# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1175 data_pdfuall _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H22 Cl2 O2 Pd2 Se4' _chemical_formula_weight 833.87 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' 'O' 'O' 0.0106 0.0060 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.640(2) _cell_length_b 11.557(2) _cell_length_c 12.535(3) _cell_angle_alpha 100.17(3) _cell_angle_beta 105.38(3) _cell_angle_gamma 113.52(3) _cell_volume 1170.0(4) _cell_formula_units_Z 2 _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 2.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 7.995 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 14164 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_av_sigmaI/netI 0.0788 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4310 _reflns_number_gt 2992 _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^)+(0.0750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0003(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4310 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1508 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 1.114 _refine_ls_shift/su_mean 0.028 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 Pd1 Pd 0.05894(8) 0.00865(7) 0.17387(6) 0.0412(2) Uani 1 d . . . Pd2 Pd 0.30086(8) 0.03475(7) 0.42642(6) 0.0419(2) Uani 1 d . . . Se1 Se 0.32953(12) 0.17726(10) 0.30608(9) 0.0471(3) Uani 1 d . . . Se2 Se 0.16736(11) -0.13188(10) 0.23809(8) 0.0451(3) Uani 1 d . . . Se11 Se -0.20534(11) -0.16882(10) 0.03370(8) 0.0467(3) Uani 1 d . . . Se21 Se 0.26768(12) -0.11340(11) 0.54457(9) 0.0532(3) Uani 1 d . . . Cl1 Cl -0.0435(3) 0.1548(3) 0.1282(2) 0.0593(7) Uani 1 d . . . Cl2 Cl 0.4104(4) 0.2033(3) 0.6041(2) 0.0677(8) Uani 1 d . . . O11 O -0.2313(7) -0.3660(6) 0.1370(6) 0.0479(16) Uani 1 d . . . O21 O -0.0091(8) -0.3385(6) 0.3785(6) 0.0495(16) Uani 1 d . . . C1 C 0.3105(14) 0.3299(10) 0.3802(11) 0.067(3) Uani 1 d . . . H1A H 0.2095 0.2997 0.3925 0.101 Uiso 1 calc R . . H1B H 0.3129 0.3848 0.3307 0.101 Uiso 1 calc R . . H1C H 0.3997 0.3807 0.4539 0.101 Uiso 1 calc R . . C2 C 0.3387(13) -0.0993(12) 0.1733(9) 0.062(3) Uani 1 d . . . H2A H 0.4042 -0.0051 0.1918 0.093 Uiso 1 calc R . . H2B H 0.2897 -0.1403 0.0901 0.093 Uiso 1 calc R . . H2C H 0.4060 -0.1366 0.2064 0.093 Uiso 1 calc R . . C11 C -0.2197(12) -0.3361(10) 0.0388(9) 0.051(2) Uani 1 d . . . C12 C -0.2119(15) -0.4295(11) -0.0326(10) 0.066(3) Uani 1 d . . . H12 H -0.2040 -0.4311 -0.1051 0.079 Uiso 1 calc R . . C13 C -0.2179(15) -0.5275(11) 0.0232(11) 0.070(3) Uani 1 d . . . H13 H -0.2128 -0.6048 -0.0061 0.084 Uiso 1 calc R . . C14 C -0.2323(12) -0.4888(10) 0.1257(9) 0.052(2) Uani 1 d . . . C15 C -0.3474(13) -0.1665(12) 0.1185(10) 0.067(3) Uani 1 d . . . H15A H -0.4562 -0.2365 0.0731 0.101 Uiso 1 calc R . . H15B H -0.3475 -0.0822 0.1323 0.101 Uiso 1 calc R . . H15C H -0.3085 -0.1798 0.1918 0.101 Uiso 1 calc R . . C21 C 0.1492(11) -0.2937(10) 0.4482(9) 0.051(3) Uani 1 d . . . C22 C 0.1935(14) -0.3891(12) 0.4310(11) 0.069(3) Uani 1 d . . . H22 H 0.2945 -0.3833 0.4678 0.083 Uiso 1 calc R . . C23 C 0.0536(13) -0.5007(11) 0.3447(11) 0.066(3) Uani 1 d . . . H23 H 0.0467 -0.5828 0.3129 0.079 Uiso 1 calc R . . C24 C -0.0653(12) -0.4691(9) 0.3169(9) 0.048(2) Uani 1 d . . . C25 C 0.0888(15) -0.1039(12) 0.5852(11) 0.075(3) Uani 1 d . . . H25A H -0.0134 -0.1676 0.5241 0.112 Uiso 1 calc R . . H25B H 0.0999 -0.0160 0.5946 0.112 Uiso 1 calc R . . H25C H 0.0924 -0.1234 0.6569 0.112 Uiso 1 calc R . . C31 C -0.2383(12) -0.5410(10) 0.2254(10) 0.056(3) Uani 1 d . . . C32 C -0.2951(13) -0.6882(10) 0.1889(11) 0.071(3) Uani 1 d . . . H32A H -0.4064 -0.7341 0.1353 0.106 Uiso 1 calc R . . H32B H -0.2871 -0.7173 0.2564 0.106 Uiso 1 calc R . . H32C H -0.2282 -0.7075 0.1516 0.106 Uiso 1 calc R . . C33 C -0.3531(13) -0.5093(11) 0.2799(10) 0.064(3) Uani 1 d . . . H33A H -0.3141 -0.4148 0.3053 0.096 Uiso 1 calc R . . H33B H -0.3537 -0.5414 0.3455 0.096 Uiso 1 calc R . . H33C H -0.4617 -0.5523 0.2223 0.096 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 Pd1 0.0375(4) 0.0453(4) 0.0466(5) 0.0208(4) 0.0238(3) 0.0171(4) Pd2 0.0370(4) 0.0426(4) 0.0438(5) 0.0158(4) 0.0204(3) 0.0124(4) Se1 0.0414(6) 0.0446(6) 0.0557(6) 0.0209(5) 0.0263(5) 0.0134(5) Se2 0.0403(6) 0.0427(5) 0.0490(6) 0.0148(5) 0.0169(4) 0.0161(5) Se11 0.0406(6) 0.0574(6) 0.0430(6) 0.0218(5) 0.0198(4) 0.0190(5) Se21 0.0444(6) 0.0536(6) 0.0474(6) 0.0214(5) 0.0134(5) 0.0099(5) Cl1 0.0675(17) 0.0651(17) 0.0658(17) 0.0326(14) 0.0337(14) 0.0398(15) Cl2 0.078(2) 0.0538(16) 0.0522(16) 0.0077(13) 0.0262(14) 0.0161(15) O11 0.045(4) 0.046(4) 0.052(4) 0.018(3) 0.021(3) 0.018(3) O21 0.037(4) 0.049(4) 0.055(4) 0.019(4) 0.016(3) 0.014(3) C1 0.060(7) 0.049(6) 0.091(9) 0.017(6) 0.023(6) 0.029(6) C2 0.060(7) 0.082(8) 0.057(7) 0.022(6) 0.033(6) 0.038(7) C11 0.042(6) 0.047(6) 0.045(6) 0.008(5) 0.015(5) 0.007(5) C12 0.078(8) 0.051(7) 0.054(7) 0.010(6) 0.025(6) 0.020(6) C13 0.088(9) 0.052(7) 0.078(8) 0.020(6) 0.047(7) 0.032(7) C14 0.041(6) 0.043(6) 0.063(7) 0.017(5) 0.022(5) 0.011(5) C15 0.046(6) 0.091(9) 0.069(8) 0.027(7) 0.036(6) 0.027(6) C21 0.034(5) 0.055(6) 0.056(6) 0.025(5) 0.014(5) 0.012(5) C22 0.047(7) 0.068(8) 0.095(9) 0.044(7) 0.017(6) 0.028(7) C23 0.052(7) 0.048(6) 0.092(9) 0.022(6) 0.020(6) 0.022(6) C24 0.043(6) 0.040(6) 0.062(7) 0.025(5) 0.020(5) 0.016(5) C25 0.084(9) 0.076(8) 0.077(8) 0.027(7) 0.061(7) 0.027(7) C31 0.044(6) 0.046(6) 0.073(8) 0.023(6) 0.024(5) 0.013(5) C32 0.046(6) 0.044(6) 0.097(9) 0.020(6) 0.012(6) 0.008(5) C33 0.056(7) 0.066(7) 0.077(8) 0.030(6) 0.034(6) 0.026(6) _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 Cl1 2.351(3) . ? Pd1 Se2 2.3976(13) . ? Pd1 Se1 2.420(2) . ? Pd1 Se11 2.443(2) . ? Pd2 Cl2 2.334(3) . ? Pd2 Se2 2.3964(18) . ? Pd2 Se1 2.4082(13) . ? Pd2 Se21 2.4366(13) . ? Se1 C1 1.944(10) . ? Se2 C2 1.962(10) . ? Se11 C11 1.896(10) . ? Se11 C15 1.948(10) . ? Se21 C21 1.893(11) . ? Se21 C25 1.960(11) . ? O11 C11 1.357(11) . ? O11 C14 1.397(11) . ? O21 C24 1.372(12) . ? O21 C21 1.364(11) . ? C11 C12 1.315(15) . ? C12 C13 1.423(15) . ? C13 C14 1.346(15) . ? C14 C31 1.486(14) . ? C21 C22 1.336(15) . ? C22 C23 1.413(16) . ? C23 C24 1.318(13) . ? C24 C31 1.526(14) . ? C31 C32 1.501(14) . ? C31 C33 1.569(14) . ? 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 Cl1 Pd1 Se2 174.95(8) . . ? Cl1 Pd1 Se1 96.98(8) . . ? Se2 Pd1 Se1 80.52(5) . . ? Cl1 Pd1 Se11 85.64(8) . . ? Se2 Pd1 Se11 97.09(5) . . ? Se1 Pd1 Se11 176.04(4) . . ? Cl2 Pd2 Se2 174.23(8) . . ? Cl2 Pd2 Se1 96.51(8) . . ? Se2 Pd2 Se1 80.79(5) . . ? Cl2 Pd2 Se21 84.62(8) . . ? Se2 Pd2 Se21 98.05(5) . . ? Se1 Pd2 Se21 178.80(5) . . ? C1 Se1 Pd2 107.9(4) . . ? C1 Se1 Pd1 107.4(4) . . ? Pd2 Se1 Pd1 85.47(5) . . ? C2 Se2 Pd2 104.4(3) . . ? C2 Se2 Pd1 101.8(3) . . ? Pd2 Se2 Pd1 86.24(5) . . ? C11 Se11 C15 96.6(5) . . ? C11 Se11 Pd1 109.3(3) . . ? C15 Se11 Pd1 101.5(4) . . ? C21 Se21 C25 96.9(5) . . ? C21 Se21 Pd2 110.6(3) . . ? C25 Se21 Pd2 99.6(4) . . ? C11 O11 C14 106.9(8) . . ? C24 O21 C21 105.9(8) . . ? C12 C11 O11 111.2(10) . . ? C12 C11 Se11 132.7(9) . . ? O11 C11 Se11 116.0(7) . . ? C11 C12 C13 106.4(11) . . ? C14 C13 C12 108.1(10) . . ? C13 C14 O11 107.4(8) . . ? C13 C14 C31 135.5(10) . . ? O11 C14 C31 117.0(9) . . ? C22 C21 O21 111.0(10) . . ? C22 C21 Se21 131.6(8) . . ? O21 C21 Se21 117.4(8) . . ? C21 C22 C23 105.1(9) . . ? C24 C23 C22 108.6(10) . . ? C23 C24 O21 109.4(9) . . ? C23 C24 C31 133.8(10) . . ? O21 C24 C31 116.5(8) . . ? C14 C31 C32 111.5(10) . . ? C14 C31 C24 106.9(8) . . ? C32 C31 C24 109.3(9) . . ? C14 C31 C33 110.3(9) . . ? C32 C31 C33 109.9(9) . . ? C24 C31 C33 108.9(9) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 1.651 _refine_diff_density_min -1.923 _refine_diff_density_rms 0.250