# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1333 data_1 _publ_contact_author ; Prof K R Koch Department of Chemistry University of Cape Town Rondebosch 7701 South Africa ; _publ_contact_author_email ; kkoch@psipsy.uct.ac.za ; loop_ _publ_author_name 'Koch, Klaus R' 'Coetzee, Anita' 'Wang, Yali' _publ_author_address ; Department of Chemistry University of Cape Town Rondebosch 7701 South Africa ; _publ_requested_journal 'J Chem Soc, Dalton Trans' _audit_creation_method SHELXL-97 _chemical_name_systematic 'trans-bis(N-benzoyl-N'-propylthioureato)dibromopalladium(II)' _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H28 Br2 N4 O2 Pd S2' _chemical_formula_weight 710.84 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' 'O' 'O' 0.0106 0.0060 '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' -1.1770 1.0070 '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 8.7678(10) _cell_length_b 8.9525(9) _cell_length_c 9.8668(8) _cell_angle_alpha 104.034(8) _cell_angle_beta 113.016(8) _cell_angle_gamma 99.226(9) _cell_volume 662.72(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'psi scan' _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 22.54 _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 348 _exptl_absorpt_coefficient_mu 3.849 _exptl_absorpt_correction_type 'Lorenz-polarisation as well as empirical absorption corrections ' _exptl_absorpt_correction_T_min 0.7837 _exptl_absorpt_correction_T_max 0.9976 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w - 2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% ? _diffrn_reflns_number 1867 _diffrn_reflns_av_R_equivalents 0.0137 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 22.54 _reflns_number_total 1744 _reflns_number_gt 1542 _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 w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.3740P] 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 1744 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0740 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.006 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.0000 0.0000 0.0000 0.03944(16) Uani 1 d S . . Br Br 0.05827(6) 0.24090(5) 0.21385(5) 0.05501(18) Uani 1 d . . . S S 0.13936(14) 0.17199(14) -0.08422(12) 0.0577(3) Uani 1 d . . . N1 N -0.1267(4) 0.0410(4) -0.3727(4) 0.0423(8) Uani 1 d . . . H1 H -0.145(5) -0.029(5) -0.339(4) 0.035(11) Uiso 1 d . . . N2 N 0.0793(4) 0.2694(4) -0.3236(4) 0.0441(8) Uani 1 d . . . H2 H 0.015(5) 0.255(5) -0.419(5) 0.048(12) Uiso 1 d . . . C1 C 0.0247(5) 0.1608(4) -0.2712(4) 0.0403(9) Uani 1 d . . . C11 C -0.2376(5) 0.0284(4) -0.5225(4) 0.0400(9) Uani 1 d . . . C12 C -0.4019(5) -0.1052(4) -0.6068(4) 0.0397(9) Uani 1 d . . . C13 C -0.4533(5) -0.2132(5) -0.5422(5) 0.0486(10) Uani 1 d . . . H131 H -0.3833 -0.2049 -0.4399 0.069(6) Uiso 1 calc R . . C14 C -0.6083(6) -0.3331(5) -0.6298(5) 0.0583(11) Uani 1 d . . . H141 H -0.6414 -0.4065 -0.5869 0.069(6) Uiso 1 calc R . . C15 C -0.7134(5) -0.3441(6) -0.7797(5) 0.0599(12) Uani 1 d . . . H151 H -0.8176 -0.4250 -0.8384 0.069(6) Uiso 1 calc R . . C16 C -0.6648(6) -0.2359(6) -0.8429(5) 0.0585(12) Uani 1 d . . . H161 H -0.7375 -0.2427 -0.9439 0.069(6) Uiso 1 calc R . . C17 C -0.5089(5) -0.1167(5) -0.7582(5) 0.0519(10) Uani 1 d . . . H171 H -0.4761 -0.0447 -0.8025 0.069(6) Uiso 1 calc R . . O11 O -0.2026(4) 0.1237(4) -0.5831(3) 0.0582(8) Uani 1 d . . . C21 C 0.2327(5) 0.4070(5) -0.2272(5) 0.0480(10) Uani 1 d . . . H211 H 0.3347 0.3696 -0.1933 0.068(7) Uiso 1 calc R . . H212 H 0.2246 0.4656 -0.1349 0.068(7) Uiso 1 calc R . . C22 C 0.2496(5) 0.5168(5) -0.3172(5) 0.0492(10) Uani 1 d . . . H221 H 0.1512 0.5598 -0.3448 0.068(7) Uiso 1 calc R . . H222 H 0.2491 0.4560 -0.4133 0.068(7) Uiso 1 calc R . . C23 C 0.4150(6) 0.6544(5) -0.2229(6) 0.0629(12) Uani 1 d . . . H231 H 0.4231 0.7210 -0.2842 0.097(10) Uiso 1 calc R . . H232 H 0.5126 0.6121 -0.1953 0.097(10) Uiso 1 calc R . . H233 H 0.4139 0.7171 -0.1295 0.097(10) Uiso 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 Pd 0.0401(3) 0.0392(3) 0.0262(2) 0.01030(18) 0.00681(19) 0.00076(18) Br 0.0695(3) 0.0457(3) 0.0378(3) 0.0107(2) 0.0161(2) 0.0117(2) S 0.0544(6) 0.0602(7) 0.0332(6) 0.0152(5) 0.0066(5) -0.0136(5) N1 0.044(2) 0.0401(19) 0.0335(19) 0.0145(16) 0.0118(16) 0.0007(16) N2 0.0475(19) 0.045(2) 0.0295(19) 0.0102(16) 0.0141(17) -0.0004(15) C1 0.042(2) 0.039(2) 0.035(2) 0.0086(18) 0.0164(18) 0.0052(18) C11 0.045(2) 0.042(2) 0.033(2) 0.0101(18) 0.0174(19) 0.0128(18) C12 0.041(2) 0.039(2) 0.034(2) 0.0066(17) 0.0156(18) 0.0122(17) C13 0.047(2) 0.049(2) 0.041(2) 0.011(2) 0.016(2) 0.007(2) C14 0.051(3) 0.055(3) 0.055(3) 0.012(2) 0.020(2) -0.001(2) C15 0.038(2) 0.055(3) 0.059(3) 0.000(2) 0.010(2) 0.002(2) C16 0.049(2) 0.060(3) 0.041(2) 0.004(2) 0.004(2) 0.014(2) C17 0.056(3) 0.052(3) 0.036(2) 0.013(2) 0.011(2) 0.014(2) O11 0.0593(18) 0.0618(19) 0.0418(17) 0.0244(15) 0.0135(14) 0.0005(15) C21 0.050(2) 0.040(2) 0.043(2) 0.0088(19) 0.018(2) -0.0022(19) C22 0.051(2) 0.044(2) 0.049(2) 0.016(2) 0.021(2) 0.0071(19) C23 0.063(3) 0.051(3) 0.063(3) 0.020(2) 0.023(2) 0.000(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 Pd S 2.3164(10) 2 ? Pd S 2.3164(10) . ? Pd Br 2.4415(5) . ? Pd Br 2.4415(5) 2 ? S C1 1.689(4) . ? N1 C1 1.378(5) . ? N1 C11 1.379(5) . ? N2 C1 1.315(5) . ? N2 C21 1.460(5) . ? C11 O11 1.220(5) . ? C11 C12 1.492(5) . ? C12 C17 1.386(5) . ? C12 C13 1.388(6) . ? C13 C14 1.382(6) . ? C14 C15 1.371(6) . ? C15 C16 1.370(7) . ? C16 C17 1.383(6) . ? C21 C22 1.502(6) . ? C22 C23 1.517(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 S Pd S 180.0 2 . ? S Pd Br 94.54(3) 2 . ? S Pd Br 85.46(3) . . ? S Pd Br 85.46(3) 2 2 ? S Pd Br 94.54(3) . 2 ? Br Pd Br 180.0 . 2 ? C1 S Pd 114.83(13) . . ? C1 N1 C11 126.9(3) . . ? C1 N2 C21 123.9(3) . . ? N2 C1 N1 118.0(3) . . ? N2 C1 S 119.8(3) . . ? N1 C1 S 122.2(3) . . ? O11 C11 N1 121.0(3) . . ? O11 C11 C12 121.4(3) . . ? N1 C11 C12 117.6(3) . . ? C17 C12 C13 119.5(4) . . ? C17 C12 C11 116.2(4) . . ? C13 C12 C11 124.3(3) . . ? C14 C13 C12 120.1(4) . . ? C15 C14 C13 120.2(4) . . ? C16 C15 C14 119.9(4) . . ? C15 C16 C17 120.8(4) . . ? C16 C17 C12 119.5(4) . . ? N2 C21 C22 110.7(3) . . ? C21 C22 C23 111.5(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S Pd S C1 0.00(5) 2 . . . ? Br Pd S C1 -125.94(15) . . . . ? Br Pd S C1 54.06(15) 2 . . . ? C21 N2 C1 N1 177.0(3) . . . . ? C21 N2 C1 S -2.7(5) . . . . ? C11 N1 C1 N2 -5.7(6) . . . . ? C11 N1 C1 S 174.0(3) . . . . ? Pd S C1 N2 169.4(3) . . . . ? Pd S C1 N1 -10.2(4) . . . . ? C1 N1 C11 O11 4.4(6) . . . . ? C1 N1 C11 C12 -175.2(3) . . . . ? O11 C11 C12 C17 1.7(5) . . . . ? N1 C11 C12 C17 -178.7(3) . . . . ? O11 C11 C12 C13 -176.9(4) . . . . ? N1 C11 C12 C13 2.7(5) . . . . ? C17 C12 C13 C14 1.4(6) . . . . ? C11 C12 C13 C14 179.9(4) . . . . ? C12 C13 C14 C15 -1.2(7) . . . . ? C13 C14 C15 C16 -0.1(7) . . . . ? C14 C15 C16 C17 1.2(7) . . . . ? C15 C16 C17 C12 -1.0(6) . . . . ? C13 C12 C17 C16 -0.3(6) . . . . ? C11 C12 C17 C16 -179.0(4) . . . . ? C1 N2 C21 C22 -174.3(4) . . . . ? N2 C21 C22 C23 -176.0(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.54 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.492 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.079