# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Pierre Braunstein' _publ_contact_author_email BRAUNST@CHIMIE.U-STRASBG.FR _publ_section_title ; Versatile coordination modes of novel hemilabile S-NHC ligands ; loop_ _publ_author_name 'Pierre Braunstein' 'Christophe Fliedel' 'Gilles Schnee' # Attachment 'Complex_5.cif' data_flied27 _database_code_depnum_ccdc_archive 'CCDC 710767' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H14 Cl2 N2 Pd S' _chemical_formula_sum 'C8 H14 Cl2 N2 Pd S' _chemical_formula_weight 347.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9199(6) _cell_length_b 8.3242(4) _cell_length_c 14.8290(9) _cell_angle_alpha 90.00 _cell_angle_beta 118.849(4) _cell_angle_gamma 90.00 _cell_volume 1180.66(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3634 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.986 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 2.164 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_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 4371 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0707 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.50 _reflns_number_total 2443 _reflns_number_gt 1717 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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^)+(0.0891P)^2^+2.4353P] 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 2443 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1671 _refine_ls_wR_factor_gt 0.1379 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 0.22831(6) -0.17449(7) -0.09829(4) 0.0209(2) Uani 1 1 d . . . S1 S 0.2121(2) -0.3658(2) -0.21347(15) 0.0247(5) Uani 1 1 d . . . C1 C 0.1893(8) -0.0034(9) -0.2018(5) 0.0196(16) Uani 1 1 d . . . C2 C 0.0889(9) 0.1183(10) -0.3558(6) 0.0284(19) Uani 1 1 d . . . H2 H 0.0294 0.1389 -0.4252 0.034 Uiso 1 1 calc R . . C3 C 0.1946(9) 0.2105(10) -0.2903(6) 0.0254(18) Uani 1 1 d . . . H3 H 0.2226 0.3075 -0.3058 0.030 Uiso 1 1 calc R . . C4 C 0.0025(9) -0.1596(10) -0.3440(6) 0.0281(19) Uani 1 1 d . . . H4A H -0.0702 -0.1388 -0.4139 0.034 Uiso 1 1 calc R . . H4B H -0.0418 -0.1918 -0.3038 0.034 Uiso 1 1 calc R . . C5 C 0.0985(9) -0.2943(10) -0.3438(6) 0.0279(19) Uani 1 1 d . . . H5A H 0.1550 -0.2546 -0.3732 0.033 Uiso 1 1 calc R . . H5B H 0.0421 -0.3826 -0.3861 0.033 Uiso 1 1 calc R . . C6 C 0.3850(9) -0.3803(11) -0.2053(7) 0.036(2) Uani 1 1 d . . . H6A H 0.4462 -0.4400 -0.1435 0.043 Uiso 1 1 calc R . . H6B H 0.3756 -0.4423 -0.2637 0.043 Uiso 1 1 calc R . . C7 C 0.4544(10) -0.2246(12) -0.2033(7) 0.041(2) Uani 1 1 d . . . H7A H 0.3902 -0.1575 -0.2586 0.061 Uiso 1 1 calc R . . H7B H 0.5353 -0.2447 -0.2111 0.061 Uiso 1 1 calc R . . H7C H 0.4822 -0.1715 -0.1388 0.061 Uiso 1 1 calc R . . C8 C 0.3799(9) 0.1973(10) -0.1036(7) 0.033(2) Uani 1 1 d . . . H8A H 0.3556 0.2929 -0.0796 0.049 Uiso 1 1 calc R . . H8B H 0.4516 0.2218 -0.1213 0.049 Uiso 1 1 calc R . . H8C H 0.4137 0.1175 -0.0502 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.2850(2) -0.3908(2) 0.01958(15) 0.0299(5) Uani 1 1 d . . . Cl2 Cl 0.2274(2) 0.0137(2) 0.01713(15) 0.0290(5) Uani 1 1 d . . . N1 N 0.0849(6) -0.0144(8) -0.3002(5) 0.0222(14) Uani 1 1 d . . . N2 N 0.2551(7) 0.1352(8) -0.1953(5) 0.0236(15) 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 0.0222(4) 0.0220(4) 0.0187(4) 0.0005(2) 0.0099(3) -0.0011(3) S1 0.0273(11) 0.0241(10) 0.0225(11) -0.0012(8) 0.0117(9) -0.0019(8) C1 0.019(4) 0.021(4) 0.016(4) -0.003(3) 0.006(3) 0.004(3) C2 0.029(5) 0.032(5) 0.025(5) 0.008(4) 0.013(4) 0.008(4) C3 0.030(5) 0.031(4) 0.019(4) 0.008(4) 0.015(4) 0.001(4) C4 0.021(4) 0.041(5) 0.016(4) -0.004(4) 0.004(3) -0.009(4) C5 0.029(5) 0.028(4) 0.024(4) -0.006(4) 0.011(4) -0.005(4) C6 0.028(5) 0.038(5) 0.041(6) -0.009(4) 0.016(4) 0.010(4) C7 0.035(5) 0.055(6) 0.034(5) -0.003(5) 0.019(5) -0.011(5) C8 0.026(5) 0.034(5) 0.030(5) -0.007(4) 0.008(4) -0.006(4) Cl1 0.0331(11) 0.0272(11) 0.0256(11) 0.0053(9) 0.0111(9) -0.0022(9) Cl2 0.0374(12) 0.0291(11) 0.0215(10) -0.0033(8) 0.0150(9) 0.0009(9) N1 0.018(3) 0.030(4) 0.017(3) 0.004(3) 0.007(3) 0.001(3) N2 0.025(4) 0.025(4) 0.021(4) 0.002(3) 0.011(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.984(7) . ? Pd1 S1 2.279(2) . ? Pd1 Cl2 2.3239(19) . ? Pd1 Cl1 2.374(2) . ? S1 C5 1.821(8) . ? S1 C6 1.837(8) . ? C1 N2 1.339(10) . ? C1 N1 1.353(9) . ? C2 C3 1.335(12) . ? C2 N1 1.391(10) . ? C2 H2 0.9300 . ? C3 N2 1.384(9) . ? C3 H3 0.9300 . ? C4 N1 1.459(10) . ? C4 C5 1.534(11) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.495(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N2 1.478(10) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? 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 90.7(2) . . ? C1 Pd1 Cl2 90.6(2) . . ? S1 Pd1 Cl2 175.39(7) . . ? C1 Pd1 Cl1 175.3(2) . . ? S1 Pd1 Cl1 85.41(7) . . ? Cl2 Pd1 Cl1 93.52(7) . . ? C5 S1 C6 104.1(4) . . ? C5 S1 Pd1 109.5(3) . . ? C6 S1 Pd1 106.9(3) . . ? N2 C1 N1 106.2(6) . . ? N2 C1 Pd1 131.0(6) . . ? N1 C1 Pd1 122.8(5) . . ? C3 C2 N1 106.8(7) . . ? C3 C2 H2 126.6 . . ? N1 C2 H2 126.6 . . ? C2 C3 N2 107.5(7) . . ? C2 C3 H3 126.2 . . ? N2 C3 H3 126.2 . . ? N1 C4 C5 109.3(6) . . ? N1 C4 H4A 109.8 . . ? C5 C4 H4A 109.8 . . ? N1 C4 H4B 109.8 . . ? C5 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? C4 C5 S1 110.9(5) . . ? C4 C5 H5A 109.5 . . ? S1 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? S1 C5 H5B 109.5 . . ? H5A C5 H5B 108.0 . . ? C7 C6 S1 116.0(6) . . ? C7 C6 H6A 108.3 . . ? S1 C6 H6A 108.3 . . ? C7 C6 H6B 108.3 . . ? S1 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C1 N1 C2 109.5(6) . . ? C1 N1 C4 123.6(6) . . ? C2 N1 C4 125.6(7) . . ? C1 N2 C3 109.9(7) . . ? C1 N2 C8 126.4(7) . . ? C3 N2 C8 123.6(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.844 _refine_diff_density_min -1.012 _refine_diff_density_rms 0.221 # Attachment 'Complex_6.cif' data_gillesw2 _database_code_depnum_ccdc_archive 'CCDC 710768' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H28 Cl2 N4 Pd S2' _chemical_formula_sum 'C16 H28 Cl2 N4 Pd S2' _chemical_formula_weight 517.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' C C 0.0033 0.0016 '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' S S 0.1246 0.1234 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8872(8) _cell_length_b 7.9205(9) _cell_length_c 9.8308(7) _cell_angle_alpha 96.521(6) _cell_angle_beta 91.623(6) _cell_angle_gamma 114.409(4) _cell_volume 553.7(1) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4822 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.986 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 264 _exptl_absorpt_coefficient_mu 1.275 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4911 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_sigmaI/netI 0.1052 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2172 _reflns_number_gt 1528 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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^)+(0.0737P)^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 2172 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1492 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 1.0000 0.0000 0.5000 0.0333(3) Uani 1 2 d S . . Cl1 Cl 0.7333(2) -0.2718(2) 0.50169(18) 0.0487(5) Uani 1 1 d . . . C1 C 0.8805(8) 0.1483(8) 0.6102(5) 0.0313(14) Uani 1 1 d . . . C2 C 0.7084(9) 0.3064(9) 0.6638(6) 0.0375(15) Uani 1 1 d . . . H2 H 0.6249 0.3606 0.6552 0.045 Uiso 1 1 calc R . . C3 C 0.8046(9) 0.3097(9) 0.7796(6) 0.0399(16) Uani 1 1 d . . . H3 H 0.8006 0.3668 0.8668 0.048 Uiso 1 1 calc R . . C4 C 0.6854(8) 0.1692(9) 0.4168(6) 0.0363(15) Uani 1 1 d . . . H4A H 0.5621 0.1684 0.4111 0.044 Uiso 1 1 calc R . . H4B H 0.6733 0.0460 0.3783 0.044 Uiso 1 1 calc R . . C5 C 0.8105(9) 0.3120(9) 0.3331(6) 0.0451(17) Uani 1 1 d . . . H5A H 0.9384 0.3290 0.3519 0.054 Uiso 1 1 calc R . . H5B H 0.8050 0.4309 0.3611 0.054 Uiso 1 1 calc R . . C6 C 0.4976(15) 0.1973(15) 0.1286(10) 0.101(4) Uani 1 1 d . . . H6A H 0.4505 0.1449 0.0340 0.121 Uiso 1 1 calc R . . H6B H 0.4269 0.1064 0.1872 0.121 Uiso 1 1 calc R . . C7 C 0.4738(19) 0.3663(17) 0.1626(10) 0.114(4) Uani 1 1 d . . . H7A H 0.3435 0.3395 0.1513 0.171 Uiso 1 1 calc R . . H7B H 0.5413 0.4548 0.1029 0.171 Uiso 1 1 calc R . . H7C H 0.5207 0.4179 0.2562 0.171 Uiso 1 1 calc R . . C8 C 1.0399(11) 0.1823(12) 0.8408(7) 0.061(2) Uani 1 1 d . . . H8A H 1.0400 0.2418 0.9315 0.092 Uiso 1 1 calc R . . H8B H 1.1637 0.2348 0.8109 0.092 Uiso 1 1 calc R . . H8C H 1.0002 0.0504 0.8421 0.092 Uiso 1 1 calc R . . N1 N 0.9097(7) 0.2129(8) 0.7448(5) 0.0395(13) Uani 1 1 d . . . N2 N 0.7572(6) 0.2075(7) 0.5606(5) 0.0315(11) Uani 1 1 d . . . S1 S 0.7471(3) 0.2459(3) 0.15202(18) 0.0650(6) 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 0.0330(4) 0.0341(4) 0.0382(4) 0.0054(3) 0.0080(3) 0.0191(3) Cl1 0.0368(9) 0.0365(10) 0.0737(12) 0.0062(9) 0.0138(8) 0.0161(8) C1 0.026(3) 0.035(3) 0.036(3) 0.008(3) 0.010(2) 0.015(3) C2 0.041(4) 0.038(4) 0.043(4) 0.006(3) 0.013(3) 0.026(3) C3 0.049(4) 0.041(4) 0.040(3) 0.007(3) 0.021(3) 0.027(3) C4 0.034(3) 0.040(4) 0.042(3) 0.004(3) 0.008(3) 0.023(3) C5 0.045(4) 0.040(4) 0.050(4) 0.007(3) 0.009(3) 0.018(3) C6 0.139(10) 0.077(7) 0.072(6) 0.005(5) -0.008(6) 0.033(7) C7 0.184(13) 0.109(9) 0.080(7) 0.027(6) 0.038(7) 0.087(9) C8 0.074(6) 0.076(6) 0.046(4) 0.009(4) 0.001(4) 0.044(5) N1 0.045(3) 0.048(3) 0.033(3) 0.008(2) 0.007(2) 0.026(3) N2 0.030(3) 0.032(3) 0.036(3) 0.005(2) 0.008(2) 0.016(2) S1 0.0702(14) 0.0881(17) 0.0401(10) 0.0067(10) 0.0074(9) 0.0368(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 2.031(6) 2_756 ? Pd1 C1 2.031(6) . ? Pd1 Cl1 2.3081(16) 2_756 ? Pd1 Cl1 2.3081(16) . ? C1 N1 1.341(7) . ? C1 N2 1.344(7) . ? C2 C3 1.342(8) . ? C2 N2 1.372(7) . ? C2 H2 0.9300 . ? C3 N1 1.369(8) . ? C3 H3 0.9300 . ? C4 N2 1.458(7) . ? C4 C5 1.505(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 S1 1.793(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.431(13) . ? C6 S1 1.845(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N1 1.486(8) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? 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 C1 180.000(1) 2_756 . ? C1 Pd1 Cl1 90.21(16) 2_756 2_756 ? C1 Pd1 Cl1 89.79(16) . 2_756 ? C1 Pd1 Cl1 89.79(16) 2_756 . ? C1 Pd1 Cl1 90.21(16) . . ? Cl1 Pd1 Cl1 180.0 2_756 . ? N1 C1 N2 105.1(5) . . ? N1 C1 Pd1 128.5(4) . . ? N2 C1 Pd1 126.4(4) . . ? C3 C2 N2 106.7(5) . . ? C3 C2 H2 126.7 . . ? N2 C2 H2 126.6 . . ? C2 C3 N1 106.8(5) . . ? C2 C3 H3 126.6 . . ? N1 C3 H3 126.6 . . ? N2 C4 C5 112.2(5) . . ? N2 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? N2 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C4 C5 S1 112.8(5) . . ? C4 C5 H5A 109.0 . . ? S1 C5 H5A 109.0 . . ? C4 C5 H5B 109.0 . . ? S1 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C7 C6 S1 110.0(8) . . ? C7 C6 H6A 109.7 . . ? S1 C6 H6A 109.7 . . ? C7 C6 H6B 109.7 . . ? S1 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C1 N1 C3 110.8(5) . . ? C1 N1 C8 123.7(5) . . ? C3 N1 C8 125.6(5) . . ? C1 N2 C2 110.6(5) . . ? C1 N2 C4 124.0(5) . . ? C2 N2 C4 125.4(5) . . ? C5 S1 C6 105.7(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.933 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.255 # Attachment 'Complex_8_revised.cif' data_Complex8 _database_code_depnum_ccdc_archive 'CCDC 710769' _audit_creation_date 2008-09-30T17:09:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Compound X' _chemical_formula_sum 'C29 H35 Cl2 N2 P Pd S' _chemical_formula_weight 651.92 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# 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 12.8722(6) _cell_length_b 17.6615(5) _cell_length_c 18.3472(6) _cell_angle_alpha 90 _cell_angle_beta 133.128(2) _cell_angle_gamma 90 _cell_volume 3044.18(22) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15176 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_special_details ; ? ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.927 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.0243255 _diffrn_orient_matrix_ub_12 0.0536066 _diffrn_orient_matrix_ub_13 0.0061789 _diffrn_orient_matrix_ub_21 -0.0487208 _diffrn_orient_matrix_ub_22 0.0083023 _diffrn_orient_matrix_ub_23 0.0559706 _diffrn_orient_matrix_ub_31 0.0554387 _diffrn_orient_matrix_ub_32 -0.0162254 _diffrn_orient_matrix_ub_33 0.0490534 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_unetI/netI 0.0545 _diffrn_reflns_number 16443 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 5669 _reflns_number_gt 4361 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. In 8, the butyl and the ethyl moieties were severely disordered. Attempts to refine a satisfactory model for this disorder failed and the atoms were refined with restrained C-C distances (1.54 A) and anisotropic thermal parameters restrained to isotropic ones. ; _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^)+(0.1119P)^2^+4.9714P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0092(9) _refine_ls_number_reflns 5669 _refine_ls_number_parameters 329 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.083 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1874 _refine_ls_wR_factor_gt 0.1665 _refine_ls_goodness_of_fit_ref 1.1 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.245 _refine_diff_density_min -1.11 _refine_diff_density_rms 0.26 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 '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' Cl Cl 0.1484 0.1585 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 1.05257(4) 0.68705(2) 1.14164(3) 0.0247(2) Uani 1 1 d . . . P1 P 0.89423(16) 0.78300(8) 1.06649(11) 0.0275(4) Uani 1 1 d . . . Cl1 Cl 1.09210(16) 0.70195(9) 1.28655(10) 0.0329(4) Uani 1 1 d . . . Cl2 Cl 1.22163(16) 0.58866(8) 1.21404(11) 0.0381(4) Uani 1 1 d . . . N1 N 0.9250(5) 0.6085(3) 0.9535(4) 0.0331(11) Uani 1 1 d . . . N2 N 1.0639(6) 0.6970(3) 0.9827(4) 0.0341(12) Uani 1 1 d . . . S1 S 1.4353(3) 0.81665(16) 1.1522(2) 0.0895(9) Uani 1 1 d . . . C1 C 0.8566(7) 0.8241(3) 0.9598(5) 0.0338(14) Uani 1 1 d . . . C2 C 0.7740(7) 0.7848(4) 0.8695(5) 0.0382(15) Uani 1 1 d . . . H2 H 0.7261 0.7401 0.8614 0.046 Uiso 1 1 calc R . . C3 C 0.7601(8) 0.8090(4) 0.7918(5) 0.0443(17) Uani 1 1 d . . . H3 H 0.7027 0.7817 0.7307 0.053 Uiso 1 1 calc R . . C4 C 0.8305(8) 0.8734(4) 0.8041(5) 0.0524(19) Uani 1 1 d . . . H4 H 0.8236 0.8899 0.7516 0.063 Uiso 1 1 calc R . . C5 C 0.9109(10) 0.9143(4) 0.8913(6) 0.060(2) Uani 1 1 d . . . H5 H 0.958 0.9591 0.8986 0.072 Uiso 1 1 calc R . . C6 C 0.9230(8) 0.8899(4) 0.9691(5) 0.0484(18) Uani 1 1 d . . . H6 H 0.9774 0.9186 1.0289 0.058 Uiso 1 1 calc R . . C7 C 0.9511(7) 0.8645(3) 1.1470(5) 0.0355(14) Uani 1 1 d . . . C8 C 1.0938(8) 0.8797(4) 1.2242(5) 0.0435(16) Uani 1 1 d . . . H8 H 1.163 0.8465 1.2373 0.052 Uiso 1 1 calc R . . C9 C 1.1363(10) 0.9438(4) 1.2828(6) 0.057(2) Uani 1 1 d . . . H9 H 1.2347 0.9541 1.3366 0.068 Uiso 1 1 calc R . . C10 C 1.0357(12) 0.9920(4) 1.2629(7) 0.061(2) Uani 1 1 d . . . H10 H 1.0653 1.0356 1.3034 0.073 Uiso 1 1 calc R . . C11 C 0.8958(11) 0.9785(4) 1.1866(7) 0.059(2) Uani 1 1 d . . . H11 H 0.8278 1.013 1.173 0.071 Uiso 1 1 calc R . . C12 C 0.8505(9) 0.9146(4) 1.1279(6) 0.0497(18) Uani 1 1 d . . . H12 H 0.7517 0.9048 1.0749 0.06 Uiso 1 1 calc R . . C13 C 0.7224(6) 0.7547(4) 1.0195(4) 0.0346(14) Uani 1 1 d . . . C14 C 0.5941(7) 0.7899(4) 0.9371(5) 0.0491(18) Uani 1 1 d . . . H14 H 0.5954 0.8299 0.9031 0.059 Uiso 1 1 calc R . . C15 C 0.4667(8) 0.7663(5) 0.9056(6) 0.059(2) Uani 1 1 d . . . H15 H 0.3813 0.7916 0.8513 0.07 Uiso 1 1 calc R . . C16 C 0.4610(8) 0.7084(5) 0.9501(5) 0.0515(18) Uani 1 1 d U . . H16 H 0.3717 0.692 0.9257 0.062 Uiso 1 1 calc R . . C17 C 0.5838(7) 0.6727(4) 1.0308(5) 0.0474(17) Uani 1 1 d . . . H17 H 0.5794 0.6326 1.0632 0.057 Uiso 1 1 calc R . . C18 C 0.7152(7) 0.6951(4) 1.0652(5) 0.0383(15) Uani 1 1 d . . . H18 H 0.7997 0.6695 1.12 0.046 Uiso 1 1 calc R . . C19 C 1.0112(6) 0.6645(3) 1.0183(4) 0.0308(13) Uani 1 1 d . . . C20 C 0.9257(7) 0.6054(4) 0.8787(5) 0.0382(15) Uani 1 1 d . . . H20 H 0.8748 0.5704 0.8248 0.046 Uiso 1 1 calc R . . C21 C 1.0116(8) 0.6609(4) 0.8962(5) 0.0400(15) Uani 1 1 d . . . H21 H 1.0325 0.673 0.857 0.048 Uiso 1 1 calc R . . C22 C 0.8469(8) 0.5552(4) 0.9639(6) 0.0554(14) Uani 1 1 d U . . H22A H 0.8827 0.5611 1.0315 0.066 Uiso 1 1 calc R . . H22B H 0.8685 0.5028 0.9585 0.066 Uiso 1 1 calc R . . C23 C 0.6895(8) 0.5654(4) 0.8890(6) 0.0623(13) Uani 1 1 d DU . . H23A H 0.6524 0.5577 0.8213 0.075 Uiso 1 1 calc R . . H23B H 0.6671 0.618 0.893 0.075 Uiso 1 1 calc R . . C24 C 0.6124(7) 0.5088(5) 0.9055(6) 0.0705(15) Uani 1 1 d DU . . H24A H 0.6488 0.4567 0.9158 0.085 Uiso 1 1 calc R . . H24B H 0.629 0.5237 0.9647 0.085 Uiso 1 1 calc R . . C25 C 0.4543(8) 0.5125(6) 0.8116(7) 0.103(3) Uani 1 1 d DU . . H25A H 0.425 0.5656 0.7933 0.155 Uiso 1 1 calc R . . H25B H 0.3997 0.488 0.8243 0.155 Uiso 1 1 calc R . . H25C H 0.4366 0.4864 0.7569 0.155 Uiso 1 1 calc R . . C26 C 1.1628(7) 0.7599(4) 1.0289(6) 0.0497(14) Uani 1 1 d U . . H26A H 1.157 0.787 1.0733 0.06 Uiso 1 1 calc R A . H26B H 1.1333 0.7957 0.9761 0.06 Uiso 1 1 calc R . . C27 C 1.3146(8) 0.7371(4) 1.0886(6) 0.0552(14) Uani 1 1 d U . . H27A H 1.3225 0.7139 1.0434 0.066 Uiso 1 1 calc R . . H27B H 1.3426 0.6986 1.1385 0.066 Uiso 1 1 calc R . . C29 C 1.5007(15) 0.9225(8) 1.0852(11) 0.134(4) Uani 1 1 d U A 1 H29A H 1.5248 0.9567 1.1369 0.201 Uiso 1 1 calc R A 1 H29B H 1.4742 0.9523 1.0295 0.201 Uiso 1 1 calc R A 1 H29C H 1.5833 0.8908 1.1131 0.201 Uiso 1 1 calc R A 1 C28 C 1.3823(14) 0.8747(8) 1.0496(10) 0.124(4) Uani 1 1 d U A 1 H28A H 1.3541 0.8419 0.9948 0.149 Uiso 1 1 calc R A 1 H28B H 1.2996 0.9065 1.0235 0.149 Uiso 1 1 calc R A 1 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 0.0267(3) 0.0267(3) 0.0232(3) -0.00113(16) 0.0181(2) -0.00056(16) P1 0.0326(8) 0.0284(8) 0.0261(8) 0.0020(6) 0.0219(7) 0.0028(6) Cl1 0.0353(8) 0.0420(8) 0.0236(7) -0.0003(6) 0.0210(7) 0.0015(6) Cl2 0.0411(8) 0.0344(8) 0.0387(8) 0.0031(6) 0.0273(7) 0.0086(6) N1 0.042(3) 0.029(3) 0.031(3) -0.004(2) 0.026(2) -0.003(2) N2 0.044(3) 0.039(3) 0.035(3) -0.004(2) 0.033(3) -0.003(2) S1 0.0627(15) 0.099(2) 0.0692(17) 0.0015(13) 0.0305(14) -0.0226(13) C1 0.038(3) 0.037(3) 0.032(3) 0.008(3) 0.026(3) 0.006(3) C2 0.047(4) 0.034(3) 0.034(3) 0.003(3) 0.028(3) 0.003(3) C3 0.058(4) 0.043(4) 0.034(4) 0.005(3) 0.032(4) 0.002(3) C4 0.078(5) 0.048(4) 0.046(4) 0.005(3) 0.048(4) -0.004(4) C5 0.100(6) 0.044(4) 0.059(5) -0.006(4) 0.063(5) -0.019(4) C6 0.078(5) 0.034(4) 0.045(4) -0.006(3) 0.047(4) -0.010(3) C7 0.059(4) 0.027(3) 0.038(4) 0.002(3) 0.040(3) 0.003(3) C8 0.063(5) 0.036(3) 0.038(4) -0.003(3) 0.038(4) -0.006(3) C9 0.086(6) 0.045(4) 0.046(4) -0.006(3) 0.047(4) -0.019(4) C10 0.131(8) 0.018(3) 0.086(6) -0.009(3) 0.095(7) -0.012(4) C11 0.108(7) 0.032(4) 0.087(6) -0.003(4) 0.086(6) 0.004(4) C12 0.070(5) 0.042(4) 0.060(5) 0.002(3) 0.053(4) 0.011(3) C13 0.036(3) 0.044(4) 0.030(3) 0.003(3) 0.025(3) 0.007(3) C14 0.045(4) 0.059(4) 0.045(4) 0.023(3) 0.031(4) 0.020(3) C15 0.034(4) 0.087(6) 0.044(4) 0.017(4) 0.022(3) 0.019(4) C16 0.036(3) 0.074(4) 0.045(4) 0.005(3) 0.028(3) -0.002(3) C17 0.037(4) 0.069(5) 0.038(4) 0.000(3) 0.026(3) -0.011(3) C18 0.031(3) 0.051(4) 0.030(3) 0.006(3) 0.020(3) 0.004(3) C19 0.034(3) 0.030(3) 0.031(3) -0.002(2) 0.023(3) -0.001(3) C20 0.051(4) 0.040(4) 0.029(3) -0.005(3) 0.030(3) 0.002(3) C21 0.060(4) 0.042(4) 0.040(4) -0.001(3) 0.043(4) 0.001(3) C22 0.057(3) 0.056(3) 0.061(3) -0.004(2) 0.043(2) -0.019(2) C23 0.059(3) 0.058(3) 0.064(3) -0.003(2) 0.040(2) -0.020(2) C24 0.061(3) 0.059(3) 0.068(3) -0.002(2) 0.035(2) -0.022(2) C25 0.076(4) 0.086(4) 0.094(4) 0.002(4) 0.037(4) -0.024(4) C26 0.048(3) 0.056(3) 0.059(3) -0.005(3) 0.042(3) -0.009(2) C27 0.050(3) 0.056(3) 0.061(3) -0.005(3) 0.039(3) -0.008(2) C29 0.134(5) 0.140(5) 0.122(5) 0.007(4) 0.085(4) -0.044(4) C28 0.127(5) 0.135(5) 0.118(5) 0.007(4) 0.086(4) -0.040(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C19 1.978(6) . ? Pd1 P1 2.2549(15) . ? Pd1 Cl1 2.3554(15) . ? Pd1 Cl2 2.3596(15) . ? P1 C13 1.811(6) . ? P1 C1 1.816(6) . ? P1 C7 1.821(6) . ? N1 C19 1.350(7) . ? N1 C20 1.379(8) . ? N1 C22 1.482(8) . ? N2 C19 1.350(8) . ? N2 C21 1.385(8) . ? N2 C26 1.448(9) . ? S1 C27 1.808(8) . ? S1 C28 1.818(12) . ? C1 C6 1.382(9) . ? C1 C2 1.397(9) . ? C2 C3 1.377(9) . ? C2 H2 0.95 . ? C3 C4 1.373(10) . ? C3 H3 0.95 . ? C4 C5 1.375(10) . ? C4 H4 0.95 . ? C5 C6 1.393(10) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C8 1.376(9) . ? C7 C12 1.400(9) . ? C8 C9 1.389(10) . ? C8 H8 0.95 . ? C9 C10 1.375(12) . ? C9 H9 0.95 . ? C10 C11 1.347(12) . ? C10 H10 0.95 . ? C11 C12 1.383(10) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 C18 1.387(9) . ? C13 C14 1.409(9) . ? C14 C15 1.379(10) . ? C14 H14 0.95 . ? C15 C16 1.342(11) . ? C15 H15 0.95 . ? C16 C17 1.374(10) . ? C16 H16 0.95 . ? C17 C18 1.399(9) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? C20 C21 1.342(9) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C22 C23 1.489(11) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 C24 1.577(15) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 C25 1.523(14) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 C27 1.501(10) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C29 C28 1.450(15) . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? 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 C19 Pd1 P1 91.62(17) . . ? C19 Pd1 Cl1 174.25(18) . . ? P1 Pd1 Cl1 90.78(5) . . ? C19 Pd1 Cl2 85.35(17) . . ? P1 Pd1 Cl2 176.32(6) . . ? Cl1 Pd1 Cl2 92.43(5) . . ? C13 P1 C1 105.0(3) . . ? C13 P1 C7 106.7(3) . . ? C1 P1 C7 102.8(3) . . ? C13 P1 Pd1 112.5(2) . . ? C1 P1 Pd1 115.0(2) . . ? C7 P1 Pd1 113.8(2) . . ? C19 N1 C20 110.2(5) . . ? C19 N1 C22 124.9(5) . . ? C20 N1 C22 124.8(5) . . ? C19 N2 C21 110.3(5) . . ? C19 N2 C26 125.1(5) . . ? C21 N2 C26 124.6(6) . . ? C27 S1 C28 102.8(5) . . ? C6 C1 C2 118.0(6) . . ? C6 C1 P1 121.1(5) . . ? C2 C1 P1 120.4(5) . . ? C3 C2 C1 121.9(6) . . ? C3 C2 H2 119 . . ? C1 C2 H2 119 . . ? C4 C3 C2 118.9(7) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 120.9(7) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 119.9(7) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 120.5(6) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C8 C7 C12 119.3(6) . . ? C8 C7 P1 120.2(5) . . ? C12 C7 P1 120.4(5) . . ? C7 C8 C9 119.8(7) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 119.9(8) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.9(7) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 120.4(7) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 119.6(8) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C18 C13 C14 118.0(6) . . ? C18 C13 P1 119.1(5) . . ? C14 C13 P1 122.9(5) . . ? C15 C14 C13 120.1(7) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 121.3(7) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 120.3(7) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 120.1(7) . . ? C16 C17 H17 120 . . ? C18 C17 H17 120 . . ? C13 C18 C17 120.1(6) . . ? C13 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? N1 C19 N2 105.5(5) . . ? N1 C19 Pd1 124.9(4) . . ? N2 C19 Pd1 129.5(4) . . ? C21 C20 N1 107.3(5) . . ? C21 C20 H20 126.3 . . ? N1 C20 H20 126.3 . . ? C20 C21 N2 106.6(5) . . ? C20 C21 H21 126.7 . . ? N2 C21 H21 126.7 . . ? N1 C22 C23 114.8(6) . . ? N1 C22 H22A 108.6 . . ? C23 C22 H22A 108.6 . . ? N1 C22 H22B 108.6 . . ? C23 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? C22 C23 C24 112.6(6) . . ? C22 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? C22 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C23 106.6(7) . . ? C25 C24 H24A 110.4 . . ? C23 C24 H24A 110.4 . . ? C25 C24 H24B 110.4 . . ? C23 C24 H24B 110.4 . . ? H24A C24 H24B 108.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N2 C26 C27 114.0(6) . . ? N2 C26 H26A 108.8 . . ? C27 C26 H26A 108.8 . . ? N2 C26 H26B 108.8 . . ? C27 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? C26 C27 S1 112.3(5) . . ? C26 C27 H27A 109.2 . . ? S1 C27 H27A 109.2 . . ? C26 C27 H27B 109.2 . . ? S1 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C29 C28 S1 109.1(10) . . ? C29 C28 H28A 109.9 . . ? S1 C28 H28A 109.9 . . ? C29 C28 H28B 109.9 . . ? S1 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? # Attachment 'Complex_9_revised.cif' data_Complex9 _database_code_depnum_ccdc_archive 'CCDC 710770' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30.75 H30.50 Cl3.50 N2 P Pd S' _chemical_formula_weight 721.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 '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' C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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' H H 0.0000 0.0000 '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' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1476(2) _cell_length_b 14.9042(5) _cell_length_c 20.9556(6) _cell_angle_alpha 97.8810(10) _cell_angle_beta 90.739(2) _cell_angle_gamma 97.207(2) _cell_volume 3113.16(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 29832 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.48 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1462 _exptl_absorpt_coefficient_mu 1.039 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31306 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0775 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 26.50 _reflns_number_total 12890 _reflns_number_gt 8792 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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. The asymmetric unit of 9.0.75CH2Cl2 consisted in two crystallographically independent molecules of 9 and two dichloromethane molecules, one of which was found disordered in two positions close to the symmetry center, with an occupancy factor of 0.5. The latter was refined with restrained anisotropic thermal parameters and C-Cl distances (1.74 A). ; _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^)+(0.0994P)^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 12890 _refine_ls_number_parameters 711 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1677 _refine_ls_wR_factor_gt 0.1388 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.035 _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 C17B C 0.7006(6) 0.9956(4) 0.2210(3) 0.0434(15) Uani 1 1 d . . . H17B H 0.7586 1.0411 0.2453 0.052 Uiso 1 1 calc R . . Pd1A Pd 0.17935(3) 0.14388(3) 0.369538(17) 0.02250(12) Uani 1 1 d . . . P1A P 0.01430(12) 0.23025(9) 0.39171(6) 0.0235(3) Uani 1 1 d . . . C1A C 0.0697(4) 0.3412(3) 0.4404(2) 0.0261(11) Uani 1 1 d . . . C2A C 0.1367(5) 0.4095(4) 0.4091(3) 0.0310(12) Uani 1 1 d . . . H2A H 0.1416 0.4010 0.3644 0.037 Uiso 1 1 calc R . . C3A C 0.1963(5) 0.4904(4) 0.4449(3) 0.0369(13) Uani 1 1 d . . . H3A H 0.2416 0.5360 0.4244 0.044 Uiso 1 1 calc R . . C4A C 0.1873(5) 0.5019(4) 0.5110(3) 0.0394(15) Uani 1 1 d . . . H4A H 0.2295 0.5549 0.5352 0.047 Uiso 1 1 calc R . . C5A C 0.1188(5) 0.4379(4) 0.5411(3) 0.0356(14) Uani 1 1 d . . . H5A H 0.1108 0.4482 0.5856 0.043 Uiso 1 1 calc R . . C6A C 0.0597(5) 0.3564(4) 0.5062(2) 0.0310(12) Uani 1 1 d . . . H6A H 0.0133 0.3121 0.5275 0.037 Uiso 1 1 calc R . . C7A C -0.0698(4) 0.2601(3) 0.3228(2) 0.0247(11) Uani 1 1 d . . . C8A C -0.1467(5) 0.3321(4) 0.3300(3) 0.0308(12) Uani 1 1 d . . . H8A H -0.1516 0.3658 0.3705 0.037 Uiso 1 1 calc R . . C9A C -0.2154(5) 0.3540(4) 0.2786(3) 0.0333(12) Uani 1 1 d . . . H9A H -0.2664 0.4020 0.2844 0.040 Uiso 1 1 calc R . . C10A C -0.2083(5) 0.3039(4) 0.2181(3) 0.0356(13) Uani 1 1 d . . . H10A H -0.2550 0.3183 0.1831 0.043 Uiso 1 1 calc R . . C11A C -0.1330(5) 0.2336(4) 0.2096(3) 0.0345(13) Uani 1 1 d . . . H11A H -0.1289 0.2004 0.1689 0.041 Uiso 1 1 calc R . . C12A C -0.0624(5) 0.2111(4) 0.2612(3) 0.0312(12) Uani 1 1 d . . . H12A H -0.0105 0.1636 0.2548 0.037 Uiso 1 1 calc R . . C13A C -0.1124(4) 0.1721(3) 0.4380(2) 0.0244(11) Uani 1 1 d . . . C14A C -0.2476(5) 0.1697(4) 0.4243(3) 0.0345(13) Uani 1 1 d . . . H14A H -0.2758 0.1997 0.3915 0.041 Uiso 1 1 calc R . . C15A C -0.3398(5) 0.1227(4) 0.4597(3) 0.0346(13) Uani 1 1 d . . . H15A H -0.4300 0.1212 0.4504 0.042 Uiso 1 1 calc R . . C16A C -0.2996(5) 0.0780(4) 0.5084(3) 0.0380(14) Uani 1 1 d . . . H16A H -0.3626 0.0466 0.5318 0.046 Uiso 1 1 calc R . . C17A C -0.1650(5) 0.0798(4) 0.5226(3) 0.0368(13) Uani 1 1 d . . . H17A H -0.1374 0.0500 0.5556 0.044 Uiso 1 1 calc R . . C18A C -0.0738(5) 0.1259(4) 0.4874(3) 0.0323(12) Uani 1 1 d . . . H18A H 0.0162 0.1265 0.4966 0.039 Uiso 1 1 calc R . . C19A C 0.3176(4) 0.2486(3) 0.3990(2) 0.0249(11) Uani 1 1 d . . . C20A C 0.4676(5) 0.3486(4) 0.4593(3) 0.0385(14) Uani 1 1 d . . . H20A H 0.5192 0.3783 0.4948 0.046 Uiso 1 1 calc R . . C21A C 0.4733(5) 0.3697(4) 0.3990(3) 0.0397(14) Uani 1 1 d . . . H21A H 0.5287 0.4171 0.3849 0.048 Uiso 1 1 calc R . . C22A C 0.3563(5) 0.3028(4) 0.2925(3) 0.0357(13) Uani 1 1 d . . . H22A H 0.3750 0.3635 0.2804 0.043 Uiso 1 1 calc R . . H22B H 0.2636 0.2805 0.2816 0.043 Uiso 1 1 calc R . . C23A C 0.4445(5) 0.2395(4) 0.2552(3) 0.0374(13) Uani 1 1 d . . . H23A H 0.4231 0.1784 0.2664 0.045 Uiso 1 1 calc R . . H23B H 0.5367 0.2604 0.2679 0.045 Uiso 1 1 calc R . . C24A C 0.2681(5) 0.1649(4) 0.1500(3) 0.0352(13) Uani 1 1 d . . . C25A C 0.1959(6) 0.1806(5) 0.0969(3) 0.0503(16) Uani 1 1 d . . . H25A H 0.2273 0.2280 0.0743 0.060 Uiso 1 1 calc R . . C26A C 0.0762(7) 0.1258(6) 0.0771(3) 0.0610(19) Uani 1 1 d . . . H26A H 0.0278 0.1369 0.0416 0.073 Uiso 1 1 calc R . . C27A C 0.0314(6) 0.0561(5) 0.1100(3) 0.0553(18) Uani 1 1 d . . . H27A H -0.0468 0.0184 0.0964 0.066 Uiso 1 1 calc R . . C28A C 0.1013(6) 0.0413(4) 0.1632(3) 0.0454(15) Uani 1 1 d . . . H28A H 0.0689 -0.0054 0.1862 0.055 Uiso 1 1 calc R . . C29A C 0.2181(6) 0.0946(4) 0.1827(3) 0.0431(15) Uani 1 1 d . . . H29A H 0.2647 0.0833 0.2187 0.052 Uiso 1 1 calc R . . C30A C 0.3345(5) 0.2300(4) 0.5144(2) 0.0342(13) Uani 1 1 d . . . H30A H 0.2576 0.1857 0.5035 0.051 Uiso 1 1 calc R . . H30B H 0.3147 0.2747 0.5493 0.051 Uiso 1 1 calc R . . H30C H 0.4069 0.2000 0.5273 0.051 Uiso 1 1 calc R . . Cl1A Cl 0.35360(12) 0.05339(9) 0.35184(7) 0.0344(3) Uani 1 1 d . . . Cl2A Cl 0.01832(12) 0.02068(9) 0.33176(6) 0.0329(3) Uani 1 1 d . . . N1A N 0.3716(4) 0.2750(3) 0.4586(2) 0.0280(10) Uani 1 1 d . . . N2A N 0.3803(4) 0.3070(3) 0.3620(2) 0.0282(10) Uani 1 1 d . . . S1A S 0.42360(15) 0.23551(12) 0.16892(7) 0.0457(4) Uani 1 1 d . . . Pd1B Pd 0.65512(3) 0.65169(3) 0.249100(17) 0.02264(12) Uani 1 1 d . . . P1B P 0.68598(12) 0.72297(9) 0.16118(6) 0.0252(3) Uani 1 1 d . . . C1B C 0.5859(5) 0.6677(4) 0.0912(2) 0.0298(12) Uani 1 1 d . . . C2B C 0.4553(5) 0.6302(4) 0.1009(3) 0.0384(14) Uani 1 1 d . . . H2B H 0.4251 0.6300 0.1426 0.046 Uiso 1 1 calc R . . C3B C 0.3715(6) 0.5937(4) 0.0491(3) 0.0487(16) Uani 1 1 d . . . H3B H 0.2843 0.5698 0.0556 0.058 Uiso 1 1 calc R . . C4B C 0.4184(7) 0.5929(4) -0.0133(3) 0.0497(17) Uani 1 1 d . . . H4B H 0.3622 0.5696 -0.0486 0.060 Uiso 1 1 calc R . . C5B C 0.5471(7) 0.6266(4) -0.0221(3) 0.0495(16) Uani 1 1 d . . . H5B H 0.5782 0.6240 -0.0637 0.059 Uiso 1 1 calc R . . C6B C 0.6338(6) 0.6649(4) 0.0297(3) 0.0404(14) Uani 1 1 d . . . H6B H 0.7212 0.6878 0.0229 0.048 Uiso 1 1 calc R . . C7B C 0.8605(5) 0.7357(4) 0.1385(3) 0.0321(12) Uani 1 1 d . . . C8B C 0.9453(6) 0.6792(5) 0.1607(3) 0.0493(17) Uani 1 1 d . . . H8B H 0.9126 0.6333 0.1845 0.059 Uiso 1 1 calc R . . C9B C 1.0789(6) 0.6922(5) 0.1470(3) 0.062(2) Uani 1 1 d . . . H9B H 1.1366 0.6564 0.1630 0.074 Uiso 1 1 calc R . . C10B C 1.1266(6) 0.7567(5) 0.1104(3) 0.0503(17) Uani 1 1 d . . . H10B H 1.2159 0.7632 0.1001 0.060 Uiso 1 1 calc R . . C11B C 1.0432(5) 0.8126(4) 0.0884(3) 0.0411(14) Uani 1 1 d . . . H11B H 1.0766 0.8575 0.0640 0.049 Uiso 1 1 calc R . . C12B C 0.9118(5) 0.8022(4) 0.1022(3) 0.0350(13) Uani 1 1 d . . . H12B H 0.8559 0.8401 0.0871 0.042 Uiso 1 1 calc R . . C13B C 0.6475(5) 0.8401(4) 0.1712(2) 0.0277(11) Uani 1 1 d . . . C14B C 0.5270(6) 0.8615(4) 0.1492(3) 0.0452(16) Uani 1 1 d . . . H14B H 0.4680 0.8164 0.1251 0.054 Uiso 1 1 calc R . . C15B C 0.4947(7) 0.9475(5) 0.1625(4) 0.064(2) Uani 1 1 d . . . H15B H 0.4142 0.9613 0.1473 0.077 Uiso 1 1 calc R . . C16B C 0.5826(7) 1.0152(5) 0.1989(4) 0.0610(19) Uani 1 1 d . . . H16B H 0.5602 1.0741 0.2083 0.073 Uiso 1 1 calc R . . C18B C 0.7347(5) 0.9088(4) 0.2076(2) 0.0313(12) Uani 1 1 d . . . H18B H 0.8158 0.8957 0.2227 0.038 Uiso 1 1 calc R . . C19B C 0.6545(4) 0.7700(3) 0.3044(2) 0.0229(10) Uani 1 1 d . . . C20B C 0.7271(5) 0.8999(3) 0.3696(2) 0.0279(11) Uani 1 1 d . . . H20B H 0.7839 0.9455 0.3946 0.033 Uiso 1 1 calc R . . C21B C 0.5964(5) 0.8988(3) 0.3589(2) 0.0291(12) Uani 1 1 d . . . H21B H 0.5452 0.9435 0.3756 0.035 Uiso 1 1 calc R . . C22B C 0.4118(5) 0.7872(4) 0.3031(3) 0.0378(14) Uani 1 1 d . . . H22C H 0.4038 0.7477 0.2621 0.045 Uiso 1 1 calc R . . H22D H 0.3639 0.8386 0.2993 0.045 Uiso 1 1 calc R . . C23B C 0.3482(6) 0.7318(5) 0.3583(3) 0.0530(18) Uani 1 1 d . . . H23C H 0.3572 0.7721 0.3991 0.064 Uiso 1 1 calc R . . H23D H 0.3986 0.6817 0.3624 0.064 Uiso 1 1 calc R . . C24B C 0.1847(6) 0.5927(4) 0.2863(3) 0.0436(15) Uani 1 1 d . . . C25B C 0.0597(6) 0.5466(5) 0.2650(3) 0.0497(16) Uani 1 1 d . . . H25B H -0.0170 0.5650 0.2836 0.060 Uiso 1 1 calc R . . C26B C 0.0516(7) 0.4757(6) 0.2176(4) 0.068(2) Uani 1 1 d . . . H26B H -0.0319 0.4468 0.2027 0.082 Uiso 1 1 calc R . . C27B C 0.1626(8) 0.4442(5) 0.1902(4) 0.066(2) Uani 1 1 d . . . H27B H 0.1549 0.3950 0.1573 0.079 Uiso 1 1 calc R . . C28B C 0.2849(7) 0.4873(5) 0.2127(3) 0.0520(17) Uani 1 1 d . . . H28B H 0.3609 0.4666 0.1949 0.062 Uiso 1 1 calc R . . C29B C 0.2979(5) 0.5606(4) 0.2610(3) 0.0409(14) Uani 1 1 d . . . H29B H 0.3817 0.5882 0.2765 0.049 Uiso 1 1 calc R . . C30B C 0.8937(5) 0.7912(4) 0.3361(3) 0.0346(13) Uani 1 1 d . . . H30D H 0.8960 0.7444 0.3632 0.052 Uiso 1 1 calc R . . H30E H 0.9579 0.8426 0.3521 0.052 Uiso 1 1 calc R . . H30F H 0.9144 0.7679 0.2929 0.052 Uiso 1 1 calc R . . Cl1B Cl 0.66531(14) 0.51171(9) 0.18421(6) 0.0399(3) Uani 1 1 d . . . Cl2B Cl 0.63295(12) 0.58182(9) 0.34406(6) 0.0322(3) Uani 1 1 d . . . N1B N 0.7608(4) 0.8199(3) 0.33634(19) 0.0248(9) Uani 1 1 d . . . N2B N 0.5519(4) 0.8199(3) 0.31885(19) 0.0259(9) Uani 1 1 d . . . S1B S 0.18215(15) 0.68836(13) 0.34455(9) 0.0521(4) Uani 1 1 d . . . C31 C 0.3632(11) 0.9008(7) -0.0498(6) 0.126(4) Uani 1 1 d . . . H31A H 0.3526 0.9065 -0.0951 0.151 Uiso 1 1 calc R . . H31B H 0.4578 0.9070 -0.0397 0.151 Uiso 1 1 calc R . . Cl3 Cl 0.2979(2) 0.98872(19) -0.00521(13) 0.1039(9) Uani 1 1 d . . . Cl4 Cl 0.2946(3) 0.7951(2) -0.03804(13) 0.1277(12) Uani 1 1 d . . . C32 C -0.019(2) 0.5584(10) 0.0197(9) 0.1373(19) Uani 0.50 1 d PDU A -1 H32A H 0.0175 0.5925 0.0602 0.165 Uiso 0.50 1 calc PR A -1 H32B H -0.1146 0.5560 0.0207 0.165 Uiso 0.50 1 calc PR A -1 Cl5 Cl 0.0375(7) 0.6193(5) -0.0426(3) 0.1373(19) Uani 0.50 1 d PDU A -1 Cl6 Cl 0.0201(8) 0.4481(6) 0.0154(3) 0.1373(19) Uani 0.50 1 d PDU A -1 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 C17B 0.064(4) 0.032(3) 0.034(3) 0.006(3) 0.004(3) 0.004(3) Pd1A 0.0230(2) 0.0205(2) 0.0252(2) 0.00526(16) 0.00110(15) 0.00474(15) P1A 0.0248(6) 0.0224(7) 0.0248(7) 0.0050(5) 0.0021(5) 0.0068(5) C1A 0.026(2) 0.023(3) 0.031(3) 0.001(2) 0.003(2) 0.010(2) C2A 0.037(3) 0.028(3) 0.028(3) 0.001(2) 0.002(2) 0.005(2) C3A 0.040(3) 0.021(3) 0.049(4) 0.002(3) 0.001(3) 0.001(2) C4A 0.033(3) 0.034(3) 0.046(4) -0.017(3) -0.009(3) 0.009(3) C5A 0.034(3) 0.040(4) 0.030(3) -0.009(3) -0.005(2) 0.011(3) C6A 0.028(3) 0.036(3) 0.031(3) 0.006(2) 0.001(2) 0.010(2) C7A 0.023(2) 0.024(3) 0.028(3) 0.006(2) 0.0032(19) 0.006(2) C8A 0.036(3) 0.031(3) 0.027(3) 0.006(2) 0.002(2) 0.010(2) C9A 0.034(3) 0.028(3) 0.042(3) 0.014(3) 0.004(2) 0.007(2) C10A 0.039(3) 0.036(3) 0.033(3) 0.015(3) -0.009(2) 0.001(3) C11A 0.044(3) 0.031(3) 0.029(3) 0.003(2) -0.001(2) 0.004(3) C12A 0.032(3) 0.023(3) 0.040(3) 0.010(2) 0.001(2) 0.003(2) C13A 0.024(2) 0.022(3) 0.026(3) -0.001(2) 0.0019(19) 0.004(2) C14A 0.032(3) 0.037(3) 0.037(3) 0.006(3) 0.002(2) 0.012(2) C15A 0.029(3) 0.039(3) 0.036(3) 0.004(3) 0.005(2) 0.007(2) C16A 0.047(3) 0.031(3) 0.034(3) 0.000(3) 0.013(3) -0.002(3) C17A 0.044(3) 0.038(3) 0.030(3) 0.010(3) 0.004(2) 0.005(3) C18A 0.033(3) 0.030(3) 0.036(3) 0.008(2) 0.002(2) 0.007(2) C19A 0.025(2) 0.025(3) 0.027(3) 0.006(2) 0.002(2) 0.010(2) C20A 0.028(3) 0.039(4) 0.044(4) -0.003(3) -0.004(2) 0.001(2) C21A 0.027(3) 0.028(3) 0.061(4) 0.002(3) 0.005(3) -0.003(2) C22A 0.042(3) 0.032(3) 0.036(3) 0.013(3) 0.007(2) 0.006(2) C23A 0.036(3) 0.044(4) 0.033(3) 0.008(3) 0.005(2) 0.006(3) C24A 0.044(3) 0.037(3) 0.027(3) 0.006(3) 0.008(2) 0.010(3) C25A 0.063(4) 0.054(4) 0.038(4) 0.021(3) 0.003(3) 0.008(3) C26A 0.070(5) 0.074(6) 0.040(4) 0.014(4) -0.016(3) 0.010(4) C27A 0.049(4) 0.060(5) 0.055(4) -0.005(4) 0.002(3) 0.012(3) C28A 0.057(4) 0.040(4) 0.037(4) 0.003(3) 0.004(3) 0.005(3) C29A 0.056(4) 0.043(4) 0.035(3) 0.008(3) 0.001(3) 0.020(3) C30A 0.041(3) 0.040(3) 0.024(3) 0.012(2) -0.003(2) 0.005(3) Cl1A 0.0312(6) 0.0319(8) 0.0440(8) 0.0093(6) 0.0040(5) 0.0147(6) Cl2A 0.0320(6) 0.0255(7) 0.0394(8) 0.0029(6) -0.0011(5) -0.0008(5) N1A 0.026(2) 0.029(3) 0.029(2) 0.0034(19) -0.0024(17) 0.0035(18) N2A 0.030(2) 0.027(2) 0.028(2) 0.0085(19) 0.0063(18) 0.0030(18) S1A 0.0491(8) 0.0554(11) 0.0335(8) 0.0110(7) 0.0143(6) 0.0033(7) Pd1B 0.0262(2) 0.0209(2) 0.0220(2) 0.00379(16) 0.00087(15) 0.00686(15) P1B 0.0289(6) 0.0257(7) 0.0232(7) 0.0066(6) 0.0034(5) 0.0088(5) C1B 0.039(3) 0.028(3) 0.025(3) 0.006(2) -0.001(2) 0.011(2) C2B 0.045(3) 0.041(4) 0.029(3) -0.001(3) -0.003(2) 0.010(3) C3B 0.041(3) 0.050(4) 0.054(4) -0.001(3) -0.008(3) 0.012(3) C4B 0.075(5) 0.043(4) 0.032(4) 0.002(3) -0.014(3) 0.017(3) C5B 0.087(5) 0.039(4) 0.023(3) 0.006(3) 0.002(3) 0.008(3) C6B 0.056(3) 0.037(4) 0.029(3) 0.008(3) 0.003(3) 0.003(3) C7B 0.035(3) 0.034(3) 0.030(3) 0.008(2) 0.005(2) 0.012(2) C8B 0.045(3) 0.059(4) 0.056(4) 0.031(3) 0.016(3) 0.028(3) C9B 0.041(3) 0.090(6) 0.072(5) 0.047(4) 0.019(3) 0.034(4) C10B 0.036(3) 0.068(5) 0.052(4) 0.020(4) 0.014(3) 0.014(3) C11B 0.037(3) 0.050(4) 0.038(3) 0.012(3) 0.013(2) 0.005(3) C12B 0.036(3) 0.034(3) 0.037(3) 0.012(3) 0.003(2) 0.007(2) C13B 0.034(3) 0.027(3) 0.025(3) 0.010(2) 0.008(2) 0.009(2) C14B 0.043(3) 0.039(4) 0.056(4) 0.004(3) -0.008(3) 0.018(3) C15B 0.053(4) 0.049(5) 0.094(6) -0.001(4) -0.004(4) 0.033(4) C16B 0.079(5) 0.030(4) 0.079(5) 0.006(4) 0.011(4) 0.025(4) C18B 0.039(3) 0.025(3) 0.031(3) 0.011(2) 0.005(2) 0.004(2) C19B 0.030(2) 0.023(3) 0.018(2) 0.007(2) 0.0033(19) 0.007(2) C20B 0.037(3) 0.022(3) 0.024(3) 0.003(2) 0.000(2) 0.001(2) C21B 0.042(3) 0.021(3) 0.025(3) 0.000(2) 0.002(2) 0.009(2) C22B 0.027(3) 0.034(3) 0.052(4) 0.002(3) -0.002(2) 0.008(2) C23B 0.071(4) 0.052(4) 0.038(4) -0.010(3) -0.017(3) 0.031(3) C24B 0.045(3) 0.039(4) 0.053(4) 0.027(3) 0.010(3) 0.006(3) C25B 0.037(3) 0.058(5) 0.058(4) 0.028(4) 0.002(3) 0.002(3) C26B 0.052(4) 0.067(6) 0.088(6) 0.039(5) -0.011(4) -0.014(4) C27B 0.078(5) 0.041(4) 0.073(5) 0.019(4) -0.022(4) -0.023(4) C28B 0.058(4) 0.041(4) 0.060(4) 0.021(3) -0.004(3) 0.004(3) C29B 0.034(3) 0.038(4) 0.052(4) 0.010(3) -0.001(3) 0.006(3) C30B 0.030(3) 0.035(3) 0.040(3) 0.006(3) -0.003(2) 0.007(2) Cl1B 0.0635(9) 0.0276(8) 0.0305(7) -0.0011(6) -0.0059(6) 0.0194(7) Cl2B 0.0436(7) 0.0270(7) 0.0276(7) 0.0089(5) -0.0009(5) 0.0053(6) N1B 0.026(2) 0.023(2) 0.025(2) 0.0005(18) 0.0004(17) 0.0052(17) N2B 0.026(2) 0.025(2) 0.027(2) 0.0011(19) 0.0006(17) 0.0071(18) S1B 0.0380(8) 0.0567(11) 0.0630(11) 0.0112(9) 0.0123(7) 0.0075(7) C31 0.121(8) 0.095(9) 0.147(10) -0.023(7) 0.061(7) -0.007(6) Cl3 0.0882(15) 0.109(2) 0.1032(19) -0.0185(16) 0.0125(13) 0.0046(14) Cl4 0.198(3) 0.112(2) 0.1000(19) 0.0518(17) 0.082(2) 0.074(2) C32 0.140(4) 0.135(5) 0.117(4) -0.017(4) -0.034(3) -0.018(3) Cl5 0.140(4) 0.135(5) 0.117(4) -0.017(4) -0.034(3) -0.018(3) Cl6 0.140(4) 0.135(5) 0.117(4) -0.017(4) -0.034(3) -0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C17B C16B 1.358(9) . ? C17B C18B 1.374(8) . ? C17B H17B 0.9300 . ? Pd1A C19A 1.987(5) . ? Pd1A P1A 2.2528(12) . ? Pd1A Cl2A 2.3417(13) . ? Pd1A Cl1A 2.3583(12) . ? P1A C7A 1.804(5) . ? P1A C13A 1.825(5) . ? P1A C1A 1.838(5) . ? C1A C6A 1.374(7) . ? C1A C2A 1.397(7) . ? C2A C3A 1.392(7) . ? C2A H2A 0.9300 . ? C3A C4A 1.378(8) . ? C3A H3A 0.9300 . ? C4A C5A 1.342(8) . ? C4A H4A 0.9300 . ? C5A C6A 1.390(7) . ? C5A H5A 0.9300 . ? C6A H6A 0.9300 . ? C7A C8A 1.397(7) . ? C7A C12A 1.402(7) . ? C8A C9A 1.373(7) . ? C8A H8A 0.9300 . ? C9A C10A 1.389(7) . ? C9A H9A 0.9300 . ? C10A C11A 1.368(7) . ? C10A H10A 0.9300 . ? C11A C12A 1.390(7) . ? C11A H11A 0.9300 . ? C12A H12A 0.9300 . ? C13A C14A 1.394(7) . ? C13A C18A 1.396(7) . ? C14A C15A 1.382(8) . ? C14A H14A 0.9300 . ? C15A C16A 1.377(8) . ? C15A H15A 0.9300 . ? C16A C17A 1.390(8) . ? C16A H16A 0.9300 . ? C17A C18A 1.368(7) . ? C17A H17A 0.9300 . ? C18A H18A 0.9300 . ? C19A N1A 1.346(6) . ? C19A N2A 1.350(6) . ? C20A C21A 1.343(8) . ? C20A N1A 1.371(7) . ? C20A H20A 0.9300 . ? C21A N2A 1.389(7) . ? C21A H21A 0.9300 . ? C22A N2A 1.466(6) . ? C22A C23A 1.526(7) . ? C22A H22A 0.9700 . ? C22A H22B 0.9700 . ? C23A S1A 1.811(5) . ? C23A H23A 0.9700 . ? C23A H23B 0.9700 . ? C24A C29A 1.377(8) . ? C24A C25A 1.386(8) . ? C24A S1A 1.791(6) . ? C25A C26A 1.401(9) . ? C25A H25A 0.9300 . ? C26A C27A 1.358(10) . ? C26A H26A 0.9300 . ? C27A C28A 1.371(9) . ? C27A H27A 0.9300 . ? C28A C29A 1.366(8) . ? C28A H28A 0.9300 . ? C29A H29A 0.9300 . ? C30A N1A 1.457(7) . ? C30A H30A 0.9600 . ? C30A H30B 0.9600 . ? C30A H30C 0.9600 . ? Pd1B C19B 1.973(5) . ? Pd1B P1B 2.2559(14) . ? Pd1B Cl1B 2.3437(13) . ? Pd1B Cl2B 2.3698(13) . ? P1B C1B 1.811(5) . ? P1B C13B 1.821(5) . ? P1B C7B 1.833(5) . ? C1B C6B 1.381(7) . ? C1B C2B 1.400(8) . ? C2B C3B 1.377(8) . ? C2B H2B 0.9300 . ? C3B C4B 1.396(9) . ? C3B H3B 0.9300 . ? C4B C5B 1.363(9) . ? C4B H4B 0.9300 . ? C5B C6B 1.399(8) . ? C5B H5B 0.9300 . ? C6B H6B 0.9300 . ? C7B C12B 1.386(8) . ? C7B C8B 1.395(8) . ? C8B C9B 1.385(8) . ? C8B H8B 0.9300 . ? C9B C10B 1.357(9) . ? C9B H9B 0.9300 . ? C10B C11B 1.376(8) . ? C10B H10B 0.9300 . ? C11B C12B 1.363(7) . ? C11B H11B 0.9300 . ? C12B H12B 0.9300 . ? C13B C14B 1.391(7) . ? C13B C18B 1.398(7) . ? C14B C15B 1.356(8) . ? C14B H14B 0.9300 . ? C15B C16B 1.393(10) . ? C15B H15B 0.9300 . ? C16B H16B 0.9300 . ? C18B H18B 0.9300 . ? C19B N1B 1.345(6) . ? C19B N2B 1.368(6) . ? C20B C21B 1.339(7) . ? C20B N1B 1.380(6) . ? C20B H20B 0.9300 . ? C21B N2B 1.370(6) . ? C21B H21B 0.9300 . ? C22B N2B 1.462(6) . ? C22B C23B 1.607(9) . ? C22B H22C 0.9700 . ? C22B H22D 0.9700 . ? C23B S1B 1.733(7) . ? C23B H23C 0.9700 . ? C23B H23D 0.9700 . ? C24B C29B 1.383(8) . ? C24B C25B 1.401(8) . ? C24B S1B 1.749(7) . ? C25B C26B 1.341(10) . ? C25B H25B 0.9300 . ? C26B C27B 1.378(11) . ? C26B H26B 0.9300 . ? C27B C28B 1.370(9) . ? C27B H27B 0.9300 . ? C28B C29B 1.376(9) . ? C28B H28B 0.9300 . ? C29B H29B 0.9300 . ? C30B N1B 1.466(6) . ? C30B H30D 0.9600 . ? C30B H30E 0.9600 . ? C30B H30F 0.9600 . ? C31 Cl4 1.692(11) . ? C31 Cl3 1.711(9) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 Cl6 1.728(9) . ? C32 Cl5 1.750(10) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? 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 C16B C17B C18B 120.4(6) . . ? C16B C17B H17B 119.8 . . ? C18B C17B H17B 119.8 . . ? C19A Pd1A P1A 92.01(13) . . ? C19A Pd1A Cl2A 178.32(15) . . ? P1A Pd1A Cl2A 88.56(5) . . ? C19A Pd1A Cl1A 87.24(13) . . ? P1A Pd1A Cl1A 177.17(5) . . ? Cl2A Pd1A Cl1A 92.26(5) . . ? C7A P1A C13A 106.9(2) . . ? C7A P1A C1A 103.7(2) . . ? C13A P1A C1A 106.1(2) . . ? C7A P1A Pd1A 115.72(15) . . ? C13A P1A Pd1A 110.29(16) . . ? C1A P1A Pd1A 113.50(15) . . ? C6A C1A C2A 119.1(5) . . ? C6A C1A P1A 123.1(4) . . ? C2A C1A P1A 117.5(4) . . ? C3A C2A C1A 119.9(5) . . ? C3A C2A H2A 120.0 . . ? C1A C2A H2A 120.0 . . ? C4A C3A C2A 119.1(6) . . ? C4A C3A H3A 120.4 . . ? C2A C3A H3A 120.4 . . ? C5A C4A C3A 121.2(5) . . ? C5A C4A H4A 119.4 . . ? C3A C4A H4A 119.4 . . ? C4A C5A C6A 120.4(5) . . ? C4A C5A H5A 119.8 . . ? C6A C5A H5A 119.8 . . ? C1A C6A C5A 120.1(5) . . ? C1A C6A H6A 119.9 . . ? C5A C6A H6A 119.9 . . ? C8A C7A C12A 118.3(5) . . ? C8A C7A P1A 120.4(4) . . ? C12A C7A P1A 121.3(4) . . ? C9A C8A C7A 121.4(5) . . ? C9A C8A H8A 119.3 . . ? C7A C8A H8A 119.3 . . ? C8A C9A C10A 119.5(5) . . ? C8A C9A H9A 120.2 . . ? C10A C9A H9A 120.2 . . ? C11A C10A C9A 120.2(5) . . ? C11A C10A H10A 119.9 . . ? C9A C10A H10A 119.9 . . ? C10A C11A C12A 120.7(5) . . ? C10A C11A H11A 119.6 . . ? C12A C11A H11A 119.6 . . ? C11A C12A C7A 119.8(5) . . ? C11A C12A H12A 120.1 . . ? C7A C12A H12A 120.1 . . ? C14A C13A C18A 118.5(5) . . ? C14A C13A P1A 121.9(4) . . ? C18A C13A P1A 119.6(4) . . ? C15A C14A C13A 119.8(5) . . ? C15A C14A H14A 120.1 . . ? C13A C14A H14A 120.1 . . ? C16A C15A C14A 120.7(5) . . ? C16A C15A H15A 119.6 . . ? C14A C15A H15A 119.6 . . ? C15A C16A C17A 120.1(5) . . ? C15A C16A H16A 119.9 . . ? C17A C16A H16A 119.9 . . ? C18A C17A C16A 119.1(5) . . ? C18A C17A H17A 120.5 . . ? C16A C17A H17A 120.5 . . ? C17A C18A C13A 121.7(5) . . ? C17A C18A H18A 119.1 . . ? C13A C18A H18A 119.1 . . ? N1A C19A N2A 105.3(4) . . ? N1A C19A Pd1A 128.1(4) . . ? N2A C19A Pd1A 126.6(4) . . ? C21A C20A N1A 107.1(5) . . ? C21A C20A H20A 126.4 . . ? N1A C20A H20A 126.4 . . ? C20A C21A N2A 106.6(5) . . ? C20A C21A H21A 126.7 . . ? N2A C21A H21A 126.7 . . ? N2A C22A C23A 110.3(4) . . ? N2A C22A H22A 109.6 . . ? C23A C22A H22A 109.6 . . ? N2A C22A H22B 109.6 . . ? C23A C22A H22B 109.6 . . ? H22A C22A H22B 108.1 . . ? C22A C23A S1A 112.1(4) . . ? C22A C23A H23A 109.2 . . ? S1A C23A H23A 109.2 . . ? C22A C23A H23B 109.2 . . ? S1A C23A H23B 109.2 . . ? H23A C23A H23B 107.9 . . ? C29A C24A C25A 118.2(6) . . ? C29A C24A S1A 124.8(4) . . ? C25A C24A S1A 117.0(5) . . ? C24A C25A C26A 120.6(6) . . ? C24A C25A H25A 119.7 . . ? C26A C25A H25A 119.7 . . ? C27A C26A C25A 119.4(6) . . ? C27A C26A H26A 120.3 . . ? C25A C26A H26A 120.3 . . ? C26A C27A C28A 120.1(7) . . ? C26A C27A H27A 119.9 . . ? C28A C27A H27A 119.9 . . ? C29A C28A C27A 120.6(7) . . ? C29A C28A H28A 119.7 . . ? C27A C28A H28A 119.7 . . ? C28A C29A C24A 121.0(6) . . ? C28A C29A H29A 119.5 . . ? C24A C29A H29A 119.5 . . ? N1A C30A H30A 109.5 . . ? N1A C30A H30B 109.5 . . ? H30A C30A H30B 109.5 . . ? N1A C30A H30C 109.5 . . ? H30A C30A H30C 109.5 . . ? H30B C30A H30C 109.5 . . ? C19A N1A C20A 110.8(5) . . ? C19A N1A C30A 124.4(4) . . ? C20A N1A C30A 124.8(4) . . ? C19A N2A C21A 110.2(4) . . ? C19A N2A C22A 124.7(4) . . ? C21A N2A C22A 125.1(5) . . ? C24A S1A C23A 103.8(3) . . ? C19B Pd1B P1B 90.77(14) . . ? C19B Pd1B Cl1B 177.66(13) . . ? P1B Pd1B Cl1B 89.26(5) . . ? C19B Pd1B Cl2B 87.46(14) . . ? P1B Pd1B Cl2B 176.93(5) . . ? Cl1B Pd1B Cl2B 92.41(5) . . ? C1B P1B C13B 104.0(2) . . ? C1B P1B C7B 108.3(2) . . ? C13B P1B C7B 102.8(2) . . ? C1B P1B Pd1B 114.02(19) . . ? C13B P1B Pd1B 114.88(16) . . ? C7B P1B Pd1B 111.99(18) . . ? C6B C1B C2B 120.4(5) . . ? C6B C1B P1B 121.7(4) . . ? C2B C1B P1B 117.9(4) . . ? C3B C2B C1B 120.4(5) . . ? C3B C2B H2B 119.8 . . ? C1B C2B H2B 119.8 . . ? C2B C3B C4B 119.4(6) . . ? C2B C3B H3B 120.3 . . ? C4B C3B H3B 120.3 . . ? C5B C4B C3B 119.7(6) . . ? C5B C4B H4B 120.2 . . ? C3B C4B H4B 120.2 . . ? C4B C5B C6B 122.0(6) . . ? C4B C5B H5B 119.0 . . ? C6B C5B H5B 119.0 . . ? C1B C6B C5B 118.1(6) . . ? C1B C6B H6B 121.0 . . ? C5B C6B H6B 121.0 . . ? C12B C7B C8B 119.1(5) . . ? C12B C7B P1B 121.9(4) . . ? C8B C7B P1B 118.9(4) . . ? C9B C8B C7B 119.1(6) . . ? C9B C8B H8B 120.5 . . ? C7B C8B H8B 120.5 . . ? C10B C9B C8B 120.8(6) . . ? C10B C9B H9B 119.6 . . ? C8B C9B H9B 119.6 . . ? C9B C10B C11B 120.2(5) . . ? C9B C10B H10B 119.9 . . ? C11B C10B H10B 119.9 . . ? C12B C11B C10B 120.1(6) . . ? C12B C11B H11B 119.9 . . ? C10B C11B H11B 119.9 . . ? C11B C12B C7B 120.6(5) . . ? C11B C12B H12B 119.7 . . ? C7B C12B H12B 119.7 . . ? C14B C13B C18B 118.8(5) . . ? C14B C13B P1B 121.5(4) . . ? C18B C13B P1B 119.3(4) . . ? C15B C14B C13B 120.7(6) . . ? C15B C14B H14B 119.6 . . ? C13B C14B H14B 119.6 . . ? C14B C15B C16B 119.8(6) . . ? C14B C15B H15B 120.1 . . ? C16B C15B H15B 120.1 . . ? C17B C16B C15B 120.4(6) . . ? C17B C16B H16B 119.8 . . ? C15B C16B H16B 119.8 . . ? C17B C18B C13B 119.9(5) . . ? C17B C18B H18B 120.0 . . ? C13B C18B H18B 120.0 . . ? N1B C19B N2B 104.6(4) . . ? N1B C19B Pd1B 125.6(3) . . ? N2B C19B Pd1B 129.8(3) . . ? C21B C20B N1B 106.5(4) . . ? C21B C20B H20B 126.8 . . ? N1B C20B H20B 126.8 . . ? C20B C21B N2B 107.7(4) . . ? C20B C21B H21B 126.2 . . ? N2B C21B H21B 126.2 . . ? N2B C22B C23B 110.2(4) . . ? N2B C22B H22C 109.6 . . ? C23B C22B H22C 109.6 . . ? N2B C22B H22D 109.6 . . ? C23B C22B H22D 109.6 . . ? H22C C22B H22D 108.1 . . ? C22B C23B S1B 114.5(4) . . ? C22B C23B H23C 108.6 . . ? S1B C23B H23C 108.6 . . ? C22B C23B H23D 108.6 . . ? S1B C23B H23D 108.6 . . ? H23C C23B H23D 107.6 . . ? C29B C24B C25B 119.4(6) . . ? C29B C24B S1B 125.3(5) . . ? C25B C24B S1B 115.2(5) . . ? C26B C25B C24B 119.4(6) . . ? C26B C25B H25B 120.3 . . ? C24B C25B H25B 120.3 . . ? C25B C26B C27B 122.3(7) . . ? C25B C26B H26B 118.9 . . ? C27B C26B H26B 118.9 . . ? C28B C27B C26B 118.2(7) . . ? C28B C27B H27B 120.9 . . ? C26B C27B H27B 120.9 . . ? C27B C28B C29B 121.6(7) . . ? C27B C28B H28B 119.2 . . ? C29B C28B H28B 119.2 . . ? C28B C29B C24B 119.0(6) . . ? C28B C29B H29B 120.5 . . ? C24B C29B H29B 120.5 . . ? N1B C30B H30D 109.5 . . ? N1B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? N1B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C19B N1B C20B 111.1(4) . . ? C19B N1B C30B 123.7(4) . . ? C20B N1B C30B 125.2(4) . . ? C19B N2B C21B 110.1(4) . . ? C19B N2B C22B 124.8(4) . . ? C21B N2B C22B 124.3(4) . . ? C23B S1B C24B 104.2(3) . . ? Cl4 C31 Cl3 114.9(6) . . ? Cl4 C31 H31A 108.5 . . ? Cl3 C31 H31A 108.5 . . ? Cl4 C31 H31B 108.5 . . ? Cl3 C31 H31B 108.5 . . ? H31A C31 H31B 107.5 . . ? Cl6 C32 Cl5 116.6(11) . . ? Cl6 C32 H32A 108.1 . . ? Cl5 C32 H32A 108.1 . . ? Cl6 C32 H32B 108.1 . . ? Cl5 C32 H32B 108.1 . . ? H32A C32 H32B 107.3 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.079 _refine_diff_density_min -1.653 _refine_diff_density_rms 0.189 # Attachment 'Complex_10.cif' data_CF_GS3 _database_code_depnum_ccdc_archive 'CCDC 710771' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H35 Cl2 N2 P Pd S' _chemical_formula_sum 'C33 H35 Cl2 N2 P Pd S' _chemical_formula_weight 699.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 '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' C C 0.0033 0.0016 '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' S S 0.1246 0.1234 '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' H H 0.0000 0.0000 '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' _symmetry_int_tables_number 14 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 19.5332(10) _cell_length_b 9.1372(5) _cell_length_c 20.1256(8) _cell_angle_alpha 90.00 _cell_angle_beta 117.700(2) _cell_angle_gamma 90.00 _cell_volume 3180.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20012 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.988 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.893 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20288 _diffrn_reflns_av_R_equivalents 0.0927 _diffrn_reflns_av_sigmaI/netI 0.1223 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6256 _reflns_number_gt 3611 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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^)+(0.0750P)^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 6256 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1196 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1539 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.003 _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 0.67931(3) 0.02767(5) 0.82459(2) 0.02262(16) Uani 1 1 d . . . P1 P 0.74512(9) 0.07298(17) 0.94910(8) 0.0239(4) Uani 1 1 d . . . C1 C 0.8338(3) 0.1740(7) 0.9730(3) 0.0281(15) Uani 1 1 d . . . C2 C 0.8822(4) 0.1235(8) 0.9436(4) 0.0385(17) Uani 1 1 d . . . H2 H 0.8673 0.0436 0.9112 0.046 Uiso 1 1 calc R . . C3 C 0.9519(4) 0.1925(8) 0.9626(4) 0.0429(18) Uani 1 1 d . . . H3 H 0.9838 0.1581 0.9433 0.051 Uiso 1 1 calc R . . C4 C 0.9741(4) 0.3089(9) 1.0089(4) 0.049(2) Uani 1 1 d . . . H4 H 1.0211 0.3543 1.0213 0.059 Uiso 1 1 calc R . . C5 C 0.9268(4) 0.3617(8) 1.0384(4) 0.051(2) Uani 1 1 d . . . H5 H 0.9424 0.4419 1.0706 0.061 Uiso 1 1 calc R . . C6 C 0.8570(4) 0.2948(7) 1.0199(4) 0.0422(18) Uani 1 1 d . . . H6 H 0.8253 0.3311 1.0390 0.051 Uiso 1 1 calc R . . C7 C 0.6898(4) 0.1812(6) 0.9834(3) 0.0257(14) Uani 1 1 d . . . C8 C 0.6229(4) 0.2505(6) 0.9333(3) 0.0282(15) Uani 1 1 d . . . H8 H 0.6061 0.2413 0.8821 0.034 Uiso 1 1 calc R . . C9 C 0.5803(4) 0.3338(7) 0.9587(4) 0.0336(16) Uani 1 1 d . . . H9 H 0.5356 0.3812 0.9244 0.040 Uiso 1 1 calc R . . C10 C 0.6040(4) 0.3462(7) 1.0339(4) 0.0375(17) Uani 1 1 d . . . H10 H 0.5755 0.4019 1.0509 0.045 Uiso 1 1 calc R . . C11 C 0.6701(4) 0.2763(7) 1.0843(4) 0.0388(18) Uani 1 1 d . . . H11 H 0.6862 0.2857 1.1354 0.047 Uiso 1 1 calc R . . C12 C 0.7129(4) 0.1922(7) 1.0600(3) 0.0335(16) Uani 1 1 d . . . H12 H 0.7569 0.1434 1.0945 0.040 Uiso 1 1 calc R . . C13 C 0.7767(4) -0.0876(7) 1.0102(3) 0.0249(14) Uani 1 1 d . . . C14 C 0.8529(4) -0.1328(7) 1.0463(3) 0.0325(16) Uani 1 1 d . . . H14 H 0.8906 -0.0758 1.0429 0.039 Uiso 1 1 calc R . . C15 C 0.8742(4) -0.2608(7) 1.0873(3) 0.0393(17) Uani 1 1 d . . . H15 H 0.9257 -0.2898 1.1105 0.047 Uiso 1 1 calc R . . C16 C 0.8198(4) -0.3456(7) 1.0940(3) 0.0364(17) Uani 1 1 d . . . H16 H 0.8343 -0.4319 1.1217 0.044 Uiso 1 1 calc R . . C17 C 0.7426(4) -0.3018(7) 1.0590(3) 0.0370(17) Uani 1 1 d . . . H17 H 0.7055 -0.3587 1.0635 0.044 Uiso 1 1 calc R . . C18 C 0.7209(4) -0.1732(7) 1.0175(3) 0.0320(16) Uani 1 1 d . . . H18 H 0.6695 -0.1438 0.9945 0.038 Uiso 1 1 calc R . . C19 C 0.6506(3) -0.1722(6) 0.8410(3) 0.0227(14) Uani 1 1 d . . . C20 C 0.5823(4) -0.3606(7) 0.8486(3) 0.0351(17) Uani 1 1 d . . . H20 H 0.5416 -0.4147 0.8479 0.042 Uiso 1 1 calc R . . C21 C 0.6524(4) -0.4122(7) 0.8636(3) 0.0333(16) Uani 1 1 d . . . H21 H 0.6694 -0.5084 0.8751 0.040 Uiso 1 1 calc R . . C22 C 0.7713(3) -0.3060(7) 0.8636(3) 0.0283(15) Uani 1 1 d . . . H22A H 0.8025 -0.3741 0.9031 0.034 Uiso 1 1 calc R . . H22B H 0.7962 -0.2110 0.8764 0.034 Uiso 1 1 calc R . . C23 C 0.7668(4) -0.3577(7) 0.7897(3) 0.0333(16) Uani 1 1 d . . . H23A H 0.7327 -0.2928 0.7499 0.040 Uiso 1 1 calc R . . H23B H 0.7441 -0.4548 0.7785 0.040 Uiso 1 1 calc R . . C24 C 0.8811(4) -0.1776(8) 0.7835(3) 0.0353(17) Uani 1 1 d . . . C25 C 0.8298(4) -0.0635(8) 0.7650(3) 0.0374(17) Uani 1 1 d . . . H25 H 0.7796 -0.0811 0.7567 0.045 Uiso 1 1 calc R . . C26 C 0.8522(4) 0.0792(8) 0.7586(4) 0.0446(19) Uani 1 1 d . . . H26 H 0.8174 0.1562 0.7475 0.053 Uiso 1 1 calc R . . C27 C 0.9252(5) 0.1050(9) 0.7686(4) 0.052(2) Uani 1 1 d . . . H27 H 0.9401 0.1992 0.7634 0.062 Uiso 1 1 calc R . . C28 C 0.9767(5) -0.0093(9) 0.7865(4) 0.050(2) Uani 1 1 d . . . H28 H 1.0263 0.0081 0.7929 0.060 Uiso 1 1 calc R . . C29 C 0.9557(4) -0.1482(9) 0.7949(4) 0.0459(19) Uani 1 1 d . . . H29 H 0.9916 -0.2237 0.8084 0.055 Uiso 1 1 calc R . . C30 C 0.5144(3) -0.1163(7) 0.8118(3) 0.0316(16) Uani 1 1 d . . . H30A H 0.4691 -0.1669 0.7746 0.038 Uiso 1 1 calc R . . H30B H 0.5220 -0.0298 0.7881 0.038 Uiso 1 1 calc R . . C31 C 0.4990(4) -0.0690(7) 0.8757(3) 0.0328(16) Uani 1 1 d . . . H31A H 0.5453 -0.0246 0.9149 0.039 Uiso 1 1 calc R . . H31B H 0.4864 -0.1540 0.8968 0.039 Uiso 1 1 calc R . . C33 C 0.4153(4) 0.0915(8) 0.9107(4) 0.0453(19) Uani 1 1 d . . . H33A H 0.4031 0.0088 0.9327 0.068 Uiso 1 1 calc R . . H33B H 0.3720 0.1572 0.8901 0.068 Uiso 1 1 calc R . . H33C H 0.4595 0.1413 0.9484 0.068 Uiso 1 1 calc R . . C32 C 0.4330(4) 0.0396(8) 0.8488(3) 0.0396(17) Uani 1 1 d . . . H32A H 0.3871 -0.0055 0.8095 0.047 Uiso 1 1 calc R . . H32B H 0.4459 0.1236 0.8272 0.047 Uiso 1 1 calc R . . Cl1 Cl 0.70606(10) 0.26667(17) 0.80075(9) 0.0339(4) Uani 1 1 d . . . Cl2 Cl 0.60974(9) -0.02657(18) 0.69550(8) 0.0325(4) Uani 1 1 d . . . S1 S 0.85868(11) -0.3634(2) 0.79012(11) 0.0448(5) Uani 1 1 d . . . N1 N 0.5818(3) -0.2124(6) 0.8345(3) 0.0271(12) Uani 1 1 d . . . N2 N 0.6943(3) -0.2954(5) 0.8586(3) 0.0271(12) 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 0.0260(3) 0.0212(3) 0.0233(3) 0.0006(2) 0.0136(2) 0.0000(2) P1 0.0244(9) 0.0236(9) 0.0258(8) -0.0006(7) 0.0135(7) -0.0005(7) C1 0.030(4) 0.023(4) 0.028(3) 0.004(3) 0.011(3) 0.001(3) C2 0.037(4) 0.042(5) 0.041(4) -0.012(3) 0.022(4) -0.007(4) C3 0.036(5) 0.046(5) 0.052(5) 0.001(4) 0.026(4) -0.004(4) C4 0.031(4) 0.048(5) 0.066(5) 0.009(4) 0.021(4) -0.014(4) C5 0.050(5) 0.035(5) 0.069(5) -0.017(4) 0.028(4) -0.021(4) C6 0.042(5) 0.031(4) 0.056(5) -0.002(4) 0.025(4) 0.000(4) C7 0.030(4) 0.020(4) 0.027(3) 0.001(3) 0.014(3) 0.003(3) C8 0.032(4) 0.028(4) 0.027(3) -0.001(3) 0.015(3) -0.003(3) C9 0.037(4) 0.027(4) 0.041(4) 0.005(3) 0.021(3) 0.005(3) C10 0.044(5) 0.029(4) 0.054(5) -0.005(3) 0.034(4) 0.001(3) C11 0.054(5) 0.042(5) 0.034(4) -0.015(3) 0.031(4) -0.009(4) C12 0.035(4) 0.034(4) 0.029(4) -0.004(3) 0.013(3) 0.000(3) C13 0.032(4) 0.029(4) 0.016(3) -0.001(3) 0.013(3) 0.005(3) C14 0.025(4) 0.034(4) 0.036(4) 0.003(3) 0.012(3) 0.000(3) C15 0.042(5) 0.038(5) 0.035(4) 0.009(3) 0.015(3) 0.013(4) C16 0.051(5) 0.032(4) 0.029(3) 0.006(3) 0.021(4) 0.011(4) C17 0.048(5) 0.034(4) 0.036(4) 0.002(3) 0.026(4) -0.007(4) C18 0.033(4) 0.032(4) 0.034(4) 0.002(3) 0.019(3) -0.003(3) C19 0.028(4) 0.024(4) 0.019(3) 0.001(3) 0.013(3) -0.002(3) C20 0.042(5) 0.027(4) 0.043(4) -0.002(3) 0.026(4) -0.015(3) C21 0.045(5) 0.023(4) 0.042(4) -0.002(3) 0.028(4) -0.006(3) C22 0.028(4) 0.023(4) 0.032(3) 0.000(3) 0.013(3) 0.003(3) C23 0.037(4) 0.030(4) 0.047(4) -0.011(3) 0.031(3) -0.011(3) C24 0.034(4) 0.043(5) 0.034(4) -0.006(3) 0.021(3) -0.006(4) C25 0.032(4) 0.046(5) 0.043(4) -0.007(3) 0.024(3) -0.008(4) C26 0.060(5) 0.041(5) 0.039(4) -0.001(3) 0.027(4) 0.001(4) C27 0.055(6) 0.057(6) 0.055(5) -0.013(4) 0.035(4) -0.023(5) C28 0.035(5) 0.066(6) 0.052(5) -0.016(4) 0.024(4) -0.023(4) C29 0.035(5) 0.062(6) 0.043(4) -0.004(4) 0.021(4) -0.004(4) C30 0.023(4) 0.036(4) 0.035(4) 0.001(3) 0.012(3) -0.001(3) C31 0.032(4) 0.039(4) 0.032(4) -0.008(3) 0.019(3) -0.004(3) C33 0.047(5) 0.043(5) 0.055(5) -0.001(4) 0.032(4) 0.003(4) C32 0.035(4) 0.047(5) 0.038(4) -0.009(3) 0.018(3) 0.003(4) Cl1 0.0455(11) 0.0217(9) 0.0405(9) 0.0041(7) 0.0251(8) 0.0017(8) Cl2 0.0329(9) 0.0398(10) 0.0237(8) 0.0004(7) 0.0124(7) -0.0020(8) S1 0.0439(12) 0.0412(12) 0.0651(12) -0.0084(9) 0.0385(10) -0.0012(9) N1 0.028(3) 0.028(3) 0.028(3) -0.003(2) 0.016(2) -0.004(3) N2 0.028(3) 0.022(3) 0.035(3) -0.002(2) 0.018(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C19 1.982(6) . ? Pd1 P1 2.2601(15) . ? Pd1 Cl1 2.3463(16) . ? Pd1 Cl2 2.3580(15) . ? P1 C1 1.818(6) . ? P1 C7 1.821(6) . ? P1 C13 1.828(6) . ? C1 C6 1.384(9) . ? C1 C2 1.408(8) . ? C2 C3 1.382(9) . ? C2 H2 0.9300 . ? C3 C4 1.346(10) . ? C3 H3 0.9300 . ? C4 C5 1.395(9) . ? C4 H4 0.9300 . ? C5 C6 1.378(9) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.379(8) . ? C7 C12 1.393(8) . ? C8 C9 1.387(8) . ? C8 H8 0.9300 . ? C9 C10 1.367(8) . ? C9 H9 0.9300 . ? C10 C11 1.372(9) . ? C10 H10 0.9300 . ? C11 C12 1.382(8) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.382(8) . ? C13 C18 1.402(8) . ? C14 C15 1.379(8) . ? C14 H14 0.9300 . ? C15 C16 1.372(9) . ? C15 H15 0.9300 . ? C16 C17 1.394(9) . ? C16 H16 0.9300 . ? C17 C18 1.389(8) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 N1 1.340(7) . ? C19 N2 1.356(7) . ? C20 C21 1.343(9) . ? C20 N1 1.383(8) . ? C20 H20 0.9300 . ? C21 N2 1.377(8) . ? C21 H21 0.9300 . ? C22 N2 1.464(7) . ? C22 C23 1.523(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 S1 1.791(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.372(9) . ? C24 C29 1.391(9) . ? C24 S1 1.774(7) . ? C25 C26 1.400(10) . ? C25 H25 0.9300 . ? C26 C27 1.365(9) . ? C26 H26 0.9300 . ? C27 C28 1.376(10) . ? C27 H27 0.9300 . ? C28 C29 1.369(10) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 N1 1.467(7) . ? C30 C31 1.514(7) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.513(9) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C33 C32 1.516(8) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? 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 C19 Pd1 P1 92.48(16) . . ? C19 Pd1 Cl1 176.86(18) . . ? P1 Pd1 Cl1 89.44(6) . . ? C19 Pd1 Cl2 85.82(16) . . ? P1 Pd1 Cl2 178.30(6) . . ? Cl1 Pd1 Cl2 92.26(6) . . ? C1 P1 C7 106.5(3) . . ? C1 P1 C13 104.3(3) . . ? C7 P1 C13 104.7(2) . . ? C1 P1 Pd1 111.57(19) . . ? C7 P1 Pd1 112.8(2) . . ? C13 P1 Pd1 116.06(19) . . ? C6 C1 C2 118.5(6) . . ? C6 C1 P1 123.8(5) . . ? C2 C1 P1 117.8(5) . . ? C3 C2 C1 120.1(6) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.7(6) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120.3(7) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 119.9(7) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 120.6(6) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C8 C7 C12 119.0(5) . . ? C8 C7 P1 120.0(4) . . ? C12 C7 P1 120.9(5) . . ? C7 C8 C9 120.7(6) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 120.0(6) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 119.9(6) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 120.9(6) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C7 119.5(6) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C14 C13 C18 118.5(6) . . ? C14 C13 P1 122.5(5) . . ? C18 C13 P1 118.9(5) . . ? C15 C14 C13 121.3(6) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C16 C15 C14 120.4(6) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 119.6(6) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 120.2(6) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C13 120.0(6) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? N1 C19 N2 106.2(5) . . ? N1 C19 Pd1 125.8(4) . . ? N2 C19 Pd1 128.0(4) . . ? C21 C20 N1 107.4(6) . . ? C21 C20 H20 126.3 . . ? N1 C20 H20 126.3 . . ? C20 C21 N2 106.9(6) . . ? C20 C21 H21 126.6 . . ? N2 C21 H21 126.6 . . ? N2 C22 C23 111.3(5) . . ? N2 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? N2 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C22 C23 S1 113.7(4) . . ? C22 C23 H23A 108.8 . . ? S1 C23 H23A 108.8 . . ? C22 C23 H23B 108.8 . . ? S1 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? C25 C24 C29 118.4(7) . . ? C25 C24 S1 124.9(5) . . ? C29 C24 S1 116.7(6) . . ? C24 C25 C26 120.8(6) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C27 C26 C25 119.8(7) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 119.6(7) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C29 C28 C27 120.7(7) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C24 120.7(7) . . ? C28 C29 H29 119.7 . . ? C24 C29 H29 119.7 . . ? N1 C30 C31 114.2(5) . . ? N1 C30 H30A 108.7 . . ? C31 C30 H30A 108.7 . . ? N1 C30 H30B 108.7 . . ? C31 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? C30 C31 C32 110.8(5) . . ? C30 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C32 C33 113.1(5) . . ? C31 C32 H32A 109.0 . . ? C33 C32 H32A 109.0 . . ? C31 C32 H32B 109.0 . . ? C33 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C24 S1 C23 104.7(3) . . ? C19 N1 C20 109.7(5) . . ? C19 N1 C30 125.5(5) . . ? C20 N1 C30 124.7(5) . . ? C19 N2 C21 109.9(5) . . ? C19 N2 C22 125.1(5) . . ? C21 N2 C22 124.8(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.244 _refine_diff_density_min -1.481 _refine_diff_density_rms 0.236