807(8) . ? P3 C34 1.817(10) . ? P3 C40 1.835(8) . ? C1 C3 1.417(11) . ? C1 C2 1.426(11) . ? C2 C9 1.455(12) . ? C2 P1 1.722(9) . ? C3 C4 1.444(11) . ? C4 C5 1.405(11) . ? C4 C9 1.442(11) . ? C5 C6 1.385(11) . ? C6 C7 1.422(12) . ? C7 C8 1.394(12) . ? C8 C9 1.372(11) . ? P1 C10' 1.800(9) . ? P1 C10 1.803(9) . ? P1 C16 1.821(9) . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C10' C11' 1.3900 . ? C10' C15' 1.3900 . ? C11' C12' 1.3900 . ? C12' C13' 1.3900 . ? C13' C14' 1.3900 . ? C14' C15' 1.3900 . ? C16 C17 1.339(12) . ? C16 C21 1.354(12) . ? C17 C18 1.402(14) . ? C18 C19 1.357(14) . ? C19 C20 1.334(14) . ? C20 C21 1.428(13) . ? C22 C27 1.391(11) . ? C22 C23 1.412(11) . ? C23 C24 1.389(12) . ? C24 C25 1.381(13) . ? C25 C26 1.370(13) . ? C26 C27 1.382(12) . ? C28 C33 1.371(13) . ? C28 C29 1.377(11) . ? C29 C30 1.374(14) . ? C30 C31 1.367(14) . ? C31 C32 1.358(13) . ? C32 C33 1.381(13) . ? C34 C39 1.400(12) . ? C34 C35 1.409(12) . ? C35 C36 1.389(13) . ? C36 C37 1.386(13) . ? C37 C38 1.360(13) . ? C38 C39 1.386(12) . ? C40 C45 1.368(12) . ? C40 C41 1.374(12) . ? C41 C42 1.371(11) . ? C42 C43 1.352(14) . ? C43 C44 1.338(14) . ? C44 C45 1.374(12) . ? C46 C47 1.392(10) . ? C46 C51 1.411(10) . ? C47 C48 1.395(11) . ? C48 C49 1.370(12) . ? C49 C50 1.368(12) . ? C50 C51 1.394(12) . ? C52 Cl1 1.72(2) . ? C52 Cl2 1.83(2) . ? C52' Cl1' 1.727(17) . ? C52' Cl2' 1.849(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 C1 Pd1 S2 88.3(3) . . ? C1 Pd1 S1 87.5(3) . . ? S2 Pd1 S1 173.83(9) . . ? C1 Pd1 P3 176.9(3) . . ? S2 Pd1 P3 94.35(9) . . ? S1 Pd1 P3 90.02(9) . . ? P2 S1 Pd1 101.82(12) . . ? P1 S2 Pd1 102.43(13) . . ? C3 P2 C22 111.9(4) . . ? C3 P2 C28 112.2(4) . . ? C22 P2 C28 104.8(4) . . ? C3 P2 S1 105.8(3) . . ? C22 P2 S1 110.9(3) . . ? C28 P2 S1 111.3(3) . . ? C46 P3 C34 103.2(4) . . ? C46 P3 C40 103.4(4) . . ? C34 P3 C40 102.5(4) . . ? C46 P3 Pd1 110.6(3) . . ? C34 P3 Pd1 120.0(3) . . ? C40 P3 Pd1 115.2(3) . . ? C3 C1 C2 106.8(8) . . ? C3 C1 Pd1 127.5(6) . . ? C2 C1 Pd1 125.7(7) . . ? C1 C2 C9 109.8(8) . . ? C1 C2 P1 117.9(7) . . ? C9 C2 P1 131.9(7) . . ? C1 C3 C4 109.4(7) . . ? C1 C3 P2 116.2(7) . . ? C4 C3 P2 133.4(7) . . ? C5 C4 C9 120.1(8) . . ? C5 C4 C3 132.1(9) . . ? C9 C4 C3 107.8(8) . . ? C6 C5 C4 119.4(9) . . ? C5 C6 C7 119.9(9) . . ? C8 C7 C6 120.8(9) . . ? C9 C8 C7 119.9(10) . . ? C8 C9 C4 119.7(9) . . ? C8 C9 C2 134.2(9) . . ? C4 C9 C2 105.9(8) . . ? C2 P1 C10' 112.8(7) . . ? C2 P1 C10 113.2(7) . . ? C10' P1 C10 5.4(11) . . ? C2 P1 C16 114.5(4) . . ? C10' P1 C16 107.1(6) . . ? C10 P1 C16 102.5(7) . . ? C2 P1 S2 105.3(3) . . ? C10' P1 S2 107.1(6) . . ? C10 P1 S2 111.7(6) . . ? C16 P1 S2 109.7(3) . . ? C11 C10 C15 120.0 . . ? C11 C10 P1 120.0(9) . . ? C15 C10 P1 120.0(9) . . ? C12 C11 C10 120.0 . . ? C11 C12 C13 120.0 . . ? C12 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C10 120.0 . . ? C11' C10' C15' 120.0 . . ? C11' C10' P1 118.4(9) . . ? C15' C10' P1 121.5(9) . . ? C10' C11' C12' 120.0 . . ? C11' C12' C13' 120.0 . . ? C14' C13' C12' 120.0 . . ? C13' C14' C15' 120.0 . . ? C14' C15' C10' 120.0 . . ? C17 C16 C21 119.8(10) . . ? C17 C16 P1 122.9(8) . . ? C21 C16 P1 117.3(7) . . ? C16 C17 C18 119.7(11) . . ? C19 C18 C17 120.4(11) . . ? C20 C19 C18 121.0(12) . . ? C19 C20 C21 118.0(12) . . ? C16 C21 C20 121.0(10) . . ? C27 C22 C23 118.8(8) . . ? C27 C22 P2 121.0(7) . . ? C23 C22 P2 120.1(7) . . ? C24 C23 C22 120.3(9) . . ? C25 C24 C23 119.5(10) . . ? C26 C25 C24 120.4(11) . . ? C25 C26 C27 121.1(10) . . ? C26 C27 C22 119.8(10) . . ? C33 C28 C29 117.3(9) . . ? C33 C28 P2 121.8(7) . . ? C29 C28 P2 120.6(8) . . ? C30 C29 C28 120.7(11) . . ? C31 C30 C29 120.8(10) . . ? C32 C31 C30 119.6(10) . . ? C31 C32 C33 119.2(11) . . ? C28 C33 C32 122.3(10) . . ? C39 C34 C35 118.0(9) . . ? C39 C34 P3 123.1(7) . . ? C35 C34 P3 118.9(8) . . ? C36 C35 C34 120.4(10) . . ? C37 C36 C35 120.0(10) . . ? C38 C37 C36 120.1(11) . . ? C37 C38 C39 121.1(11) . . ? C38 C39 C34 120.3(10) . . ? C45 C40 C41 117.3(8) . . ? C45 C40 P3 123.0(8) . . ? C41 C40 P3 119.7(7) . . ? C42 C41 C40 120.3(10) . . ? C43 C42 C41 120.7(11) . . ? C44 C43 C42 120.0(10) . . ? C43 C44 C45 119.8(11) . . ? C40 C45 C44 121.6(10) . . ? C47 C46 C51 118.1(8) . . ? C47 C46 P3 124.7(6) . . ? C51 C46 P3 117.2(7) . . ? C46 C47 C48 120.9(8) . . ? C49 C48 C47 120.2(9) . . ? C50 C49 C48 120.1(10) . . ? C49 C50 C51 121.0(9) . . ? C50 C51 C46 119.8(9) . . ? Cl1 C52 Cl2 107.7(14) . . ? Cl1' C52' Cl2' 106.6(9) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.971 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.130 _vrf_RINTA01_noel10m ; PROBLEM: The value of Rint is greater than 0.25 RESPONSE: The crystal is very weakly diffracting and the quality of the data is poor due to the crystal quality. ; _vrf_PLAT020_noel10m ; PROBLEM: The value of Rint is greater than 0.12 ......... 0.25 RESPONSE: The crystal is very weakly diffracting and the quality of the data is poor due to the crystal quality. ; # end Validation Reply Form data_7 _database_code_depnum_ccdc_archive 'CCDC 800699' #TrackingRef '- RX_Bourissou-DT-pincer.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H42 B Cl2 F4 P3 Pd S2' _chemical_formula_weight 1088.00 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1914(3) _cell_length_b 14.4571(3) _cell_length_c 14.9919(3) _cell_angle_alpha 110.9630(10) _cell_angle_beta 97.9850(10) _cell_angle_gamma 93.245(2) _cell_volume 2427.34(9) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4421 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 29.58 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.729 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.890 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36403 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.0799 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8875 _reflns_number_gt 6190 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.4137P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8875 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8650(3) 0.9090(3) -0.0136(3) 0.0193(9) Uani 1 1 d . . . H1 H 0.9039 0.9185 -0.0647 0.023 Uiso 1 1 calc R . . C2 C 0.7730(3) 0.9760(3) 0.0062(3) 0.0216(9) Uani 1 1 d . . . C3 C 0.6809(3) 0.9838(3) -0.0556(3) 0.0276(10) Uani 1 1 d . . . H3 H 0.6665 0.9420 -0.1222 0.033 Uiso 1 1 calc R . . C4 C 0.6101(3) 1.0547(3) -0.0168(3) 0.0323(11) Uani 1 1 d . . . H4 H 0.5470 1.0617 -0.0578 0.039 Uiso 1 1 calc R . . C5 C 0.6305(3) 1.1146(3) 0.0802(3) 0.0325(11) Uani 1 1 d . . . H5 H 0.5803 1.1615 0.1050 0.039 Uiso 1 1 calc R . . C6 C 0.7227(3) 1.1082(3) 0.1426(3) 0.0295(10) Uani 1 1 d . . . H6 H 0.7357 1.1497 0.2094 0.035 Uiso 1 1 calc R . . C7 C 0.7957(3) 1.0389(3) 0.1044(3) 0.0223(9) Uani 1 1 d . . . C8 C 0.9024(3) 1.0166(3) 0.1481(3) 0.0204(9) Uani 1 1 d . . . C9 C 0.9446(3) 0.9419(3) 0.0827(3) 0.0190(9) Uani 1 1 d . . . C10 C 0.7547(3) 0.7105(3) -0.1584(3) 0.0228(9) Uani 1 1 d . . . C11 C 0.7493(3) 0.7494(3) -0.2315(3) 0.0261(10) Uani 1 1 d . . . H11 H 0.7846 0.8143 -0.2182 0.031 Uiso 1 1 calc R . . C12 C 0.6926(4) 0.6930(4) -0.3232(3) 0.0362(11) Uani 1 1 d . . . H12 H 0.6893 0.7188 -0.3735 0.043 Uiso 1 1 calc R . . C13 C 0.6406(4) 0.5994(4) -0.3419(3) 0.0433(13) Uani 1 1 d . . . H13 H 0.6013 0.5611 -0.4051 0.052 Uiso 1 1 calc R . . C14 C 0.6449(4) 0.5608(4) -0.2706(4) 0.0495(14) Uani 1 1 d . . . H14 H 0.6088 0.4960 -0.2846 0.059 Uiso 1 1 calc R . . C15 C 0.7010(4) 0.6152(3) -0.1789(3) 0.0377(12) Uani 1 1 d . . . H15 H 0.7035 0.5883 -0.1295 0.045 Uiso 1 1 calc R . . C16 C 0.7453(3) 0.7627(3) 0.0445(3) 0.0191(9) Uani 1 1 d . . . C17 C 0.6317(3) 0.7734(3) 0.0269(3) 0.0322(11) Uani 1 1 d . . . H17 H 0.6020 0.7885 -0.0276 0.039 Uiso 1 1 calc R . . C18 C 0.5628(4) 0.7619(3) 0.0890(4) 0.0370(12) Uani 1 1 d . . . H18 H 0.4858 0.7693 0.0770 0.044 Uiso 1 1 calc R . . C19 C 0.6057(4) 0.7396(3) 0.1687(3) 0.0338(11) Uani 1 1 d . . . H19 H 0.5580 0.7314 0.2109 0.041 Uiso 1 1 calc R . . C20 C 0.7177(4) 0.7294(3) 0.1866(3) 0.0332(11) Uani 1 1 d . . . H20 H 0.7472 0.7149 0.2415 0.040 Uiso 1 1 calc R . . C21 C 0.7874(3) 0.7404(3) 0.1242(3) 0.0250(10) Uani 1 1 d . . . H21 H 0.8642 0.7326 0.1364 0.030 Uiso 1 1 calc R . . C22 C 1.0043(3) 1.1997(3) 0.3120(3) 0.0217(9) Uani 1 1 d . . . C23 C 0.9710(4) 1.2503(3) 0.2514(3) 0.0304(10) Uani 1 1 d . . . H23 H 0.9350 1.2146 0.1865 0.036 Uiso 1 1 calc R . . C24 C 0.9908(4) 1.3536(3) 0.2868(4) 0.0383(12) Uani 1 1 d . . . H24 H 0.9679 1.3888 0.2460 0.046 Uiso 1 1 calc R . . C25 C 1.0434(4) 1.4053(3) 0.3804(4) 0.0425(13) Uani 1 1 d . . . H25 H 1.0553 1.4760 0.4044 0.051 Uiso 1 1 calc R . . C26 C 1.0791(4) 1.3552(3) 0.4399(3) 0.0354(11) Uani 1 1 d . . . H26 H 1.1169 1.3914 0.5041 0.042 Uiso 1 1 calc R . . C27 C 1.0600(3) 1.2528(3) 0.4063(3) 0.0277(10) Uani 1 1 d . . . H27 H 1.0848 1.2183 0.4473 0.033 Uiso 1 1 calc R . . C28 C 0.9068(3) 1.0341(3) 0.3512(3) 0.0228(9) Uani 1 1 d . . . C29 C 0.8415(3) 1.1007(3) 0.4060(3) 0.0307(10) Uani 1 1 d . . . H29 H 0.8358 1.1636 0.4001 0.037 Uiso 1 1 calc R . . C30 C 0.7849(4) 1.0747(4) 0.4692(3) 0.0399(12) Uani 1 1 d . . . H30 H 0.7402 1.1199 0.5067 0.048 Uiso 1 1 calc R . . C31 C 0.7935(4) 0.9830(4) 0.4778(3) 0.0422(13) Uani 1 1 d . . . H31 H 0.7563 0.9660 0.5224 0.051 Uiso 1 1 calc R . . C32 C 0.8555(4) 0.9169(4) 0.4219(4) 0.0446(13) Uani 1 1 d . . . H32 H 0.8592 0.8532 0.4265 0.054 Uiso 1 1 calc R . . C33 C 0.9128(4) 0.9418(3) 0.3591(3) 0.0362(11) Uani 1 1 d . . . H33 H 0.9564 0.8958 0.3212 0.043 Uiso 1 1 calc R . . C34 C 1.3104(3) 0.8161(3) 0.2518(3) 0.0234(9) Uani 1 1 d . . . C35 C 1.3674(3) 0.9055(3) 0.2601(3) 0.0324(11) Uani 1 1 d . . . H35 H 1.3419 0.9384 0.2179 0.039 Uiso 1 1 calc R . . C38 C 1.4455(4) 0.8088(4) 0.3827(3) 0.0478(14) Uani 1 1 d . . . H38 H 1.4728 0.7756 0.4242 0.057 Uiso 1 1 calc R . . C39 C 1.3504(3) 0.7671(3) 0.3131(3) 0.0300(10) Uani 1 1 d . . . H39 H 1.3125 0.7054 0.3070 0.036 Uiso 1 1 calc R . . C40 C 1.2495(3) 0.6742(3) 0.0563(3) 0.0212(9) Uani 1 1 d . . . C41 C 1.2500(3) 0.6910(3) -0.0287(3) 0.0237(9) Uani 1 1 d . . . H41 H 1.2172 0.7463 -0.0366 0.028 Uiso 1 1 calc R . . C42 C 1.2981(3) 0.6274(3) -0.1031(3) 0.0329(11) Uani 1 1 d . . . H42 H 1.2982 0.6392 -0.1615 0.040 Uiso 1 1 calc R . . C43 C 1.3459(4) 0.5470(3) -0.0912(3) 0.0384(12) Uani 1 1 d . . . H43 H 1.3777 0.5027 -0.1420 0.046 Uiso 1 1 calc R . . C44 C 1.3474(4) 0.5311(3) -0.0060(3) 0.0370(12) Uani 1 1 d . . . H44 H 1.3814 0.4765 0.0021 0.044 Uiso 1 1 calc R . . C45 C 1.2999(3) 0.5939(3) 0.0679(3) 0.0285(10) Uani 1 1 d . . . H45 H 1.3014 0.5825 0.1266 0.034 Uiso 1 1 calc R . . C46 C 1.1034(3) 0.6852(3) 0.1981(3) 0.0207(9) Uani 1 1 d . . . C47 C 1.0475(3) 0.5932(3) 0.1366(3) 0.0270(10) Uani 1 1 d . . . H47 H 1.0646 0.5632 0.0733 0.032 Uiso 1 1 calc R . . C48 C 0.9677(4) 0.5450(3) 0.1662(3) 0.0334(11) Uani 1 1 d . . . H48 H 0.9304 0.4821 0.1231 0.040 Uiso 1 1 calc R . . C49 C 0.9411(4) 0.5871(3) 0.2579(4) 0.0340(11) Uani 1 1 d . . . H49 H 0.8852 0.5543 0.2779 0.041 Uiso 1 1 calc R . . C50 C 0.9976(4) 0.6780(3) 0.3198(3) 0.0350(11) Uani 1 1 d . . . H50 H 0.9812 0.7072 0.3834 0.042 Uiso 1 1 calc R . . C51 C 1.0775(3) 0.7269(3) 0.2905(3) 0.0269(10) Uani 1 1 d . . . H51 H 1.1150 0.7897 0.3339 0.032 Uiso 1 1 calc R . . P1 P 0.83159(8) 0.77633(8) -0.03879(8) 0.0186(2) Uani 1 1 d . . . P2 P 0.98054(9) 1.06585(7) 0.26780(8) 0.0198(2) Uani 1 1 d . . . P3 P 1.19040(8) 0.76121(7) 0.15487(8) 0.0188(2) Uani 1 1 d . . . S1 S 0.98279(8) 0.72764(7) -0.02354(7) 0.0219(2) Uani 1 1 d . . . S2 S 1.12656(8) 1.00420(7) 0.25637(8) 0.0237(2) Uani 1 1 d . . . Pd1 Pd 1.06687(2) 0.86501(2) 0.11353(2) 0.01724(9) Uani 1 1 d . . . C36 C 1.4621(4) 0.9466(4) 0.3306(4) 0.0530(15) Uani 1 1 d . . . H36 H 1.5010 1.0080 0.3370 0.064 Uiso 1 1 calc R . . C37 C 1.4995(4) 0.8977(5) 0.3912(4) 0.0567(16) Uani 1 1 d . . . H37 H 1.5637 0.9265 0.4395 0.068 Uiso 1 1 calc R . . C52 C 0.3672(5) 0.6455(4) 0.5620(5) 0.0690(18) Uani 1 1 d . . . H52A H 0.3531 0.5966 0.5926 0.083 Uiso 1 1 calc R . . H52B H 0.4280 0.6247 0.5242 0.083 Uiso 1 1 calc R . . B1 B 0.6442(5) 0.6099(4) 0.3778(4) 0.0393(14) Uani 1 1 d . . . F1 F 0.5754(2) 0.6077(2) 0.29541(19) 0.0524(8) Uani 1 1 d . . . F2 F 0.5783(3) 0.6015(3) 0.4426(2) 0.0694(10) Uani 1 1 d . . . F3 F 0.7063(3) 0.5302(2) 0.3552(3) 0.0740(10) Uani 1 1 d . . . F4 F 0.7148(3) 0.6970(3) 0.4171(3) 0.0844(12) Uani 1 1 d . . . Cl1 Cl 0.24517(14) 0.64547(12) 0.48309(15) 0.0875(6) Uani 1 1 d . . . Cl2 Cl 0.40918(16) 0.76352(15) 0.65245(15) 0.1050(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.021(2) 0.017(2) 0.021(2) 0.0090(18) 0.0050(18) 0.0014(17) C2 0.019(2) 0.021(2) 0.028(2) 0.013(2) 0.0036(19) 0.0011(17) C3 0.025(2) 0.026(2) 0.036(3) 0.018(2) 0.000(2) 0.0023(19) C4 0.024(2) 0.032(3) 0.046(3) 0.024(2) -0.002(2) 0.004(2) C5 0.021(2) 0.029(3) 0.051(3) 0.018(2) 0.008(2) 0.010(2) C6 0.028(2) 0.028(2) 0.032(3) 0.008(2) 0.007(2) 0.008(2) C7 0.021(2) 0.025(2) 0.027(2) 0.016(2) 0.0059(19) 0.0032(18) C8 0.021(2) 0.018(2) 0.021(2) 0.0060(18) 0.0045(18) 0.0025(17) C9 0.018(2) 0.018(2) 0.022(2) 0.0087(18) 0.0045(18) -0.0011(17) C10 0.021(2) 0.025(2) 0.020(2) 0.0056(19) 0.0019(18) 0.0051(18) C11 0.026(2) 0.031(2) 0.021(2) 0.009(2) 0.0045(19) 0.0018(19) C12 0.038(3) 0.051(3) 0.020(2) 0.015(2) -0.001(2) 0.008(2) C13 0.043(3) 0.046(3) 0.026(3) 0.001(3) -0.008(2) 0.006(3) C14 0.058(4) 0.032(3) 0.041(3) 0.005(3) -0.017(3) -0.016(2) C15 0.046(3) 0.033(3) 0.031(3) 0.014(2) -0.007(2) -0.009(2) C16 0.022(2) 0.017(2) 0.019(2) 0.0060(18) 0.0072(18) 0.0009(17) C17 0.029(2) 0.041(3) 0.035(3) 0.024(2) 0.007(2) 0.007(2) C18 0.026(2) 0.045(3) 0.047(3) 0.023(3) 0.010(2) 0.007(2) C19 0.036(3) 0.036(3) 0.038(3) 0.018(2) 0.019(2) 0.006(2) C20 0.039(3) 0.038(3) 0.026(3) 0.016(2) 0.006(2) 0.002(2) C21 0.025(2) 0.030(2) 0.023(2) 0.013(2) 0.0030(19) 0.0051(19) C22 0.025(2) 0.018(2) 0.023(2) 0.0071(19) 0.0098(19) 0.0047(18) C23 0.038(3) 0.024(2) 0.026(2) 0.008(2) 0.002(2) 0.002(2) C24 0.051(3) 0.027(3) 0.043(3) 0.020(2) 0.008(3) 0.006(2) C25 0.055(3) 0.017(2) 0.050(3) 0.006(2) 0.012(3) 0.002(2) C26 0.040(3) 0.031(3) 0.029(3) 0.003(2) 0.008(2) 0.001(2) C27 0.035(3) 0.024(2) 0.023(2) 0.009(2) 0.005(2) 0.003(2) C28 0.026(2) 0.024(2) 0.019(2) 0.0090(19) 0.0036(19) -0.0003(18) C29 0.035(3) 0.028(2) 0.030(3) 0.010(2) 0.011(2) 0.005(2) C30 0.030(3) 0.052(3) 0.032(3) 0.007(3) 0.013(2) 0.000(2) C31 0.034(3) 0.067(4) 0.027(3) 0.024(3) 0.001(2) -0.012(3) C32 0.051(3) 0.046(3) 0.050(3) 0.033(3) 0.009(3) 0.000(3) C33 0.040(3) 0.036(3) 0.040(3) 0.020(2) 0.014(2) 0.008(2) C34 0.017(2) 0.027(2) 0.021(2) 0.001(2) 0.0037(18) 0.0059(18) C35 0.026(2) 0.030(3) 0.037(3) 0.008(2) 0.007(2) 0.001(2) C38 0.035(3) 0.075(4) 0.026(3) 0.010(3) 0.000(2) 0.019(3) C39 0.026(2) 0.041(3) 0.024(2) 0.011(2) 0.004(2) 0.013(2) C40 0.019(2) 0.017(2) 0.025(2) 0.0034(19) 0.0061(18) 0.0029(17) C41 0.022(2) 0.028(2) 0.022(2) 0.009(2) 0.0043(19) -0.0006(18) C42 0.028(3) 0.042(3) 0.028(3) 0.011(2) 0.010(2) 0.000(2) C43 0.038(3) 0.035(3) 0.033(3) -0.001(2) 0.016(2) 0.000(2) C44 0.042(3) 0.027(3) 0.044(3) 0.011(2) 0.018(2) 0.015(2) C45 0.032(3) 0.027(2) 0.030(3) 0.012(2) 0.012(2) 0.008(2) C46 0.022(2) 0.022(2) 0.020(2) 0.0099(19) 0.0032(18) 0.0063(18) C47 0.030(2) 0.024(2) 0.027(3) 0.008(2) 0.008(2) 0.0024(19) C48 0.035(3) 0.025(2) 0.045(3) 0.017(2) 0.013(2) 0.001(2) C49 0.033(3) 0.031(3) 0.050(3) 0.024(3) 0.016(2) 0.006(2) C50 0.045(3) 0.038(3) 0.032(3) 0.018(2) 0.024(2) 0.014(2) C51 0.030(2) 0.023(2) 0.029(3) 0.010(2) 0.010(2) 0.0057(19) P1 0.0202(6) 0.0193(6) 0.0164(6) 0.0071(5) 0.0024(5) 0.0017(4) P2 0.0241(6) 0.0160(5) 0.0185(6) 0.0045(5) 0.0051(5) 0.0039(4) P3 0.0200(6) 0.0176(5) 0.0188(6) 0.0061(5) 0.0040(5) 0.0033(4) S1 0.0222(5) 0.0200(5) 0.0205(6) 0.0038(5) 0.0030(5) 0.0048(4) S2 0.0219(6) 0.0223(6) 0.0221(6) 0.0032(5) 0.0012(5) 0.0048(4) Pd1 0.01852(17) 0.01613(17) 0.01674(17) 0.00537(13) 0.00331(13) 0.00337(12) C36 0.032(3) 0.047(3) 0.060(4) -0.003(3) 0.007(3) -0.008(3) C37 0.025(3) 0.080(4) 0.037(3) -0.007(3) -0.007(2) 0.000(3) C52 0.072(4) 0.053(4) 0.093(5) 0.031(4) 0.029(4) 0.027(3) B1 0.049(4) 0.044(4) 0.029(3) 0.019(3) 0.005(3) 0.002(3) F1 0.072(2) 0.0568(19) 0.0327(16) 0.0226(15) 0.0059(15) 0.0062(16) F2 0.067(2) 0.110(3) 0.0367(18) 0.0309(19) 0.0195(17) 0.0039(19) F3 0.077(2) 0.070(2) 0.088(3) 0.037(2) 0.026(2) 0.0316(19) F4 0.085(3) 0.069(2) 0.088(3) 0.035(2) -0.021(2) -0.033(2) Cl1 0.0756(12) 0.0537(10) 0.1171(16) 0.0151(10) 0.0074(11) 0.0103(9) Cl2 0.0837(13) 0.1003(15) 0.0945(15) -0.0112(12) 0.0110(11) 0.0446(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.515(5) . ? C1 C9 1.524(5) . ? C1 P1 1.826(4) . ? C1 H1 1.0000 . ? C2 C3 1.389(5) . ? C2 C7 1.403(6) . ? C3 C4 1.395(6) . ? C3 H3 0.9500 . ? C4 C5 1.379(6) . ? C4 H4 0.9500 . ? C5 C6 1.388(6) . ? C5 H5 0.9500 . ? C6 C7 1.399(5) . ? C6 H6 0.9500 . ? C7 C8 1.479(5) . ? C8 C9 1.355(5) . ? C8 P2 1.780(4) . ? C9 Pd1 2.009(4) . ? C10 C11 1.395(5) . ? C10 C15 1.401(6) . ? C10 P1 1.792(4) . ? C11 C12 1.380(6) . ? C11 H11 0.9500 . ? C12 C13 1.376(6) . ? C12 H12 0.9500 . ? C13 C14 1.369(6) . ? C13 H13 0.9500 . ? C14 C15 1.371(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.385(5) . ? C16 C17 1.401(5) . ? C16 P1 1.796(4) . ? C17 C18 1.382(6) . ? C17 H17 0.9500 . ? C18 C19 1.388(6) . ? C18 H18 0.9500 . ? C19 C20 1.382(6) . ? C19 H19 0.9500 . ? C20 C21 1.390(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.391(5) . ? C22 C27 1.394(5) . ? C22 P2 1.798(4) . ? C23 C24 1.388(6) . ? C23 H23 0.9500 . ? C24 C25 1.373(6) . ? C24 H24 0.9500 . ? C25 C26 1.377(6) . ? C25 H25 0.9500 . ? C26 C27 1.376(6) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.385(5) . ? C28 C29 1.392(6) . ? C28 P2 1.806(4) . ? C29 C30 1.386(6) . ? C29 H29 0.9500 . ? C30 C31 1.386(6) . ? C30 H30 0.9500 . ? C31 C32 1.368(7) . ? C31 H31 0.9500 . ? C32 C33 1.379(6) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.388(6) . ? C34 C39 1.401(5) . ? C34 P3 1.826(4) . ? C35 C36 1.391(6) . ? C35 H35 0.9500 . ? C38 C37 1.367(7) . ? C38 C39 1.389(6) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.381(5) . ? C40 C45 1.397(5) . ? C40 P3 1.831(4) . ? C41 C42 1.394(6) . ? C41 H41 0.9500 . ? C42 C43 1.385(6) . ? C42 H42 0.9500 . ? C43 C44 1.374(6) . ? C43 H43 0.9500 . ? C44 C45 1.380(6) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C51 1.389(5) . ? C46 C47 1.389(5) . ? C46 P3 1.822(4) . ? C47 C48 1.376(6) . ? C47 H47 0.9500 . ? C48 C49 1.384(6) . ? C48 H48 0.9500 . ? C49 C50 1.382(6) . ? C49 H49 0.9500 . ? C50 C51 1.379(6) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? P1 S1 2.0226(14) . ? P2 S2 2.0366(14) . ? P3 Pd1 2.3593(10) . ? S1 Pd1 2.3414(11) . ? S2 Pd1 2.3414(11) . ? C36 C37 1.383(7) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C52 Cl2 1.750(6) . ? C52 Cl1 1.768(6) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? B1 F4 1.371(6) . ? B1 F2 1.377(6) . ? B1 F3 1.381(6) . ? B1 F1 1.383(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C9 104.7(3) . . ? C2 C1 P1 118.5(3) . . ? C9 C1 P1 101.4(2) . . ? C2 C1 H1 110.5 . . ? C9 C1 H1 110.5 . . ? P1 C1 H1 110.5 . . ? C3 C2 C7 121.2(4) . . ? C3 C2 C1 130.7(4) . . ? C7 C2 C1 108.1(3) . . ? C2 C3 C4 118.1(4) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C5 C4 C3 120.9(4) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 121.7(4) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C7 118.1(4) . . ? C5 C6 H6 121.0 . . ? C7 C6 H6 121.0 . . ? C6 C7 C2 120.1(4) . . ? C6 C7 C8 132.1(4) . . ? C2 C7 C8 107.8(3) . . ? C9 C8 C7 111.5(4) . . ? C9 C8 P2 116.0(3) . . ? C7 C8 P2 132.5(3) . . ? C8 C9 C1 107.8(3) . . ? C8 C9 Pd1 125.9(3) . . ? C1 C9 Pd1 124.6(3) . . ? C11 C10 C15 119.5(4) . . ? C11 C10 P1 122.6(3) . . ? C15 C10 P1 117.9(3) . . ? C12 C11 C10 119.7(4) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C11 120.0(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 120.8(4) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.4(5) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C10 119.7(4) . . ? C14 C15 H15 120.1 . . ? C10 C15 H15 120.1 . . ? C21 C16 C17 119.4(4) . . ? C21 C16 P1 122.0(3) . . ? C17 C16 P1 118.6(3) . . ? C18 C17 C16 119.9(4) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.2(4) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 120.0(4) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.1(4) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C16 C21 C20 120.3(4) . . ? C16 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C27 119.8(4) . . ? C23 C22 P2 120.2(3) . . ? C27 C22 P2 120.0(3) . . ? C24 C23 C22 119.3(4) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C25 C24 C23 120.4(4) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.5(4) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C27 C26 C25 120.0(4) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C22 120.0(4) . . ? C26 C27 H27 120.0 . . ? C22 C27 H27 120.0 . . ? C33 C28 C29 119.7(4) . . ? C33 C28 P2 119.9(3) . . ? C29 C28 P2 120.4(3) . . ? C30 C29 C28 119.6(4) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C31 C30 C29 120.1(4) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 C30 120.0(4) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.6(4) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C28 120.1(4) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? C35 C34 C39 119.5(4) . . ? C35 C34 P3 118.6(3) . . ? C39 C34 P3 121.7(3) . . ? C34 C35 C36 119.7(4) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C37 C38 C39 119.6(5) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C38 C39 C34 120.1(4) . . ? C38 C39 H39 119.9 . . ? C34 C39 H39 119.9 . . ? C41 C40 C45 119.3(4) . . ? C41 C40 P3 119.8(3) . . ? C45 C40 P3 120.8(3) . . ? C40 C41 C42 120.4(4) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C43 C42 C41 119.5(4) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C44 C43 C42 120.2(4) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 120.5(4) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C44 C45 C40 120.0(4) . . ? C44 C45 H45 120.0 . . ? C40 C45 H45 120.0 . . ? C51 C46 C47 118.3(4) . . ? C51 C46 P3 119.0(3) . . ? C47 C46 P3 121.8(3) . . ? C48 C47 C46 120.8(4) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C47 C48 C49 120.7(4) . . ? C47 C48 H48 119.6 . . ? C49 C48 H48 119.6 . . ? C50 C49 C48 118.6(4) . . ? C50 C49 H49 120.7 . . ? C48 C49 H49 120.7 . . ? C51 C50 C49 121.0(4) . . ? C51 C50 H50 119.5 . . ? C49 C50 H50 119.5 . . ? C50 C51 C46 120.5(4) . . ? C50 C51 H51 119.8 . . ? C46 C51 H51 119.8 . . ? C10 P1 C16 106.87(19) . . ? C10 P1 C1 112.45(18) . . ? C16 P1 C1 108.91(18) . . ? C10 P1 S1 110.86(13) . . ? C16 P1 S1 114.26(13) . . ? C1 P1 S1 103.60(13) . . ? C8 P2 C22 111.20(18) . . ? C8 P2 C28 111.10(19) . . ? C22 P2 C28 106.79(19) . . ? C8 P2 S2 104.76(13) . . ? C22 P2 S2 111.30(13) . . ? C28 P2 S2 111.78(14) . . ? C46 P3 C34 105.20(18) . . ? C46 P3 C40 106.42(18) . . ? C34 P3 C40 103.67(18) . . ? C46 P3 Pd1 103.52(12) . . ? C34 P3 Pd1 119.86(13) . . ? C40 P3 Pd1 116.94(13) . . ? P1 S1 Pd1 97.17(5) . . ? P2 S2 Pd1 98.89(5) . . ? C9 Pd1 S1 87.99(11) . . ? C9 Pd1 S2 86.86(11) . . ? S1 Pd1 S2 172.14(4) . . ? C9 Pd1 P3 171.76(11) . . ? S1 Pd1 P3 88.96(4) . . ? S2 Pd1 P3 95.33(4) . . ? C37 C36 C35 119.9(5) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C38 C37 C36 121.1(5) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? Cl2 C52 Cl1 111.5(3) . . ? Cl2 C52 H52A 109.3 . . ? Cl1 C52 H52A 109.3 . . ? Cl2 C52 H52B 109.3 . . ? Cl1 C52 H52B 109.3 . . ? H52A C52 H52B 108.0 . . ? F4 B1 F2 110.8(5) . . ? F4 B1 F3 109.2(5) . . ? F2 B1 F3 108.4(4) . . ? F4 B1 F1 110.1(4) . . ? F2 B1 F1 108.3(4) . . ? F3 B1 F1 110.1(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.096 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.092 #===END data_1-Me _database_code_depnum_ccdc_archive 'CCDC 800700' #TrackingRef '- RX_Bourissou-DT-pincer.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 P2 S2' _chemical_formula_weight 562.62 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 9.3107(2) _cell_length_b 15.8384(3) _cell_length_c 20.4529(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.5710(10) _cell_angle_gamma 90.00 _cell_volume 2890.85(10) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4864 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 25.27 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.317 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.925 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33762 _diffrn_reflns_av_R_equivalents 0.0904 _diffrn_reflns_av_sigmaI/netI 0.0836 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.66 _reflns_number_total 6721 _reflns_number_gt 4104 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6721 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.885 _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 S1 S 0.73866(7) 0.53981(3) 0.43650(3) 0.04039(16) Uani 1 1 d . . . S2 S 1.04281(6) 0.96784(4) 0.41088(3) 0.03469(15) Uani 1 1 d . . . P1 P 0.74172(6) 0.66062(3) 0.45662(3) 0.02734(14) Uani 1 1 d . . . P2 P 0.87425(6) 0.92852(3) 0.33559(3) 0.02490(13) Uani 1 1 d . . . C1 C 0.5684(2) 0.69658(12) 0.47082(10) 0.0263(5) Uani 1 1 d . . . C2 C 0.4988(2) 0.64460(13) 0.50778(10) 0.0327(5) Uani 1 1 d . . . H2 H 0.5407 0.5910 0.5233 0.039 Uiso 1 1 calc R . . C3 C 0.3694(3) 0.67093(14) 0.52177(11) 0.0384(6) Uani 1 1 d . . . H3 H 0.3227 0.6354 0.5471 0.046 Uiso 1 1 calc R . . C4 C 0.3072(2) 0.74882(15) 0.49906(10) 0.0347(5) Uani 1 1 d . . . H4 H 0.2187 0.7669 0.5093 0.042 Uiso 1 1 calc R . . C5 C 0.3735(2) 0.79964(15) 0.46181(11) 0.0375(6) Uani 1 1 d . . . H5 H 0.3295 0.8525 0.4454 0.045 Uiso 1 1 calc R . . C6 C 0.5042(2) 0.77468(13) 0.44784(10) 0.0335(5) Uani 1 1 d . . . H6 H 0.5502 0.8107 0.4226 0.040 Uiso 1 1 calc R . . C7 C 0.8883(2) 0.69199(13) 0.53242(10) 0.0279(5) Uani 1 1 d . . . C8 C 0.9957(2) 0.63337(14) 0.56564(11) 0.0342(5) Uani 1 1 d . . . H8 H 0.9921 0.5773 0.5488 0.041 Uiso 1 1 calc R . . C9 C 1.1076(3) 0.65694(16) 0.62305(11) 0.0435(6) Uani 1 1 d . . . H9 H 1.1798 0.6165 0.6460 0.052 Uiso 1 1 calc R . . C10 C 1.1156(3) 0.73779(17) 0.64731(11) 0.0435(6) Uani 1 1 d . . . H10 H 1.1943 0.7535 0.6863 0.052 Uiso 1 1 calc R . . C11 C 1.0090(3) 0.79684(16) 0.61503(11) 0.0450(6) Uani 1 1 d . . . H11 H 1.0143 0.8528 0.6322 0.054 Uiso 1 1 calc R . . C12 C 0.8946(3) 0.77430(14) 0.55768(11) 0.0372(6) Uani 1 1 d . . . H12 H 0.8210 0.8146 0.5357 0.045 Uiso 1 1 calc R . . C13 C 0.7737(2) 0.72385(12) 0.38850(10) 0.0251(5) Uani 1 1 d . . . C14 C 0.8911(2) 0.77478(12) 0.39383(10) 0.0260(5) Uani 1 1 d . . . H14 H 0.9652 0.7867 0.4355 0.031 Uiso 1 1 calc R . . C15 C 0.8916(2) 0.81117(12) 0.32532(10) 0.0262(5) Uani 1 1 d . . . C16 C 0.7562(2) 0.76865(12) 0.27797(10) 0.0278(5) Uani 1 1 d . . . C17 C 0.7051(3) 0.76968(13) 0.20732(11) 0.0374(6) Uani 1 1 d . . . H17 H 0.7547 0.8023 0.1814 0.045 Uiso 1 1 calc R . . C18 C 0.5796(3) 0.72190(15) 0.17543(12) 0.0466(7) Uani 1 1 d . . . H18 H 0.5429 0.7218 0.1271 0.056 Uiso 1 1 calc R . . C19 C 0.5071(3) 0.67427(15) 0.21333(12) 0.0459(6) Uani 1 1 d . . . H19 H 0.4204 0.6429 0.1904 0.055 Uiso 1 1 calc R . . C20 C 0.5586(2) 0.67141(13) 0.28403(11) 0.0360(5) Uani 1 1 d . . . H20 H 0.5090 0.6384 0.3097 0.043 Uiso 1 1 calc R . . C21 C 0.6852(2) 0.71847(12) 0.31598(10) 0.0274(5) Uani 1 1 d . . . C22 C 1.0361(2) 0.79396(14) 0.30631(11) 0.0353(5) Uani 1 1 d . . . H22A H 1.0510 0.7329 0.3042 0.053 Uiso 1 1 calc R . . H22B H 1.1210 0.8189 0.3408 0.053 Uiso 1 1 calc R . . H22C H 1.0289 0.8191 0.2617 0.053 Uiso 1 1 calc R . . C23 C 0.6937(2) 0.94865(12) 0.35050(10) 0.0263(5) Uani 1 1 d . . . C24 C 0.5566(2) 0.92051(13) 0.30721(11) 0.0312(5) Uani 1 1 d . . . H24 H 0.5558 0.8865 0.2689 0.037 Uiso 1 1 calc R . . C25 C 0.4233(2) 0.94156(14) 0.31950(12) 0.0382(6) Uani 1 1 d . . . H25 H 0.3311 0.9229 0.2893 0.046 Uiso 1 1 calc R . . C26 C 0.4233(3) 0.99015(15) 0.37618(13) 0.0429(6) Uani 1 1 d . . . H26 H 0.3316 1.0051 0.3848 0.052 Uiso 1 1 calc R . . C27 C 0.5584(3) 1.01641(15) 0.41984(12) 0.0413(6) Uani 1 1 d . . . H27 H 0.5588 1.0488 0.4590 0.050 Uiso 1 1 calc R . . C28 C 0.6919(3) 0.99646(14) 0.40766(11) 0.0341(5) Uani 1 1 d . . . H28 H 0.7835 1.0152 0.4382 0.041 Uiso 1 1 calc R . . C29 C 0.8712(2) 0.97926(12) 0.25483(10) 0.0280(5) Uani 1 1 d . . . C30 C 0.7413(3) 0.99163(14) 0.20141(11) 0.0393(6) Uani 1 1 d . . . H30 H 0.6476 0.9730 0.2059 0.047 Uiso 1 1 calc R . . C31 C 0.7479(3) 1.03076(15) 0.14214(11) 0.0475(7) Uani 1 1 d . . . H31 H 0.6585 1.0396 0.1062 0.057 Uiso 1 1 calc R . . C32 C 0.8838(3) 1.05713(15) 0.13467(12) 0.0468(7) Uani 1 1 d . . . H32 H 0.8880 1.0827 0.0932 0.056 Uiso 1 1 calc R . . C33 C 1.0132(3) 1.04638(15) 0.18730(12) 0.0454(6) Uani 1 1 d . . . H33 H 1.1066 1.0652 0.1825 0.054 Uiso 1 1 calc R . . C34 C 1.0062(3) 1.00792(14) 0.24730(11) 0.0364(5) Uani 1 1 d . . . H34 H 1.0953 1.0011 0.2837 0.044 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 S1 0.0544(4) 0.0210(3) 0.0519(4) -0.0010(3) 0.0250(3) 0.0034(3) S2 0.0287(3) 0.0416(4) 0.0310(3) -0.0013(2) 0.0040(2) -0.0033(3) P1 0.0329(3) 0.0208(3) 0.0318(3) 0.0034(2) 0.0149(2) 0.0030(2) P2 0.0241(3) 0.0275(3) 0.0242(3) 0.0026(2) 0.0085(2) 0.0005(2) C1 0.0302(12) 0.0241(11) 0.0264(10) -0.0011(9) 0.0109(9) -0.0009(9) C2 0.0412(13) 0.0252(12) 0.0366(12) -0.0009(9) 0.0189(10) 0.0001(10) C3 0.0413(14) 0.0380(14) 0.0422(13) -0.0037(11) 0.0220(11) -0.0121(11) C4 0.0243(11) 0.0452(15) 0.0359(12) -0.0070(11) 0.0107(10) -0.0001(11) C5 0.0333(13) 0.0389(14) 0.0398(13) 0.0031(11) 0.0098(11) 0.0101(11) C6 0.0360(13) 0.0297(12) 0.0395(12) 0.0075(10) 0.0182(10) 0.0029(10) C7 0.0328(12) 0.0281(12) 0.0277(11) 0.0049(9) 0.0164(9) 0.0003(10) C8 0.0348(13) 0.0346(13) 0.0380(12) 0.0090(10) 0.0181(10) 0.0071(10) C9 0.0376(14) 0.0564(17) 0.0380(13) 0.0149(12) 0.0134(11) 0.0080(12) C10 0.0397(14) 0.0612(18) 0.0311(12) 0.0066(12) 0.0127(11) -0.0091(13) C11 0.0568(16) 0.0408(15) 0.0392(14) -0.0036(11) 0.0164(12) -0.0075(13) C12 0.0447(14) 0.0296(13) 0.0383(13) 0.0045(10) 0.0134(11) 0.0044(11) C13 0.0284(11) 0.0221(11) 0.0284(10) 0.0020(9) 0.0138(9) 0.0036(9) C14 0.0270(11) 0.0275(12) 0.0242(10) 0.0039(9) 0.0084(9) 0.0049(9) C15 0.0277(11) 0.0260(12) 0.0264(11) 0.0033(8) 0.0100(9) 0.0020(9) C16 0.0319(12) 0.0241(11) 0.0277(11) -0.0007(9) 0.0093(9) 0.0077(9) C17 0.0513(15) 0.0294(12) 0.0306(12) 0.0012(10) 0.0100(11) 0.0043(11) C18 0.0610(17) 0.0409(15) 0.0297(12) -0.0061(11) -0.0001(12) 0.0053(13) C19 0.0436(15) 0.0375(14) 0.0473(14) -0.0099(12) -0.0022(12) -0.0014(12) C20 0.0362(13) 0.0270(12) 0.0444(13) -0.0040(10) 0.0111(11) -0.0006(10) C21 0.0286(11) 0.0234(11) 0.0314(11) -0.0017(9) 0.0106(9) 0.0045(9) C22 0.0352(13) 0.0363(13) 0.0407(13) 0.0059(10) 0.0207(11) 0.0075(10) C23 0.0258(11) 0.0263(12) 0.0296(11) 0.0062(9) 0.0123(9) 0.0025(9) C24 0.0302(12) 0.0283(12) 0.0365(12) 0.0031(9) 0.0115(10) 0.0021(10) C25 0.0248(12) 0.0358(14) 0.0545(14) 0.0072(11) 0.0120(11) 0.0023(10) C26 0.0354(14) 0.0394(14) 0.0641(16) 0.0149(12) 0.0304(13) 0.0094(11) C27 0.0518(16) 0.0395(15) 0.0420(13) 0.0007(11) 0.0282(12) 0.0026(12) C28 0.0372(13) 0.0363(13) 0.0318(12) 0.0013(10) 0.0145(10) 0.0016(11) C29 0.0359(12) 0.0233(11) 0.0273(10) 0.0036(9) 0.0129(9) 0.0033(9) C30 0.0415(14) 0.0395(14) 0.0357(12) 0.0064(10) 0.0090(11) -0.0036(11) C31 0.0618(18) 0.0478(16) 0.0285(12) 0.0102(11) 0.0057(12) 0.0029(14) C32 0.078(2) 0.0344(14) 0.0357(13) 0.0090(11) 0.0278(14) 0.0046(13) C33 0.0550(16) 0.0383(14) 0.0556(16) 0.0103(12) 0.0362(14) 0.0004(12) C34 0.0350(13) 0.0375(13) 0.0406(13) 0.0068(10) 0.0171(10) 0.0032(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 P1 1.9558(8) . ? S2 P2 1.9605(7) . ? P1 C13 1.808(2) . ? P1 C1 1.811(2) . ? P1 C7 1.818(2) . ? P2 C23 1.821(2) . ? P2 C29 1.830(2) . ? P2 C15 1.883(2) . ? C1 C6 1.396(3) . ? C1 C2 1.396(3) . ? C2 C3 1.380(3) . ? C2 H2 0.9500 . ? C3 C4 1.386(3) . ? C3 H3 0.9500 . ? C4 C5 1.371(3) . ? C4 H4 0.9500 . ? C5 C6 1.384(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.392(3) . ? C7 C12 1.397(3) . ? C8 C9 1.380(3) . ? C8 H8 0.9500 . ? C9 C10 1.368(3) . ? C9 H9 0.9500 . ? C10 C11 1.386(3) . ? C10 H10 0.9500 . ? C11 C12 1.388(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.338(3) . ? C13 C21 1.479(3) . ? C14 C15 1.516(3) . ? C14 H14 0.9500 . ? C15 C16 1.511(3) . ? C15 C22 1.528(3) . ? C16 C17 1.386(3) . ? C16 C21 1.402(3) . ? C17 C18 1.389(3) . ? C17 H17 0.9500 . ? C18 C19 1.387(3) . ? C18 H18 0.9500 . ? C19 C20 1.388(3) . ? C19 H19 0.9500 . ? C20 C21 1.390(3) . ? C20 H20 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C28 1.397(3) . ? C23 C24 1.402(3) . ? C24 C25 1.376(3) . ? C24 H24 0.9500 . ? C25 C26 1.391(3) . ? C25 H25 0.9500 . ? C26 C27 1.383(3) . ? C26 H26 0.9500 . ? C27 C28 1.373(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.386(3) . ? C29 C30 1.393(3) . ? C30 C31 1.378(3) . ? C30 H30 0.9500 . ? C31 C32 1.382(3) . ? C31 H31 0.9500 . ? C32 C33 1.378(3) . ? C32 H32 0.9500 . ? C33 C34 1.388(3) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? 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 C13 P1 C1 107.42(9) . . ? C13 P1 C7 104.90(9) . . ? C1 P1 C7 105.29(9) . . ? C13 P1 S1 112.05(7) . . ? C1 P1 S1 112.41(7) . . ? C7 P1 S1 114.15(7) . . ? C23 P2 C29 107.27(9) . . ? C23 P2 C15 107.71(9) . . ? C29 P2 C15 108.22(9) . . ? C23 P2 S2 112.55(7) . . ? C29 P2 S2 111.87(7) . . ? C15 P2 S2 109.05(6) . . ? C6 C1 C2 119.0(2) . . ? C6 C1 P1 122.70(16) . . ? C2 C1 P1 118.26(16) . . ? C3 C2 C1 120.1(2) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.4(2) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.8(2) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.6(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 120.1(2) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C8 C7 C12 119.5(2) . . ? C8 C7 P1 119.62(16) . . ? C12 C7 P1 120.83(16) . . ? C9 C8 C7 119.9(2) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C10 C9 C8 120.8(2) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 120.1(2) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 120.1(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 119.6(2) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C14 C13 C21 108.95(17) . . ? C14 C13 P1 125.56(15) . . ? C21 C13 P1 125.01(15) . . ? C13 C14 C15 111.81(17) . . ? C13 C14 H14 124.1 . . ? C15 C14 H14 124.1 . . ? C16 C15 C14 101.60(16) . . ? C16 C15 C22 113.06(17) . . ? C14 C15 C22 113.72(16) . . ? C16 C15 P2 115.41(13) . . ? C14 C15 P2 104.43(13) . . ? C22 C15 P2 108.31(14) . . ? C17 C16 C21 120.58(19) . . ? C17 C16 C15 129.7(2) . . ? C21 C16 C15 109.64(17) . . ? C16 C17 C18 118.4(2) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C19 C18 C17 120.8(2) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 121.4(2) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C19 C20 C21 117.8(2) . . ? C19 C20 H20 121.1 . . ? C21 C20 H20 121.1 . . ? C20 C21 C16 120.91(19) . . ? C20 C21 C13 131.1(2) . . ? C16 C21 C13 107.92(17) . . ? C15 C22 H22A 109.5 . . ? C15 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C15 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 118.4(2) . . ? C28 C23 P2 117.82(16) . . ? C24 C23 P2 123.80(16) . . ? C25 C24 C23 120.9(2) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 120.0(2) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 119.3(2) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C28 C27 C26 121.2(2) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C23 120.3(2) . . ? C27 C28 H28 119.9 . . ? C23 C28 H28 119.9 . . ? C34 C29 C30 118.6(2) . . ? C34 C29 P2 117.58(15) . . ? C30 C29 P2 123.80(17) . . ? C31 C30 C29 120.4(2) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 120.3(2) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C33 C32 C31 120.0(2) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 119.6(2) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C29 C34 C33 121.0(2) . . ? C29 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.427 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.057 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 800701' #TrackingRef '- RX_Bourissou-DT-pincer.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H29 Cl3 P2 Pd S2' _chemical_formula_weight 788.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 9.4787(3) _cell_length_b 33.9812(9) _cell_length_c 10.6863(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.622(2) _cell_angle_gamma 90.00 _cell_volume 3371.46(17) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 2916 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 20.42 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 1.032 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.615085 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35458 _diffrn_reflns_av_R_equivalents 0.1307 _diffrn_reflns_av_sigmaI/netI 0.1146 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 5.17 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6823 _reflns_number_gt 3913 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+5.5705P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6823 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1236 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1155 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 0.58418(5) 0.365653(13) 0.42491(4) 0.02290(13) Uani 1 1 d . . . Cl1 Cl 0.63204(18) 0.39144(5) 0.23076(14) 0.0403(4) Uani 1 1 d . . . P1 P 0.52475(16) 0.41927(4) 0.66952(14) 0.0241(3) Uani 1 1 d . . . P2 P 0.42831(15) 0.28459(4) 0.47511(14) 0.0221(3) Uani 1 1 d . . . S1 S 0.61245(18) 0.42838(4) 0.51417(15) 0.0324(4) Uani 1 1 d . . . S2 S 0.52563(16) 0.30320(4) 0.33476(14) 0.0307(4) Uani 1 1 d . . . C1 C 0.5541(5) 0.34591(15) 0.5900(5) 0.0192(12) Uani 1 1 d . . . C2 C 0.5164(5) 0.36747(16) 0.6856(5) 0.0209(11) Uani 1 1 d . . . C3 C 0.5464(5) 0.30253(15) 0.6225(5) 0.0200(12) Uani 1 1 d . . . C4 C 0.6943(6) 0.28181(17) 0.6419(5) 0.0288(14) Uani 1 1 d . . . H4A H 0.7630 0.2955 0.7085 0.043 Uiso 1 1 calc R . . H4B H 0.7295 0.2823 0.5617 0.043 Uiso 1 1 calc R . . H4C H 0.6843 0.2544 0.6678 0.043 Uiso 1 1 calc R . . C5 C 0.4909(5) 0.30262(15) 0.7466(5) 0.0182(12) Uani 1 1 d . . . C6 C 0.4626(6) 0.27154(16) 0.8226(5) 0.0257(13) Uani 1 1 d . . . H6 H 0.4720 0.2450 0.7972 0.031 Uiso 1 1 calc R . . C7 C 0.4201(6) 0.28026(18) 0.9366(6) 0.0304(14) Uani 1 1 d . . . H7 H 0.4003 0.2595 0.9900 0.036 Uiso 1 1 calc R . . C8 C 0.4062(6) 0.31907(19) 0.9735(6) 0.0326(15) Uani 1 1 d . . . H8 H 0.3754 0.3244 1.0511 0.039 Uiso 1 1 calc R . . C9 C 0.4362(6) 0.34998(17) 0.8993(5) 0.0285(14) Uani 1 1 d . . . H9 H 0.4291 0.3764 0.9265 0.034 Uiso 1 1 calc R . . C10 C 0.4771(5) 0.34191(16) 0.7840(5) 0.0228(13) Uani 1 1 d . . . C11 C 0.6351(6) 0.44099(15) 0.8080(5) 0.0249(13) Uani 1 1 d . . . C12 C 0.7822(6) 0.44560(17) 0.8145(6) 0.0329(15) Uani 1 1 d . . . H12 H 0.8226 0.4392 0.7426 0.040 Uiso 1 1 calc R . . C13 C 0.8701(7) 0.45947(19) 0.9250(7) 0.0438(17) Uani 1 1 d . . . H13 H 0.9705 0.4622 0.9286 0.053 Uiso 1 1 calc R . . C14 C 0.8139(8) 0.46922(19) 1.0287(7) 0.0458(18) Uani 1 1 d . . . H14 H 0.8756 0.4787 1.1040 0.055 Uiso 1 1 calc R . . C15 C 0.6676(8) 0.46544(18) 1.0251(6) 0.0426(17) Uani 1 1 d . . . H15 H 0.6291 0.4723 1.0976 0.051 Uiso 1 1 calc R . . C16 C 0.5775(7) 0.45161(16) 0.9149(5) 0.0291(13) Uani 1 1 d . . . H16 H 0.4769 0.4493 0.9118 0.035 Uiso 1 1 calc R . . C17 C 0.3468(6) 0.43939(17) 0.6560(5) 0.0261(13) Uani 1 1 d . . . C18 C 0.3285(6) 0.48045(16) 0.6568(5) 0.0290(14) Uani 1 1 d . . . H18 H 0.4097 0.4973 0.6649 0.035 Uiso 1 1 calc R . . C19 C 0.1919(7) 0.49620(19) 0.6457(6) 0.0383(16) Uani 1 1 d . . . H19 H 0.1796 0.5239 0.6463 0.046 Uiso 1 1 calc R . . C20 C 0.0737(7) 0.47187(19) 0.6338(6) 0.0384(16) Uani 1 1 d . . . H20 H -0.0196 0.4828 0.6285 0.046 Uiso 1 1 calc R . . C21 C 0.0908(7) 0.4315(2) 0.6298(7) 0.0433(17) Uani 1 1 d . . . H21 H 0.0087 0.4149 0.6190 0.052 Uiso 1 1 calc R . . C22 C 0.2274(6) 0.41504(17) 0.6413(6) 0.0346(15) Uani 1 1 d . . . H22 H 0.2386 0.3873 0.6390 0.042 Uiso 1 1 calc R . . C23 C 0.4161(6) 0.23159(16) 0.4747(5) 0.0247(13) Uani 1 1 d . . . C24 C 0.5186(7) 0.20956(18) 0.4283(6) 0.0367(15) Uani 1 1 d . . . H24 H 0.5924 0.2224 0.3956 0.044 Uiso 1 1 calc R . . C25 C 0.5125(8) 0.16880(19) 0.4300(7) 0.0486(19) Uani 1 1 d . . . H25 H 0.5818 0.1537 0.3980 0.058 Uiso 1 1 calc R . . C26 C 0.4054(8) 0.1503(2) 0.4783(7) 0.0492(19) Uani 1 1 d . . . H26 H 0.4010 0.1223 0.4781 0.059 Uiso 1 1 calc R . . C27 C 0.3054(7) 0.17139(18) 0.5265(6) 0.0394(16) Uani 1 1 d . . . H27 H 0.2333 0.1583 0.5610 0.047 Uiso 1 1 calc R . . C28 C 0.3104(6) 0.21173(17) 0.5243(6) 0.0329(15) Uani 1 1 d . . . H28 H 0.2407 0.2264 0.5571 0.039 Uiso 1 1 calc R . . C29 C 0.2513(5) 0.30597(16) 0.4650(5) 0.0257(13) Uani 1 1 d . . . C30 C 0.1900(7) 0.32612(17) 0.3537(6) 0.0371(16) Uani 1 1 d . . . H30 H 0.2399 0.3286 0.2854 0.045 Uiso 1 1 calc R . . C31 C 0.0513(7) 0.3429(2) 0.3448(8) 0.051(2) Uani 1 1 d . . . H31 H 0.0080 0.3567 0.2695 0.061 Uiso 1 1 calc R . . C32 C -0.0206(7) 0.3395(2) 0.4421(9) 0.055(2) Uani 1 1 d . . . H32 H -0.1139 0.3506 0.4341 0.066 Uiso 1 1 calc R . . C33 C 0.0417(6) 0.32010(19) 0.5517(7) 0.0429(17) Uani 1 1 d . . . H33 H -0.0080 0.3185 0.6204 0.051 Uiso 1 1 calc R . . C34 C 0.1755(6) 0.30287(17) 0.5636(6) 0.0314(14) Uani 1 1 d . . . H34 H 0.2161 0.2889 0.6392 0.038 Uiso 1 1 calc R . . C35 C 0.8020(8) 0.0563(2) 0.7030(7) 0.058(2) Uani 1 1 d . . . H35A H 0.8913 0.0695 0.7472 0.070 Uiso 1 1 calc R . . H35B H 0.8279 0.0294 0.6797 0.070 Uiso 1 1 calc R . . Cl2 Cl 0.6828(3) 0.05296(8) 0.8075(2) 0.0992(9) Uani 1 1 d . . . Cl3 Cl 0.7312(2) 0.08193(8) 0.5657(3) 0.0953(9) 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 0.0239(2) 0.0279(2) 0.0189(2) 0.0033(2) 0.00909(17) 0.0019(2) Cl1 0.0557(10) 0.0436(10) 0.0281(8) 0.0107(7) 0.0238(8) 0.0097(8) P1 0.0265(8) 0.0226(8) 0.0248(8) -0.0011(7) 0.0094(7) -0.0018(6) P2 0.0214(8) 0.0238(8) 0.0205(8) 0.0003(6) 0.0027(6) 0.0001(6) S1 0.0447(10) 0.0265(8) 0.0310(9) 0.0049(7) 0.0198(8) -0.0034(7) S2 0.0377(9) 0.0347(9) 0.0217(8) -0.0028(7) 0.0108(7) -0.0019(7) C1 0.015(3) 0.022(3) 0.021(3) 0.000(2) 0.003(2) -0.001(2) C2 0.017(3) 0.022(3) 0.024(3) 0.002(3) 0.005(2) 0.000(2) C3 0.020(3) 0.022(3) 0.019(3) 0.001(2) 0.006(2) 0.001(2) C4 0.020(3) 0.040(4) 0.026(3) -0.002(3) 0.004(3) 0.004(3) C5 0.010(3) 0.023(3) 0.020(3) 0.002(2) 0.000(2) -0.004(2) C6 0.020(3) 0.024(3) 0.032(3) 0.009(3) 0.004(3) -0.001(2) C7 0.027(3) 0.035(4) 0.031(3) 0.015(3) 0.011(3) -0.003(3) C8 0.024(3) 0.055(4) 0.024(3) 0.004(3) 0.017(3) 0.003(3) C9 0.033(3) 0.029(3) 0.027(3) 0.004(3) 0.014(3) 0.001(3) C10 0.017(3) 0.029(3) 0.023(3) 0.006(3) 0.002(2) 0.001(2) C11 0.032(3) 0.018(3) 0.025(3) 0.005(2) 0.004(3) -0.001(2) C12 0.028(4) 0.034(4) 0.036(4) 0.001(3) 0.006(3) -0.004(3) C13 0.031(4) 0.042(4) 0.050(5) 0.004(4) -0.010(3) -0.009(3) C14 0.054(5) 0.038(4) 0.038(4) -0.002(3) -0.006(4) -0.010(3) C15 0.061(5) 0.039(4) 0.027(4) 0.005(3) 0.007(3) -0.006(3) C16 0.032(3) 0.029(3) 0.025(3) -0.001(3) 0.004(3) -0.012(3) C17 0.027(3) 0.032(3) 0.022(3) -0.001(3) 0.011(3) 0.000(3) C18 0.029(3) 0.028(3) 0.030(3) 0.001(3) 0.004(3) 0.000(3) C19 0.044(4) 0.033(4) 0.039(4) 0.004(3) 0.010(3) 0.010(3) C20 0.034(4) 0.047(4) 0.036(4) 0.002(3) 0.012(3) 0.013(3) C21 0.020(3) 0.055(5) 0.054(5) -0.002(4) 0.008(3) 0.000(3) C22 0.036(4) 0.024(3) 0.047(4) 0.004(3) 0.014(3) 0.001(3) C23 0.023(3) 0.030(3) 0.017(3) -0.001(3) -0.003(2) 0.000(3) C24 0.036(4) 0.036(4) 0.040(4) -0.008(3) 0.010(3) -0.002(3) C25 0.049(4) 0.037(4) 0.059(5) -0.014(4) 0.009(4) 0.011(3) C26 0.055(5) 0.028(4) 0.060(5) 0.001(4) 0.000(4) -0.001(3) C27 0.036(4) 0.031(4) 0.047(4) 0.007(3) 0.000(3) -0.009(3) C28 0.024(3) 0.032(4) 0.039(4) 0.005(3) -0.001(3) 0.001(3) C29 0.012(3) 0.029(3) 0.032(3) 0.004(3) -0.005(3) 0.000(2) C30 0.033(4) 0.034(4) 0.040(4) 0.003(3) -0.003(3) 0.000(3) C31 0.036(4) 0.044(4) 0.062(5) 0.007(4) -0.015(4) 0.006(3) C32 0.022(4) 0.048(5) 0.087(6) -0.010(4) -0.008(4) 0.008(3) C33 0.017(3) 0.046(4) 0.066(5) -0.017(4) 0.009(3) -0.004(3) C34 0.022(3) 0.033(3) 0.039(4) -0.004(3) 0.004(3) -0.004(3) C35 0.044(5) 0.064(5) 0.065(5) 0.016(4) 0.007(4) -0.007(4) Cl2 0.130(2) 0.1052(19) 0.0761(16) -0.0188(15) 0.0535(16) -0.0422(17) Cl3 0.0571(14) 0.120(2) 0.1005(19) 0.0650(17) -0.0045(13) -0.0193(13) _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 1.961(5) . ? Pd1 S1 2.3285(16) . ? Pd1 S2 2.3503(16) . ? Pd1 Cl1 2.3785(15) . ? P1 C2 1.772(6) . ? P1 C11 1.790(6) . ? P1 C17 1.799(6) . ? P1 S1 2.025(2) . ? P2 C23 1.805(6) . ? P2 C29 1.812(5) . ? P2 C3 1.842(5) . ? P2 S2 2.015(2) . ? C1 C2 1.362(7) . ? C1 C3 1.520(7) . ? C2 C10 1.469(7) . ? C3 C5 1.522(7) . ? C3 C4 1.545(7) . ? C5 C6 1.391(7) . ? C5 C10 1.407(7) . ? C6 C7 1.390(8) . ? C7 C8 1.390(8) . ? C8 C9 1.380(8) . ? C9 C10 1.391(7) . ? C11 C12 1.391(8) . ? C11 C16 1.409(8) . ? C12 C13 1.383(8) . ? C13 C14 1.364(9) . ? C14 C15 1.385(9) . ? C15 C16 1.389(8) . ? C17 C22 1.385(8) . ? C17 C18 1.406(8) . ? C18 C19 1.384(8) . ? C19 C20 1.378(8) . ? C20 C21 1.382(8) . ? C21 C22 1.393(8) . ? C23 C24 1.394(8) . ? C23 C28 1.398(8) . ? C24 C25 1.386(8) . ? C25 C26 1.380(9) . ? C26 C27 1.370(9) . ? C27 C28 1.372(8) . ? C29 C30 1.393(8) . ? C29 C34 1.394(8) . ? C30 C31 1.418(9) . ? C31 C32 1.358(10) . ? C32 C33 1.371(10) . ? C33 C34 1.379(8) . ? C35 Cl3 1.722(7) . ? C35 Cl2 1.745(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 S1 88.30(16) . . ? C1 Pd1 S2 89.70(16) . . ? S1 Pd1 S2 173.03(6) . . ? C1 Pd1 Cl1 176.86(16) . . ? S1 Pd1 Cl1 89.64(6) . . ? S2 Pd1 Cl1 92.63(6) . . ? C2 P1 C11 111.1(2) . . ? C2 P1 C17 109.0(2) . . ? C11 P1 C17 107.0(3) . . ? C2 P1 S1 105.37(18) . . ? C11 P1 S1 110.3(2) . . ? C17 P1 S1 114.17(19) . . ? C23 P2 C29 110.0(3) . . ? C23 P2 C3 111.1(2) . . ? C29 P2 C3 108.3(2) . . ? C23 P2 S2 110.51(19) . . ? C29 P2 S2 112.8(2) . . ? C3 P2 S2 104.01(17) . . ? P1 S1 Pd1 99.41(7) . . ? P2 S2 Pd1 94.82(7) . . ? C2 C1 C3 108.5(4) . . ? C2 C1 Pd1 126.8(4) . . ? C3 C1 Pd1 124.0(4) . . ? C1 C2 C10 111.2(5) . . ? C1 C2 P1 116.0(4) . . ? C10 C2 P1 132.8(4) . . ? C1 C3 C5 103.8(4) . . ? C1 C3 C4 112.8(4) . . ? C5 C3 C4 110.3(4) . . ? C1 C3 P2 100.1(3) . . ? C5 C3 P2 119.2(4) . . ? C4 C3 P2 110.0(4) . . ? C6 C5 C10 121.0(5) . . ? C6 C5 C3 130.4(5) . . ? C10 C5 C3 108.5(4) . . ? C7 C6 C5 118.3(5) . . ? C8 C7 C6 120.7(5) . . ? C9 C8 C7 121.1(5) . . ? C8 C9 C10 119.0(5) . . ? C9 C10 C5 119.8(5) . . ? C9 C10 C2 132.4(5) . . ? C5 C10 C2 107.8(5) . . ? C12 C11 C16 118.6(5) . . ? C12 C11 P1 120.1(4) . . ? C16 C11 P1 121.2(4) . . ? C13 C12 C11 120.4(6) . . ? C14 C13 C12 120.7(6) . . ? C13 C14 C15 120.4(6) . . ? C14 C15 C16 119.8(6) . . ? C15 C16 C11 120.0(6) . . ? C22 C17 C18 119.6(5) . . ? C22 C17 P1 120.9(4) . . ? C18 C17 P1 119.4(4) . . ? C19 C18 C17 119.8(5) . . ? C20 C19 C18 120.4(6) . . ? C19 C20 C21 120.0(6) . . ? C20 C21 C22 120.6(6) . . ? C17 C22 C21 119.6(6) . . ? C24 C23 C28 118.6(5) . . ? C24 C23 P2 119.2(4) . . ? C28 C23 P2 122.1(4) . . ? C25 C24 C23 119.9(6) . . ? C26 C25 C24 119.8(6) . . ? C27 C26 C25 121.2(6) . . ? C26 C27 C28 119.2(6) . . ? C27 C28 C23 121.3(6) . . ? C30 C29 C34 119.5(5) . . ? C30 C29 P2 118.1(5) . . ? C34 C29 P2 122.5(4) . . ? C29 C30 C31 118.5(6) . . ? C32 C31 C30 121.0(7) . . ? C31 C32 C33 119.9(6) . . ? C32 C33 C34 120.9(7) . . ? C33 C34 C29 120.2(6) . . ? Cl3 C35 Cl2 112.7(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.643 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.124 #===END