# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Prof. T. S. Andy Hor' _publ_contact_author_email andyhor@nus.edu.sg loop_ _publ_author_name A.Hor 'Shi Bai' data_HOR _database_code_depnum_ccdc_archive 'CCDC 676819' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H31 Cl2 N O2 Pd S2' _chemical_formula_weight 462.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' O O 0.0106 0.0060 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.3641(7) _cell_length_b 13.4053(17) _cell_length_c 15.300(2) _cell_angle_alpha 67.357(2) _cell_angle_beta 84.856(2) _cell_angle_gamma 80.298(2) _cell_volume 1000.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3737 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 27.38 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 1.404 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6036 _exptl_absorpt_correction_T_max 0.9205 _exptl_absorpt_process_details 'Sababs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8989 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3524 _reflns_number_gt 3093 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+0.9973P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3524 _refine_ls_number_parameters 200 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1161 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.15315(6) 0.26900(3) 0.24947(2) 0.02101(15) Uani 1 1 d . . . S1 S 0.2398(2) 0.08787(9) 0.26865(8) 0.0272(3) Uani 1 1 d . . . S2 S 0.1008(2) 0.44590(10) 0.24205(9) 0.0299(3) Uani 1 1 d . . . Cl1 Cl -0.1015(2) 0.31200(11) 0.12360(9) 0.0355(3) Uani 1 1 d . . . Cl2 Cl 0.0099(2) 0.15543(11) 0.53918(9) 0.0368(3) Uani 1 1 d . . . N1 N 0.3748(7) 0.2298(3) 0.3610(3) 0.0270(9) Uani 1 1 d D . . H1N H 0.264(8) 0.208(4) 0.409(3) 0.032 Uiso 1 1 d D . . C1 C 0.5663(8) 0.1333(4) 0.3711(3) 0.0283(11) Uani 1 1 d . . . H1A H 0.6581 0.1106 0.4298 0.034 Uiso 1 1 calc R . . H1B H 0.6883 0.1504 0.3176 0.034 Uiso 1 1 calc R . . C2 C 0.4273(9) 0.0429(4) 0.3732(3) 0.0290(11) Uani 1 1 d . . . H2A H 0.3168 0.0220 0.4300 0.035 Uiso 1 1 calc R . . H2B H 0.5497 -0.0213 0.3761 0.035 Uiso 1 1 calc R . . C3 C 0.4778(9) 0.0922(4) 0.1751(3) 0.0328(11) Uani 1 1 d . . . H3A H 0.3916 0.1180 0.1149 0.039 Uiso 1 1 calc R . . H3B H 0.5861 0.1461 0.1706 0.039 Uiso 1 1 calc R . . C4 C 0.6416(13) -0.0127(5) 0.1871(5) 0.0621(19) Uani 1 1 d . . . H4 H 0.7574 -0.0270 0.2388 0.074 Uiso 1 1 calc R . . C5 C 0.8052(15) 0.0013(6) 0.0991(5) 0.082(3) Uani 1 1 d . . . H5A H 0.9315 -0.0630 0.1103 0.123 Uiso 1 1 calc R . . H5B H 0.8886 0.0651 0.0832 0.123 Uiso 1 1 calc R . . H5C H 0.7009 0.0107 0.0471 0.123 Uiso 1 1 calc R . . C6 C 0.5087(18) -0.1089(7) 0.2157(8) 0.103(3) Uani 1 1 d . . . H6A H 0.4083 -0.1152 0.2731 0.155 Uiso 1 1 calc R . . H6B H 0.6317 -0.1743 0.2274 0.155 Uiso 1 1 calc R . . H6C H 0.3988 -0.1004 0.1656 0.155 Uiso 1 1 calc R . . C7 C 0.4866(9) 0.3249(4) 0.3600(3) 0.0304(11) Uani 1 1 d . . . H7A H 0.5700 0.3062 0.4199 0.036 Uiso 1 1 calc R . . H7B H 0.6127 0.3453 0.3082 0.036 Uiso 1 1 calc R . . C8 C 0.2772(10) 0.4177(4) 0.3467(4) 0.0357(12) Uani 1 1 d . . . H8A H 0.3476 0.4831 0.3406 0.043 Uiso 1 1 calc R . . H8B H 0.1629 0.3998 0.4025 0.043 Uiso 1 1 calc R . . C9 C 0.3191(9) 0.5063(4) 0.1460(3) 0.0311(11) Uani 1 1 d . . . H9A H 0.4701 0.4523 0.1500 0.037 Uiso 1 1 calc R . . H9B H 0.2395 0.5230 0.0857 0.037 Uiso 1 1 calc R . . C10 C 0.4008(10) 0.6102(4) 0.1452(4) 0.0398(13) Uani 1 1 d . . . H10 H 0.4973 0.5921 0.2028 0.048 Uiso 1 1 calc R . . C11 C 0.5752(11) 0.6519(5) 0.0579(4) 0.0583(19) Uani 1 1 d . . . H11A H 0.7227 0.5972 0.0627 0.087 Uiso 1 1 calc R . . H11B H 0.6285 0.7189 0.0545 0.087 Uiso 1 1 calc R . . H11C H 0.4850 0.6658 0.0012 0.087 Uiso 1 1 calc R . . C12 C 0.1760(14) 0.6962(5) 0.1429(6) 0.069(2) Uani 1 1 d . . . H12A H 0.2352 0.7617 0.1407 0.103 Uiso 1 1 calc R . . H12B H 0.0704 0.6687 0.1994 0.103 Uiso 1 1 calc R . . H12C H 0.0785 0.7134 0.0872 0.103 Uiso 1 1 calc R . . O1W O 0.7971(12) 0.3714(4) 0.5688(5) 0.0891(18) Uani 1 1 d D . . H2W H 0.932(11) 0.348(6) 0.602(6) 0.107 Uiso 1 1 d D . . H1W H 0.805(16) 0.306(3) 0.570(6) 0.107 Uiso 1 1 d D . . O2W O 0.7353(12) 0.5602(5) 0.4014(5) 0.0916(18) Uani 1 1 d D . . H4W H 0.728(15) 0.527(3) 0.4598(17) 0.110 Uiso 1 1 d D . . H3W H 0.596(5) 0.601(4) 0.402(4) 0.110 Uiso 1 1 d 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 0.0101(2) 0.0258(2) 0.0242(2) -0.00629(15) 0.00015(13) -0.00266(13) S1 0.0168(6) 0.0280(6) 0.0327(6) -0.0067(5) 0.0000(5) -0.0042(5) S2 0.0193(6) 0.0305(6) 0.0391(7) -0.0138(5) 0.0032(5) -0.0021(5) Cl1 0.0260(6) 0.0432(7) 0.0344(7) -0.0101(5) -0.0121(5) -0.0019(5) Cl2 0.0249(6) 0.0432(7) 0.0369(7) -0.0110(6) 0.0064(5) -0.0047(5) N1 0.020(2) 0.032(2) 0.026(2) -0.0080(17) 0.0028(16) -0.0034(17) C1 0.016(2) 0.037(3) 0.025(2) -0.005(2) -0.0039(18) 0.001(2) C2 0.024(2) 0.028(2) 0.027(2) -0.002(2) -0.001(2) 0.001(2) C3 0.022(3) 0.044(3) 0.032(3) -0.015(2) 0.003(2) -0.008(2) C4 0.057(4) 0.048(4) 0.069(4) -0.018(3) 0.015(3) 0.007(3) C5 0.066(5) 0.087(5) 0.072(5) -0.028(4) 0.027(4) 0.024(4) C6 0.085(6) 0.067(5) 0.186(10) -0.084(6) 0.037(7) -0.022(5) C7 0.024(3) 0.041(3) 0.031(3) -0.015(2) 0.001(2) -0.013(2) C8 0.040(3) 0.037(3) 0.036(3) -0.019(2) 0.006(2) -0.010(2) C9 0.022(2) 0.033(3) 0.032(3) -0.005(2) -0.001(2) -0.004(2) C10 0.031(3) 0.036(3) 0.048(3) -0.007(2) -0.013(2) -0.010(2) C11 0.037(3) 0.065(4) 0.054(4) 0.011(3) -0.012(3) -0.031(3) C12 0.061(5) 0.036(3) 0.116(6) -0.032(4) -0.021(4) -0.008(3) O1W 0.091(5) 0.065(3) 0.121(5) -0.052(4) 0.008(4) -0.003(3) O2W 0.078(4) 0.107(5) 0.098(4) -0.055(4) 0.012(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 N1 2.016(4) . ? Pd1 Cl1 2.2932(12) . ? Pd1 S2 2.2998(13) . ? Pd1 S1 2.3007(13) . ? S1 C2 1.810(5) . ? S1 C3 1.821(5) . ? S2 C9 1.812(5) . ? S2 C8 1.813(5) . ? N1 C1 1.476(6) . ? N1 C7 1.493(6) . ? C1 C2 1.514(7) . ? C3 C4 1.483(8) . ? C4 C6 1.477(10) . ? C4 C5 1.505(9) . ? C7 C8 1.492(7) . ? C9 C10 1.525(7) . ? C10 C12 1.514(9) . ? C10 C11 1.532(8) . ? 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 N1 Pd1 Cl1 179.33(12) . . ? N1 Pd1 S2 86.89(12) . . ? Cl1 Pd1 S2 93.53(5) . . ? N1 Pd1 S1 86.91(12) . . ? Cl1 Pd1 S1 92.68(5) . . ? S2 Pd1 S1 173.70(4) . . ? C2 S1 C3 103.0(2) . . ? C2 S1 Pd1 96.49(16) . . ? C3 S1 Pd1 101.47(17) . . ? C9 S2 C8 103.1(2) . . ? C9 S2 Pd1 101.55(17) . . ? C8 S2 Pd1 96.62(17) . . ? C1 N1 C7 112.9(4) . . ? C1 N1 Pd1 111.8(3) . . ? C7 N1 Pd1 112.5(3) . . ? N1 C1 C2 107.3(4) . . ? C1 C2 S1 110.4(3) . . ? C4 C3 S1 115.7(4) . . ? C6 C4 C3 115.4(6) . . ? C6 C4 C5 112.5(7) . . ? C3 C4 C5 109.1(5) . . ? C8 C7 N1 107.9(4) . . ? C7 C8 S2 111.0(3) . . ? C10 C9 S2 114.4(4) . . ? C12 C10 C9 111.8(5) . . ? C12 C10 C11 110.9(5) . . ? C9 C10 C11 107.3(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N Cl2 0.895(19) 2.25(2) 3.140(4) 175(5) . O1W H2W O2W 0.87(2) 2.32(7) 2.939(10) 129(7) 2_766 O1W H1W Cl2 0.86(2) 2.32(5) 3.114(5) 152(8) 1_655 O2W H4W O1W 0.831(19) 2.106(19) 2.820(9) 144(4) . O2W H3W O1W 0.850(18) 2.115(19) 2.900(8) 153(5) 2_666 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.481 _refine_diff_density_min -1.176 _refine_diff_density_rms 0.144 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 676820' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H23 Cl2 N Pd S2' _chemical_formula_weight 494.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3815(6) _cell_length_b 5.6441(3) _cell_length_c 28.7929(15) _cell_angle_alpha 90.00 _cell_angle_beta 99.3760(10) _cell_angle_gamma 90.00 _cell_volume 1985.24(18) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5492 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 27.44 _exptl_crystal_description BLOCK _exptl_crystal_colour BLUE _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 1.415 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4376 _exptl_absorpt_correction_T_max 0.8715 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13376 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4540 _reflns_number_gt 4076 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+0.8159P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4540 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0621 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.617448(11) 0.20442(3) 0.132441(5) 0.02214(6) Uani 1 1 d . . . Cl1 Cl 0.71794(5) -0.07170(11) 0.18041(2) 0.04043(14) Uani 1 1 d . . . Cl2 Cl 0.36054(4) 0.07727(9) 0.038524(19) 0.03346(12) Uani 1 1 d . . . S1 S 0.48487(4) 0.22022(9) 0.179396(18) 0.02587(11) Uani 1 1 d . . . S2 S 0.74400(4) 0.22918(10) 0.082698(19) 0.02758(12) Uani 1 1 d . . . N1 N 0.52691(13) 0.4438(3) 0.09013(6) 0.0227(3) Uani 1 1 d . . . C1 C 0.45795(17) 0.5904(4) 0.11663(7) 0.0285(4) Uani 1 1 d . . . H1A H 0.4077 0.6882 0.0948 0.034 Uiso 1 1 calc R . . H1B H 0.5043 0.6956 0.1385 0.034 Uiso 1 1 calc R . . C2 C 0.39388(16) 0.4264(4) 0.14356(7) 0.0294(5) Uani 1 1 d . . . H2A H 0.3403 0.3377 0.1214 0.035 Uiso 1 1 calc R . . H2B H 0.3538 0.5201 0.1638 0.035 Uiso 1 1 calc R . . C3 C 0.54675(17) 0.4045(4) 0.22908(7) 0.0320(5) Uani 1 1 d . . . H3A H 0.6128 0.3274 0.2457 0.038 Uiso 1 1 calc R . . H3B H 0.5677 0.5585 0.2176 0.038 Uiso 1 1 calc R . . C4 C 0.46613(17) 0.4393(4) 0.26200(7) 0.0272(4) Uani 1 1 d . . . C5 C 0.39947(19) 0.6391(4) 0.25933(8) 0.0331(5) Uani 1 1 d . . . H5 H 0.4086 0.7604 0.2379 0.040 Uiso 1 1 calc R . . C6 C 0.3202(2) 0.6619(4) 0.28765(8) 0.0365(5) Uani 1 1 d . . . H6 H 0.2749 0.7965 0.2850 0.044 Uiso 1 1 calc R . . C7 C 0.30729(18) 0.4859(4) 0.31999(8) 0.0340(5) Uani 1 1 d . . . H7 H 0.2533 0.5009 0.3393 0.041 Uiso 1 1 calc R . . C8 C 0.37411(18) 0.2889(4) 0.32364(8) 0.0316(5) Uani 1 1 d . . . H8 H 0.3662 0.1705 0.3458 0.038 Uiso 1 1 calc R . . C9 C 0.45272(18) 0.2646(4) 0.29490(8) 0.0305(5) Uani 1 1 d . . . H9 H 0.4975 0.1293 0.2976 0.037 Uiso 1 1 calc R . . C10 C 0.59495(16) 0.5913(4) 0.06333(7) 0.0269(4) Uani 1 1 d . . . H10A H 0.6392 0.7023 0.0847 0.032 Uiso 1 1 calc R . . H10B H 0.5476 0.6833 0.0393 0.032 Uiso 1 1 calc R . . C11 C 0.66896(17) 0.4324(4) 0.04015(7) 0.0293(4) Uani 1 1 d . . . H11A H 0.7208 0.5297 0.0262 0.035 Uiso 1 1 calc R . . H11B H 0.6249 0.3418 0.0148 0.035 Uiso 1 1 calc R . . C12 C 0.84558(17) 0.4202(4) 0.11765(8) 0.0354(5) Uani 1 1 d . . . H12A H 0.8104 0.5681 0.1249 0.043 Uiso 1 1 calc R . . H12B H 0.8739 0.3413 0.1475 0.043 Uiso 1 1 calc R . . C13 C 0.93917(16) 0.4763(4) 0.09212(7) 0.0268(4) Uani 1 1 d . . . C14 C 0.9452(2) 0.6894(4) 0.06872(9) 0.0377(5) Uani 1 1 d . . . H14 H 0.8877 0.7994 0.0670 0.045 Uiso 1 1 calc R . . C15 C 1.0353(3) 0.7403(5) 0.04792(9) 0.0496(7) Uani 1 1 d . . . H15 H 1.0396 0.8864 0.0327 0.059 Uiso 1 1 calc R . . C16 C 1.1187(2) 0.5786(5) 0.04944(9) 0.0501(7) Uani 1 1 d . . . H16 H 1.1805 0.6155 0.0358 0.060 Uiso 1 1 calc R . . C17 C 1.11180(18) 0.3642(5) 0.07080(9) 0.0440(6) Uani 1 1 d . . . H17 H 1.1675 0.2510 0.0707 0.053 Uiso 1 1 calc R . . C18 C 1.02318(17) 0.3143(4) 0.09239(8) 0.0321(5) Uani 1 1 d . . . H18 H 1.0196 0.1678 0.1076 0.039 Uiso 1 1 calc R . . H1N H 0.4839(19) 0.349(4) 0.0716(9) 0.032(6) Uiso 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 0.01949(8) 0.02390(9) 0.02304(9) -0.00004(6) 0.00355(6) 0.00122(6) Cl1 0.0394(3) 0.0413(3) 0.0378(3) 0.0068(2) -0.0022(2) 0.0129(3) Cl2 0.0350(3) 0.0298(3) 0.0356(3) -0.0024(2) 0.0058(2) -0.0017(2) S1 0.0245(2) 0.0296(3) 0.0243(3) 0.0022(2) 0.0061(2) -0.0021(2) S2 0.0218(2) 0.0329(3) 0.0288(3) -0.0064(2) 0.0065(2) 0.0005(2) N1 0.0212(8) 0.0241(9) 0.0231(8) 0.0010(7) 0.0040(7) -0.0002(7) C1 0.0275(10) 0.0295(11) 0.0292(11) 0.0019(9) 0.0074(8) 0.0066(9) C2 0.0205(9) 0.0410(12) 0.0268(11) 0.0010(9) 0.0040(8) 0.0037(9) C3 0.0285(10) 0.0418(13) 0.0252(11) -0.0014(9) 0.0027(8) -0.0050(10) C4 0.0287(10) 0.0309(11) 0.0211(10) -0.0028(8) 0.0011(8) -0.0024(9) C5 0.0440(13) 0.0259(11) 0.0286(11) 0.0013(9) 0.0038(9) -0.0005(10) C6 0.0409(13) 0.0291(12) 0.0384(13) -0.0052(9) 0.0036(10) 0.0083(10) C7 0.0335(11) 0.0409(13) 0.0281(11) -0.0080(9) 0.0065(9) 0.0018(10) C8 0.0353(11) 0.0355(12) 0.0240(11) 0.0034(9) 0.0046(9) -0.0002(10) C9 0.0322(11) 0.0313(11) 0.0266(11) 0.0013(9) 0.0006(9) 0.0078(9) C10 0.0277(10) 0.0280(11) 0.0263(10) 0.0026(8) 0.0080(8) -0.0018(9) C11 0.0289(10) 0.0369(12) 0.0228(10) 0.0003(9) 0.0066(8) -0.0021(9) C12 0.0234(10) 0.0487(14) 0.0344(12) -0.0141(10) 0.0052(9) -0.0038(10) C13 0.0227(9) 0.0307(11) 0.0263(10) -0.0080(8) 0.0018(8) -0.0018(8) C14 0.0418(13) 0.0291(12) 0.0392(13) -0.0047(10) -0.0020(10) 0.0049(10) C15 0.076(2) 0.0426(14) 0.0303(13) -0.0005(11) 0.0078(13) -0.0226(14) C16 0.0457(14) 0.071(2) 0.0381(14) -0.0239(13) 0.0213(12) -0.0251(14) C17 0.0235(10) 0.0534(16) 0.0550(16) -0.0262(13) 0.0056(10) 0.0003(11) C18 0.0259(10) 0.0312(12) 0.0376(12) -0.0046(9) 0.0000(9) 0.0015(9) _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 N1 2.0300(16) . ? Pd1 S1 2.2920(5) . ? Pd1 S2 2.2929(5) . ? Pd1 Cl1 2.3075(6) . ? S1 C2 1.819(2) . ? S1 C3 1.833(2) . ? S2 C11 1.819(2) . ? S2 C12 1.829(2) . ? N1 C1 1.486(2) . ? N1 C10 1.487(2) . ? C1 C2 1.513(3) . ? C3 C4 1.497(3) . ? C4 C5 1.392(3) . ? C4 C9 1.396(3) . ? C5 C6 1.380(3) . ? C6 C7 1.388(3) . ? C7 C8 1.380(3) . ? C8 C9 1.383(3) . ? C10 C11 1.513(3) . ? C12 C13 1.504(3) . ? C13 C18 1.384(3) . ? C13 C14 1.387(3) . ? C14 C15 1.380(4) . ? C15 C16 1.374(4) . ? C16 C17 1.367(4) . ? C17 C18 1.376(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 S1 87.11(5) . . ? N1 Pd1 S2 87.21(5) . . ? S1 Pd1 S2 173.75(2) . . ? N1 Pd1 Cl1 179.07(5) . . ? S1 Pd1 Cl1 92.37(2) . . ? S2 Pd1 Cl1 93.34(2) . . ? C2 S1 C3 102.78(11) . . ? C2 S1 Pd1 97.31(7) . . ? C3 S1 Pd1 103.54(7) . . ? C11 S2 C12 103.24(11) . . ? C11 S2 Pd1 97.65(7) . . ? C12 S2 Pd1 99.84(7) . . ? C1 N1 C10 112.10(16) . . ? C1 N1 Pd1 111.71(12) . . ? C10 N1 Pd1 112.33(12) . . ? N1 C1 C2 108.40(17) . . ? C1 C2 S1 110.74(14) . . ? C4 C3 S1 109.36(14) . . ? C5 C4 C9 118.3(2) . . ? C5 C4 C3 121.4(2) . . ? C9 C4 C3 120.16(19) . . ? C6 C5 C4 121.0(2) . . ? C5 C6 C7 120.0(2) . . ? C8 C7 C6 119.6(2) . . ? C7 C8 C9 120.4(2) . . ? C8 C9 C4 120.6(2) . . ? N1 C10 C11 109.40(17) . . ? C10 C11 S2 110.87(14) . . ? C13 C12 S2 111.76(15) . . ? C18 C13 C14 118.4(2) . . ? C18 C13 C12 119.8(2) . . ? C14 C13 C12 121.8(2) . . ? C15 C14 C13 120.2(2) . . ? C16 C15 C14 120.3(2) . . ? C17 C16 C15 120.1(2) . . ? C16 C17 C18 119.8(2) . . ? C17 C18 C13 121.1(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.426 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.075 #===END