# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2302 data_jain100 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Triphenylphosphine chloro 2(N,N-dimethylamino)ethylselenolato palladium(II) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H25 Cl N P Pd Se' _chemical_formula_weight 555.21 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 9.5268(19) _cell_length_b 19.827(4) _cell_length_c 11.661(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.77(3) _cell_angle_gamma 90.00 _cell_volume 2191.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 2.710 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 7291 _diffrn_reflns_av_R_equivalents 0.0861 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 30.04 _reflns_number_total 5997 _reflns_number_gt 5050 _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5997 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1354 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 Pd Pd 0.83108(3) 0.134033(13) 0.56891(2) 0.01784(11) Uani 1 1 d . . . Se Se 0.68441(5) 0.040196(19) 0.51596(4) 0.02783(13) Uani 1 1 d . . . P P 0.92612(10) 0.07533(5) 0.72328(8) 0.01844(19) Uani 1 1 d . . . N N 0.7160(4) 0.18835(16) 0.4290(3) 0.0227(6) Uani 1 1 d . . . C13 C 0.8688(4) 0.11543(18) 0.8508(3) 0.0208(7) Uani 1 1 d . . . C7 C 1.1181(4) 0.06821(19) 0.7457(3) 0.0223(7) Uani 1 1 d . . . C18 C 0.9451(4) 0.1119(2) 0.9603(3) 0.0257(7) Uani 1 1 d . . . H18A H 1.0307 0.0889 0.9698 0.031 Uiso 1 1 calc R . . C1 C 0.8711(4) -0.01282(17) 0.7344(3) 0.0215(7) Uani 1 1 d . . . C5 C 0.8650(5) -0.1249(2) 0.6527(4) 0.0325(9) Uani 1 1 d . . . H5A H 0.8919 -0.1551 0.5980 0.039 Uiso 1 1 calc R . . C2 C 0.7838(4) -0.03465(19) 0.8166(4) 0.0250(7) Uani 1 1 d . . . H2A H 0.7567 -0.0047 0.8716 0.030 Uiso 1 1 calc R . . C14 C 0.7413(5) 0.1516(2) 0.8399(4) 0.0297(8) Uani 1 1 d . . . H14A H 0.6901 0.1556 0.7680 0.036 Uiso 1 1 calc R . . C6 C 0.9127(5) -0.0589(2) 0.6527(4) 0.0276(8) Uani 1 1 d . . . H6A H 0.9722 -0.0451 0.5987 0.033 Uiso 1 1 calc R . . C4 C 0.7776(5) -0.1462(2) 0.7335(4) 0.0348(10) Uani 1 1 d . . . H4A H 0.7457 -0.1905 0.7326 0.042 Uiso 1 1 calc R . . C3 C 0.7376(5) -0.1016(2) 0.8156(4) 0.0318(9) Uani 1 1 d . . . H3A H 0.6798 -0.1163 0.8703 0.038 Uiso 1 1 calc R . . C17 C 0.8928(5) 0.1426(2) 1.0545(4) 0.0321(9) Uani 1 1 d . . . H17A H 0.9442 0.1399 1.1265 0.039 Uiso 1 1 calc R . . C15 C 0.6908(5) 0.1816(3) 0.9356(4) 0.0376(10) Uani 1 1 d . . . H15A H 0.6057 0.2049 0.9273 0.045 Uiso 1 1 calc R . . C20 C 0.6430(5) 0.1409(2) 0.3422(4) 0.0287(8) Uani 1 1 d . . . H20A H 0.7126 0.1186 0.3002 0.034 Uiso 1 1 calc R . . H20B H 0.5804 0.1663 0.2873 0.034 Uiso 1 1 calc R . . C19 C 0.5586(5) 0.0885(2) 0.4001(4) 0.0308(9) Uani 1 1 d . . . H19A H 0.5163 0.0569 0.3432 0.037 Uiso 1 1 calc R . . H19B H 0.4835 0.1102 0.4368 0.037 Uiso 1 1 calc R . . C8 C 1.2058(5) 0.1087(2) 0.6855(4) 0.0315(9) Uani 1 1 d . . . H8A H 1.1667 0.1399 0.6320 0.038 Uiso 1 1 calc R . . C21 C 0.8033(6) 0.2340(2) 0.3646(4) 0.0368(10) Uani 1 1 d . . . H21A H 0.7444 0.2561 0.3043 0.055 Uiso 1 1 calc R . . H21B H 0.8745 0.2083 0.3316 0.055 Uiso 1 1 calc R . . H21C H 0.8474 0.2672 0.4162 0.055 Uiso 1 1 calc R . . C12 C 1.1795(5) 0.0212(2) 0.8253(4) 0.0327(9) Uani 1 1 d . . . H12A H 1.1220 -0.0068 0.8644 0.039 Uiso 1 1 calc R . . C16 C 0.7666(6) 0.1770(2) 1.0433(4) 0.0348(10) Uani 1 1 d . . . H16A H 0.7325 0.1969 1.1072 0.042 Uiso 1 1 calc R . . C22 C 0.6091(5) 0.2301(2) 0.4811(4) 0.0348(10) Uani 1 1 d . . . H22A H 0.5551 0.2553 0.4218 0.052 Uiso 1 1 calc R . . H22B H 0.6560 0.2607 0.5362 0.052 Uiso 1 1 calc R . . H22C H 0.5473 0.2013 0.5191 0.052 Uiso 1 1 calc R . . C10 C 1.4104(5) 0.0565(3) 0.7859(6) 0.0464(13) Uani 1 1 d . . . H10A H 1.5080 0.0529 0.7996 0.056 Uiso 1 1 calc R . . C9 C 1.3520(5) 0.1021(3) 0.7056(5) 0.0434(12) Uani 1 1 d . . . H9A H 1.4103 0.1286 0.6647 0.052 Uiso 1 1 calc R . . C11 C 1.3246(5) 0.0160(3) 0.8464(5) 0.0430(12) Uani 1 1 d . . . H11A H 1.3644 -0.0145 0.9009 0.052 Uiso 1 1 calc R . . Cl Cl 0.95980(12) 0.23248(5) 0.63216(9) 0.0297(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.02102(16) 0.01560(15) 0.01521(15) 0.00126(8) -0.00651(10) -0.00105(9) Se 0.0311(2) 0.01952(19) 0.0289(2) 0.00496(14) -0.01629(16) -0.00616(15) P 0.0197(4) 0.0177(4) 0.0163(4) 0.0012(3) -0.0062(3) 0.0004(3) N 0.0265(16) 0.0204(14) 0.0192(14) 0.0035(11) -0.0076(12) -0.0017(12) C13 0.0223(17) 0.0188(14) 0.0198(16) 0.0017(12) -0.0060(13) -0.0012(13) C7 0.0195(16) 0.0219(16) 0.0239(17) -0.0028(13) -0.0052(14) 0.0010(13) C18 0.0251(18) 0.0274(18) 0.0228(18) 0.0004(14) -0.0063(14) 0.0044(15) C1 0.0202(16) 0.0167(14) 0.0250(17) 0.0032(13) -0.0108(13) 0.0001(13) C5 0.041(2) 0.0236(18) 0.030(2) -0.0015(15) -0.0105(18) 0.0009(17) C2 0.0235(18) 0.0254(17) 0.0246(18) 0.0055(14) -0.0048(15) 0.0013(15) C14 0.0253(19) 0.040(2) 0.0220(18) 0.0018(16) -0.0063(15) 0.0071(17) C6 0.036(2) 0.0221(17) 0.0231(18) 0.0006(14) -0.0064(16) 0.0021(16) C4 0.038(2) 0.0215(17) 0.041(2) 0.0055(17) -0.0173(19) -0.0044(17) C3 0.029(2) 0.0265(19) 0.038(2) 0.0096(16) -0.0068(17) -0.0062(16) C17 0.039(2) 0.038(2) 0.0177(17) 0.0014(16) -0.0056(16) -0.0010(19) C15 0.036(2) 0.043(3) 0.034(2) 0.0014(18) 0.0019(19) 0.014(2) C20 0.038(2) 0.0231(17) 0.0216(18) 0.0040(14) -0.0125(16) -0.0021(16) C19 0.030(2) 0.0256(18) 0.033(2) 0.0069(15) -0.0164(17) -0.0030(16) C8 0.026(2) 0.030(2) 0.038(2) -0.0019(17) -0.0008(17) -0.0027(16) C21 0.044(3) 0.034(2) 0.029(2) 0.0139(17) -0.0121(19) -0.0138(19) C12 0.027(2) 0.035(2) 0.034(2) 0.0064(17) -0.0072(17) 0.0073(17) C16 0.046(3) 0.034(2) 0.0237(19) -0.0016(16) -0.0017(18) 0.0036(19) C22 0.039(2) 0.0261(19) 0.037(2) -0.0044(17) -0.0114(19) 0.0102(18) C10 0.020(2) 0.046(3) 0.070(4) -0.018(3) -0.012(2) 0.002(2) C9 0.023(2) 0.044(3) 0.063(4) -0.006(2) 0.004(2) -0.007(2) C11 0.029(2) 0.044(3) 0.052(3) -0.002(2) -0.017(2) 0.012(2) Cl 0.0361(5) 0.0210(4) 0.0294(5) -0.0015(3) -0.0087(4) -0.0071(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N 2.160(3) . ? Pd P 2.2554(11) . ? Pd Se 2.3710(6) . ? Pd Cl 2.3823(10) . ? Se C19 1.963(4) . ? P C13 1.817(4) . ? P C7 1.827(4) . ? P C1 1.833(4) . ? N C21 1.484(5) . ? N C22 1.489(6) . ? N C20 1.500(5) . ? C13 C14 1.406(6) . ? C13 C18 1.406(5) . ? C7 C8 1.397(6) . ? C7 C12 1.401(6) . ? C18 C17 1.392(6) . ? C1 C2 1.398(6) . ? C1 C6 1.405(6) . ? C5 C4 1.385(7) . ? C5 C6 1.385(6) . ? C2 C3 1.399(5) . ? C14 C15 1.392(6) . ? C4 C3 1.385(7) . ? C17 C16 1.377(7) . ? C15 C16 1.387(7) . ? C20 C19 1.514(6) . ? C8 C9 1.395(6) . ? C12 C11 1.383(7) . ? C10 C9 1.377(9) . ? C10 C11 1.389(9) . ? 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 N Pd P 173.13(10) . . ? N Pd Se 87.33(9) . . ? P Pd Se 88.95(3) . . ? N Pd Cl 91.82(9) . . ? P Pd Cl 91.31(4) . . ? Se Pd Cl 174.29(3) . . ? C19 Se Pd 95.71(13) . . ? C13 P C7 107.20(18) . . ? C13 P C1 104.33(18) . . ? C7 P C1 101.86(17) . . ? C13 P Pd 107.31(12) . . ? C7 P Pd 118.02(13) . . ? C1 P Pd 116.99(12) . . ? C21 N C22 107.9(4) . . ? C21 N C20 106.6(3) . . ? C22 N C20 109.6(3) . . ? C21 N Pd 114.8(3) . . ? C22 N Pd 106.6(3) . . ? C20 N Pd 111.3(2) . . ? C14 C13 C18 118.1(4) . . ? C14 C13 P 118.6(3) . . ? C18 C13 P 123.4(3) . . ? C8 C7 C12 119.0(4) . . ? C8 C7 P 121.6(3) . . ? C12 C7 P 119.4(3) . . ? C17 C18 C13 120.1(4) . . ? C2 C1 C6 119.4(3) . . ? C2 C1 P 122.5(3) . . ? C6 C1 P 118.0(3) . . ? C4 C5 C6 120.5(4) . . ? C1 C2 C3 119.8(4) . . ? C15 C14 C13 120.8(4) . . ? C5 C6 C1 119.9(4) . . ? C3 C4 C5 120.2(4) . . ? C4 C3 C2 120.2(4) . . ? C16 C17 C18 121.4(4) . . ? C16 C15 C14 120.5(4) . . ? N C20 C19 111.1(3) . . ? C20 C19 Se 109.1(3) . . ? C9 C8 C7 119.9(5) . . ? C11 C12 C7 120.7(5) . . ? C17 C16 C15 119.2(4) . . ? C9 C10 C11 120.4(5) . . ? C10 C9 C8 120.2(5) . . ? C12 C11 C10 119.7(5) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 1.771 _refine_diff_density_min -1.864 _refine_diff_density_rms 0.159 data_indien _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Tris[chloro 2(N,N-dimtehylamino)ethylselenato palladium(II)] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H30 Cl3 N3 Pd3 Se3' _chemical_formula_weight 878.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 10.7805(5) _cell_length_b 13.1187(9) _cell_length_c 16.6749(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.899(5) _cell_angle_gamma 90.00 _cell_volume 2345.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 7.274 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _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 22492 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.02 _reflns_number_total 5593 _reflns_number_gt 3983 _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^)+(0.0531P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00211(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5593 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_restrained_S_all 0.884 _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 0.10708(3) 0.95957(3) 0.85709(2) 0.03843(11) Uani 1 1 d . . . Pd2 Pd 0.12545(3) 1.03272(3) 0.63622(2) 0.03585(11) Uani 1 1 d . . . Pd3 Pd 0.40406(3) 1.00103(3) 0.76387(2) 0.03508(10) Uani 1 1 d . . . Se3 Se 0.24869(5) 0.89432(4) 0.69711(3) 0.04083(14) Uani 1 1 d . . . Se1 Se 0.24831(5) 1.09171(4) 0.83059(4) 0.04605(15) Uani 1 1 d . . . Se2 Se -0.01510(5) 0.98857(5) 0.73069(3) 0.04428(15) Uani 1 1 d . . . Cl2 Cl 0.26339(15) 1.07587(13) 0.53986(10) 0.0567(4) Uani 1 1 d . . . Cl3 Cl 0.55569(13) 1.11778(12) 0.81848(9) 0.0526(3) Uani 1 1 d . . . Cl1 Cl -0.03128(16) 0.82628(13) 0.87742(10) 0.0599(4) Uani 1 1 d . . . N2 N 0.0039(4) 1.1574(3) 0.6025(3) 0.0394(10) Uani 1 1 d . . . N3 N 0.5382(4) 0.9132(3) 0.7075(3) 0.0431(10) Uani 1 1 d . . . N1 N 0.2184(5) 0.9327(4) 0.9683(3) 0.0526(12) Uani 1 1 d . . . C5 C -0.0808(6) 1.1262(5) 0.7339(4) 0.0572(16) Uani 1 1 d . . . H13A H -0.1557 1.1274 0.7615 0.069 Uiso 1 1 calc R . . H13B H -0.0197 1.1715 0.7618 0.069 Uiso 1 1 calc R . . C9 C 0.3591(5) 0.8392(5) 0.6202(4) 0.0547(15) Uani 1 1 d . . . C10 C 0.4825(5) 0.8194(5) 0.6705(4) 0.0521(14) Uani 1 1 d . . . H15A H 0.4692 0.7709 0.7127 0.063 Uiso 1 1 calc R . . H15B H 0.5404 0.7891 0.6365 0.063 Uiso 1 1 calc R . . C6 C -0.1095(5) 1.1581(5) 0.6472(4) 0.0529(15) Uani 1 1 d . . . H16A H -0.1713 1.1123 0.6207 0.063 Uiso 1 1 calc R . . H16B H -0.1448 1.2262 0.6453 0.063 Uiso 1 1 calc R . . C12 C 0.5885(7) 0.9777(5) 0.6461(4) 0.0609(16) Uani 1 1 d . . . H17A H 0.6244 1.0383 0.6712 0.073 Uiso 1 1 calc R . . H17B H 0.5224 0.9962 0.6057 0.073 Uiso 1 1 calc R . . H17C H 0.6514 0.9408 0.6215 0.073 Uiso 1 1 calc R . . C8 C -0.0400(6) 1.1551(5) 0.5150(4) 0.0579(16) Uani 1 1 d . . . H18A H -0.0862 1.0935 0.5026 0.069 Uiso 1 1 calc R . . H18B H 0.0305 1.1574 0.4842 0.069 Uiso 1 1 calc R . . H18C H -0.0928 1.2129 0.5016 0.069 Uiso 1 1 calc R . . C11 C 0.6420(5) 0.8818(5) 0.7684(4) 0.0579(17) Uani 1 1 d . . . H19A H 0.6096 0.8397 0.8086 0.070 Uiso 1 1 calc R . . H19B H 0.6804 0.9413 0.7937 0.070 Uiso 1 1 calc R . . H19C H 0.7028 0.8441 0.7424 0.070 Uiso 1 1 calc R . . C7 C 0.0738(6) 1.2518(5) 0.6194(5) 0.0610(17) Uani 1 1 d . . . H20A H 0.1030 1.2548 0.6757 0.073 Uiso 1 1 calc R . . H20B H 0.0205 1.3091 0.6054 0.073 Uiso 1 1 calc R . . H20C H 0.1437 1.2536 0.5881 0.073 Uiso 1 1 calc R . . C1 C 0.3291(8) 1.0900(7) 0.9426(4) 0.087(3) Uani 1 1 d . . . H39 H 0.3772 1.1442 0.9642 0.104 Uiso 1 1 calc R . . C3 C 0.2821(10) 0.8368(8) 0.9621(5) 0.113(4) Uani 1 1 d . . . H40A H 0.3302 0.8387 0.9168 0.136 Uiso 1 1 calc R . . H40B H 0.2220 0.7827 0.9549 0.136 Uiso 1 1 calc R . . H H 0.3365 0.8250 1.0105 0.136 Uiso 1 1 calc R . . C4 C 0.1472(8) 0.9276(11) 1.0366(5) 0.123(5) Uani 1 1 d . . . H41A H 0.1040 0.9909 1.0417 0.148 Uiso 1 1 calc R . . H41B H 0.2022 0.9154 1.0847 0.148 Uiso 1 1 calc R . . H41C H 0.0877 0.8731 1.0290 0.148 Uiso 1 1 calc R . . C2 C 0.3115(16) 1.0116(11) 0.9824(9) 0.236(12) Uani 1 1 d . . . H42 H 0.3670 1.0027 1.0284 0.283 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 0.03471(19) 0.0412(2) 0.0400(2) 0.00014(16) 0.00687(16) 0.00198(15) Pd2 0.03251(18) 0.0398(2) 0.0349(2) -0.00187(15) 0.00193(15) -0.00215(15) Pd3 0.03296(18) 0.0360(2) 0.0359(2) 0.00111(15) 0.00192(15) -0.00099(15) Se3 0.0373(3) 0.0387(3) 0.0459(3) -0.0041(2) 0.0009(2) -0.0004(2) Se1 0.0422(3) 0.0424(3) 0.0545(3) -0.0078(2) 0.0098(2) -0.0030(2) Se2 0.0346(3) 0.0539(3) 0.0442(3) 0.0060(2) 0.0032(2) -0.0052(2) Cl2 0.0538(8) 0.0648(9) 0.0545(9) 0.0053(7) 0.0200(7) -0.0007(7) Cl3 0.0477(7) 0.0540(8) 0.0541(8) 0.0018(6) -0.0038(6) -0.0136(6) Cl1 0.0625(9) 0.0600(9) 0.0599(9) 0.0037(7) 0.0186(8) -0.0165(7) N2 0.037(2) 0.038(2) 0.041(2) 0.0007(18) -0.0043(19) 0.0003(17) N3 0.043(2) 0.042(2) 0.044(2) -0.001(2) 0.008(2) 0.0026(19) N1 0.047(3) 0.058(3) 0.052(3) 0.003(2) -0.001(2) 0.009(2) C5 0.045(3) 0.072(4) 0.058(4) 0.008(3) 0.018(3) 0.017(3) C9 0.048(3) 0.059(4) 0.056(4) -0.017(3) 0.000(3) 0.009(3) C10 0.046(3) 0.048(3) 0.062(4) -0.011(3) 0.006(3) 0.010(2) C6 0.033(3) 0.058(4) 0.067(4) 0.016(3) 0.005(3) 0.009(2) C12 0.060(4) 0.067(4) 0.059(4) 0.003(3) 0.022(3) -0.003(3) C8 0.062(4) 0.067(4) 0.042(3) 0.002(3) -0.006(3) 0.003(3) C11 0.041(3) 0.060(4) 0.069(4) -0.004(3) -0.011(3) 0.014(3) C7 0.050(3) 0.043(3) 0.088(5) -0.010(3) 0.000(3) -0.007(3) C1 0.101(6) 0.116(7) 0.044(4) -0.030(4) 0.015(4) -0.056(5) C3 0.131(8) 0.133(9) 0.073(5) 0.001(5) -0.004(5) 0.096(7) C4 0.075(5) 0.256(15) 0.039(4) -0.023(6) 0.008(4) 0.050(7) C2 0.294(19) 0.198(14) 0.171(12) 0.130(11) -0.193(14) -0.179(14) _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 2.133(5) . ? Pd1 Cl1 2.3455(16) . ? Pd1 Se1 2.3783(7) . ? Pd1 Se2 2.3982(7) . ? Pd2 N2 2.135(4) . ? Pd2 Se2 2.3672(7) . ? Pd2 Cl2 2.3673(16) . ? Pd2 Se3 2.4115(6) . ? Pd3 N3 2.141(5) . ? Pd3 Cl3 2.3540(14) . ? Pd3 Se3 2.3709(6) . ? Pd3 Se1 2.4199(7) . ? Se3 C9 1.975(6) . ? Se1 C1 1.978(7) . ? Se2 C5 1.942(7) . ? N2 C7 1.462(7) . ? N2 C8 1.487(7) . ? N2 C6 1.496(7) . ? N3 C12 1.474(8) . ? N3 C10 1.476(7) . ? N3 C11 1.490(7) . ? N1 C4 1.439(10) . ? N1 C3 1.442(9) . ? N1 C2 1.444(11) . ? C5 C6 1.507(9) . ? C9 C10 1.520(8) . ? C1 C2 1.250(13) . ? 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 93.46(16) . . ? N1 Pd1 Se1 88.19(15) . . ? Cl1 Pd1 Se1 177.41(5) . . ? N1 Pd1 Se2 178.94(15) . . ? Cl1 Pd1 Se2 86.86(5) . . ? Se1 Pd1 Se2 91.45(2) . . ? N2 Pd2 Se2 86.88(13) . . ? N2 Pd2 Cl2 92.81(13) . . ? Se2 Pd2 Cl2 178.98(5) . . ? N2 Pd2 Se3 169.91(13) . . ? Se2 Pd2 Se3 84.16(2) . . ? Cl2 Pd2 Se3 96.23(4) . . ? N3 Pd3 Cl3 92.66(13) . . ? N3 Pd3 Se3 87.28(12) . . ? Cl3 Pd3 Se3 174.15(4) . . ? N3 Pd3 Se1 176.85(13) . . ? Cl3 Pd3 Se1 89.39(5) . . ? Se3 Pd3 Se1 90.92(2) . . ? C9 Se3 Pd3 94.45(17) . . ? C9 Se3 Pd2 110.18(19) . . ? Pd3 Se3 Pd2 94.89(2) . . ? C1 Se1 Pd1 92.6(2) . . ? C1 Se1 Pd3 99.8(3) . . ? Pd1 Se1 Pd3 102.41(2) . . ? C5 Se2 Pd2 92.9(2) . . ? C5 Se2 Pd1 107.0(2) . . ? Pd2 Se2 Pd1 107.00(2) . . ? C7 N2 C8 108.2(5) . . ? C7 N2 C6 109.3(5) . . ? C8 N2 C6 107.1(4) . . ? C7 N2 Pd2 108.0(3) . . ? C8 N2 Pd2 111.6(4) . . ? C6 N2 Pd2 112.6(3) . . ? C12 N3 C10 110.6(5) . . ? C12 N3 C11 109.2(5) . . ? C10 N3 C11 107.4(4) . . ? C12 N3 Pd3 108.0(4) . . ? C10 N3 Pd3 111.6(4) . . ? C11 N3 Pd3 110.1(4) . . ? C4 N1 C3 108.3(8) . . ? C4 N1 C2 108.8(10) . . ? C3 N1 C2 108.0(10) . . ? C4 N1 Pd1 113.4(4) . . ? C3 N1 Pd1 108.1(5) . . ? C2 N1 Pd1 110.0(5) . . ? C6 C5 Se2 105.8(5) . . ? C10 C9 Se3 104.8(4) . . ? N3 C10 C9 112.6(5) . . ? N2 C6 C5 112.3(4) . . ? C2 C1 Se1 115.8(6) . . ? C1 C2 N1 130.2(8) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.216 _refine_diff_density_min -1.012 _refine_diff_density_rms 0.151