# Electronic Supplementary Material for CrystEngComm # 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 'T. S. Andy Hor' _publ_contact_author_email ANDYHOR@NUS.EDU.SG _publ_section_title ; Crystallographic Analysis of Different Water-Halide Cluster Blends in Cationic [(SNS)PdII] Pincer Complexes ; loop_ _publ_author_name 'Andy Hor' 'Shi Bai' 'Lip Lin Koh' 'Gabriel Y. H. Quek' # Attachment 'Dalton-CIF.cif' data_8249 _database_code_depnum_ccdc_archive 'CCDC 729211' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H21 Cl2 N O Pd S2' _chemical_formula_weight 388.68 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.1868(3) _cell_length_b 11.4095(6) _cell_length_c 12.8769(7) _cell_angle_alpha 86.3600(10) _cell_angle_beta 89.3090(10) _cell_angle_gamma 77.1710(10) _cell_volume 741.52(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5672 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.52 _exptl_crystal_description PLATE _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 392 _exptl_absorpt_coefficient_mu 1.871 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.3998 _exptl_absorpt_correction_T_max 0.8647 _exptl_absorpt_process_details 'Sababs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 9699 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3401 _reflns_number_gt 3182 _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^)+(0.0195P)^2^+0.2670P] 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 3401 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0211 _refine_ls_wR_factor_ref 0.0505 _refine_ls_wR_factor_gt 0.0497 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 0.41336(3) 0.293603(12) 0.726704(11) 0.02333(5) Uani 1 1 d . . . S1 S 0.29073(9) 0.49950(4) 0.73730(4) 0.02840(11) Uani 1 1 d . . . S2 S 0.50090(10) 0.08736(4) 0.72670(4) 0.03241(11) Uani 1 1 d . . . Cl1 Cl 0.66265(11) 0.30784(5) 0.57991(4) 0.03710(12) Uani 1 1 d . . . N1 N 0.1928(3) 0.27880(16) 0.85625(13) 0.0279(3) Uani 1 1 d . . . C1 C -0.0225(4) 0.3884(2) 0.86433(16) 0.0338(4) Uani 1 1 d . . . H1A H -0.1123 0.3846 0.9306 0.041 Uiso 1 1 calc R . . H1B H -0.1508 0.3931 0.8092 0.041 Uiso 1 1 calc R . . C2 C 0.0958(4) 0.4978(2) 0.85547(16) 0.0343(5) Uani 1 1 d . . . H2A H 0.2074 0.4975 0.9155 0.041 Uiso 1 1 calc R . . H2B H -0.0444 0.5700 0.8547 0.041 Uiso 1 1 calc R . . C3 C 0.0415(4) 0.54070(19) 0.63538(16) 0.0344(4) Uani 1 1 d . . . H3A H 0.1279 0.5330 0.5682 0.041 Uiso 1 1 calc R . . H3B H -0.0755 0.4851 0.6409 0.041 Uiso 1 1 calc R . . C4 C -0.1200(5) 0.6672(2) 0.6410(2) 0.0504(6) Uani 1 1 d . . . H4A H -0.2237 0.6727 0.7035 0.076 Uiso 1 1 calc R . . H4B H -0.2352 0.6874 0.5817 0.076 Uiso 1 1 calc R . . H4C H -0.0042 0.7221 0.6415 0.076 Uiso 1 1 calc R . . C5 C 0.0987(5) 0.1652(2) 0.86207(17) 0.0380(5) Uani 1 1 d . . . H5A H -0.0328 0.1683 0.8085 0.046 Uiso 1 1 calc R . . H5B H 0.0177 0.1542 0.9292 0.046 Uiso 1 1 calc R . . C6 C 0.3297(5) 0.0620(2) 0.84715(17) 0.0404(5) Uani 1 1 d . . . H6A H 0.2679 -0.0121 0.8453 0.048 Uiso 1 1 calc R . . H6B H 0.4509 0.0536 0.9053 0.048 Uiso 1 1 calc R . . C7 C 0.2743(4) 0.06300(19) 0.62793(17) 0.0371(5) Uani 1 1 d . . . H7A H 0.1000 0.1125 0.6399 0.045 Uiso 1 1 calc R . . H7B H 0.3335 0.0879 0.5600 0.045 Uiso 1 1 calc R . . C8 C 0.2560(6) -0.0673(2) 0.6285(2) 0.0572(7) Uani 1 1 d . . . H8A H 0.4307 -0.1176 0.6265 0.086 Uiso 1 1 calc R . . H8B H 0.1578 -0.0789 0.5687 0.086 Uiso 1 1 calc R . . H8C H 0.1679 -0.0882 0.6907 0.086 Uiso 1 1 calc R . . H1N H 0.283(4) 0.2740(18) 0.9057(17) 0.022(5) Uiso 1 1 d . . . Cl2 Cl 0.51179(10) 0.28828(5) 1.06170(4) 0.03788(12) Uani 1 1 d . . . O1W O 1.0815(5) 0.1334(2) 1.13178(18) 0.0614(6) Uani 1 1 d . . . H2W H 1.189(7) 0.172(3) 1.117(3) 0.070(11) Uiso 1 1 d . . . H1W H 0.941(7) 0.177(3) 1.116(2) 0.066(10) 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 0.02144(8) 0.02504(8) 0.02472(8) -0.00220(5) 0.00085(5) -0.00758(6) S1 0.0273(2) 0.0281(2) 0.0318(2) -0.00654(19) 0.00051(19) -0.00924(19) S2 0.0286(2) 0.0267(2) 0.0410(3) 0.0021(2) -0.0021(2) -0.0051(2) Cl1 0.0402(3) 0.0365(3) 0.0366(3) -0.0054(2) 0.0150(2) -0.0128(2) N1 0.0275(8) 0.0365(9) 0.0219(8) -0.0011(7) -0.0015(7) -0.0117(7) C1 0.0267(10) 0.0467(12) 0.0284(10) -0.0054(9) 0.0054(8) -0.0081(9) C2 0.0338(11) 0.0393(12) 0.0286(10) -0.0106(9) 0.0020(8) -0.0035(9) C3 0.0410(12) 0.0324(11) 0.0313(10) 0.0009(8) -0.0045(9) -0.0117(9) C4 0.0530(15) 0.0377(13) 0.0560(15) 0.0015(11) -0.0089(12) -0.0014(11) C5 0.0433(12) 0.0476(13) 0.0301(11) -0.0016(9) 0.0060(9) -0.0256(10) C6 0.0541(14) 0.0348(11) 0.0351(11) 0.0076(9) -0.0057(10) -0.0184(10) C7 0.0416(12) 0.0348(11) 0.0363(11) -0.0094(9) 0.0001(9) -0.0096(9) C8 0.085(2) 0.0397(13) 0.0544(16) -0.0147(12) 0.0051(14) -0.0260(14) Cl2 0.0308(3) 0.0508(3) 0.0340(3) -0.0027(2) -0.0034(2) -0.0128(2) O1W 0.0462(12) 0.0562(12) 0.0799(15) 0.0234(11) -0.0090(10) -0.0146(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.0307(16) . ? Pd1 Cl1 2.2949(5) . ? Pd1 S2 2.2954(5) . ? Pd1 S1 2.3058(5) . ? S1 C2 1.818(2) . ? S1 C3 1.819(2) . ? S2 C6 1.817(2) . ? S2 C7 1.817(2) . ? N1 C5 1.481(3) . ? N1 C1 1.488(3) . ? C1 C2 1.507(3) . ? C3 C4 1.505(3) . ? C5 C6 1.501(3) . ? C7 C8 1.510(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 Cl1 179.27(5) . . ? N1 Pd1 S2 87.31(5) . . ? Cl1 Pd1 S2 91.980(19) . . ? N1 Pd1 S1 87.33(5) . . ? Cl1 Pd1 S1 93.372(19) . . ? S2 Pd1 S1 174.359(18) . . ? C2 S1 C3 103.29(10) . . ? C2 S1 Pd1 96.78(7) . . ? C3 S1 Pd1 101.32(7) . . ? C6 S2 C7 102.78(11) . . ? C6 S2 Pd1 96.72(8) . . ? C7 S2 Pd1 102.31(7) . . ? C5 N1 C1 113.71(17) . . ? C5 N1 Pd1 111.47(13) . . ? C1 N1 Pd1 110.77(12) . . ? N1 C1 C2 108.89(16) . . ? C1 C2 S1 110.68(14) . . ? C4 C3 S1 112.76(16) . . ? N1 C5 C6 108.95(17) . . ? C5 C6 S2 110.48(15) . . ? C8 C7 S2 112.05(17) . . ? 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 0.79(2) 2.38(2) 3.1574(18) 171(2) . O1W H2W Cl2 0.80(3) 2.43(3) 3.228(2) 177(3) 1_655 O1W H1W Cl2 0.81(3) 2.39(3) 3.196(2) 174(3) . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.459 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.066 #===END data_8303 _database_code_depnum_ccdc_archive 'CCDC 729212' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H30 Cl2 N O1.50 Pd S2' _chemical_formula_weight 453.79 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.9875(16) _cell_length_b 8.9087(4) _cell_length_c 14.1037(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.9110(10) _cell_angle_gamma 90.00 _cell_volume 3980.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5295 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.15 _exptl_crystal_description PLATE _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7660 _exptl_absorpt_correction_T_max 0.8957 _exptl_absorpt_process_details 'Sababs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 13800 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4567 _reflns_number_gt 4015 _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^)+(0.0400P)^2^+0.6586P] 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 4567 _refine_ls_number_parameters 199 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.369329(5) 0.805281(18) 0.629584(11) 0.03723(7) Uani 1 1 d . . . Cl1 Cl 0.31029(2) 0.94906(7) 0.63667(5) 0.05936(18) Uani 1 1 d . . . Cl2 Cl 0.42664(3) 0.48932(9) 0.44902(5) 0.0754(2) Uani 1 1 d . . . S1 S 0.34455(2) 0.60180(7) 0.70721(4) 0.05009(16) Uani 1 1 d . . . S2 S 0.403975(19) 0.99771(7) 0.56151(4) 0.04378(14) Uani 1 1 d . . . H1N H 0.4216(8) 0.644(3) 0.5810(18) 0.038(7) Uiso 1 1 d . . . N1 N 0.42355(7) 0.6855(2) 0.63015(14) 0.0429(5) Uani 1 1 d . . . C1 C 0.42801(8) 0.5669(3) 0.70486(17) 0.0520(6) Uani 1 1 d . . . H1A H 0.4329 0.6124 0.7679 0.062 Uiso 1 1 calc R . . H1B H 0.4519 0.5030 0.6975 0.062 Uiso 1 1 calc R . . C2 C 0.38849(9) 0.4759(3) 0.6947(2) 0.0564(7) Uani 1 1 d . . . H2A H 0.3905 0.3988 0.7437 0.068 Uiso 1 1 calc R . . H2B H 0.3841 0.4275 0.6326 0.068 Uiso 1 1 calc R . . C3 C 0.29825(10) 0.5134(3) 0.6332(3) 0.0674(8) Uani 1 1 d . . . C4 C 0.29703(14) 0.3487(4) 0.6640(3) 0.1036(14) Uani 1 1 d . . . H4A H 0.2979 0.3434 0.7322 0.155 Uiso 1 1 calc R . . H4B H 0.3209 0.2967 0.6456 0.155 Uiso 1 1 calc R . . H4C H 0.2715 0.3029 0.6334 0.155 Uiso 1 1 calc R . . C5 C 0.26022(11) 0.5976(4) 0.6600(4) 0.1086(14) Uani 1 1 d . . . H5A H 0.2350 0.5602 0.6228 0.163 Uiso 1 1 calc R . . H5B H 0.2632 0.7027 0.6475 0.163 Uiso 1 1 calc R . . H5C H 0.2585 0.5831 0.7268 0.163 Uiso 1 1 calc R . . C6 C 0.30155(12) 0.5286(4) 0.5277(3) 0.0879(11) Uani 1 1 d . . . H6A H 0.2784 0.4770 0.4911 0.132 Uiso 1 1 calc R . . H6B H 0.3277 0.4856 0.5147 0.132 Uiso 1 1 calc R . . H6C H 0.3007 0.6329 0.5104 0.132 Uiso 1 1 calc R . . C7 C 0.46057(8) 0.7869(3) 0.63685(18) 0.0528(6) Uani 1 1 d . . . H7A H 0.4859 0.7290 0.6324 0.063 Uiso 1 1 calc R . . H7B H 0.4641 0.8384 0.6980 0.063 Uiso 1 1 calc R . . C8 C 0.45388(8) 0.8994(3) 0.55685(19) 0.0548(6) Uani 1 1 d . . . H8A H 0.4531 0.8487 0.4958 0.066 Uiso 1 1 calc R . . H8B H 0.4770 0.9708 0.5633 0.066 Uiso 1 1 calc R . . C9 C 0.38185(8) 1.0177(3) 0.43214(17) 0.0476(6) Uani 1 1 d . . . C10 C 0.36523(10) 0.8686(3) 0.39121(19) 0.0633(8) Uani 1 1 d . . . H10A H 0.3546 0.8807 0.3246 0.095 Uiso 1 1 calc R . . H10B H 0.3430 0.8345 0.4251 0.095 Uiso 1 1 calc R . . H10C H 0.3877 0.7961 0.3980 0.095 Uiso 1 1 calc R . . C11 C 0.34669(10) 1.1325(3) 0.4317(2) 0.0651(8) Uani 1 1 d . . . H11A H 0.3322 1.1435 0.3677 0.098 Uiso 1 1 calc R . . H11B H 0.3585 1.2273 0.4539 0.098 Uiso 1 1 calc R . . H11C H 0.3271 1.0991 0.4731 0.098 Uiso 1 1 calc R . . C12 C 0.41640(10) 1.0789(4) 0.37888(19) 0.0642(7) Uani 1 1 d . . . H12A H 0.4380 1.0042 0.3776 0.096 Uiso 1 1 calc R . . H12B H 0.4284 1.1671 0.4109 0.096 Uiso 1 1 calc R . . H12C H 0.4046 1.1040 0.3145 0.096 Uiso 1 1 calc R . . O1W O 0.5000 0.1120(4) 0.7500 0.1104(14) Uani 1 2 d SD . . H1W H 0.494(2) 0.177(8) 0.705(4) 0.080 Uiso 0.50 1 d PD . . H2W H 0.495(3) 0.155(8) 0.802(3) 0.080 Uiso 0.50 1 d PD . . O2W O 0.49480(11) 0.3069(4) 0.5906(2) 0.1030(10) Uani 1 1 d D . . H3W H 0.5141(9) 0.370(4) 0.599(3) 0.080 Uiso 1 1 d D . . H4W H 0.4776(10) 0.340(4) 0.547(2) 0.080 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 0.03984(12) 0.03846(11) 0.03344(11) -0.00145(6) 0.00522(7) 0.00115(7) Cl1 0.0538(4) 0.0512(4) 0.0761(5) 0.0052(3) 0.0196(3) 0.0119(3) Cl2 0.1091(7) 0.0700(5) 0.0461(4) -0.0154(3) 0.0068(4) 0.0044(4) S1 0.0609(4) 0.0450(3) 0.0472(3) 0.0043(3) 0.0174(3) 0.0018(3) S2 0.0471(3) 0.0447(3) 0.0396(3) -0.0037(2) 0.0061(2) -0.0065(3) N1 0.0477(12) 0.0500(12) 0.0302(10) -0.0031(8) 0.0023(8) 0.0079(9) C1 0.0566(16) 0.0583(15) 0.0402(13) 0.0058(11) 0.0039(11) 0.0167(12) C2 0.0717(19) 0.0453(14) 0.0528(15) 0.0087(11) 0.0107(12) 0.0099(13) C3 0.0566(18) 0.0483(15) 0.098(2) 0.0017(15) 0.0146(15) -0.0122(13) C4 0.102(3) 0.0544(19) 0.154(4) 0.014(2) 0.015(3) -0.022(2) C5 0.055(2) 0.074(2) 0.200(5) -0.007(3) 0.030(2) -0.0085(18) C6 0.084(2) 0.083(2) 0.089(3) -0.0062(19) -0.0199(19) -0.0139(19) C7 0.0405(14) 0.0711(18) 0.0450(14) -0.0032(12) -0.0006(10) 0.0012(12) C8 0.0422(14) 0.0708(18) 0.0525(15) -0.0003(13) 0.0103(11) -0.0035(12) C9 0.0573(15) 0.0460(13) 0.0391(12) 0.0041(10) 0.0050(10) -0.0033(11) C10 0.082(2) 0.0562(16) 0.0468(15) -0.0014(12) -0.0072(13) -0.0098(15) C11 0.072(2) 0.0616(17) 0.0612(17) 0.0138(14) 0.0077(14) 0.0097(15) C12 0.073(2) 0.0691(18) 0.0526(16) 0.0092(13) 0.0154(13) -0.0081(15) O1W 0.179(5) 0.072(3) 0.077(2) 0.000 0.005(3) 0.000 O2W 0.107(3) 0.109(3) 0.096(2) 0.0314(17) 0.0258(18) 0.0223(16) _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 2.035(2) . ? Pd1 Cl1 2.2954(7) . ? Pd1 S1 2.3135(6) . ? Pd1 S2 2.3199(6) . ? S1 C2 1.826(3) . ? S1 C3 1.865(3) . ? S2 C8 1.830(3) . ? S2 C9 1.872(2) . ? N1 C7 1.482(3) . ? N1 C1 1.485(3) . ? C1 C2 1.492(4) . ? C3 C6 1.512(5) . ? C3 C5 1.521(5) . ? C3 C4 1.532(4) . ? C7 C8 1.502(4) . ? C9 C10 1.515(3) . ? C9 C11 1.520(4) . ? C9 C12 1.520(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 Cl1 176.44(6) . . ? N1 Pd1 S1 86.25(6) . . ? Cl1 Pd1 S1 94.54(2) . . ? N1 Pd1 S2 86.20(6) . . ? Cl1 Pd1 S2 92.77(2) . . ? S1 Pd1 S2 171.58(2) . . ? C2 S1 C3 104.44(14) . . ? C2 S1 Pd1 96.73(9) . . ? C3 S1 Pd1 111.31(10) . . ? C8 S2 C9 103.01(12) . . ? C8 S2 Pd1 97.47(9) . . ? C9 S2 Pd1 109.61(8) . . ? C7 N1 C1 112.98(19) . . ? C7 N1 Pd1 110.71(16) . . ? C1 N1 Pd1 111.98(16) . . ? N1 C1 C2 108.7(2) . . ? C1 C2 S1 108.09(18) . . ? C6 C3 C5 111.6(3) . . ? C6 C3 C4 111.9(3) . . ? C5 C3 C4 110.5(3) . . ? C6 C3 S1 110.8(2) . . ? C5 C3 S1 104.7(2) . . ? C4 C3 S1 107.2(2) . . ? N1 C7 C8 109.2(2) . . ? C7 C8 S2 109.09(18) . . ? C10 C9 C11 111.6(2) . . ? C10 C9 C12 111.5(2) . . ? C11 C9 C12 110.2(2) . . ? C10 C9 S2 110.70(16) . . ? C11 C9 S2 104.40(18) . . ? C12 C9 S2 108.22(17) . . ? 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 0.78(2) 2.34(3) 3.108(2) 169(2) . O1W H1W O2W 0.863(19) 1.99(2) 2.827(4) 163(7) . O1W H2W O2W 0.86(2) 2.02(4) 2.827(4) 155(7) 2_656 O2W H3W Cl2 0.830(18) 2.45(2) 3.211(4) 154(4) 5_666 O2W H4W Cl2 0.824(17) 2.39(2) 3.191(3) 165(4) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.540 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.072 #===END data_8581 _database_code_depnum_ccdc_archive 'CCDC 729213' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H35 Cl2 N O2 Pd S2' _chemical_formula_weight 514.87 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.835(3) _cell_length_b 5.1827(5) _cell_length_c 25.391(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.190(2) _cell_angle_gamma 90.00 _cell_volume 4379.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 1.292 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5112 _exptl_absorpt_correction_T_max 0.9265 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14635 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5022 _reflns_number_gt 4237 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+22.9107P] 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 5022 _refine_ls_number_parameters 238 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1252 _refine_ls_wR_factor_gt 0.1195 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.143 _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 O1S O 0.5457(2) 0.6290(14) 0.8523(3) 0.0239(16) Uani 0.50 1 d P A -1 O2S O 0.5218(3) 0.9515(15) 0.7610(3) 0.040(2) Uani 0.50 1 d P B -3 O3S O 0.4496(3) 0.8744(17) 0.6831(4) 0.039(2) Uani 0.50 1 d P C -2 O4S O 0.4502(3) 0.3549(18) 0.6672(3) 0.042(2) Uani 0.50 1 d P D -4 Pd1 Pd 0.609338(10) 0.23336(6) 0.636553(14) 0.01039(11) Uani 1 1 d . . . S1 S 0.61150(4) 0.2544(2) 0.72854(5) 0.0156(2) Uani 1 1 d . . . S2 S 0.60087(3) 0.2495(2) 0.54270(5) 0.0146(2) Uani 1 1 d . . . Cl1 Cl 0.66112(3) -0.0592(2) 0.65222(5) 0.0151(2) Uani 1 1 d . . . Cl2 Cl 0.48058(4) 0.1041(3) 0.58360(7) 0.0319(3) Uani 1 1 d . . . N1 N 0.55854(12) 0.4522(8) 0.62101(16) 0.0146(8) Uani 1 1 d D . . H1N H 0.5397(13) 0.332(8) 0.618(2) 0.022 Uiso 1 1 d D . . C1 C 0.55077(14) 0.6027(9) 0.5695(2) 0.0179(10) Uani 1 1 d . . . H1A H 0.5712 0.7399 0.5738 0.022 Uiso 1 1 calc R . . H1B H 0.5239 0.6845 0.5605 0.022 Uiso 1 1 calc R . . C2 C 0.55271(14) 0.4172(10) 0.52421(19) 0.0170(10) Uani 1 1 d . . . H2A H 0.5491 0.5136 0.4894 0.020 Uiso 1 1 calc R . . H2B H 0.5307 0.2897 0.5181 0.020 Uiso 1 1 calc R . . C3 C 0.55731(17) 0.6075(11) 0.6694(2) 0.0260(12) Uani 1 1 d . . . H3A H 0.5307 0.6917 0.6622 0.031 Uiso 1 1 calc R . . H3B H 0.5782 0.7436 0.6766 0.031 Uiso 1 1 calc R . . C4 C 0.56466(15) 0.4330(12) 0.7182(2) 0.0260(13) Uani 1 1 d . . . H4A H 0.5420 0.3102 0.7126 0.031 Uiso 1 1 calc R . . H4B H 0.5661 0.5366 0.7515 0.031 Uiso 1 1 calc R . . C5 C 0.63380(14) 0.5086(9) 0.53158(18) 0.0127(9) Uani 1 1 d . . . H5 H 0.6283 0.6695 0.5498 0.015 Uiso 1 1 calc R . . C6 C 0.62432(15) 0.5581(9) 0.46984(19) 0.0168(10) Uani 1 1 d . . . H6A H 0.5957 0.6077 0.4544 0.020 Uiso 1 1 calc R . . H6B H 0.6289 0.3988 0.4511 0.020 Uiso 1 1 calc R . . C7 C 0.65116(16) 0.7739(10) 0.4600(2) 0.0204(11) Uani 1 1 d . . . H7A H 0.6447 0.9365 0.4760 0.024 Uiso 1 1 calc R . . H7B H 0.6457 0.8002 0.4198 0.024 Uiso 1 1 calc R . . C8 C 0.69578(15) 0.7111(10) 0.4858(2) 0.0199(10) Uani 1 1 d . . . H8A H 0.7031 0.5610 0.4667 0.024 Uiso 1 1 calc R . . H8B H 0.7122 0.8600 0.4810 0.024 Uiso 1 1 calc R . . C9 C 0.70480(14) 0.6506(10) 0.5468(2) 0.0163(10) Uani 1 1 d . . . H9A H 0.7007 0.8080 0.5666 0.020 Uiso 1 1 calc R . . H9B H 0.7333 0.5983 0.5618 0.020 Uiso 1 1 calc R . . C10 C 0.67773(14) 0.4336(9) 0.55701(19) 0.0141(10) Uani 1 1 d . . . H10A H 0.6834 0.2711 0.5403 0.017 Uiso 1 1 calc R . . H10B H 0.6832 0.4053 0.5971 0.017 Uiso 1 1 calc R . . C11 C 0.64867(14) 0.5029(9) 0.76061(18) 0.0124(9) Uani 1 1 d . . . H11 H 0.6412 0.6682 0.7398 0.015 Uiso 1 1 calc R . . C12 C 0.69016(14) 0.4189(9) 0.7582(2) 0.0161(10) Uani 1 1 d . . . H12A H 0.6900 0.4034 0.7193 0.019 Uiso 1 1 calc R . . H12B H 0.6969 0.2479 0.7759 0.019 Uiso 1 1 calc R . . C13 C 0.72174(15) 0.6172(11) 0.7879(2) 0.0211(11) Uani 1 1 d . . . H13A H 0.7487 0.5568 0.7878 0.025 Uiso 1 1 calc R . . H13B H 0.7164 0.7832 0.7678 0.025 Uiso 1 1 calc R . . C14 C 0.72146(16) 0.6595(12) 0.8473(2) 0.0264(12) Uani 1 1 d . . . H14A H 0.7294 0.4980 0.8686 0.032 Uiso 1 1 calc R . . H14B H 0.7412 0.7948 0.8646 0.032 Uiso 1 1 calc R . . C15 C 0.68015(17) 0.7400(10) 0.8489(2) 0.0247(12) Uani 1 1 d . . . H15A H 0.6734 0.9103 0.8309 0.030 Uiso 1 1 calc R . . H15B H 0.6802 0.7579 0.8878 0.030 Uiso 1 1 calc R . . C16 C 0.64798(15) 0.5433(10) 0.81976(19) 0.0182(10) Uani 1 1 d . . . H16A H 0.6531 0.3771 0.8398 0.022 Uiso 1 1 calc R . . H16B H 0.6211 0.6063 0.8198 0.022 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1S 0.023(4) 0.020(4) 0.028(4) 0.001(3) 0.007(3) 0.001(3) O2S 0.078(7) 0.021(4) 0.024(4) -0.003(3) 0.020(5) -0.011(4) O3S 0.050(6) 0.037(5) 0.041(5) 0.010(4) 0.029(5) 0.001(4) O4S 0.067(7) 0.040(5) 0.026(4) 0.000(4) 0.023(5) 0.020(5) Pd1 0.00878(18) 0.00981(17) 0.01096(18) 0.00050(13) 0.00040(13) -0.00010(13) S1 0.0134(6) 0.0175(6) 0.0158(6) -0.0002(5) 0.0039(5) -0.0007(5) S2 0.0124(5) 0.0158(6) 0.0132(5) 0.0023(4) 0.0001(4) -0.0022(5) Cl1 0.0147(6) 0.0163(6) 0.0131(5) 0.0005(4) 0.0024(4) 0.0050(4) Cl2 0.0125(6) 0.0289(7) 0.0516(9) 0.0236(7) 0.0053(6) 0.0000(5) N1 0.0098(19) 0.014(2) 0.016(2) -0.0040(16) -0.0018(16) 0.0001(15) C1 0.009(2) 0.016(2) 0.026(3) 0.004(2) 0.001(2) -0.0029(18) C2 0.008(2) 0.026(3) 0.012(2) 0.0099(19) -0.0037(18) 0.0014(19) C3 0.021(3) 0.029(3) 0.024(3) -0.009(2) -0.001(2) 0.008(2) C4 0.007(2) 0.047(4) 0.023(3) -0.012(2) 0.004(2) 0.007(2) C5 0.012(2) 0.013(2) 0.015(2) 0.0011(18) 0.0068(18) -0.0039(18) C6 0.016(2) 0.017(2) 0.015(2) 0.0011(19) 0.003(2) -0.0014(19) C7 0.024(3) 0.022(3) 0.017(2) 0.000(2) 0.009(2) -0.002(2) C8 0.021(3) 0.019(2) 0.024(3) 0.001(2) 0.012(2) -0.001(2) C9 0.011(2) 0.021(2) 0.017(2) 0.0009(19) 0.0040(19) 0.0002(19) C10 0.014(2) 0.013(2) 0.012(2) 0.0021(17) -0.0015(19) 0.0010(18) C11 0.015(2) 0.010(2) 0.010(2) -0.0014(17) -0.0011(18) -0.0023(18) C12 0.014(2) 0.015(2) 0.016(2) -0.0036(19) -0.0001(19) -0.0009(19) C13 0.008(2) 0.028(3) 0.024(3) -0.006(2) -0.001(2) -0.002(2) C14 0.021(3) 0.031(3) 0.021(3) -0.009(2) -0.002(2) -0.001(2) C15 0.031(3) 0.022(3) 0.017(2) -0.004(2) 0.001(2) 0.003(2) C16 0.019(3) 0.022(3) 0.012(2) -0.0036(19) 0.0008(19) -0.001(2) _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 2.040(4) . ? Pd1 Cl1 2.2994(11) . ? Pd1 S2 2.3146(12) . ? Pd1 S1 2.3172(12) . ? S1 C4 1.826(5) . ? S1 C11 1.837(5) . ? S2 C2 1.823(5) . ? S2 C5 1.841(5) . ? N1 C1 1.476(6) . ? N1 C3 1.479(6) . ? C1 C2 1.517(7) . ? C3 C4 1.495(8) . ? C5 C10 1.525(6) . ? C5 C6 1.525(6) . ? C6 C7 1.525(7) . ? C7 C8 1.533(7) . ? C8 C9 1.520(7) . ? C9 C10 1.538(6) . ? C11 C16 1.524(6) . ? C11 C12 1.528(6) . ? C12 C13 1.532(7) . ? C13 C14 1.527(7) . ? C14 C15 1.511(7) . ? C15 C16 1.534(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 Cl1 172.53(12) . . ? N1 Pd1 S2 86.64(12) . . ? Cl1 Pd1 S2 93.26(4) . . ? N1 Pd1 S1 86.37(12) . . ? Cl1 Pd1 S1 93.82(4) . . ? S2 Pd1 S1 172.93(4) . . ? C4 S1 C11 101.0(2) . . ? C4 S1 Pd1 96.78(17) . . ? C11 S1 Pd1 106.77(15) . . ? C2 S2 C5 100.4(2) . . ? C2 S2 Pd1 96.32(15) . . ? C5 S2 Pd1 106.78(15) . . ? C1 N1 C3 113.9(4) . . ? C1 N1 Pd1 112.7(3) . . ? C3 N1 Pd1 112.2(3) . . ? N1 C1 C2 107.4(4) . . ? C1 C2 S2 110.5(3) . . ? N1 C3 C4 108.7(4) . . ? C3 C4 S1 110.6(4) . . ? C10 C5 C6 111.3(4) . . ? C10 C5 S2 110.0(3) . . ? C6 C5 S2 109.0(3) . . ? C5 C6 C7 109.6(4) . . ? C6 C7 C8 111.5(4) . . ? C9 C8 C7 111.0(4) . . ? C8 C9 C10 111.7(4) . . ? C5 C10 C9 109.3(4) . . ? C16 C11 C12 111.7(4) . . ? C16 C11 S1 108.6(3) . . ? C12 C11 S1 109.5(3) . . ? C11 C12 C13 109.8(4) . . ? C14 C13 C12 111.7(4) . . ? C15 C14 C13 110.5(4) . . ? C14 C15 C16 111.7(4) . . ? C11 C16 C15 110.2(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.423 _refine_diff_density_min -1.161 _refine_diff_density_rms 0.143 #===end data_8640 _database_code_depnum_ccdc_archive 'CCDC 729214' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H31 Br2 N O2 Pd S2' _chemical_formula_weight 551.72 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.4127(4) _cell_length_b 13.6387(10) _cell_length_c 15.2316(12) _cell_angle_alpha 67.5880(10) _cell_angle_beta 85.211(2) _cell_angle_gamma 80.964(2) _cell_volume 1026.25(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5168 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 5.002 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1533 _exptl_absorpt_correction_T_max 0.6904 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 13428 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4683 _reflns_number_gt 4140 _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^)+(0.0754P)^2^+0.3211P] 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 4683 _refine_ls_number_parameters 201 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1163 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.053 _refine_ls_shift/su_mean 0.002 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 0.83881(5) 0.72496(2) 0.750148(19) 0.01476(11) Uani 1 1 d . . . Br1 Br 1.10182(7) 0.67264(3) 0.88592(3) 0.02160(12) Uani 1 1 d . . . Br2 Br 0.98776(8) 0.84923(3) 0.44716(3) 0.02436(13) Uani 1 1 d . . . S1 S 0.89073(18) 0.55479(8) 0.74864(7) 0.0190(2) Uani 1 1 d . . . S2 S 0.76231(18) 0.90109(8) 0.73706(7) 0.0173(2) Uani 1 1 d . . . N1 N 0.6152(6) 0.7694(3) 0.6362(2) 0.0180(7) Uani 1 1 d . . . H1N H 0.711(10) 0.790(4) 0.586(4) 0.029(13) Uiso 1 1 d . . . C1 C 0.5011(8) 0.6779(3) 0.6347(3) 0.0223(8) Uani 1 1 d . . . H1A H 0.4117 0.6990 0.5748 0.027 Uiso 1 1 calc R . . H1B H 0.3797 0.6551 0.6885 0.027 Uiso 1 1 calc R . . C2 C 0.7082(9) 0.5878(3) 0.6426(3) 0.0252(9) Uani 1 1 d . . . H2A H 0.8192 0.6088 0.5854 0.030 Uiso 1 1 calc R . . H2B H 0.6362 0.5239 0.6462 0.030 Uiso 1 1 calc R . . C3 C 0.4321(7) 0.8651(3) 0.6295(3) 0.0207(8) Uani 1 1 d . . . H3A H 0.3109 0.8470 0.6839 0.025 Uiso 1 1 calc R . . H3B H 0.3386 0.8908 0.5700 0.025 Uiso 1 1 calc R . . C4 C 0.5771(8) 0.9508(3) 0.6308(3) 0.0203(8) Uani 1 1 d . . . H4A H 0.4594 1.0147 0.6294 0.024 Uiso 1 1 calc R . . H4B H 0.6887 0.9722 0.5737 0.024 Uiso 1 1 calc R . . C5 C 0.6810(8) 0.4863(3) 0.8445(3) 0.0210(8) Uani 1 1 d . . . H5A H 0.7599 0.4691 0.9059 0.025 Uiso 1 1 calc R . . H5B H 0.5245 0.5356 0.8424 0.025 Uiso 1 1 calc R . . C6 C 0.6149(8) 0.3832(3) 0.8407(3) 0.0241(9) Uani 1 1 d . . . H6 H 0.5215 0.4017 0.7813 0.029 Uiso 1 1 calc R . . C7 C 0.8472(9) 0.3038(4) 0.8400(4) 0.0385(12) Uani 1 1 d . . . H7A H 0.9628 0.3393 0.7887 0.058 Uiso 1 1 calc R . . H7B H 0.7978 0.2430 0.8297 0.058 Uiso 1 1 calc R . . H7C H 0.9299 0.2783 0.9010 0.058 Uiso 1 1 calc R . . C8 C 0.4420(9) 0.3347(4) 0.9261(3) 0.0351(11) Uani 1 1 d . . . H8A H 0.5332 0.3134 0.9849 0.053 Uiso 1 1 calc R . . H8B H 0.3849 0.2718 0.9223 0.053 Uiso 1 1 calc R . . H8C H 0.2971 0.3879 0.9258 0.053 Uiso 1 1 calc R . . C9 C 0.5250(7) 0.8954(3) 0.8308(3) 0.0196(8) Uani 1 1 d . . . H9A H 0.4172 0.8413 0.8352 0.023 Uiso 1 1 calc R . . H9B H 0.6097 0.8711 0.8921 0.023 Uiso 1 1 calc R . . C10 C 0.3597(8) 1.0014(3) 0.8163(3) 0.0231(8) Uani 1 1 d . . . H10 H 0.2527 1.0192 0.7603 0.028 Uiso 1 1 calc R . . C11 C 0.5084(9) 1.0940(4) 0.7972(4) 0.0350(11) Uani 1 1 d . . . H11A H 0.6194 1.0768 0.8502 0.053 Uiso 1 1 calc R . . H11B H 0.3928 1.1591 0.7909 0.053 Uiso 1 1 calc R . . H11C H 0.6085 1.1054 0.7384 0.053 Uiso 1 1 calc R . . C12 C 0.1879(9) 0.9844(4) 0.9049(4) 0.0348(11) Uani 1 1 d . . . H12A H 0.0965 0.9241 0.9155 0.052 Uiso 1 1 calc R . . H12B H 0.0685 1.0493 0.8954 0.052 Uiso 1 1 calc R . . H12C H 0.2891 0.9689 0.9602 0.052 Uiso 1 1 calc R . . O2W O 0.7721(11) 0.3754(4) 0.5738(4) 0.0660(13) Uani 1 1 d D . . H2WA H 0.830(14) 0.313(3) 0.573(4) 0.079 Uiso 1 1 d D . . H2WB H 0.746(15) 0.416(4) 0.516(2) 0.079 Uiso 1 1 d D . . O1W O 0.7391(10) 0.5566(4) 0.4059(4) 0.0661(13) Uani 1 1 d D . . H1WA H 0.883(7) 0.557(5) 0.424(5) 0.079 Uiso 1 1 d D . . H1WB H 0.666(11) 0.621(3) 0.396(6) 0.079 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 0.01145(16) 0.01399(17) 0.01674(17) -0.00371(12) 0.00076(11) -0.00151(11) Br1 0.0176(2) 0.0221(2) 0.0224(2) -0.00507(17) -0.00475(15) -0.00149(16) Br2 0.0184(2) 0.0251(2) 0.0231(2) -0.00309(17) 0.00277(16) -0.00154(16) S1 0.0164(5) 0.0159(5) 0.0230(5) -0.0064(4) 0.0031(4) -0.0013(4) S2 0.0141(5) 0.0155(5) 0.0200(5) -0.0042(4) 0.0013(3) -0.0023(3) N1 0.0182(17) 0.0172(17) 0.0158(16) -0.0038(13) 0.0027(13) -0.0028(13) C1 0.020(2) 0.027(2) 0.0194(19) -0.0066(17) -0.0006(15) -0.0081(17) C2 0.035(2) 0.022(2) 0.020(2) -0.0094(17) 0.0045(17) -0.0067(18) C3 0.0156(19) 0.023(2) 0.0192(19) -0.0037(16) -0.0006(15) -0.0015(16) C4 0.0189(19) 0.0182(19) 0.0184(19) -0.0019(15) -0.0003(15) -0.0005(15) C5 0.0178(19) 0.020(2) 0.0202(19) -0.0014(16) 0.0014(15) -0.0041(15) C6 0.019(2) 0.024(2) 0.026(2) -0.0037(17) -0.0039(16) -0.0063(16) C7 0.030(3) 0.022(2) 0.064(3) -0.014(2) -0.004(2) -0.0078(19) C8 0.027(2) 0.040(3) 0.031(2) 0.002(2) -0.0031(19) -0.020(2) C9 0.0168(19) 0.020(2) 0.0215(19) -0.0070(16) 0.0015(15) -0.0028(15) C10 0.020(2) 0.024(2) 0.025(2) -0.0099(17) 0.0018(16) -0.0017(16) C11 0.030(3) 0.027(2) 0.052(3) -0.021(2) 0.007(2) -0.0058(19) C12 0.025(2) 0.041(3) 0.038(3) -0.020(2) 0.005(2) 0.003(2) O2W 0.091(4) 0.039(3) 0.074(3) -0.032(2) -0.001(3) 0.002(2) O1W 0.059(3) 0.086(4) 0.069(3) -0.049(3) 0.005(3) -0.007(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 2.040(3) . ? Pd1 S1 2.3023(10) . ? Pd1 S2 2.3061(10) . ? Pd1 Br1 2.4208(5) . ? S1 C5 1.819(4) . ? S1 C2 1.833(5) . ? S2 C4 1.818(4) . ? S2 C9 1.826(4) . ? N1 C3 1.485(5) . ? N1 C1 1.486(5) . ? C1 C2 1.502(6) . ? C3 C4 1.514(6) . ? C5 C6 1.526(6) . ? C6 C7 1.527(7) . ? C6 C8 1.530(6) . ? C9 C10 1.524(6) . ? C10 C11 1.525(6) . ? C10 C12 1.536(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 S1 86.91(10) . . ? N1 Pd1 S2 86.93(10) . . ? S1 Pd1 S2 173.83(4) . . ? N1 Pd1 Br1 179.62(10) . . ? S1 Pd1 Br1 93.29(3) . . ? S2 Pd1 Br1 92.87(3) . . ? C5 S1 C2 102.7(2) . . ? C5 S1 Pd1 103.00(14) . . ? C2 S1 Pd1 96.59(14) . . ? C4 S2 C9 102.69(19) . . ? C4 S2 Pd1 96.63(14) . . ? C9 S2 Pd1 101.89(13) . . ? C3 N1 C1 114.2(3) . . ? C3 N1 Pd1 111.1(2) . . ? C1 N1 Pd1 111.7(2) . . ? N1 C1 C2 107.8(3) . . ? C1 C2 S1 110.6(3) . . ? N1 C3 C4 107.6(3) . . ? C3 C4 S2 110.2(3) . . ? C6 C5 S1 114.2(3) . . ? C5 C6 C7 112.2(4) . . ? C5 C6 C8 107.9(4) . . ? C7 C6 C8 111.1(4) . . ? C10 C9 S2 114.4(3) . . ? C9 C10 C11 113.2(4) . . ? C9 C10 C12 107.4(3) . . ? C11 C10 C12 111.5(4) . . ? 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 O2W H2WA Br2 0.855(19) 2.41(2) 3.256(4) 173(6) 2_766 O2W H2WB O1W 0.850(19) 2.01(4) 2.792(8) 152(7) . O1W H1WA O2W 0.85(2) 2.22(4) 3.014(8) 156(7) 2_766 O1W H1WB O2W 0.865(19) 2.38(7) 2.807(8) 111(5) 2_666 N1 H1N Br2 0.87(5) 2.43(5) 3.297(3) 179(5) . C5 H5B Br1 0.99 2.92 3.883(4) 165.0 1_455 C9 H9A Br1 0.99 2.91 3.887(4) 169.4 1_455 C1 H1B Pd1 0.99 3.12 3.930(4) 140.4 1_455 C3 H3A Pd1 0.99 3.15 3.950(4) 138.5 1_455 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.641 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.211 #===end data_7584 _database_code_depnum_ccdc_archive 'CCDC 729215' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H27 Cl N2 O3 Pd S2' _chemical_formula_weight 453.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.7601(4) _cell_length_b 11.4786(7) _cell_length_c 15.2346(10) _cell_angle_alpha 70.5740(10) _cell_angle_beta 85.4230(10) _cell_angle_gamma 77.6310(10) _cell_volume 927.85(11) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2478 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 26.02 _exptl_crystal_description PLATE _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 1.378 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8096 _exptl_absorpt_correction_T_max 0.8860 _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 8462 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.45 _reflns_number_total 4208 _reflns_number_gt 3663 _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^)+(0.0516P)^2^+0.5761P] 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 4208 _refine_ls_number_parameters 198 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _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 0.39549(6) 0.33181(3) 0.27855(2) 0.02454(12) Uani 1 1 d . . . Cl1 Cl 0.6955(2) 0.33026(12) 0.16927(9) 0.0410(3) Uani 1 1 d . . . S1 S 0.2803(2) 0.54775(11) 0.22101(8) 0.0342(3) Uani 1 1 d . . . S2 S 0.4746(2) 0.11621(11) 0.34855(8) 0.0308(2) Uani 1 1 d . . . O1 O 0.5640(8) 0.2111(4) 0.5342(3) 0.0698(13) Uani 1 1 d . . . O2 O 0.5457(10) 0.3024(5) 0.6385(4) 0.0839(16) Uani 1 1 d . . . O3 O 0.2954(10) 0.3712(5) 0.5298(3) 0.0900(18) Uani 1 1 d . . . N1 N 0.1303(7) 0.3350(4) 0.3736(3) 0.0326(8) Uani 1 1 d D . . H1N H 0.193(9) 0.327(5) 0.427(2) 0.053(17) Uiso 1 1 d D . . N2 N 0.4732(9) 0.2955(5) 0.5668(3) 0.0489(11) Uani 1 1 d . . . C1 C -0.0570(9) 0.4507(5) 0.3444(3) 0.0375(11) Uani 1 1 d . . . H1A H -0.1628 0.4562 0.3972 0.045 Uiso 1 1 calc R . . H1B H -0.1521 0.4483 0.2947 0.045 Uiso 1 1 calc R . . C2 C 0.0584(9) 0.5631(5) 0.3103(3) 0.0394(11) Uani 1 1 d . . . H2A H 0.1339 0.5719 0.3626 0.047 Uiso 1 1 calc R . . H2B H -0.0630 0.6394 0.2849 0.047 Uiso 1 1 calc R . . C3 C 0.0316(9) 0.2182(5) 0.3989(4) 0.0403(12) Uani 1 1 d . . . H3A H -0.0434 0.2146 0.3446 0.048 Uiso 1 1 calc R . . H3B H -0.0892 0.2180 0.4480 0.048 Uiso 1 1 calc R . . C4 C 0.2305(9) 0.1061(5) 0.4324(3) 0.0398(11) Uani 1 1 d . . . H4A H 0.1722 0.0287 0.4415 0.048 Uiso 1 1 calc R . . H4B H 0.2872 0.1025 0.4924 0.048 Uiso 1 1 calc R . . C5 C 0.1010(8) 0.5629(4) 0.1224(3) 0.0328(10) Uani 1 1 d . . . H5A H 0.2075 0.5447 0.0731 0.039 Uiso 1 1 calc R . . H5B H 0.0006 0.4995 0.1424 0.039 Uiso 1 1 calc R . . C6 C -0.0564(8) 0.6919(4) 0.0826(3) 0.0342(10) Uani 1 1 d . . . H6 H -0.1588 0.7120 0.1331 0.041 Uiso 1 1 calc R . . C7 C 0.0900(10) 0.7935(5) 0.0414(4) 0.0437(12) Uani 1 1 d . . . H7A H 0.1862 0.7966 0.0897 0.066 Uiso 1 1 calc R . . H7B H -0.0156 0.8746 0.0159 0.066 Uiso 1 1 calc R . . H7C H 0.1926 0.7742 -0.0076 0.066 Uiso 1 1 calc R . . C8 C -0.2136(9) 0.6867(5) 0.0088(4) 0.0469(13) Uani 1 1 d . . . H8A H -0.1153 0.6703 -0.0422 0.070 Uiso 1 1 calc R . . H8B H -0.3239 0.7666 -0.0143 0.070 Uiso 1 1 calc R . . H8C H -0.3018 0.6198 0.0359 0.070 Uiso 1 1 calc R . . C9 C 0.3742(8) 0.0471(4) 0.2702(3) 0.0333(10) Uani 1 1 d . . . H9A H 0.3290 -0.0328 0.3069 0.040 Uiso 1 1 calc R . . H9B H 0.2327 0.1039 0.2373 0.040 Uiso 1 1 calc R . . C10 C 0.5626(9) 0.0233(5) 0.1994(4) 0.0426(12) Uani 1 1 d . . . H10 H 0.5928 0.1052 0.1569 0.051 Uiso 1 1 calc R . . C11 C 0.7943(10) -0.0564(6) 0.2455(5) 0.0598(17) Uani 1 1 d . . . H11A H 0.8589 -0.0113 0.2783 0.090 Uiso 1 1 calc R . . H11B H 0.9072 -0.0735 0.1983 0.090 Uiso 1 1 calc R . . H11C H 0.7648 -0.1354 0.2892 0.090 Uiso 1 1 calc R . . C12 C 0.4618(11) -0.0430(6) 0.1432(4) 0.0541(15) Uani 1 1 d . . . H12A H 0.4447 -0.1265 0.1833 0.081 Uiso 1 1 calc R . . H12B H 0.5692 -0.0504 0.0921 0.081 Uiso 1 1 calc R . . H12C H 0.3077 0.0057 0.1188 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02355(18) 0.02521(19) 0.02611(18) -0.00940(13) 0.00088(12) -0.00622(13) Cl1 0.0415(7) 0.0428(7) 0.0456(7) -0.0201(6) 0.0181(5) -0.0205(6) S1 0.0388(6) 0.0276(6) 0.0393(6) -0.0132(5) -0.0015(5) -0.0088(5) S2 0.0282(6) 0.0308(6) 0.0306(6) -0.0084(5) -0.0022(4) -0.0020(5) O1 0.063(3) 0.064(3) 0.076(3) -0.024(3) 0.019(2) -0.004(2) O2 0.099(4) 0.084(4) 0.075(3) -0.018(3) -0.034(3) -0.034(3) O3 0.102(4) 0.098(4) 0.070(3) -0.056(3) -0.033(3) 0.038(3) N1 0.030(2) 0.035(2) 0.032(2) -0.0128(18) 0.0022(16) -0.0038(17) N2 0.050(3) 0.056(3) 0.044(3) -0.018(2) 0.001(2) -0.014(2) C1 0.035(3) 0.040(3) 0.040(3) -0.019(2) 0.006(2) -0.004(2) C2 0.048(3) 0.036(3) 0.037(3) -0.021(2) 0.001(2) -0.002(2) C3 0.036(3) 0.034(3) 0.047(3) -0.009(2) 0.012(2) -0.009(2) C4 0.044(3) 0.033(3) 0.032(2) -0.001(2) 0.010(2) -0.005(2) C5 0.039(3) 0.030(2) 0.033(2) -0.013(2) -0.0012(19) -0.010(2) C6 0.035(2) 0.031(3) 0.035(2) -0.010(2) 0.0030(19) -0.007(2) C7 0.052(3) 0.030(3) 0.048(3) -0.009(2) -0.006(2) -0.011(2) C8 0.038(3) 0.047(3) 0.051(3) -0.008(3) -0.005(2) -0.008(3) C9 0.030(2) 0.027(2) 0.044(3) -0.011(2) -0.007(2) -0.005(2) C10 0.047(3) 0.040(3) 0.045(3) -0.017(2) 0.007(2) -0.016(3) C11 0.037(3) 0.071(4) 0.089(5) -0.050(4) 0.015(3) -0.015(3) C12 0.066(4) 0.050(4) 0.057(3) -0.029(3) 0.002(3) -0.016(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 2.022(4) . ? Pd1 S1 2.3011(12) . ? Pd1 Cl1 2.3034(11) . ? Pd1 S2 2.3040(12) . ? S1 C2 1.817(5) . ? S1 C5 1.831(4) . ? S2 C4 1.818(5) . ? S2 C9 1.823(4) . ? O1 N2 1.233(6) . ? O2 N2 1.232(6) . ? O3 N2 1.228(6) . ? N1 C1 1.482(6) . ? N1 C3 1.489(6) . ? C1 C2 1.497(7) . ? C3 C4 1.502(7) . ? C5 C6 1.516(6) . ? C6 C7 1.521(7) . ? C6 C8 1.523(7) . ? C9 C10 1.516(7) . ? C10 C11 1.521(8) . ? C10 C12 1.533(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 S1 87.14(12) . . ? N1 Pd1 Cl1 179.38(13) . . ? S1 Pd1 Cl1 92.29(5) . . ? N1 Pd1 S2 86.12(12) . . ? S1 Pd1 S2 173.26(4) . . ? Cl1 Pd1 S2 94.45(4) . . ? C2 S1 C5 103.0(2) . . ? C2 S1 Pd1 96.55(17) . . ? C5 S1 Pd1 99.88(15) . . ? C4 S2 C9 100.1(2) . . ? C4 S2 Pd1 97.93(16) . . ? C9 S2 Pd1 107.51(16) . . ? C1 N1 C3 112.2(4) . . ? C1 N1 Pd1 113.1(3) . . ? C3 N1 Pd1 110.6(3) . . ? O3 N2 O2 118.4(5) . . ? O3 N2 O1 119.0(5) . . ? O2 N2 O1 122.5(6) . . ? N1 C1 C2 108.9(4) . . ? C1 C2 S1 111.1(3) . . ? N1 C3 C4 108.7(4) . . ? C3 C4 S2 110.5(3) . . ? C6 C5 S1 114.0(3) . . ? C5 C6 C7 111.5(4) . . ? C5 C6 C8 108.2(4) . . ? C7 C6 C8 110.7(4) . . ? C10 C9 S2 112.7(3) . . ? C9 C10 C11 111.9(4) . . ? C9 C10 C12 107.1(4) . . ? C11 C10 C12 110.7(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 O3 0.882(19) 1.97(3) 2.817(6) 161(5) . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.250 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.125 #===END