# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Hauz Khas, New Delhi 110016 India ; _publ_contact_author_email aksingh@chemistry.iitd.ac.in _publ_contact_author_fax +91-11-26582277 _publ_contact_author_phone +91-11-26591379 #TrackingRef '- CCDC-765901-revised.cif' _publ_contact_author_name 'D. Das, P. Singh and A. K. Singh' loop_ _publ_author_name D.Das P.Singh A.K.Singh data_L _database_code_depnum_ccdc_archive 'CCDC 763938' #TrackingRef '- CCDC-763938.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H30 Se4' _chemical_formula_sum 'C34 H30 Se4 ' _chemical_formula_weight 754.42 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.453(5) _cell_length_b 10.808(4) _cell_length_c 11.001(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.325(9) _cell_angle_gamma 90.00 _cell_volume 1476.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 1285 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.32 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.504 _exptl_crystal_size_mid 0.314 _exptl_crystal_size_min 0.144 _exptl_crystal_density_meas 1.697 _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740.0 _exptl_absorpt_coefficient_mu 4.992 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.164 _exptl_absorpt_correction_T_max 0.489 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 13742 _diffrn_reflns_av_R_equivalents 0.0904 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2596 _reflns_number_gt 2307 _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^)+(0.0481P)^2^+5.1375P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2596 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1141 _refine_ls_R_factor_gt 0.0997 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1692 _refine_ls_goodness_of_fit_ref 1.373 _refine_ls_restrained_S_all 1.373 _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 Se1 Se 0.26384(9) 0.12914(10) 0.16989(10) 0.0488(4) Uani 1 1 d . . . Se2 Se 0.54315(9) 0.08841(11) 0.36220(9) 0.0471(4) Uani 1 1 d . . . C1 C 0.5921(7) -0.0226(9) 0.0694(8) 0.036(2) Uani 1 1 d . . . H1 H 0.6550 -0.0391 0.1177 0.043 Uiso 1 1 calc R . . C2 C 0.5312(8) 0.0781(9) 0.0994(8) 0.035(2) Uani 1 1 d . . . C3 C 0.4347(7) 0.1010(8) 0.0284(8) 0.034(2) Uani 1 1 d . . . C4 C 0.3603(8) 0.2035(10) 0.0561(9) 0.044(3) Uani 1 1 d . . . H4A H 0.3200 0.2321 -0.0174 0.053 Uiso 1 1 calc R . . H4B H 0.3999 0.2726 0.0937 0.053 Uiso 1 1 calc R . . C5 C 0.1815(7) 0.2663(9) 0.2199(8) 0.032(2) Uani 1 1 d . . . C6 C 0.1769(9) 0.3783(10) 0.1635(10) 0.053(3) Uani 1 1 d . . . H6 H 0.2166 0.3925 0.0966 0.064 Uiso 1 1 calc R . . C7 C 0.1125(9) 0.4715(11) 0.2060(12) 0.064(3) Uani 1 1 d . . . H7 H 0.1087 0.5474 0.1661 0.076 Uiso 1 1 calc R . . C8 C 0.0547(9) 0.4535(12) 0.3051(12) 0.062(3) Uani 1 1 d . . . H8 H 0.0118 0.5163 0.3329 0.074 Uiso 1 1 calc R . . C9 C 0.0612(9) 0.3408(13) 0.3631(11) 0.062(3) Uani 1 1 d . . . H9 H 0.0228 0.3280 0.4313 0.075 Uiso 1 1 calc R . . C10 C 0.1231(8) 0.2474(11) 0.3226(10) 0.051(3) Uani 1 1 d . . . H10 H 0.1266 0.1716 0.3627 0.061 Uiso 1 1 calc R . . C11 C 0.5712(8) 0.1595(9) 0.2024(8) 0.043(2) Uani 1 1 d . . . H11A H 0.5364 0.2396 0.1936 0.051 Uiso 1 1 calc R . . H11B H 0.6481 0.1720 0.1992 0.051 Uiso 1 1 calc R . . C12 C 0.6675(7) 0.1546(9) 0.4573(8) 0.031(2) Uani 1 1 d . . . C13 C 0.7112(8) 0.0826(9) 0.5524(8) 0.037(2) Uani 1 1 d . . . H13 H 0.6806 0.0069 0.5704 0.045 Uiso 1 1 calc R . . C14 C 0.8011(8) 0.1255(9) 0.6196(8) 0.042(2) Uani 1 1 d . . . H14 H 0.8318 0.0786 0.6841 0.050 Uiso 1 1 calc R . . C15 C 0.8461(8) 0.2376(10) 0.5923(10) 0.046(3) Uani 1 1 d . . . H15 H 0.9082 0.2650 0.6364 0.055 Uiso 1 1 calc R . . C16 C 0.7994(8) 0.3081(9) 0.5005(9) 0.041(2) Uani 1 1 d . . . H16 H 0.8287 0.3848 0.4837 0.049 Uiso 1 1 calc R . . C17 C 0.7094(8) 0.2672(9) 0.4325(9) 0.039(2) Uani 1 1 d . . . H17 H 0.6774 0.3159 0.3702 0.047 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 Se1 0.0517(7) 0.0401(6) 0.0577(7) 0.0104(5) 0.0249(5) 0.0080(5) Se2 0.0456(7) 0.0708(8) 0.0251(5) -0.0038(5) 0.0044(4) -0.0257(5) C1 0.025(5) 0.053(6) 0.030(5) 0.005(5) -0.004(4) 0.008(4) C2 0.046(6) 0.039(6) 0.023(5) 0.003(4) 0.011(4) -0.009(5) C3 0.035(5) 0.036(6) 0.031(5) -0.003(4) 0.003(4) -0.002(4) C4 0.041(6) 0.056(7) 0.038(6) 0.008(5) 0.018(5) 0.007(5) C5 0.019(4) 0.039(6) 0.039(5) -0.004(4) 0.003(4) -0.004(4) C6 0.059(7) 0.051(7) 0.053(7) -0.007(6) 0.016(6) 0.007(6) C7 0.060(8) 0.049(8) 0.082(9) -0.019(7) 0.003(7) 0.006(6) C8 0.042(7) 0.056(8) 0.087(9) -0.039(7) 0.001(6) 0.012(6) C9 0.043(7) 0.084(10) 0.063(8) -0.017(7) 0.017(6) -0.007(6) C10 0.041(6) 0.063(8) 0.050(7) -0.001(6) 0.009(5) 0.003(5) C11 0.049(6) 0.043(6) 0.036(6) -0.002(5) 0.000(5) 0.000(5) C12 0.024(5) 0.047(6) 0.022(5) -0.011(4) 0.003(4) -0.005(4) C13 0.048(6) 0.037(5) 0.029(5) 0.001(4) 0.008(4) -0.007(5) C14 0.050(6) 0.051(7) 0.025(5) 0.008(5) 0.006(5) 0.002(5) C15 0.030(5) 0.055(7) 0.052(7) -0.006(5) -0.004(5) -0.008(5) C16 0.044(6) 0.033(6) 0.046(6) 0.000(5) 0.010(5) -0.009(5) C17 0.043(6) 0.034(6) 0.039(6) 0.003(4) -0.002(5) -0.006(5) _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 Se1 C5 1.907(9) . ? Se1 C4 1.971(9) . ? Se2 C12 1.939(8) . ? Se2 C11 1.973(10) . ? C1 C2 1.381(13) . ? C1 C3 1.389(12) 3_655 ? C1 H1 0.9300 . ? C2 C3 1.405(13) . ? C2 C11 1.491(13) . ? C3 C1 1.389(12) 3_655 ? C3 C4 1.490(13) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.359(14) . ? C5 C10 1.404(13) . ? C6 C7 1.390(15) . ? C6 H6 0.9300 . ? C7 C8 1.365(17) . ? C7 H7 0.9300 . ? C8 C9 1.375(17) . ? C8 H8 0.9300 . ? C9 C10 1.365(15) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.360(12) . ? C12 C13 1.382(12) . ? C13 C14 1.375(13) . ? C13 H13 0.9300 . ? C14 C15 1.377(14) . ? C14 H14 0.9300 . ? C15 C16 1.360(14) . ? C15 H15 0.9300 . ? C16 C17 1.373(13) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? 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 C5 Se1 C4 103.5(4) . . ? C12 Se2 C11 98.6(4) . . ? C2 C1 C3 124.1(8) . 3_655 ? C2 C1 H1 117.9 . . ? C3 C1 H1 117.9 3_655 . ? C1 C2 C3 117.9(8) . . ? C1 C2 C11 119.3(9) . . ? C3 C2 C11 122.8(9) . . ? C1 C3 C2 117.9(8) 3_655 . ? C1 C3 C4 119.7(8) 3_655 . ? C2 C3 C4 122.4(8) . . ? C3 C4 Se1 104.2(6) . . ? C3 C4 H4A 110.9 . . ? Se1 C4 H4A 110.9 . . ? C3 C4 H4B 110.9 . . ? Se1 C4 H4B 110.9 . . ? H4A C4 H4B 108.9 . . ? C6 C5 C10 119.4(9) . . ? C6 C5 Se1 124.5(7) . . ? C10 C5 Se1 116.2(7) . . ? C5 C6 C7 119.8(11) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 121.1(12) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 118.8(11) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C10 C9 C8 121.2(11) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C5 119.6(11) . . ? C9 C10 H10 120.2 . . ? C5 C10 H10 120.2 . . ? C2 C11 Se2 112.1(7) . . ? C2 C11 H11A 109.2 . . ? Se2 C11 H11A 109.2 . . ? C2 C11 H11B 109.2 . . ? Se2 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C17 C12 C13 121.4(8) . . ? C17 C12 Se2 121.7(7) . . ? C13 C12 Se2 117.0(7) . . ? C14 C13 C12 118.4(9) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 120.5(9) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 119.8(9) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.6(9) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C12 C17 C16 119.3(9) . . ? C12 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? 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 C3 C1 C2 C3 1.7(15) 3_655 . . . ? C3 C1 C2 C11 -176.7(9) 3_655 . . . ? C1 C2 C3 C1 -1.6(14) . . . 3_655 ? C11 C2 C3 C1 176.8(8) . . . 3_655 ? C1 C2 C3 C4 177.1(8) . . . . ? C11 C2 C3 C4 -4.5(14) . . . . ? C1 C3 C4 Se1 90.0(9) 3_655 . . . ? C2 C3 C4 Se1 -88.7(9) . . . . ? C5 Se1 C4 C3 173.0(6) . . . . ? C4 Se1 C5 C6 14.1(10) . . . . ? C4 Se1 C5 C10 -165.7(7) . . . . ? C10 C5 C6 C7 -1.6(16) . . . . ? Se1 C5 C6 C7 178.7(8) . . . . ? C5 C6 C7 C8 1.1(17) . . . . ? C6 C7 C8 C9 0.1(18) . . . . ? C7 C8 C9 C10 -0.7(18) . . . . ? C8 C9 C10 C5 0.1(17) . . . . ? C6 C5 C10 C9 1.0(15) . . . . ? Se1 C5 C10 C9 -179.2(8) . . . . ? C1 C2 C11 Se2 -80.0(10) . . . . ? C3 C2 C11 Se2 101.7(9) . . . . ? C12 Se2 C11 C2 148.3(7) . . . . ? C11 Se2 C12 C17 33.5(8) . . . . ? C11 Se2 C12 C13 -147.0(7) . . . . ? C17 C12 C13 C14 -2.2(14) . . . . ? Se2 C12 C13 C14 178.4(7) . . . . ? C12 C13 C14 C15 -0.1(14) . . . . ? C13 C14 C15 C16 2.0(15) . . . . ? C14 C15 C16 C17 -1.8(15) . . . . ? C13 C12 C17 C16 2.4(14) . . . . ? Se2 C12 C17 C16 -178.2(7) . . . . ? C15 C16 C17 C12 -0.4(15) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.891 _refine_diff_density_min -0.861 _refine_diff_density_rms 0.130 # Attachment '- CCDC-763939.cif' data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 763939' #TrackingRef '- CCDC-763939.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H38 N2 Pd2 Se4, 2(B F4)' _chemical_formula_sum 'C44 H38 B2 F8 N2 Pd2 Se4' _chemical_formula_weight 1297.02 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 'C 2/c' _symmetry_space_group_name_hall '-C 2yc' 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 22.765(4) _cell_length_b 10.926(2) _cell_length_c 18.967(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.809(3) _cell_angle_gamma 90.00 _cell_volume 4600.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 5366 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.73 _exptl_crystal_description blocks _exptl_crystal_colour red _exptl_crystal_size_max 0.524 _exptl_crystal_size_mid 0.342 _exptl_crystal_size_min 0.178 _exptl_crystal_density_meas 1.873 _exptl_crystal_density_diffrn 1.873 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504.0 _exptl_absorpt_coefficient_mu 4.013 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.207 _exptl_absorpt_correction_T_max 0.493 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 21093 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4042 _reflns_number_gt 3242 _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. Distance of peak from nearest atom is 1.220. Distance restraint DFIX was applied to fix bond length B1-F2. ; _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^)+(0.0874P)^2^+10.5408P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4042 _refine_ls_number_parameters 280 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1397 _refine_ls_wR_factor_gt 0.1323 _refine_ls_goodness_of_fit_ref 1.250 _refine_ls_restrained_S_all 1.254 _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 0.28496(2) 0.37251(4) 0.17033(3) 0.0460(2) Uani 1 1 d . . . Se1 Se 0.20984(3) 0.52474(6) 0.12382(4) 0.0519(2) Uani 1 1 d . . . Se2 Se 0.35635(3) 0.20858(7) 0.20024(4) 0.0557(3) Uani 1 1 d . . . C1 C 0.0919(4) 0.4213(10) 0.0625(5) 0.081(3) Uani 1 1 d . . . H1 H 0.0982 0.4458 0.0178 0.097 Uiso 1 1 calc R . . C2 C 0.0385(5) 0.3668(12) 0.0685(7) 0.102(4) Uani 1 1 d . . . H2 H 0.0091 0.3505 0.0271 0.122 Uiso 1 1 calc R . . C3 C 0.0284(5) 0.3358(11) 0.1365(7) 0.098(3) Uani 1 1 d . . . H3 H -0.0082 0.3014 0.1402 0.117 Uiso 1 1 calc R . . C4 C 0.0708(5) 0.3554(10) 0.1956(6) 0.083(3) Uani 1 1 d . . . H4 H 0.0637 0.3348 0.2405 0.100 Uiso 1 1 calc R . . C5 C 0.1255(4) 0.4059(8) 0.1912(4) 0.065(2) Uani 1 1 d . . . H5 H 0.1553 0.4179 0.2329 0.078 Uiso 1 1 calc R . . C6 C 0.1354(3) 0.4384(6) 0.1244(4) 0.0502(16) Uani 1 1 d . . . C7 C 0.2157(4) 0.5003(6) 0.0237(4) 0.0525(17) Uani 1 1 d . . . H7A H 0.1774 0.5202 -0.0083 0.063 Uiso 1 1 calc R . . H7B H 0.2460 0.5548 0.0126 0.063 Uiso 1 1 calc R . . C8 C 0.2320(3) 0.3697(6) 0.0114(4) 0.0442(15) Uani 1 1 d . . . C9 C 0.2651(3) 0.3009(5) 0.0704(4) 0.0429(14) Uani 1 1 d . . . C10 C 0.2828(3) 0.1804(6) 0.0574(4) 0.0446(15) Uani 1 1 d . . . C11 C 0.3155(3) 0.1049(6) 0.1204(4) 0.0551(18) Uani 1 1 d . . . H11A H 0.3449 0.0532 0.1048 0.066 Uiso 1 1 calc R . . H11B H 0.2870 0.0522 0.1369 0.066 Uiso 1 1 calc R . . C12 C 0.4242(3) 0.2581(8) 0.1612(4) 0.0594(19) Uani 1 1 d . . . C13 C 0.4654(4) 0.1693(9) 0.1555(5) 0.075(2) Uani 1 1 d . . . H13 H 0.4596 0.0884 0.1676 0.090 Uiso 1 1 calc R . . C14 C 0.5163(5) 0.2043(13) 0.1310(7) 0.097(3) Uani 1 1 d . . . H14 H 0.5458 0.1466 0.1281 0.117 Uiso 1 1 calc R . . C15 C 0.5231(5) 0.3197(14) 0.1117(9) 0.122(5) Uani 1 1 d . . . H15 H 0.5566 0.3406 0.0937 0.146 Uiso 1 1 calc R . . C16 C 0.4821(6) 0.4078(12) 0.1178(10) 0.139(6) Uani 1 1 d . . . H16 H 0.4879 0.4882 0.1047 0.167 Uiso 1 1 calc R . . C17 C 0.4321(4) 0.3765(8) 0.1435(7) 0.091(3) Uani 1 1 d . . . H17 H 0.4041 0.4358 0.1486 0.109 Uiso 1 1 calc R . . C18 C 0.3336(4) 0.5499(8) 0.2960(5) 0.067(2) Uani 1 1 d . . . H18 H 0.3404 0.6007 0.2592 0.081 Uiso 1 1 calc R . . C19 C 0.3517(4) 0.5890(9) 0.3677(6) 0.080(3) Uani 1 1 d . . . H19 H 0.3693 0.6656 0.3787 0.096 Uiso 1 1 calc R . . C20 C 0.3432(4) 0.5133(11) 0.4204(5) 0.084(3) Uani 1 1 d . . . H20 H 0.3564 0.5361 0.4685 0.100 Uiso 1 1 calc R . . C21 C 0.3153(4) 0.4037(9) 0.4037(5) 0.072(2) Uani 1 1 d . . . H21 H 0.3082 0.3516 0.4397 0.086 Uiso 1 1 calc R . . C22 C 0.2981(4) 0.3728(7) 0.3325(4) 0.0588(19) Uani 1 1 d . . . H22 H 0.2789 0.2980 0.3209 0.071 Uiso 1 1 calc R . . N1 N 0.3070(3) 0.4428(5) 0.2787(3) 0.0520(14) Uani 1 1 d . . . B1 B 0.1396(5) 0.7655(10) 0.8929(7) 0.074(3) Uani 1 1 d D . . F1 F 0.1241(5) 0.6547(7) 0.8776(7) 0.212(6) Uani 1 1 d . . . F2 F 0.1959(6) 0.7689(16) 0.9153(18) 0.426(19) Uani 1 1 d D . . F3 F 0.1227(9) 0.774(2) 0.9507(7) 0.351(12) Uani 1 1 d . . . F4 F 0.1040(8) 0.8357(9) 0.8523(8) 0.252(7) 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 Pd1 0.0491(3) 0.0371(3) 0.0534(4) 0.0003(2) 0.0151(2) 0.0026(2) Se1 0.0572(5) 0.0367(4) 0.0630(5) -0.0057(3) 0.0160(3) 0.0073(3) Se2 0.0633(5) 0.0466(4) 0.0548(5) 0.0044(3) 0.0080(4) 0.0107(3) C1 0.069(6) 0.110(8) 0.062(5) 0.008(5) 0.011(4) 0.009(5) C2 0.057(6) 0.133(10) 0.101(8) -0.001(7) -0.012(5) 0.011(6) C3 0.061(6) 0.115(9) 0.121(9) 0.012(7) 0.030(6) -0.006(6) C4 0.079(6) 0.101(7) 0.079(6) 0.010(5) 0.034(5) 0.006(6) C5 0.060(5) 0.077(5) 0.058(5) -0.009(4) 0.011(4) 0.001(4) C6 0.050(4) 0.043(4) 0.059(4) -0.007(3) 0.014(3) 0.008(3) C7 0.068(5) 0.034(3) 0.059(4) 0.008(3) 0.022(4) 0.009(3) C8 0.043(4) 0.035(3) 0.059(4) 0.004(3) 0.020(3) 0.003(3) C9 0.047(4) 0.032(3) 0.053(4) -0.001(3) 0.016(3) 0.002(3) C10 0.044(4) 0.038(3) 0.053(4) 0.009(3) 0.014(3) 0.004(3) C11 0.053(4) 0.039(4) 0.068(5) 0.002(3) 0.004(3) 0.001(3) C12 0.043(4) 0.065(5) 0.065(5) -0.005(4) 0.002(3) 0.007(4) C13 0.063(5) 0.077(6) 0.083(6) 0.001(5) 0.011(4) 0.026(5) C14 0.055(6) 0.121(10) 0.112(8) -0.016(7) 0.010(5) 0.020(6) C15 0.062(7) 0.131(12) 0.180(14) -0.016(11) 0.045(7) -0.014(7) C16 0.097(9) 0.080(8) 0.26(2) -0.006(10) 0.077(11) -0.014(7) C17 0.065(6) 0.057(6) 0.154(10) 0.007(6) 0.033(6) -0.001(4) C18 0.087(6) 0.057(5) 0.062(5) -0.002(4) 0.026(4) -0.009(4) C19 0.080(6) 0.070(6) 0.091(7) -0.028(5) 0.019(5) -0.012(5) C20 0.076(6) 0.111(9) 0.064(6) -0.012(6) 0.018(5) 0.020(6) C21 0.079(6) 0.078(6) 0.067(5) 0.010(4) 0.034(5) 0.017(5) C22 0.073(5) 0.045(4) 0.060(5) 0.003(3) 0.019(4) 0.004(4) N1 0.057(3) 0.047(3) 0.054(3) -0.003(3) 0.015(3) 0.000(3) B1 0.084(7) 0.050(6) 0.088(7) -0.002(5) 0.018(6) 0.003(5) F1 0.217(10) 0.073(5) 0.279(13) -0.001(6) -0.093(9) 0.034(6) F2 0.137(10) 0.244(15) 0.95(6) -0.06(2) 0.23(2) -0.047(10) F3 0.34(2) 0.58(4) 0.129(9) -0.112(16) 0.053(12) 0.01(2) F4 0.371(19) 0.116(7) 0.301(16) 0.101(9) 0.140(14) 0.110(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 C9 2.008(7) . ? Pd1 N1 2.147(6) . ? Pd1 Se2 2.4004(9) . ? Pd1 Se1 2.4083(9) . ? Se1 C6 1.941(7) . ? Se1 C7 1.950(7) . ? Se2 C12 1.933(8) . ? Se2 C11 1.954(7) . ? C1 C6 1.370(11) . ? C1 C2 1.382(15) . ? C1 H1 0.9300 . ? C2 C3 1.402(16) . ? C2 H2 0.9300 . ? C3 C4 1.324(15) . ? C3 H3 0.9300 . ? C4 C5 1.379(13) . ? C4 H4 0.9300 . ? C5 C6 1.382(11) . ? C5 H5 0.9300 . ? C7 C8 1.507(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C10 1.387(10) 7 ? C8 C9 1.417(9) . ? C9 C10 1.414(9) . ? C10 C8 1.387(10) 7 ? C10 C11 1.506(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.359(12) . ? C12 C13 1.370(11) . ? C13 C14 1.395(15) . ? C13 H13 0.9300 . ? C14 C15 1.331(17) . ? C14 H14 0.9300 . ? C15 C16 1.364(18) . ? C15 H15 0.9300 . ? C16 C17 1.376(15) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 N1 1.325(10) . ? C18 C19 1.398(13) . ? C18 H18 0.9300 . ? C19 C20 1.344(14) . ? C19 H19 0.9300 . ? C20 C21 1.359(14) . ? C20 H20 0.9300 . ? C21 C22 1.363(12) . ? C21 H21 0.9300 . ? C22 N1 1.327(9) . ? C22 H22 0.9300 . ? B1 F3 1.243(17) . ? B1 F4 1.250(15) . ? B1 F2 1.258(19) . ? B1 F1 1.276(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 C9 Pd1 N1 178.0(2) . . ? C9 Pd1 Se2 86.07(18) . . ? N1 Pd1 Se2 92.19(16) . . ? C9 Pd1 Se1 85.99(18) . . ? N1 Pd1 Se1 95.74(16) . . ? Se2 Pd1 Se1 172.06(3) . . ? C6 Se1 C7 100.8(3) . . ? C6 Se1 Pd1 102.2(2) . . ? C7 Se1 Pd1 93.8(2) . . ? C12 Se2 C11 98.6(3) . . ? C12 Se2 Pd1 104.9(2) . . ? C11 Se2 Pd1 94.0(2) . . ? C6 C1 C2 118.0(9) . . ? C6 C1 H1 121.0 . . ? C2 C1 H1 121.0 . . ? C1 C2 C3 120.5(10) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 120.1(10) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.8(10) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 119.4(8) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C1 C6 C5 121.1(7) . . ? C1 C6 Se1 121.8(6) . . ? C5 C6 Se1 116.8(6) . . ? C8 C7 Se1 110.7(5) . . ? C8 C7 H7A 109.5 . . ? Se1 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? Se1 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C10 C8 C9 120.6(6) 7 . ? C10 C8 C7 120.2(6) 7 . ? C9 C8 C7 119.1(6) . . ? C10 C9 C8 118.6(6) . . ? C10 C9 Pd1 120.9(5) . . ? C8 C9 Pd1 120.5(4) . . ? C8 C10 C9 120.8(6) 7 . ? C8 C10 C11 120.3(6) 7 . ? C9 C10 C11 118.9(6) . . ? C10 C11 Se2 111.3(5) . . ? C10 C11 H11A 109.4 . . ? Se2 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? Se2 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C17 C12 C13 121.6(9) . . ? C17 C12 Se2 121.5(6) . . ? C13 C12 Se2 116.8(7) . . ? C12 C13 C14 117.8(10) . . ? C12 C13 H13 121.1 . . ? C14 C13 H13 121.1 . . ? C15 C14 C13 120.5(10) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 121.5(12) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 C17 119.3(12) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C12 C17 C16 119.3(10) . . ? C12 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? N1 C18 C19 122.1(8) . . ? N1 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? C20 C19 C18 118.4(9) . . ? C20 C19 H19 120.8 . . ? C18 C19 H19 120.8 . . ? C19 C20 C21 120.4(9) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C22 117.7(8) . . ? C20 C21 H21 121.1 . . ? C22 C21 H21 121.1 . . ? N1 C22 C21 124.1(8) . . ? N1 C22 H22 118.0 . . ? C21 C22 H22 118.0 . . ? C18 N1 C22 117.3(7) . . ? C18 N1 Pd1 123.4(5) . . ? C22 N1 Pd1 119.1(5) . . ? F3 B1 F4 102.3(14) . . ? F3 B1 F2 101.1(19) . . ? F4 B1 F2 131.5(16) . . ? F3 B1 F1 98.4(16) . . ? F4 B1 F1 109.5(12) . . ? F2 B1 F1 108.3(12) . . ? 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 C9 Pd1 Se1 C6 79.2(3) . . . . ? N1 Pd1 Se1 C6 -99.8(3) . . . . ? C9 Pd1 Se1 C7 -22.7(3) . . . . ? N1 Pd1 Se1 C7 158.3(3) . . . . ? C9 Pd1 Se2 C12 77.9(3) . . . . ? N1 Pd1 Se2 C12 -103.1(3) . . . . ? C9 Pd1 Se2 C11 -22.1(3) . . . . ? N1 Pd1 Se2 C11 156.9(3) . . . . ? C6 C1 C2 C3 3.2(17) . . . . ? C1 C2 C3 C4 -2.0(19) . . . . ? C2 C3 C4 C5 -0.2(18) . . . . ? C3 C4 C5 C6 1.2(15) . . . . ? C2 C1 C6 C5 -2.2(14) . . . . ? C2 C1 C6 Se1 -175.4(8) . . . . ? C4 C5 C6 C1 0.1(13) . . . . ? C4 C5 C6 Se1 173.6(7) . . . . ? C7 Se1 C6 C1 -24.7(7) . . . . ? Pd1 Se1 C6 C1 -121.0(7) . . . . ? C7 Se1 C6 C5 161.9(6) . . . . ? Pd1 Se1 C6 C5 65.5(6) . . . . ? C6 Se1 C7 C8 -72.3(5) . . . . ? Pd1 Se1 C7 C8 30.9(5) . . . . ? Se1 C7 C8 C10 155.9(5) . . . 7 ? Se1 C7 C8 C9 -26.9(8) . . . . ? C10 C8 C9 C10 0.3(10) 7 . . . ? C7 C8 C9 C10 -176.9(6) . . . . ? C10 C8 C9 Pd1 -178.7(5) 7 . . . ? C7 C8 C9 Pd1 4.1(8) . . . . ? Se2 Pd1 C9 C10 16.1(5) . . . . ? Se1 Pd1 C9 C10 -163.8(5) . . . . ? Se2 Pd1 C9 C8 -164.9(5) . . . . ? Se1 Pd1 C9 C8 15.2(5) . . . . ? C8 C9 C10 C8 -0.3(10) . . . 7 ? Pd1 C9 C10 C8 178.7(5) . . . 7 ? C8 C9 C10 C11 -177.4(6) . . . . ? Pd1 C9 C10 C11 1.6(8) . . . . ? C8 C10 C11 Se2 158.9(5) 7 . . . ? C9 C10 C11 Se2 -24.1(8) . . . . ? C12 Se2 C11 C10 -76.6(6) . . . . ? Pd1 Se2 C11 C10 29.2(5) . . . . ? C11 Se2 C12 C17 114.4(8) . . . . ? Pd1 Se2 C12 C17 18.0(8) . . . . ? C11 Se2 C12 C13 -68.5(7) . . . . ? Pd1 Se2 C12 C13 -165.0(6) . . . . ? C17 C12 C13 C14 0.3(14) . . . . ? Se2 C12 C13 C14 -176.8(7) . . . . ? C12 C13 C14 C15 -2.2(17) . . . . ? C13 C14 C15 C16 3(2) . . . . ? C14 C15 C16 C17 -1(3) . . . . ? C13 C12 C17 C16 1.2(18) . . . . ? Se2 C12 C17 C16 178.2(11) . . . . ? C15 C16 C17 C12 -1(2) . . . . ? N1 C18 C19 C20 1.9(14) . . . . ? C18 C19 C20 C21 -2.7(15) . . . . ? C19 C20 C21 C22 1.7(14) . . . . ? C20 C21 C22 N1 0.2(13) . . . . ? C19 C18 N1 C22 0.0(12) . . . . ? C19 C18 N1 Pd1 -174.8(7) . . . . ? C21 C22 N1 C18 -1.0(12) . . . . ? C21 C22 N1 Pd1 174.0(6) . . . . ? Se2 Pd1 N1 C18 113.4(6) . . . . ? Se1 Pd1 N1 C18 -66.9(6) . . . . ? Se2 Pd1 N1 C22 -61.3(6) . . . . ? Se1 Pd1 N1 C22 118.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.220 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.119 data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 765901' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H40 Pd2 Se4, 2(Cl O4)' _chemical_formula_sum 'C40 H40 Cl2 O8 Pd2 Se4' _chemical_formula_weight 1248.26 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' 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' Cl Cl 0.1484 0.1585 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.026(5) _cell_length_b 14.321(6) _cell_length_c 15.336(7) _cell_angle_alpha 91.562(7) _cell_angle_beta 104.662(5) _cell_angle_gamma 96.774(7) _cell_volume 2322.3(18) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 7890 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.05 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.203 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.065 _exptl_crystal_density_meas 1.785 _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212.0 _exptl_absorpt_coefficient_mu 4.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.482 _exptl_absorpt_correction_T_max 0.771 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 21172 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0786 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8180 _reflns_number_gt 4747 _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^)+(0.0829P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8180 _refine_ls_number_parameters 494 _refine_ls_number_restraints 118 _refine_ls_R_factor_all 0.1073 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1600 _refine_ls_wR_factor_gt 0.1410 _refine_ls_goodness_of_fit_ref 1.294 _refine_ls_restrained_S_all 1.141 _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 0.39895(7) 0.90304(6) 0.71130(5) 0.0670(3) Uani 1 1 d . . . Pd2 Pd 0.12675(7) 0.59212(6) 0.24771(5) 0.0684(3) Uani 1 1 d . . . Se1 Se 0.33951(12) 1.05916(8) 0.73833(9) 0.0878(4) Uani 1 1 d . . . Se2 Se 0.62567(9) 0.91425(7) 0.78342(7) 0.0662(3) Uani 1 1 d . . . Se3 Se -0.00332(10) 0.69219(8) 0.30765(8) 0.0747(3) Uani 1 1 d . . . Se4 Se 0.29059(9) 0.54366(8) 0.37336(6) 0.0642(3) Uani 1 1 d . . . C1 C 0.3915(14) 0.7681(9) 0.6448(8) 0.101(4) Uani 1 1 d . . . H1A H 0.4329 0.8097 0.6131 0.121 Uiso 1 1 calc R . . H1B H 0.4295 0.7172 0.6703 0.121 Uiso 1 1 calc R . . C2 C 0.2736(13) 0.7819(11) 0.6542(9) 0.101(4) Uani 1 1 d . . . H2 H 0.2350 0.7419 0.6934 0.121 Uiso 1 1 calc R . . C3 C 0.2166(12) 0.8550(9) 0.6181(8) 0.093(4) Uani 1 1 d . . . H3A H 0.1423 0.8678 0.6370 0.112 Uiso 1 1 calc R . . H3B H 0.2098 0.8629 0.5545 0.112 Uiso 1 1 calc R . . C4 C 0.1929(10) 1.0265(9) 0.7968(9) 0.139(6) Uani 1 1 d GU . . C5 C 0.1778(9) 0.9429(7) 0.8374(8) 0.114(5) Uani 1 1 d GU . . H5 H 0.2299 0.8972 0.8338 0.137 Uiso 1 1 calc R . . C6 C 0.0856(11) 0.9271(9) 0.8832(9) 0.152(6) Uani 1 1 d GU . . H6 H 0.0754 0.8706 0.9106 0.182 Uiso 1 1 calc R . . C7 C 0.0085(11) 0.9947(12) 0.8884(11) 0.211(10) Uani 1 1 d GU . . H7 H -0.0538 0.9840 0.9193 0.253 Uiso 1 1 calc R . . C8 C 0.0236(12) 1.0783(12) 0.8478(12) 0.219(9) Uani 1 1 d GU . . H8 H -0.0285 1.1241 0.8513 0.263 Uiso 1 1 calc R . . C9 C 0.1158(13) 1.0942(10) 0.8020(11) 0.202(8) Uani 1 1 d GU . . H9 H 0.1259 1.1507 0.7746 0.243 Uiso 1 1 calc R . . C10 C 0.4461(10) 1.1220(7) 0.8498(6) 0.067(3) Uani 1 1 d . . . H10A H 0.5244 1.1507 0.8383 0.080 Uiso 1 1 calc R . . H10B H 0.4040 1.1723 0.8676 0.080 Uiso 1 1 calc R . . C11 C 0.4777(8) 1.0586(6) 0.9276(6) 0.054(2) Uani 1 1 d . . . C12 C 0.5800(8) 1.0075(6) 0.9413(6) 0.051(2) Uani 1 1 d . . . C13 C 0.5995(8) 0.9522(6) 1.0142(6) 0.057(2) Uani 1 1 d . . . H13 H 0.6697 0.9198 1.0251 0.068 Uiso 1 1 calc R . . C14 C 0.6719(8) 1.0129(6) 0.8830(7) 0.060(2) Uani 1 1 d . . . H14A H 0.7556 1.0069 0.9204 0.072 Uiso 1 1 calc R . . H14B H 0.6754 1.0743 0.8578 0.072 Uiso 1 1 calc R . . C15 C 0.6413(9) 0.8083(7) 0.8575(6) 0.059(2) Uani 1 1 d . . . C16 C 0.5437(9) 0.7641(7) 0.8893(7) 0.065(3) Uani 1 1 d . . . H16 H 0.4644 0.7845 0.8728 0.078 Uiso 1 1 calc R . . C17 C 0.5617(12) 0.6925(8) 0.9434(8) 0.085(3) Uani 1 1 d . . . H17 H 0.4946 0.6624 0.9629 0.102 Uiso 1 1 calc R . . C18 C 0.6767(13) 0.6638(9) 0.9697(9) 0.096(4) Uani 1 1 d . . . H18 H 0.6894 0.6159 1.0095 0.116 Uiso 1 1 calc R . . C19 C 0.7748(12) 0.7044(11) 0.9387(10) 0.108(4) Uani 1 1 d . . . H19 H 0.8537 0.6837 0.9570 0.130 Uiso 1 1 calc R . . C20 C 0.7577(10) 0.7759(9) 0.8804(8) 0.082(3) Uani 1 1 d . . . H20 H 0.8232 0.8019 0.8569 0.098 Uiso 1 1 calc R . . C21 C 0.0355(15) 0.6172(14) 0.1131(8) 0.117(5) Uani 1 1 d . . . H21A H 0.0826 0.6740 0.1389 0.141 Uiso 1 1 calc R . . H21B H -0.0508 0.6146 0.0869 0.141 Uiso 1 1 calc R . . C22 C 0.094(2) 0.5368(17) 0.1138(9) 0.146(7) Uani 1 1 d . . . H22 H 0.0413 0.4758 0.0957 0.175 Uiso 1 1 calc R . . C23 C 0.2163(13) 0.5385(13) 0.1506(8) 0.123(6) Uani 1 1 d . . . H23A H 0.2650 0.5945 0.1767 0.148 Uiso 1 1 calc R . . H23B H 0.2537 0.4836 0.1504 0.148 Uiso 1 1 calc R . . C24 C 0.2486(11) 0.4106(8) 0.3705(8) 0.076(3) Uani 1 1 d U . . C25 C 0.1355(12) 0.3645(10) 0.3184(9) 0.091(3) Uani 1 1 d U . . H25 H 0.0754 0.3976 0.2831 0.109 Uiso 1 1 calc R . . C26 C 0.1143(18) 0.2680(12) 0.3202(12) 0.123(5) Uani 1 1 d U . . H26 H 0.0396 0.2365 0.2832 0.147 Uiso 1 1 calc R . . C27 C 0.192(2) 0.2191(12) 0.3699(13) 0.124(5) Uani 1 1 d U . . H27 H 0.1719 0.1540 0.3667 0.148 Uiso 1 1 calc R . . C28 C 0.302(2) 0.2592(15) 0.4271(14) 0.144(6) Uani 1 1 d U . . H28 H 0.3539 0.2234 0.4660 0.172 Uiso 1 1 calc R . . C29 C 0.3355(13) 0.3618(10) 0.4254(10) 0.100(4) Uani 1 1 d U . . H29 H 0.4124 0.3923 0.4600 0.120 Uiso 1 1 calc R . . C30 C 0.2528(9) 0.5742(8) 0.4895(6) 0.067(3) Uani 1 1 d . . . H30A H 0.3117 0.5475 0.5375 0.080 Uiso 1 1 calc R . . H30B H 0.2665 0.6420 0.5010 0.080 Uiso 1 1 calc R . . C31 C 0.1204(9) 0.5384(6) 0.4926(6) 0.054(2) Uani 1 1 d . . . C32 C 0.0198(10) 0.5904(7) 0.4722(6) 0.061(2) Uani 1 1 d . . . C33 C -0.0957(8) 0.5516(6) 0.4796(5) 0.050(2) Uani 1 1 d . . . H33 H -0.1622 0.5877 0.4650 0.060 Uiso 1 1 calc R . . C34 C 0.0358(11) 0.6890(7) 0.4409(7) 0.073(3) Uani 1 1 d . . . H34A H 0.1222 0.7176 0.4667 0.087 Uiso 1 1 calc R . . H34B H -0.0194 0.7263 0.4631 0.087 Uiso 1 1 calc R . . C35 C -0.1733(10) 0.6221(9) 0.2780(8) 0.080(3) Uani 1 1 d . . . C36 C -0.1976(12) 0.5304(10) 0.2471(8) 0.095(4) Uani 1 1 d . . . H36 H -0.1325 0.4985 0.2383 0.114 Uiso 1 1 calc R . . C37 C -0.3184(13) 0.4850(12) 0.2290(10) 0.116(5) Uani 1 1 d . . . H37 H -0.3359 0.4226 0.2064 0.139 Uiso 1 1 calc R . . C38 C -0.4104(17) 0.5298(19) 0.2437(13) 0.150(7) Uani 1 1 d . . . H38 H -0.4918 0.4979 0.2317 0.180 Uiso 1 1 calc R . . C39 C -0.3889(14) 0.6220(16) 0.2761(14) 0.139(7) Uani 1 1 d . . . H39 H -0.4554 0.6509 0.2870 0.167 Uiso 1 1 calc R . . C40 C -0.2686(11) 0.6733(10) 0.2932(10) 0.108(4) Uani 1 1 d . . . H40 H -0.2525 0.7366 0.3131 0.130 Uiso 1 1 calc R . . Cl1 Cl 0.8081(3) 0.3126(4) 0.0754(3) 0.1250(14) Uani 1 1 d D . . Cl2 Cl 0.6411(4) 0.1739(3) 0.6483(3) 0.1116(11) Uani 1 1 d U . . O1 O 0.7838(11) 0.2858(9) 0.1562(7) 0.179(6) Uani 1 1 d D . . O2 O 0.7764(14) 0.4003(8) 0.0551(9) 0.198(7) Uani 1 1 d D . . O3 O 0.9353(8) 0.3132(10) 0.0829(9) 0.198(7) Uani 1 1 d D . . O4 O 0.7374(11) 0.2527(9) 0.0050(8) 0.198(6) Uani 1 1 d D . . O5 O 0.683(2) 0.2140(13) 0.7361(10) 0.261(10) Uani 1 1 d . . . O6 O 0.5849(16) 0.0874(10) 0.6480(11) 0.213(7) Uani 1 1 d . . . O7 O 0.7168(19) 0.1978(17) 0.5996(11) 0.281(12) Uani 1 1 d . . . O8 O 0.562(3) 0.223(2) 0.593(2) 0.42(2) Uani 1 1 d U . . 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 0.0695(5) 0.0712(6) 0.0572(5) 0.0023(4) 0.0134(4) 0.0031(4) Pd2 0.0603(5) 0.0927(6) 0.0517(5) 0.0110(4) 0.0179(4) -0.0012(4) Se1 0.0856(8) 0.0691(7) 0.0955(9) 0.0200(6) -0.0035(6) 0.0131(6) Se2 0.0647(6) 0.0738(7) 0.0686(6) 0.0016(5) 0.0341(5) 0.0068(5) Se3 0.0706(7) 0.0738(7) 0.0836(8) 0.0282(6) 0.0241(6) 0.0103(5) Se4 0.0496(6) 0.0847(7) 0.0603(6) 0.0033(5) 0.0215(5) 0.0008(5) C1 0.117(11) 0.094(9) 0.083(8) -0.024(7) 0.019(8) -0.002(8) C2 0.085(9) 0.130(12) 0.075(8) -0.022(8) 0.010(7) -0.006(9) C3 0.089(9) 0.099(9) 0.066(7) -0.007(7) -0.016(6) -0.012(8) C4 0.080(9) 0.095(10) 0.238(16) 0.025(11) 0.018(10) 0.048(8) C5 0.063(8) 0.128(11) 0.155(12) -0.022(10) 0.040(8) 0.011(8) C6 0.083(10) 0.139(13) 0.238(17) 0.003(12) 0.064(11) -0.014(9) C7 0.095(13) 0.20(2) 0.37(3) 0.01(2) 0.118(16) 0.000(14) C8 0.122(14) 0.22(2) 0.35(3) 0.048(19) 0.103(15) 0.080(15) C9 0.127(13) 0.176(15) 0.31(2) 0.056(15) 0.047(14) 0.064(12) C10 0.077(7) 0.060(6) 0.074(7) 0.019(5) 0.034(5) 0.017(5) C11 0.053(5) 0.047(5) 0.064(6) 0.007(4) 0.021(5) 0.006(4) C12 0.052(5) 0.039(5) 0.059(6) -0.004(4) 0.012(4) -0.004(4) C13 0.054(5) 0.046(5) 0.078(7) -0.003(5) 0.027(5) 0.015(4) C14 0.051(5) 0.050(5) 0.087(7) 0.003(5) 0.036(5) -0.003(4) C15 0.057(6) 0.063(6) 0.061(6) -0.004(5) 0.019(5) 0.013(5) C16 0.051(6) 0.060(6) 0.089(7) 0.003(6) 0.025(5) 0.013(5) C17 0.081(8) 0.072(8) 0.105(9) 0.020(7) 0.023(7) 0.015(6) C18 0.100(10) 0.078(8) 0.114(10) 0.036(7) 0.021(8) 0.030(7) C19 0.069(8) 0.122(12) 0.141(12) 0.030(10) 0.031(8) 0.027(8) C20 0.070(7) 0.090(8) 0.099(8) 0.014(7) 0.042(6) 0.021(6) C21 0.113(11) 0.181(16) 0.053(7) 0.021(9) 0.007(7) 0.028(11) C22 0.18(2) 0.21(2) 0.055(8) -0.003(11) 0.052(11) 0.017(16) C23 0.062(8) 0.240(19) 0.061(7) -0.038(9) 0.017(6) 0.005(9) C24 0.067(7) 0.095(8) 0.080(7) 0.016(6) 0.041(6) 0.021(6) C25 0.085(8) 0.095(9) 0.103(9) 0.005(7) 0.050(7) -0.001(7) C26 0.151(13) 0.101(12) 0.134(12) 0.019(10) 0.066(10) 0.021(11) C27 0.175(17) 0.085(10) 0.140(14) 0.009(10) 0.085(13) 0.033(12) C28 0.138(13) 0.151(15) 0.167(14) 0.029(12) 0.061(11) 0.068(11) C29 0.095(9) 0.092(9) 0.126(10) 0.008(8) 0.044(8) 0.030(7) C30 0.063(6) 0.092(8) 0.044(5) -0.002(5) 0.016(4) -0.001(5) C31 0.064(6) 0.050(6) 0.047(5) -0.001(4) 0.019(4) 0.000(5) C32 0.073(7) 0.069(7) 0.046(5) -0.001(5) 0.021(5) 0.013(6) C33 0.050(5) 0.056(6) 0.051(5) 0.002(4) 0.024(4) 0.015(4) C34 0.085(7) 0.055(6) 0.089(8) 0.010(5) 0.039(6) 0.011(5) C35 0.056(6) 0.097(9) 0.090(8) 0.041(7) 0.015(6) 0.027(6) C36 0.076(9) 0.106(11) 0.094(9) 0.004(8) 0.007(7) 0.010(8) C37 0.058(8) 0.134(12) 0.138(12) -0.010(9) 0.005(8) -0.012(8) C38 0.080(12) 0.19(2) 0.168(17) 0.036(16) 0.016(11) 0.009(14) C39 0.063(10) 0.168(17) 0.210(19) 0.066(15) 0.054(10) 0.062(11) C40 0.064(8) 0.109(10) 0.160(13) 0.042(9) 0.030(8) 0.030(7) Cl1 0.083(2) 0.193(4) 0.101(3) 0.013(3) 0.042(2) -0.015(3) Cl2 0.121(3) 0.107(3) 0.116(3) 0.033(2) 0.056(2) -0.014(2) O1 0.151(10) 0.273(17) 0.146(10) 0.080(10) 0.087(8) 0.035(10) O2 0.299(19) 0.129(10) 0.220(15) 0.085(10) 0.136(14) 0.074(11) O3 0.078(7) 0.309(18) 0.215(14) 0.106(13) 0.046(8) 0.012(8) O4 0.159(12) 0.240(17) 0.157(11) -0.057(11) 0.003(9) -0.027(11) O5 0.38(3) 0.247(18) 0.127(11) 0.002(11) 0.090(13) -0.120(17) O6 0.271(17) 0.141(11) 0.226(15) 0.035(10) 0.102(13) -0.073(11) O7 0.249(19) 0.43(3) 0.155(13) 0.028(16) 0.115(14) -0.12(2) O8 0.43(4) 0.39(4) 0.39(4) 0.16(3) -0.04(3) 0.15(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 C2 2.103(13) . ? Pd1 C1 2.143(12) . ? Pd1 C3 2.173(11) . ? Pd1 Se2 2.4482(16) . ? Pd1 Se1 2.4561(17) . ? Pd2 C22 2.108(14) . ? Pd2 C21 2.115(12) . ? Pd2 C23 2.155(12) . ? Pd2 Se3 2.4567(15) . ? Pd2 Se4 2.4627(14) . ? Se1 C10 1.940(10) . ? Se1 C4 2.053(11) . ? Se2 C15 1.918(10) . ? Se2 C14 1.977(9) . ? Se3 C35 1.957(12) . ? Se3 C34 1.982(11) . ? Se4 C24 1.903(12) . ? Se4 C30 1.978(9) . ? C1 C2 1.379(18) . ? C1 H1A 0.9300 . ? C1 H1B 0.9300 . ? C2 C3 1.344(17) . ? C2 H2 0.9800 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C9 1.37607 . ? C4 C5 1.37654 . ? C5 C6 1.37619 . ? C5 H5 0.9300 . ? C6 C7 1.37496 . ? C6 H6 0.9300 . ? C7 C8 1.37654 . ? C7 H7 0.9300 . ? C8 C9 1.37632 . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.514(12) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C13 1.380(12) 2_677 ? C11 C12 1.391(12) . ? C12 C13 1.375(12) . ? C12 C14 1.508(12) . ? C13 C11 1.380(12) 2_677 ? C13 H13 0.9300 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.381(13) . ? C15 C16 1.385(13) . ? C16 C17 1.338(14) . ? C16 H16 0.9300 . ? C17 C18 1.346(15) . ? C17 H17 0.9300 . ? C18 C19 1.365(18) . ? C18 H18 0.9300 . ? C19 C20 1.375(17) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.38(2) . ? C21 H21A 0.9300 . ? C21 H21B 0.9300 . ? C22 C23 1.32(2) . ? C22 H22 0.9800 . ? C23 H23A 0.9300 . ? C23 H23B 0.9300 . ? C24 C29 1.377(16) . ? C24 C25 1.379(15) . ? C25 C26 1.376(19) . ? C25 H25 0.9300 . ? C26 C27 1.28(2) . ? C26 H26 0.9300 . ? C27 C28 1.36(2) . ? C27 H27 0.9300 . ? C28 C29 1.47(2) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.502(12) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.384(12) . ? C31 C33 1.388(12) 2_566 ? C32 C33 1.361(12) . ? C32 C34 1.509(14) . ? C33 C31 1.388(12) 2_566 ? C33 H33 0.9300 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.356(16) . ? C35 C40 1.412(16) . ? C36 C37 1.368(17) . ? C36 H36 0.9300 . ? C37 C38 1.32(2) . ? C37 H37 0.9300 . ? C38 C39 1.37(2) . ? C38 H38 0.9300 . ? C39 C40 1.40(2) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? Cl1 O2 1.368(9) . ? Cl1 O4 1.369(10) . ? Cl1 O3 1.377(9) . ? Cl1 O1 1.388(9) . ? Cl2 O7 1.279(13) . ? Cl2 O6 1.317(12) . ? Cl2 O8 1.34(2) . ? Cl2 O5 1.391(16) . ? 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 C2 Pd1 C1 37.9(5) . . ? C2 Pd1 C3 36.6(5) . . ? C1 Pd1 C3 66.7(5) . . ? C2 Pd1 Se2 128.0(5) . . ? C1 Pd1 Se2 93.7(4) . . ? C3 Pd1 Se2 159.4(4) . . ? C2 Pd1 Se1 125.9(4) . . ? C1 Pd1 Se1 158.4(4) . . ? C3 Pd1 Se1 92.9(4) . . ? Se2 Pd1 Se1 105.59(5) . . ? C22 Pd2 C21 38.2(6) . . ? C22 Pd2 C23 36.1(6) . . ? C21 Pd2 C23 67.0(6) . . ? C22 Pd2 Se3 127.3(7) . . ? C21 Pd2 Se3 91.7(5) . . ? C23 Pd2 Se3 157.1(5) . . ? C22 Pd2 Se4 122.7(7) . . ? C21 Pd2 Se4 157.9(5) . . ? C23 Pd2 Se4 91.1(4) . . ? Se3 Pd2 Se4 109.46(5) . . ? C10 Se1 C4 91.7(5) . . ? C10 Se1 Pd1 111.6(3) . . ? C4 Se1 Pd1 102.0(3) . . ? C15 Se2 C14 96.9(4) . . ? C15 Se2 Pd1 104.3(3) . . ? C14 Se2 Pd1 109.4(3) . . ? C35 Se3 C34 98.5(5) . . ? C35 Se3 Pd2 105.6(4) . . ? C34 Se3 Pd2 110.2(3) . . ? C24 Se4 C30 97.5(4) . . ? C24 Se4 Pd2 103.8(4) . . ? C30 Se4 Pd2 109.8(3) . . ? C2 C1 Pd1 69.5(8) . . ? C2 C1 H1A 120.0 . . ? Pd1 C1 H1A 75.9 . . ? C2 C1 H1B 120.0 . . ? Pd1 C1 H1B 126.4 . . ? H1A C1 H1B 120.0 . . ? C3 C2 C1 121.1(15) . . ? C3 C2 Pd1 74.5(8) . . ? C1 C2 Pd1 72.6(8) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? Pd1 C2 H2 119.3 . . ? C2 C3 Pd1 68.9(7) . . ? C2 C3 H3A 116.8 . . ? Pd1 C3 H3A 116.8 . . ? C2 C3 H3B 116.8 . . ? Pd1 C3 H3B 116.8 . . ? H3A C3 H3B 113.8 . . ? C9 C4 C5 120.0 . . ? C9 C4 Se1 118.2(7) . . ? C5 C4 Se1 121.6(7) . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 120.0 . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 120.0 . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C4 C9 C8 120.0 . . ? C4 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 Se1 114.7(6) . . ? C11 C10 H10A 108.6 . . ? Se1 C10 H10A 108.6 . . ? C11 C10 H10B 108.6 . . ? Se1 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? C13 C11 C12 118.1(8) 2_677 . ? C13 C11 C10 119.5(8) 2_677 . ? C12 C11 C10 122.4(8) . . ? C13 C12 C11 117.3(8) . . ? C13 C12 C14 119.1(8) . . ? C11 C12 C14 123.5(8) . . ? C12 C13 C11 124.6(8) . 2_677 ? C12 C13 H13 117.7 . . ? C11 C13 H13 117.7 2_677 . ? C12 C14 Se2 112.8(6) . . ? C12 C14 H14A 109.0 . . ? Se2 C14 H14A 109.0 . . ? C12 C14 H14B 109.0 . . ? Se2 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C20 C15 C16 119.1(10) . . ? C20 C15 Se2 117.1(8) . . ? C16 C15 Se2 123.8(7) . . ? C17 C16 C15 121.0(10) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 120.2(12) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C19 120.7(12) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C20 120.3(12) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C15 118.7(11) . . ? C19 C20 H20 120.7 . . ? C15 C20 H20 120.7 . . ? C22 C21 Pd2 70.6(8) . . ? C22 C21 H21A 120.0 . . ? Pd2 C21 H21A 73.5 . . ? C22 C21 H21B 120.0 . . ? Pd2 C21 H21B 128.0 . . ? H21A C21 H21B 120.0 . . ? C23 C22 C21 121(2) . . ? C23 C22 Pd2 73.9(9) . . ? C21 C22 Pd2 71.2(9) . . ? C23 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? Pd2 C22 H22 119.0 . . ? C22 C23 Pd2 70.0(8) . . ? C22 C23 H23A 120.0 . . ? Pd2 C23 H23A 73.0 . . ? C22 C23 H23B 120.0 . . ? Pd2 C23 H23B 129.3 . . ? H23A C23 H23B 120.0 . . ? C29 C24 C25 120.8(12) . . ? C29 C24 Se4 116.8(10) . . ? C25 C24 Se4 122.4(10) . . ? C26 C25 C24 118.1(14) . . ? C26 C25 H25 121.0 . . ? C24 C25 H25 121.0 . . ? C27 C26 C25 123.6(19) . . ? C27 C26 H26 118.2 . . ? C25 C26 H26 118.2 . . ? C26 C27 C28 122.2(18) . . ? C26 C27 H27 118.9 . . ? C28 C27 H27 118.9 . . ? C27 C28 C29 117.7(17) . . ? C27 C28 H28 121.2 . . ? C29 C28 H28 121.2 . . ? C24 C29 C28 117.4(14) . . ? C24 C29 H29 121.3 . . ? C28 C29 H29 121.3 . . ? C31 C30 Se4 114.0(6) . . ? C31 C30 H30A 108.8 . . ? Se4 C30 H30A 108.8 . . ? C31 C30 H30B 108.8 . . ? Se4 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? C32 C31 C33 116.5(8) . 2_566 ? C32 C31 C30 124.5(9) . . ? C33 C31 C30 118.9(9) 2_566 . ? C33 C32 C31 119.5(9) . . ? C33 C32 C34 119.5(9) . . ? C31 C32 C34 121.0(9) . . ? C32 C33 C31 124.0(8) . 2_566 ? C32 C33 H33 118.0 . . ? C31 C33 H33 118.0 2_566 . ? C32 C34 Se3 112.8(7) . . ? C32 C34 H34A 109.0 . . ? Se3 C34 H34A 109.0 . . ? C32 C34 H34B 109.0 . . ? Se3 C34 H34B 109.0 . . ? H34A C34 H34B 107.8 . . ? C36 C35 C40 122.3(11) . . ? C36 C35 Se3 122.6(9) . . ? C40 C35 Se3 115.0(10) . . ? C35 C36 C37 119.7(13) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C38 C37 C36 120.0(17) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 121.8(17) . . ? C37 C38 H38 119.1 . . ? C39 C38 H38 119.1 . . ? C38 C39 C40 121.0(15) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C39 C40 C35 115.1(14) . . ? C39 C40 H40 122.5 . . ? C35 C40 H40 122.5 . . ? O2 Cl1 O4 106.0(8) . . ? O2 Cl1 O3 108.8(8) . . ? O4 Cl1 O3 111.0(8) . . ? O2 Cl1 O1 111.8(8) . . ? O4 Cl1 O1 110.8(8) . . ? O3 Cl1 O1 108.4(7) . . ? O7 Cl2 O6 123.6(13) . . ? O7 Cl2 O8 84.8(18) . . ? O6 Cl2 O8 108.9(19) . . ? O7 Cl2 O5 113.0(11) . . ? O6 Cl2 O5 110.4(10) . . ? O8 Cl2 O5 113.4(18) . . ? 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 C2 Pd1 Se1 C10 143.0(6) . . . . ? C1 Pd1 Se1 C10 178.3(11) . . . . ? C3 Pd1 Se1 C10 159.9(5) . . . . ? Se2 Pd1 Se1 C10 -29.2(3) . . . . ? C2 Pd1 Se1 C4 46.2(6) . . . . ? C1 Pd1 Se1 C4 81.5(11) . . . . ? C3 Pd1 Se1 C4 63.2(5) . . . . ? Se2 Pd1 Se1 C4 -126.0(4) . . . . ? C2 Pd1 Se2 C15 -43.0(6) . . . . ? C1 Pd1 Se2 C15 -60.8(5) . . . . ? C3 Pd1 Se2 C15 -77.9(11) . . . . ? Se1 Pd1 Se2 C15 129.0(3) . . . . ? C2 Pd1 Se2 C14 -145.7(6) . . . . ? C1 Pd1 Se2 C14 -163.6(5) . . . . ? C3 Pd1 Se2 C14 179.4(11) . . . . ? Se1 Pd1 Se2 C14 26.2(3) . . . . ? C22 Pd2 Se3 C35 55.7(8) . . . . ? C21 Pd2 Se3 C35 70.8(6) . . . . ? C23 Pd2 Se3 C35 92.0(11) . . . . ? Se4 Pd2 Se3 C35 -115.8(3) . . . . ? C22 Pd2 Se3 C34 161.2(8) . . . . ? C21 Pd2 Se3 C34 176.3(6) . . . . ? C23 Pd2 Se3 C34 -162.6(11) . . . . ? Se4 Pd2 Se3 C34 -10.4(3) . . . . ? C22 Pd2 Se4 C24 -56.6(8) . . . . ? C21 Pd2 Se4 C24 -82.5(14) . . . . ? C23 Pd2 Se4 C24 -75.1(5) . . . . ? Se3 Pd2 Se4 C24 115.4(3) . . . . ? C22 Pd2 Se4 C30 -159.9(8) . . . . ? C21 Pd2 Se4 C30 174.1(14) . . . . ? C23 Pd2 Se4 C30 -178.4(6) . . . . ? Se3 Pd2 Se4 C30 12.1(3) . . . . ? C3 Pd1 C1 C2 -29.6(8) . . . . ? Se2 Pd1 C1 C2 156.9(8) . . . . ? Se1 Pd1 C1 C2 -49.6(16) . . . . ? Pd1 C1 C2 C3 59.0(11) . . . . ? C1 Pd1 C2 C3 -130.5(13) . . . . ? Se2 Pd1 C2 C3 -160.3(7) . . . . ? Se1 Pd1 C2 C3 29.3(10) . . . . ? C3 Pd1 C2 C1 130.5(13) . . . . ? Se2 Pd1 C2 C1 -29.8(10) . . . . ? Se1 Pd1 C2 C1 159.7(7) . . . . ? C1 C2 C3 Pd1 -58.0(10) . . . . ? C1 Pd1 C3 C2 30.6(9) . . . . ? Se2 Pd1 C3 C2 49.2(15) . . . . ? Se1 Pd1 C3 C2 -156.7(8) . . . . ? C10 Se1 C4 C9 82.7(6) . . . . ? Pd1 Se1 C4 C9 -164.8(6) . . . . ? C10 Se1 C4 C5 -91.4(8) . . . . ? Pd1 Se1 C4 C5 21.1(8) . . . . ? C9 C4 C5 C6 0.0 . . . . ? Se1 C4 C5 C6 174.0(9) . . . . ? C4 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C8 0.0 . . . . ? C6 C7 C8 C9 0.0 . . . . ? C5 C4 C9 C8 0.0 . . . . ? Se1 C4 C9 C8 -174.2(9) . . . . ? C7 C8 C9 C4 0.0 . . . . ? C4 Se1 C10 C11 63.4(7) . . . . ? Pd1 Se1 C10 C11 -40.2(7) . . . . ? Se1 C10 C11 C13 -90.9(9) . . . 2_677 ? Se1 C10 C11 C12 86.7(9) . . . . ? C13 C11 C12 C13 -2.3(13) 2_677 . . . ? C10 C11 C12 C13 -179.9(8) . . . . ? C13 C11 C12 C14 -179.8(8) 2_677 . . . ? C10 C11 C12 C14 2.6(13) . . . . ? C11 C12 C13 C11 2.5(14) . . . 2_677 ? C14 C12 C13 C11 -179.9(8) . . . 2_677 ? C13 C12 C14 Se2 88.9(9) . . . . ? C11 C12 C14 Se2 -93.6(9) . . . . ? C15 Se2 C14 C12 -63.0(7) . . . . ? Pd1 Se2 C14 C12 44.9(7) . . . . ? C14 Se2 C15 C20 -90.9(8) . . . . ? Pd1 Se2 C15 C20 157.0(7) . . . . ? C14 Se2 C15 C16 88.4(8) . . . . ? Pd1 Se2 C15 C16 -23.7(8) . . . . ? C20 C15 C16 C17 1.7(15) . . . . ? Se2 C15 C16 C17 -177.6(8) . . . . ? C15 C16 C17 C18 1.8(17) . . . . ? C16 C17 C18 C19 -3(2) . . . . ? C17 C18 C19 C20 1(2) . . . . ? C18 C19 C20 C15 3(2) . . . . ? C16 C15 C20 C19 -3.9(16) . . . . ? Se2 C15 C20 C19 175.4(10) . . . . ? C23 Pd2 C21 C22 28.4(12) . . . . ? Se3 Pd2 C21 C22 -160.4(12) . . . . ? Se4 Pd2 C21 C22 37(2) . . . . ? Pd2 C21 C22 C23 -56.6(12) . . . . ? C21 Pd2 C22 C23 132.0(19) . . . . ? Se3 Pd2 C22 C23 157.0(10) . . . . ? Se4 Pd2 C22 C23 -32.5(14) . . . . ? C23 Pd2 C22 C21 -132.0(19) . . . . ? Se3 Pd2 C22 C21 24.9(14) . . . . ? Se4 Pd2 C22 C21 -164.6(9) . . . . ? C21 C22 C23 Pd2 55.4(12) . . . . ? C21 Pd2 C23 C22 -29.9(12) . . . . ? Se3 Pd2 C23 C22 -53.0(18) . . . . ? Se4 Pd2 C23 C22 153.1(12) . . . . ? C30 Se4 C24 C29 -76.8(9) . . . . ? Pd2 Se4 C24 C29 170.7(8) . . . . ? C30 Se4 C24 C25 101.4(9) . . . . ? Pd2 Se4 C24 C25 -11.1(9) . . . . ? C29 C24 C25 C26 -2.5(17) . . . . ? Se4 C24 C25 C26 179.4(9) . . . . ? C24 C25 C26 C27 3(2) . . . . ? C25 C26 C27 C28 1(3) . . . . ? C26 C27 C28 C29 -5(3) . . . . ? C25 C24 C29 C28 -1.0(17) . . . . ? Se4 C24 C29 C28 177.2(10) . . . . ? C27 C28 C29 C24 5(2) . . . . ? C24 Se4 C30 C31 -56.4(8) . . . . ? Pd2 Se4 C30 C31 51.2(8) . . . . ? Se4 C30 C31 C32 -93.6(10) . . . . ? Se4 C30 C31 C33 88.6(9) . . . 2_566 ? C33 C31 C32 C33 -0.5(13) 2_566 . . . ? C30 C31 C32 C33 -178.3(8) . . . . ? C33 C31 C32 C34 -179.7(8) 2_566 . . . ? C30 C31 C32 C34 2.5(13) . . . . ? C31 C32 C33 C31 0.5(14) . . . 2_566 ? C34 C32 C33 C31 179.8(8) . . . 2_566 ? C33 C32 C34 Se3 -87.1(9) . . . . ? C31 C32 C34 Se3 92.1(10) . . . . ? C35 Se3 C34 C32 54.3(8) . . . . ? Pd2 Se3 C34 C32 -55.8(8) . . . . ? C34 Se3 C35 C36 -102.4(10) . . . . ? Pd2 Se3 C35 C36 11.4(10) . . . . ? C34 Se3 C35 C40 76.1(9) . . . . ? Pd2 Se3 C35 C40 -170.1(8) . . . . ? C40 C35 C36 C37 0.5(19) . . . . ? Se3 C35 C36 C37 178.9(10) . . . . ? C35 C36 C37 C38 -2(2) . . . . ? C36 C37 C38 C39 1(3) . . . . ? C37 C38 C39 C40 1(3) . . . . ? C38 C39 C40 C35 -2(2) . . . . ? C36 C35 C40 C39 1.5(19) . . . . ? Se3 C35 C40 C39 -177.1(11) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.196 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.119 # Attachment '- CCDC-770943.cif' data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 770943' #TrackingRef '- CCDC-770943.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H42 Cl2 Ru2 Se4, 2(F6 P)' _chemical_formula_sum 'C46 H42 Cl2 F12 P2 Ru2 Se4 ' _chemical_formula_weight 1473.62 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' F F 0.0171 0.0103 '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' Ru Ru -1.2594 0.8363 '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 Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_hall '-C 2yc ' 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 28.964(8) _cell_length_b 11.270(3) _cell_length_c 19.155(6) _cell_angle_alpha 90.00 _cell_angle_beta 115.273(5) _cell_angle_gamma 90.00 _cell_volume 5654(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 1285 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 28.32 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.524 _exptl_crystal_size_mid 0.324 _exptl_crystal_size_min 0.184 _exptl_crystal_density_meas 1.731 _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2856.0 _exptl_absorpt_coefficient_mu 3.330 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.282 _exptl_absorpt_correction_T_max 0.545 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 12769 _diffrn_reflns_av_R_equivalents 0.0850 _diffrn_reflns_av_sigmaI/netI 0.1150 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4996 _reflns_number_gt 2749 _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. ADP restraint SIMU was applied to C18, C19 and C23. Structure Contains Solvent Accessible VOIDS. SQUEEZE was not used. ; _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^)+(0.0858P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4996 _refine_ls_number_parameters 296 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1493 _refine_ls_R_factor_gt 0.0836 _refine_ls_wR_factor_ref 0.1923 _refine_ls_wR_factor_gt 0.1650 _refine_ls_goodness_of_fit_ref 1.326 _refine_ls_restrained_S_all 1.025 _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 Ru1 Ru 0.09003(4) 0.75175(9) 0.07807(5) 0.0571(3) Uani 1 1 d . . . Se1 Se 0.00185(4) 0.82980(12) 0.03890(6) 0.0528(4) Uani 1 1 d . . . Se2 Se 0.10960(4) 0.76757(11) 0.21895(6) 0.0532(4) Uani 1 1 d . . . Cl1 Cl 0.11332(11) 0.9550(3) 0.07591(18) 0.0694(9) Uani 1 1 d . . . C1 C -0.0407(4) 0.7250(11) 0.0648(6) 0.052(3) Uani 1 1 d . . . C2 C -0.0217(4) 0.6473(11) 0.1249(7) 0.060(3) Uani 1 1 d . . . H2 H 0.0132 0.6387 0.1543 0.072 Uiso 1 1 calc R . . C3 C -0.0580(5) 0.5794(12) 0.1408(7) 0.070(4) Uani 1 1 d . . . H3 H -0.0463 0.5299 0.1838 0.084 Uiso 1 1 calc R . . C4 C -0.1080(6) 0.5850(13) 0.0960(8) 0.074(4) Uani 1 1 d . . . H4 H -0.1309 0.5358 0.1046 0.088 Uiso 1 1 calc R . . C5 C -0.1249(5) 0.6667(15) 0.0359(9) 0.095(5) Uani 1 1 d . . . H5 H -0.1600 0.6744 0.0070 0.114 Uiso 1 1 calc R . . C6 C -0.0937(5) 0.7365(14) 0.0165(9) 0.090(5) Uani 1 1 d . . . H6 H -0.1063 0.7879 -0.0255 0.108 Uiso 1 1 calc R . . C7 C 0.0001(4) 0.9676(10) 0.1010(6) 0.059(3) Uani 1 1 d . . . H7A H 0.0286 1.0186 0.1076 0.071 Uiso 1 1 calc R . . H7B H -0.0309 1.0118 0.0712 0.071 Uiso 1 1 calc R . . C8 C 0.0019(5) 0.9454(10) 0.1784(6) 0.057(3) Uani 1 1 d . . . C9 C 0.0478(4) 0.9377(10) 0.2457(6) 0.046(3) Uani 1 1 d . . . C10 C 0.0452(4) 0.9404(10) 0.3161(6) 0.047(3) Uani 1 1 d . . . H10 H 0.0754 0.9390 0.3612 0.056 Uiso 1 1 calc R . . C11 C 0.0982(4) 0.9328(10) 0.2439(6) 0.050(3) Uani 1 1 d . . . H11A H 0.1247 0.9558 0.2936 0.060 Uiso 1 1 calc R . . H11B H 0.0990 0.9869 0.2050 0.060 Uiso 1 1 calc R . . C12 C 0.1827(4) 0.7569(14) 0.2680(7) 0.074(4) Uani 1 1 d . . . C13 C 0.2138(5) 0.8452(17) 0.2578(9) 0.104(6) Uani 1 1 d . . . H13 H 0.1984 0.9139 0.2311 0.125 Uiso 1 1 calc R . . C14 C 0.2638(7) 0.835(2) 0.2845(12) 0.130(8) Uani 1 1 d . . . H14 H 0.2832 0.8934 0.2757 0.156 Uiso 1 1 calc R . . C15 C 0.2860(7) 0.736(2) 0.3250(14) 0.139(9) Uani 1 1 d . . . H15 H 0.3214 0.7287 0.3455 0.167 Uiso 1 1 calc R . . C16 C 0.2569(8) 0.641(2) 0.3374(10) 0.132(8) Uani 1 1 d . . . H16 H 0.2725 0.5722 0.3636 0.158 Uiso 1 1 calc R . . C17 C 0.2053(5) 0.6572(15) 0.3090(8) 0.094(5) Uani 1 1 d . . . H17 H 0.1853 0.5996 0.3177 0.113 Uiso 1 1 calc R . . C18 C 0.0862(7) 0.6994(12) -0.0343(7) 0.152(10) Uani 1 1 d GU . . H18 H 0.0712 0.7538 -0.0782 0.182 Uiso 1 1 calc R . . C19 C 0.1371(6) 0.7101(11) 0.0159(10) 0.145(9) Uani 1 1 d GU . . H19 H 0.1576 0.7729 0.0075 0.174 Uiso 1 1 calc R . . C20 C 0.1565(4) 0.6484(13) 0.0847(9) 0.102(6) Uani 1 1 d G . . H20 H 0.1906 0.6679 0.1243 0.122 Uiso 1 1 calc R . . C21 C 0.1250(6) 0.5759(11) 0.1032(6) 0.104(5) Uani 1 1 d G . . H21 H 0.1373 0.5437 0.1556 0.124 Uiso 1 1 calc R . . C22 C 0.0741(5) 0.5652(10) 0.0530(8) 0.088(5) Uani 1 1 d GU . . H22 H 0.0508 0.5244 0.0699 0.106 Uiso 1 1 calc R . . C23 C 0.0547(4) 0.6269(13) -0.0157(7) 0.112(7) Uani 1 1 d GU . . H23 H 0.0177 0.6296 -0.0471 0.135 Uiso 1 1 calc R . . P1 P 0.91287(17) 0.6929(4) 0.7733(2) 0.0909(13) Uani 1 1 d . . . F1 F 0.8748(5) 0.7993(11) 0.7474(8) 0.177(5) Uani 1 1 d . . . F2 F 0.9081(7) 0.6893(14) 0.8528(7) 0.205(6) Uani 1 1 d . . . F3 F 0.9579(6) 0.7784(13) 0.8129(10) 0.210(7) Uani 1 1 d . . . F4 F 0.9514(4) 0.5853(11) 0.8029(7) 0.158(4) Uani 1 1 d . . . F5 F 0.9164(8) 0.6976(17) 0.6994(8) 0.242(8) Uani 1 1 d . . . F6 F 0.8685(5) 0.6116(14) 0.7433(11) 0.234(8) 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 Ru1 0.0550(6) 0.0632(8) 0.0574(6) -0.0080(5) 0.0282(5) -0.0074(5) Se1 0.0511(6) 0.0688(10) 0.0402(5) 0.0046(6) 0.0210(5) -0.0073(6) Se2 0.0430(6) 0.0629(9) 0.0544(6) 0.0035(6) 0.0214(5) -0.0021(6) Cl1 0.0613(18) 0.082(3) 0.0717(19) 0.0044(17) 0.0345(16) -0.0170(17) C1 0.053(7) 0.063(9) 0.053(6) -0.017(6) 0.034(5) -0.029(6) C2 0.057(7) 0.062(9) 0.059(7) 0.016(7) 0.024(6) 0.000(6) C3 0.083(10) 0.072(10) 0.061(7) 0.014(7) 0.036(7) -0.012(8) C4 0.081(10) 0.070(11) 0.087(10) -0.008(8) 0.053(8) -0.017(8) C5 0.043(8) 0.123(15) 0.107(12) 0.005(11) 0.020(8) -0.018(9) C6 0.047(8) 0.121(14) 0.093(10) 0.021(9) 0.020(7) -0.019(8) C7 0.060(7) 0.048(8) 0.070(7) 0.017(6) 0.028(6) 0.005(6) C8 0.086(9) 0.046(8) 0.063(7) -0.008(6) 0.054(7) -0.011(6) C9 0.035(6) 0.054(8) 0.047(6) -0.010(5) 0.015(5) -0.003(5) C10 0.044(6) 0.052(8) 0.061(7) -0.002(6) 0.038(5) 0.006(5) C11 0.042(6) 0.047(8) 0.042(6) -0.012(5) 0.000(5) -0.009(5) C12 0.044(7) 0.122(13) 0.063(8) -0.009(8) 0.031(6) -0.017(8) C13 0.051(9) 0.146(17) 0.107(12) -0.019(11) 0.025(8) -0.014(10) C14 0.066(12) 0.18(2) 0.126(16) 0.000(15) 0.026(10) 0.003(13) C15 0.050(10) 0.20(3) 0.134(17) -0.024(17) 0.009(11) -0.019(14) C16 0.123(16) 0.17(2) 0.088(12) 0.026(13) 0.035(12) 0.070(16) C17 0.060(9) 0.110(14) 0.078(9) 0.029(9) -0.004(7) 0.017(9) C18 0.28(3) 0.107(17) 0.102(15) 0.003(13) 0.118(19) 0.04(2) C19 0.24(3) 0.112(15) 0.18(2) -0.041(17) 0.18(2) -0.016(18) C20 0.077(11) 0.105(16) 0.130(15) -0.039(12) 0.051(10) 0.016(10) C21 0.127(15) 0.100(14) 0.095(11) -0.023(10) 0.058(12) 0.031(12) C22 0.088(11) 0.091(12) 0.104(11) -0.040(10) 0.058(9) -0.020(9) C23 0.092(11) 0.122(16) 0.074(10) -0.061(10) -0.012(9) 0.026(11) P1 0.104(3) 0.090(4) 0.085(3) -0.013(3) 0.046(2) -0.008(3) F1 0.210(13) 0.111(9) 0.205(13) 0.007(9) 0.086(10) 0.063(9) F2 0.33(2) 0.196(14) 0.135(10) -0.011(9) 0.148(13) 0.027(13) F3 0.204(14) 0.171(12) 0.213(15) -0.053(11) 0.050(12) -0.087(11) F4 0.145(9) 0.150(10) 0.166(10) 0.026(8) 0.055(8) 0.069(8) F5 0.35(2) 0.31(2) 0.132(10) 0.068(12) 0.159(13) 0.064(17) F6 0.151(11) 0.203(15) 0.29(2) -0.035(14) 0.044(11) -0.083(11) _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 Ru1 C22 2.162(11) . ? Ru1 C23 2.165(10) . ? Ru1 C21 2.184(11) . ? Ru1 C18 2.189(10) . ? Ru1 C20 2.208(10) . ? Ru1 C19 2.210(10) . ? Ru1 Cl1 2.394(4) . ? Ru1 Se1 2.4945(16) . ? Ru1 Se2 2.5157(17) . ? Se1 C1 1.919(10) . ? Se1 C7 1.970(12) . ? Se2 C12 1.920(12) . ? Se2 C11 1.985(11) . ? C1 C2 1.361(15) . ? C1 C6 1.421(16) . ? C2 C3 1.435(16) . ? C2 H2 0.9300 . ? C3 C4 1.334(16) . ? C3 H3 0.9300 . ? C4 C5 1.389(19) . ? C4 H4 0.9300 . ? C5 C6 1.364(19) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.482(15) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.404(14) . ? C8 C10 1.416(14) 2 ? C9 C10 1.382(14) . ? C9 C11 1.476(14) . ? C10 C8 1.416(14) 2 ? C10 H10 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.368(18) . ? C12 C13 1.410(19) . ? C13 C14 1.32(2) . ? C13 H13 0.9300 . ? C14 C15 1.35(3) . ? C14 H14 0.9300 . ? C15 C16 1.44(3) . ? C15 H15 0.9300 . ? C16 C17 1.37(2) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.37920 . ? C18 C23 1.378004 . ? C18 H18 0.9800 . ? C19 C20 1.37976 . ? C19 H19 0.9800 . ? C20 C21 1.37901 . ? C20 H20 0.9800 . ? C21 C22 1.37920 . ? C21 H21 0.9800 . ? C22 C23 1.37826 . ? C22 H22 0.9800 . ? C23 H23 0.9800 . ? P1 F5 1.462(12) . ? P1 F6 1.481(12) . ? P1 F3 1.536(13) . ? P1 F1 1.559(12) . ? P1 F4 1.581(11) . ? P1 F2 1.589(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 C22 Ru1 C23 37.2(5) . . ? C22 Ru1 C21 37.0(6) . . ? C23 Ru1 C21 66.6(3) . . ? C22 Ru1 C18 66.6(3) . . ? C23 Ru1 C18 37.0(6) . . ? C21 Ru1 C18 78.2(3) . . ? C22 Ru1 C20 66.3(3) . . ? C23 Ru1 C20 78.2(3) . . ? C21 Ru1 C20 36.6(6) . . ? C18 Ru1 C20 65.8(3) . . ? C22 Ru1 C19 78.2(3) . . ? C23 Ru1 C19 66.2(3) . . ? C21 Ru1 C19 65.9(3) . . ? C18 Ru1 C19 36.6(7) . . ? C20 Ru1 C19 36.4(6) . . ? C22 Ru1 Cl1 164.1(3) . . ? C23 Ru1 Cl1 130.1(5) . . ? C21 Ru1 Cl1 139.9(4) . . ? C18 Ru1 Cl1 97.9(4) . . ? C20 Ru1 Cl1 105.1(4) . . ? C19 Ru1 Cl1 87.2(3) . . ? C22 Ru1 Se1 100.5(4) . . ? C23 Ru1 Se1 85.4(3) . . ? C21 Ru1 Se1 134.9(4) . . ? C18 Ru1 Se1 100.6(4) . . ? C20 Ru1 Se1 163.6(3) . . ? C19 Ru1 Se1 134.5(5) . . ? Cl1 Ru1 Se1 85.25(9) . . ? C22 Ru1 Se2 103.6(4) . . ? C23 Ru1 Se2 138.3(5) . . ? C21 Ru1 Se2 87.5(3) . . ? C18 Ru1 Se2 165.4(4) . . ? C20 Ru1 Se2 100.6(4) . . ? C19 Ru1 Se2 133.2(5) . . ? Cl1 Ru1 Se2 90.83(9) . . ? Se1 Ru1 Se2 91.75(5) . . ? C1 Se1 C7 98.3(5) . . ? C1 Se1 Ru1 113.2(4) . . ? C7 Se1 Ru1 112.6(3) . . ? C12 Se2 C11 101.7(5) . . ? C12 Se2 Ru1 102.5(4) . . ? C11 Se2 Ru1 109.9(3) . . ? C2 C1 C6 122.9(11) . . ? C2 C1 Se1 122.8(8) . . ? C6 C1 Se1 114.3(9) . . ? C1 C2 C3 117.1(11) . . ? C1 C2 H2 121.5 . . ? C3 C2 H2 121.5 . . ? C4 C3 C2 122.1(12) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 117.8(12) . . ? C3 C4 H4 121.1 . . ? C5 C4 H4 121.1 . . ? C6 C5 C4 124.6(13) . . ? C6 C5 H5 117.7 . . ? C4 C5 H5 117.7 . . ? C5 C6 C1 115.3(13) . . ? C5 C6 H6 122.3 . . ? C1 C6 H6 122.3 . . ? C8 C7 Se1 118.2(8) . . ? C8 C7 H7A 107.8 . . ? Se1 C7 H7A 107.8 . . ? C8 C7 H7B 107.8 . . ? Se1 C7 H7B 107.8 . . ? H7A C7 H7B 107.1 . . ? C9 C8 C10 119.6(10) . 2 ? C9 C8 C7 123.1(10) . . ? C10 C8 C7 117.2(11) 2 . ? C10 C9 C8 118.2(9) . . ? C10 C9 C11 119.3(9) . . ? C8 C9 C11 122.5(9) . . ? C9 C10 C8 121.9(10) . 2 ? C9 C10 H10 119.1 . . ? C8 C10 H10 119.1 2 . ? C9 C11 Se2 108.0(7) . . ? C9 C11 H11A 110.1 . . ? Se2 C11 H11A 110.1 . . ? C9 C11 H11B 110.1 . . ? Se2 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? C17 C12 C13 118.9(13) . . ? C17 C12 Se2 119.3(11) . . ? C13 C12 Se2 121.6(12) . . ? C14 C13 C12 122.8(18) . . ? C14 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? C13 C14 C15 118(2) . . ? C13 C14 H14 120.9 . . ? C15 C14 H14 120.9 . . ? C14 C15 C16 122.3(18) . . ? C14 C15 H15 118.8 . . ? C16 C15 H15 118.8 . . ? C17 C16 C15 116.9(18) . . ? C17 C16 H16 121.5 . . ? C15 C16 H16 121.5 . . ? C16 C17 C12 120.8(17) . . ? C16 C17 H17 119.6 . . ? C12 C17 H17 119.6 . . ? C19 C18 C23 120.0 . . ? C19 C18 Ru1 72.6(9) . . ? C23 C18 Ru1 70.6(4) . . ? C19 C18 H18 119.5 . . ? C23 C18 H18 119.5 . . ? Ru1 C18 H18 119.5 . . ? C18 C19 C20 120.0 . . ? C18 C19 Ru1 70.9(10) . . ? C20 C19 Ru1 71.7(10) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? Ru1 C19 H19 119.5 . . ? C21 C20 C19 120.0 . . ? C21 C20 Ru1 70.8(4) . . ? C19 C20 Ru1 71.9(10) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? Ru1 C20 H20 119.5 . . ? C22 C21 C20 120.0 . . ? C22 C21 Ru1 70.6(8) . . ? C20 C21 Ru1 72.6(4) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? Ru1 C21 H21 119.5 . . ? C23 C22 C21 120.0 . . ? C23 C22 Ru1 71.5(4) . . ? C21 C22 Ru1 72.4(7) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? Ru1 C22 H22 119.6 . . ? C22 C23 C18 120.0 . . ? C22 C23 Ru1 71.3(4) . . ? C18 C23 Ru1 72.5(4) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? Ru1 C23 H23 119.6 . . ? F5 P1 F6 93.2(12) . . ? F5 P1 F3 93.5(11) . . ? F6 P1 F3 173.3(11) . . ? F5 P1 F1 89.8(9) . . ? F6 P1 F1 88.5(9) . . ? F3 P1 F1 90.6(9) . . ? F5 P1 F4 92.6(8) . . ? F6 P1 F4 91.5(9) . . ? F3 P1 F4 89.0(8) . . ? F1 P1 F4 177.6(8) . . ? F5 P1 F2 178.9(10) . . ? F6 P1 F2 86.5(10) . . ? F3 P1 F2 86.8(9) . . ? F1 P1 F2 89.2(8) . . ? F4 P1 F2 88.4(8) . . ? 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 C22 Ru1 Se1 C1 38.0(5) . . . . ? C23 Ru1 Se1 C1 72.1(6) . . . . ? C21 Ru1 Se1 C1 22.0(5) . . . . ? C18 Ru1 Se1 C1 105.9(5) . . . . ? C20 Ru1 Se1 C1 73.0(18) . . . . ? C19 Ru1 Se1 C1 121.8(6) . . . . ? Cl1 Ru1 Se1 C1 -156.9(3) . . . . ? Se2 Ru1 Se1 C1 -66.2(3) . . . . ? C22 Ru1 Se1 C7 148.3(5) . . . . ? C23 Ru1 Se1 C7 -177.6(6) . . . . ? C21 Ru1 Se1 C7 132.3(5) . . . . ? C18 Ru1 Se1 C7 -143.8(5) . . . . ? C20 Ru1 Se1 C7 -176.7(18) . . . . ? C19 Ru1 Se1 C7 -127.9(6) . . . . ? Cl1 Ru1 Se1 C7 -46.6(4) . . . . ? Se2 Ru1 Se1 C7 44.1(4) . . . . ? C22 Ru1 Se2 C12 95.0(6) . . . . ? C23 Ru1 Se2 C12 111.3(7) . . . . ? C21 Ru1 Se2 C12 61.4(7) . . . . ? C18 Ru1 Se2 C12 48(2) . . . . ? C20 Ru1 Se2 C12 27.1(6) . . . . ? C19 Ru1 Se2 C12 8.4(7) . . . . ? Cl1 Ru1 Se2 C12 -78.5(5) . . . . ? Se1 Ru1 Se2 C12 -163.7(5) . . . . ? C22 Ru1 Se2 C11 -157.4(5) . . . . ? C23 Ru1 Se2 C11 -141.2(5) . . . . ? C21 Ru1 Se2 C11 169.0(5) . . . . ? C18 Ru1 Se2 C11 156(2) . . . . ? C20 Ru1 Se2 C11 134.6(5) . . . . ? C19 Ru1 Se2 C11 116.0(5) . . . . ? Cl1 Ru1 Se2 C11 29.1(3) . . . . ? Se1 Ru1 Se2 C11 -56.2(3) . . . . ? C7 Se1 C1 C2 -91.7(11) . . . . ? Ru1 Se1 C1 C2 27.3(11) . . . . ? C7 Se1 C1 C6 87.7(10) . . . . ? Ru1 Se1 C1 C6 -153.4(9) . . . . ? C6 C1 C2 C3 -3.1(18) . . . . ? Se1 C1 C2 C3 176.2(9) . . . . ? C1 C2 C3 C4 4.7(19) . . . . ? C2 C3 C4 C5 -5(2) . . . . ? C3 C4 C5 C6 4(2) . . . . ? C4 C5 C6 C1 -3(2) . . . . ? C2 C1 C6 C5 2(2) . . . . ? Se1 C1 C6 C5 -177.1(12) . . . . ? C1 Se1 C7 C8 39.1(9) . . . . ? Ru1 Se1 C7 C8 -80.3(9) . . . . ? Se1 C7 C8 C9 89.2(13) . . . . ? Se1 C7 C8 C10 -95.3(11) . . . 2 ? C10 C8 C9 C10 -8.0(15) 2 . . . ? C7 C8 C9 C10 167.4(11) . . . . ? C10 C8 C9 C11 175.1(10) 2 . . . ? C7 C8 C9 C11 -9.5(18) . . . . ? C8 C9 C10 C8 2.9(15) . . . 2 ? C11 C9 C10 C8 179.9(11) . . . 2 ? C10 C9 C11 Se2 103.1(10) . . . . ? C8 C9 C11 Se2 -80.0(12) . . . . ? C12 Se2 C11 C9 -152.2(8) . . . . ? Ru1 Se2 C11 C9 99.7(7) . . . . ? C11 Se2 C12 C17 136.7(11) . . . . ? Ru1 Se2 C12 C17 -109.6(11) . . . . ? C11 Se2 C12 C13 -48.4(12) . . . . ? Ru1 Se2 C12 C13 65.3(12) . . . . ? C17 C12 C13 C14 2(2) . . . . ? Se2 C12 C13 C14 -173.1(14) . . . . ? C12 C13 C14 C15 -2(3) . . . . ? C13 C14 C15 C16 2(3) . . . . ? C14 C15 C16 C17 -3(3) . . . . ? C15 C16 C17 C12 3(3) . . . . ? C13 C12 C17 C16 -2(2) . . . . ? Se2 C12 C17 C16 172.8(13) . . . . ? C22 Ru1 C18 C19 -102.1(9) . . . . ? C23 Ru1 C18 C19 -131.8(12) . . . . ? C21 Ru1 C18 C19 -65.2(2) . . . . ? C20 Ru1 C18 C19 -28.8(8) . . . . ? Cl1 Ru1 C18 C19 74.3(5) . . . . ? Se1 Ru1 C18 C19 160.9(5) . . . . ? Se2 Ru1 C18 C19 -52(2) . . . . ? C22 Ru1 C18 C23 29.6(8) . . . . ? C21 Ru1 C18 C23 66.6(3) . . . . ? C20 Ru1 C18 C23 103.0(3) . . . . ? C19 Ru1 C18 C23 131.8(12) . . . . ? Cl1 Ru1 C18 C23 -153.9(5) . . . . ? Se1 Ru1 C18 C23 -67.3(5) . . . . ? Se2 Ru1 C18 C23 80(2) . . . . ? C23 C18 C19 C20 0.0 . . . . ? Ru1 C18 C19 C20 54.3(4) . . . . ? C23 C18 C19 Ru1 -54.3(4) . . . . ? C22 Ru1 C19 C18 66.4(2) . . . . ? C23 Ru1 C19 C18 29.4(8) . . . . ? C21 Ru1 C19 C18 103.2(3) . . . . ? C20 Ru1 C19 C18 132.2(12) . . . . ? Cl1 Ru1 C19 C18 -107.3(6) . . . . ? Se1 Ru1 C19 C18 -26.8(6) . . . . ? Se2 Ru1 C19 C18 164.2(6) . . . . ? C22 Ru1 C19 C20 -65.8(3) . . . . ? C23 Ru1 C19 C20 -102.9(3) . . . . ? C21 Ru1 C19 C20 -29.0(8) . . . . ? C18 Ru1 C19 C20 -132.2(12) . . . . ? Cl1 Ru1 C19 C20 120.5(5) . . . . ? Se1 Ru1 C19 C20 -159.0(6) . . . . ? Se2 Ru1 C19 C20 32.0(6) . . . . ? C18 C19 C20 C21 0.0 . . . . ? Ru1 C19 C20 C21 53.9(3) . . . . ? C18 C19 C20 Ru1 -53.9(14) . . . . ? C22 Ru1 C20 C21 -29.4(7) . . . . ? C23 Ru1 C20 C21 -66.5(3) . . . . ? C18 Ru1 C20 C21 -103.3(3) . . . . ? C19 Ru1 C20 C21 -132.1(13) . . . . ? Cl1 Ru1 C20 C21 164.7(5) . . . . ? Se1 Ru1 C20 C21 -67(2) . . . . ? Se2 Ru1 C20 C21 71.0(5) . . . . ? C22 Ru1 C20 C19 102.8(3) . . . . ? C23 Ru1 C20 C19 65.7(3) . . . . ? C21 Ru1 C20 C19 132.1(13) . . . . ? C18 Ru1 C20 C19 28.9(9) . . . . ? Cl1 Ru1 C20 C19 -63.1(5) . . . . ? Se1 Ru1 C20 C19 65(2) . . . . ? Se2 Ru1 C20 C19 -156.9(5) . . . . ? C19 C20 C21 C22 0.0 . . . . ? Ru1 C20 C21 C22 54.4(3) . . . . ? C19 C20 C21 Ru1 -54.5(13) . . . . ? C23 Ru1 C21 C22 -29.6(8) . . . . ? C18 Ru1 C21 C22 -66.6(9) . . . . ? C20 Ru1 C21 C22 -131.7(12) . . . . ? C19 Ru1 C21 C22 -102.9(3) . . . . ? Cl1 Ru1 C21 C22 -154.9(6) . . . . ? Se1 Ru1 C21 C22 26.7(6) . . . . ? Se2 Ru1 C21 C22 116.7(6) . . . . ? C22 Ru1 C21 C20 131.7(12) . . . . ? C23 Ru1 C21 C20 102.0(3) . . . . ? C18 Ru1 C21 C20 65.1(3) . . . . ? C19 Ru1 C21 C20 28.9(9) . . . . ? Cl1 Ru1 C21 C20 -23.2(6) . . . . ? Se1 Ru1 C21 C20 158.4(7) . . . . ? Se2 Ru1 C21 C20 -111.6(6) . . . . ? C20 C21 C22 C23 0.0 . . . . ? Ru1 C21 C22 C23 55.4(4) . . . . ? C20 C21 C22 Ru1 -55.4(4) . . . . ? C21 Ru1 C22 C23 -131.3(13) . . . . ? C18 Ru1 C22 C23 -29.5(9) . . . . ? C20 Ru1 C22 C23 -102.2(3) . . . . ? C19 Ru1 C22 C23 -65.9(3) . . . . ? Cl1 Ru1 C22 C23 -42.5(19) . . . . ? Se1 Ru1 C22 C23 67.6(5) . . . . ? Se2 Ru1 C22 C23 162.1(5) . . . . ? C23 Ru1 C22 C21 131.3(13) . . . . ? C18 Ru1 C22 C21 101.8(10) . . . . ? C20 Ru1 C22 C21 29.1(8) . . . . ? C19 Ru1 C22 C21 65.3(9) . . . . ? Cl1 Ru1 C22 C21 88.8(18) . . . . ? Se1 Ru1 C22 C21 -161.1(5) . . . . ? Se2 Ru1 C22 C21 -66.7(5) . . . . ? C21 C22 C23 C18 0.0 . . . . ? Ru1 C22 C23 C18 55.8(13) . . . . ? C21 C22 C23 Ru1 -55.8(3) . . . . ? C19 C18 C23 C22 0.0 . . . . ? Ru1 C18 C23 C22 -55.2(3) . . . . ? C19 C18 C23 Ru1 55.2(13) . . . . ? C21 Ru1 C23 C22 29.5(9) . . . . ? C18 Ru1 C23 C22 131.3(13) . . . . ? C20 Ru1 C23 C22 66.1(3) . . . . ? C19 Ru1 C23 C22 102.3(10) . . . . ? Cl1 Ru1 C23 C22 166.0(5) . . . . ? Se1 Ru1 C23 C22 -114.2(6) . . . . ? Se2 Ru1 C23 C22 -26.8(7) . . . . ? C22 Ru1 C23 C18 -131.3(13) . . . . ? C21 Ru1 C23 C18 -101.8(3) . . . . ? C20 Ru1 C23 C18 -65.2(3) . . . . ? C19 Ru1 C23 C18 -29.0(9) . . . . ? Cl1 Ru1 C23 C18 34.7(5) . . . . ? Se1 Ru1 C23 C18 114.5(6) . . . . ? Se2 Ru1 C23 C18 -158.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.848 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.130