Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Kyoko Nozaki' _publ_contact_author_address ; Graduate School of Engineering The University of Tokyo Department of Chemistry and Biotech Bunkyo-ku Tokyo 113-8656 JAPAN ; _publ_contact_author_email NOZAKI@CHEMBIO.T.U-TOKYO.AC.JP _publ_section_title ; Synthesis of Anionic Methylpalladium Complexes with Phosphine-Sulfonate Ligands and Their Activities for Olefin Polymerization ; loop_ _publ_author_name 'Kyoko Nozaki' 'Takuya Kochi' 'Kenji Yoshimura' # Attachment '2A.CIF' data_2a' _database_code_depnum_ccdc_archive 'CCDC 283231' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H33 Cl N O3 P Pd S' _chemical_formula_weight 600.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 14.186(6) _cell_length_b 10.679(5) _cell_length_c 17.678(8) _cell_angle_alpha 90.000 _cell_angle_beta 92.549(2) _cell_angle_gamma 90.000 _cell_volume 2675.5(19) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7413 _cell_measurement_theta_min 3.0494 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Platelet _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 0.958 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6460 _exptl_absorpt_correction_T_max 0.9537 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14896 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4364 _reflns_number_gt 4065 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0694P)^2^+7.1840P] 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 4364 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1208 _refine_ls_wR_factor_gt 0.1192 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 0.77704(2) 0.07042(3) 0.107562(16) 0.01858(13) Uani 1 1 d . . . Cl1 Cl 0.68880(8) -0.08055(10) 0.03297(6) 0.0283(3) Uani 1 1 d . . . C1 C 0.8824(3) -0.0579(4) 0.1295(3) 0.0275(10) Uani 1 1 d . . . H1 H 0.8544 -0.1396 0.1401 0.041 Uiso 1 1 calc R . . H2 H 0.9215 -0.0305 0.1735 0.041 Uiso 1 1 calc R . . H3 H 0.9215 -0.0648 0.0853 0.041 Uiso 1 1 calc R . . P1 P 0.86255(7) 0.20918(10) 0.17416(6) 0.0190(2) Uani 1 1 d . . . C2 C 0.8329(3) 0.3690(4) 0.1426(2) 0.0214(9) Uani 1 1 d . . . C3 C 0.7387(3) 0.4044(4) 0.1254(2) 0.0214(9) Uani 1 1 d . . . S1 S 0.64319(7) 0.29824(10) 0.13636(6) 0.0246(2) Uani 1 1 d . . . O1 O 0.6602(2) 0.1983(3) 0.08059(18) 0.0270(7) Uani 1 1 d . . . O2 O 0.6517(2) 0.2525(3) 0.21347(17) 0.0299(7) Uani 1 1 d . . . O3 O 0.5578(2) 0.3663(3) 0.11736(19) 0.0347(8) Uani 1 1 d . . . C4 C 0.7185(4) 0.5216(4) 0.0953(3) 0.0304(10) Uani 1 1 d . . . H4 H 0.6549 0.5449 0.0838 0.036 Uiso 1 1 calc R . . C5 C 0.7910(4) 0.6057(4) 0.0818(3) 0.0348(11) Uani 1 1 d . . . H5 H 0.7768 0.6858 0.0608 0.042 Uiso 1 1 calc R . . C6 C 0.8830(4) 0.5725(4) 0.0990(3) 0.0328(11) Uani 1 1 d . . . H6 H 0.9323 0.6301 0.0901 0.039 Uiso 1 1 calc R . . C7 C 0.9045(3) 0.4555(4) 0.1291(2) 0.0263(10) Uani 1 1 d . . . H7 H 0.9684 0.4338 0.1407 0.032 Uiso 1 1 calc R . . C8 C 0.8497(3) 0.2082(4) 0.2766(2) 0.0220(9) Uani 1 1 d . . . C9 C 0.8544(3) 0.3181(5) 0.3184(2) 0.0308(10) Uani 1 1 d . . . H8 H 0.8655 0.3958 0.2942 0.037 Uiso 1 1 calc R . . C10 C 0.8427(4) 0.3139(5) 0.3969(3) 0.0395(12) Uani 1 1 d . . . H9 H 0.8463 0.3888 0.4259 0.047 Uiso 1 1 calc R . . C11 C 0.8258(4) 0.2016(6) 0.4319(3) 0.0449(14) Uani 1 1 d . . . H10 H 0.8166 0.1994 0.4847 0.054 Uiso 1 1 calc R . . C12 C 0.8223(4) 0.0919(5) 0.3902(3) 0.0432(13) Uani 1 1 d . . . H11 H 0.8114 0.0145 0.4148 0.052 Uiso 1 1 calc R . . C13 C 0.8348(4) 0.0942(5) 0.3122(3) 0.0327(11) Uani 1 1 d . . . H12 H 0.8330 0.0187 0.2838 0.039 Uiso 1 1 calc R . . C14 C 0.9887(3) 0.2015(4) 0.1614(2) 0.0224(9) Uani 1 1 d . . . C15 C 1.0549(3) 0.2107(5) 0.2211(3) 0.0319(10) Uani 1 1 d . . . H13 H 1.0350 0.2202 0.2714 0.038 Uiso 1 1 calc R . . C16 C 1.1509(3) 0.2060(6) 0.2074(3) 0.0421(13) Uani 1 1 d . . . H14 H 1.1962 0.2108 0.2485 0.050 Uiso 1 1 calc R . . C17 C 1.1808(3) 0.1942(5) 0.1335(3) 0.0398(12) Uani 1 1 d . . . H15 H 1.2462 0.1923 0.1243 0.048 Uiso 1 1 calc R . . C18 C 1.1148(3) 0.1853(5) 0.0739(3) 0.0367(12) Uani 1 1 d . . . H16 H 1.1350 0.1774 0.0236 0.044 Uiso 1 1 calc R . . C19 C 1.0198(3) 0.1878(5) 0.0872(3) 0.0304(10) Uani 1 1 d . . . H17 H 0.9749 0.1802 0.0460 0.036 Uiso 1 1 calc R . . N1 N 0.5040(3) -0.1152(5) 0.1350(3) 0.0506(12) Uani 1 1 d . . . H18 H 0.5510 -0.1116 0.1000 0.061 Uiso 1 1 calc R . . C20 C 0.4704(4) 0.0174(6) 0.1422(4) 0.0528(15) Uani 1 1 d . . . H19 H 0.5250 0.0714 0.1566 0.063 Uiso 1 1 calc R . . H20 H 0.4446 0.0461 0.0922 0.063 Uiso 1 1 calc R . . C21 C 0.3972(4) 0.0332(6) 0.1987(4) 0.0578(17) Uani 1 1 d . . . H21 H 0.3407 -0.0144 0.1826 0.087 Uiso 1 1 calc R . . H22 H 0.3811 0.1221 0.2028 0.087 Uiso 1 1 calc R . . H23 H 0.4214 0.0023 0.2480 0.087 Uiso 1 1 calc R . . C22 C 0.5504(4) -0.1694(6) 0.2036(3) 0.0477(14) Uani 1 1 d . . . H24 H 0.5828 -0.2473 0.1891 0.057 Uiso 1 1 calc R . . H25 H 0.5009 -0.1930 0.2387 0.057 Uiso 1 1 calc R . . C23 C 0.6197(4) -0.0885(6) 0.2451(3) 0.0515(16) Uani 1 1 d . . . H26 H 0.6719 -0.0693 0.2124 0.077 Uiso 1 1 calc R . . H27 H 0.6443 -0.1321 0.2906 0.077 Uiso 1 1 calc R . . H28 H 0.5890 -0.0105 0.2596 0.077 Uiso 1 1 calc R . . C24 C 0.4294(4) -0.1995(5) 0.0994(3) 0.0447(13) Uani 1 1 d . . . H29 H 0.3794 -0.2120 0.1359 0.054 Uiso 1 1 calc R . . H30 H 0.4004 -0.1568 0.0544 0.054 Uiso 1 1 calc R . . C25 C 0.4639(6) -0.3233(7) 0.0759(4) 0.075(2) Uani 1 1 d . . . H31 H 0.5046 -0.3132 0.0330 0.113 Uiso 1 1 calc R . . H32 H 0.4101 -0.3768 0.0610 0.113 Uiso 1 1 calc R . . H33 H 0.5000 -0.3622 0.1183 0.113 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0205(2) 0.0197(2) 0.01557(19) 0.00049(12) 0.00069(13) 0.00187(12) Cl1 0.0271(6) 0.0275(6) 0.0302(6) -0.0082(4) 0.0002(4) 0.0002(4) C1 0.026(2) 0.024(2) 0.032(2) -0.0027(18) -0.0053(19) 0.0058(18) P1 0.0204(5) 0.0224(5) 0.0142(5) 0.0018(4) 0.0001(4) 0.0011(4) C2 0.029(2) 0.022(2) 0.0136(19) -0.0002(16) 0.0005(16) 0.0015(18) C3 0.025(2) 0.021(2) 0.018(2) -0.0013(16) 0.0045(17) 0.0045(17) S1 0.0219(5) 0.0264(6) 0.0257(6) 0.0006(4) 0.0015(4) 0.0048(4) O1 0.0234(16) 0.0248(16) 0.0322(17) -0.0024(13) -0.0055(13) 0.0036(13) O2 0.0235(16) 0.0380(18) 0.0286(17) 0.0052(14) 0.0037(13) 0.0001(14) O3 0.0244(17) 0.0382(19) 0.041(2) -0.0007(16) -0.0032(14) 0.0094(15) C4 0.035(3) 0.024(2) 0.032(2) -0.0012(19) 0.002(2) 0.010(2) C5 0.052(3) 0.020(2) 0.032(3) 0.004(2) 0.003(2) 0.003(2) C6 0.047(3) 0.024(2) 0.028(2) 0.0006(19) 0.005(2) -0.006(2) C7 0.030(2) 0.028(2) 0.020(2) -0.0004(18) -0.0001(18) -0.0026(19) C8 0.017(2) 0.034(2) 0.0148(19) 0.0026(17) 0.0001(15) 0.0004(18) C9 0.035(3) 0.037(3) 0.020(2) -0.0009(19) 0.0028(19) -0.003(2) C10 0.044(3) 0.055(3) 0.020(2) -0.009(2) 0.000(2) -0.006(3) C11 0.047(3) 0.072(4) 0.017(2) 0.000(2) 0.005(2) -0.010(3) C12 0.056(3) 0.050(3) 0.024(3) 0.013(2) 0.002(2) -0.014(3) C13 0.039(3) 0.036(3) 0.023(2) 0.005(2) 0.000(2) -0.005(2) C14 0.024(2) 0.023(2) 0.020(2) 0.0042(17) -0.0001(17) 0.0030(17) C15 0.028(2) 0.043(3) 0.024(2) 0.002(2) -0.0021(18) 0.002(2) C16 0.023(3) 0.068(4) 0.034(3) 0.001(3) -0.006(2) 0.000(3) C17 0.023(2) 0.056(3) 0.041(3) 0.002(2) 0.005(2) 0.001(2) C18 0.032(3) 0.050(3) 0.029(3) 0.006(2) 0.010(2) 0.003(2) C19 0.028(2) 0.043(3) 0.021(2) 0.001(2) 0.0008(18) 0.003(2) N1 0.041(3) 0.066(3) 0.045(3) 0.002(2) -0.006(2) 0.013(2) C20 0.045(3) 0.054(4) 0.059(4) 0.015(3) -0.008(3) -0.007(3) C21 0.051(4) 0.047(3) 0.075(5) -0.009(3) -0.011(3) 0.009(3) C22 0.037(3) 0.054(4) 0.051(3) 0.021(3) -0.002(3) 0.002(3) C23 0.033(3) 0.084(5) 0.037(3) 0.018(3) -0.003(2) -0.002(3) C24 0.041(3) 0.052(3) 0.041(3) 0.007(3) -0.002(2) 0.006(3) C25 0.095(6) 0.070(5) 0.059(4) -0.020(4) -0.023(4) 0.031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.051(4) . ? Pd1 O1 2.184(3) . ? Pd1 P1 2.2195(12) . ? Pd1 Cl1 2.3997(12) . ? C1 H1 0.9800 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? P1 C14 1.815(4) . ? P1 C8 1.828(4) . ? P1 C2 1.838(4) . ? C2 C7 1.401(6) . ? C2 C3 1.408(6) . ? C3 C4 1.385(6) . ? C3 S1 1.784(4) . ? S1 O3 1.439(3) . ? S1 O2 1.448(3) . ? S1 O1 1.480(3) . ? C4 C5 1.393(7) . ? C4 H4 0.9500 . ? C5 C6 1.373(7) . ? C5 H5 0.9500 . ? C6 C7 1.387(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.387(6) . ? C8 C13 1.391(6) . ? C9 C10 1.406(7) . ? C9 H8 0.9500 . ? C10 C11 1.374(8) . ? C10 H9 0.9500 . ? C11 C12 1.384(8) . ? C11 H10 0.9500 . ? C12 C13 1.398(7) . ? C12 H11 0.9500 . ? C13 H12 0.9500 . ? C14 C15 1.386(6) . ? C14 C19 1.409(6) . ? C15 C16 1.394(7) . ? C15 H13 0.9500 . ? C16 C17 1.396(7) . ? C16 H14 0.9500 . ? C17 C18 1.381(7) . ? C17 H15 0.9500 . ? C18 C19 1.379(7) . ? C18 H16 0.9500 . ? C19 H17 0.9500 . ? N1 C22 1.473(7) . ? N1 C20 1.501(8) . ? N1 C24 1.506(8) . ? N1 H18 0.9300 . ? C20 C21 1.483(9) . ? C20 H19 0.9900 . ? C20 H20 0.9900 . ? C21 H21 0.9800 . ? C21 H22 0.9800 . ? C21 H23 0.9800 . ? C22 C23 1.478(8) . ? C22 H24 0.9900 . ? C22 H25 0.9900 . ? C23 H26 0.9800 . ? C23 H27 0.9800 . ? C23 H28 0.9800 . ? C24 C25 1.476(8) . ? C24 H29 0.9900 . ? C24 H30 0.9900 . ? C25 H31 0.9800 . ? C25 H32 0.9800 . ? C25 H33 0.9800 . ? 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 O1 176.58(15) . . ? C1 Pd1 P1 88.25(13) . . ? O1 Pd1 P1 95.17(9) . . ? C1 Pd1 Cl1 90.73(13) . . ? O1 Pd1 Cl1 85.85(9) . . ? P1 Pd1 Cl1 178.15(4) . . ? Pd1 C1 H1 109.5 . . ? Pd1 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? Pd1 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? C14 P1 C8 105.39(19) . . ? C14 P1 C2 102.59(19) . . ? C8 P1 C2 105.92(19) . . ? C14 P1 Pd1 114.97(15) . . ? C8 P1 Pd1 116.46(14) . . ? C2 P1 Pd1 110.26(14) . . ? C7 C2 C3 118.3(4) . . ? C7 C2 P1 120.4(3) . . ? C3 C2 P1 121.2(3) . . ? C4 C3 C2 120.3(4) . . ? C4 C3 S1 118.1(3) . . ? C2 C3 S1 121.6(3) . . ? O3 S1 O2 115.1(2) . . ? O3 S1 O1 111.64(19) . . ? O2 S1 O1 112.01(19) . . ? O3 S1 C3 106.8(2) . . ? O2 S1 C3 106.55(19) . . ? O1 S1 C3 103.81(19) . . ? S1 O1 Pd1 116.72(17) . . ? C3 C4 C5 120.4(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 119.8(4) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 120.5(5) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C7 C2 120.7(4) . . ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? C9 C8 C13 120.2(4) . . ? C9 C8 P1 121.3(3) . . ? C13 C8 P1 118.5(3) . . ? C8 C9 C10 119.6(5) . . ? C8 C9 H8 120.2 . . ? C10 C9 H8 120.2 . . ? C11 C10 C9 120.1(5) . . ? C11 C10 H9 119.9 . . ? C9 C10 H9 119.9 . . ? C10 C11 C12 120.2(4) . . ? C10 C11 H10 119.9 . . ? C12 C11 H10 119.9 . . ? C11 C12 C13 120.4(5) . . ? C11 C12 H11 119.8 . . ? C13 C12 H11 119.8 . . ? C8 C13 C12 119.4(5) . . ? C8 C13 H12 120.3 . . ? C12 C13 H12 120.3 . . ? C15 C14 C19 119.1(4) . . ? C15 C14 P1 122.7(3) . . ? C19 C14 P1 118.2(3) . . ? C14 C15 C16 119.9(4) . . ? C14 C15 H13 120.0 . . ? C16 C15 H13 120.0 . . ? C15 C16 C17 120.4(5) . . ? C15 C16 H14 119.8 . . ? C17 C16 H14 119.8 . . ? C18 C17 C16 119.8(5) . . ? C18 C17 H15 120.1 . . ? C16 C17 H15 120.1 . . ? C19 C18 C17 120.2(4) . . ? C19 C18 H16 119.9 . . ? C17 C18 H16 119.9 . . ? C18 C19 C14 120.7(4) . . ? C18 C19 H17 119.7 . . ? C14 C19 H17 119.7 . . ? C22 N1 C20 115.6(5) . . ? C22 N1 C24 112.9(5) . . ? C20 N1 C24 112.3(4) . . ? C22 N1 H18 104.9 . . ? C20 N1 H18 104.9 . . ? C24 N1 H18 104.9 . . ? C21 C20 N1 113.5(5) . . ? C21 C20 H19 108.9 . . ? N1 C20 H19 108.9 . . ? C21 C20 H20 108.9 . . ? N1 C20 H20 108.9 . . ? H19 C20 H20 107.7 . . ? C20 C21 H21 109.5 . . ? C20 C21 H22 109.5 . . ? H21 C21 H22 109.5 . . ? C20 C21 H23 109.5 . . ? H21 C21 H23 109.5 . . ? H22 C21 H23 109.5 . . ? N1 C22 C23 116.2(5) . . ? N1 C22 H24 108.2 . . ? C23 C22 H24 108.2 . . ? N1 C22 H25 108.2 . . ? C23 C22 H25 108.2 . . ? H24 C22 H25 107.4 . . ? C22 C23 H26 109.5 . . ? C22 C23 H27 109.5 . . ? H26 C23 H27 109.5 . . ? C22 C23 H28 109.5 . . ? H26 C23 H28 109.5 . . ? H27 C23 H28 109.5 . . ? C25 C24 N1 114.7(5) . . ? C25 C24 H29 108.6 . . ? N1 C24 H29 108.6 . . ? C25 C24 H30 108.6 . . ? N1 C24 H30 108.6 . . ? H29 C24 H30 107.6 . . ? C24 C25 H31 109.5 . . ? C24 C25 H32 109.5 . . ? H31 C25 H32 109.5 . . ? C24 C25 H33 109.5 . . ? H31 C25 H33 109.5 . . ? H32 C25 H33 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pd1 P1 C14 38.7(2) . . . . ? O1 Pd1 P1 C14 -141.44(17) . . . . ? Cl1 Pd1 P1 C14 -18.0(13) . . . . ? C1 Pd1 P1 C8 -85.3(2) . . . . ? O1 Pd1 P1 C8 94.59(18) . . . . ? Cl1 Pd1 P1 C8 -142.0(12) . . . . ? C1 Pd1 P1 C2 154.0(2) . . . . ? O1 Pd1 P1 C2 -26.08(17) . . . . ? Cl1 Pd1 P1 C2 97.3(13) . . . . ? C14 P1 C2 C7 -10.7(4) . . . . ? C8 P1 C2 C7 99.6(4) . . . . ? Pd1 P1 C2 C7 -133.6(3) . . . . ? C14 P1 C2 C3 164.0(3) . . . . ? C8 P1 C2 C3 -85.7(4) . . . . ? Pd1 P1 C2 C3 41.1(4) . . . . ? C7 C2 C3 C4 0.5(6) . . . . ? P1 C2 C3 C4 -174.3(3) . . . . ? C7 C2 C3 S1 177.0(3) . . . . ? P1 C2 C3 S1 2.3(5) . . . . ? C4 C3 S1 O3 -6.1(4) . . . . ? C2 C3 S1 O3 177.3(3) . . . . ? C4 C3 S1 O2 -129.6(3) . . . . ? C2 C3 S1 O2 53.8(4) . . . . ? C4 C3 S1 O1 112.0(3) . . . . ? C2 C3 S1 O1 -64.6(4) . . . . ? O3 S1 O1 Pd1 -172.71(19) . . . . ? O2 S1 O1 Pd1 -42.0(2) . . . . ? C3 S1 O1 Pd1 72.6(2) . . . . ? C1 Pd1 O1 S1 149(3) . . . . ? P1 Pd1 O1 S1 -29.50(19) . . . . ? Cl1 Pd1 O1 S1 152.05(19) . . . . ? C2 C3 C4 C5 0.0(7) . . . . ? S1 C3 C4 C5 -176.6(4) . . . . ? C3 C4 C5 C6 -0.5(7) . . . . ? C4 C5 C6 C7 0.4(7) . . . . ? C5 C6 C7 C2 0.1(7) . . . . ? C3 C2 C7 C6 -0.5(6) . . . . ? P1 C2 C7 C6 174.3(3) . . . . ? C14 P1 C8 C9 86.0(4) . . . . ? C2 P1 C8 C9 -22.3(4) . . . . ? Pd1 P1 C8 C9 -145.2(3) . . . . ? C14 P1 C8 C13 -94.1(4) . . . . ? C2 P1 C8 C13 157.6(4) . . . . ? Pd1 P1 C8 C13 34.6(4) . . . . ? C13 C8 C9 C10 -0.9(7) . . . . ? P1 C8 C9 C10 179.0(4) . . . . ? C8 C9 C10 C11 -0.5(8) . . . . ? C9 C10 C11 C12 1.3(8) . . . . ? C10 C11 C12 C13 -0.7(9) . . . . ? C9 C8 C13 C12 1.5(7) . . . . ? P1 C8 C13 C12 -178.4(4) . . . . ? C11 C12 C13 C8 -0.7(8) . . . . ? C8 P1 C14 C15 -7.6(4) . . . . ? C2 P1 C14 C15 103.1(4) . . . . ? Pd1 P1 C14 C15 -137.2(4) . . . . ? C8 P1 C14 C19 173.6(4) . . . . ? C2 P1 C14 C19 -75.7(4) . . . . ? Pd1 P1 C14 C19 43.9(4) . . . . ? C19 C14 C15 C16 -0.2(7) . . . . ? P1 C14 C15 C16 -179.0(4) . . . . ? C14 C15 C16 C17 1.1(8) . . . . ? C15 C16 C17 C18 -1.0(9) . . . . ? C16 C17 C18 C19 -0.1(9) . . . . ? C17 C18 C19 C14 1.0(8) . . . . ? C15 C14 C19 C18 -0.9(7) . . . . ? P1 C14 C19 C18 178.0(4) . . . . ? C22 N1 C20 C21 -62.4(7) . . . . ? C24 N1 C20 C21 69.2(6) . . . . ? C20 N1 C22 C23 -44.5(7) . . . . ? C24 N1 C22 C23 -175.7(5) . . . . ? C22 N1 C24 C25 -59.5(7) . . . . ? C20 N1 C24 C25 167.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 2.660 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.111