# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Vimal K Jain' _publ_contact_author_email jainvk@barc.gov.in _publ_section_title ; Oligomeric allyl-palladium(II) complexes of ss-substituted ethylselenolates: Syntheses, structures and thermal decomposition ; _publ_author_name V.K.Jain # Attachment '- lbk-19.cif' data_lbk-19 _database_code_depnum_ccdc_archive 'CCDC 811871' #TrackingRef '- lbk-19.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H42 O6 Pd3 Se3' _chemical_formula_weight 982.66 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' 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 'P 1 21/a 1' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 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 30.966(7) _cell_length_b 6.795(3) _cell_length_c 15.901(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.15(3) _cell_angle_gamma 90.00 _cell_volume 3271(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 9.4 _cell_measurement_theta_max 12.2 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.996 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 5.003 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.4344 _exptl_absorpt_correction_T_max 0.4344 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.59 _diffrn_reflns_number 9911 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.2532 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7428 _reflns_number_gt 2287 _reflns_threshold_expression >2sigma(I) _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep 3 for Windows' _computing_publication_material 'WinGX 1.70.01' _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^)+(0.0701P)^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 7428 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2853 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.2185 _refine_ls_wR_factor_gt 0.1533 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.000 _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 C1 C 0.5507(7) 0.194(2) 1.0197(11) 0.086(6) Uani 1 1 d . . . H1A H 0.5771 0.1145 1.0381 0.103 Uiso 1 1 calc R . . H1B H 0.5361 0.2292 1.0659 0.103 Uiso 1 1 calc R . . C2 C 0.5260(7) 0.151(3) 0.9474(15) 0.102 Uani 1 1 d . . . H2 H 0.5397 0.0448 0.9203 0.123 Uiso 1 1 calc R . . C3 C 0.4957(6) 0.229(3) 0.8921(12) 0.087(5) Uani 1 1 d . . . H3A H 0.4695 0.2715 0.9116 0.104 Uiso 1 1 calc R . . H3B H 0.4893 0.1698 0.8353 0.104 Uiso 1 1 calc R . . C4 C 0.4823(4) 0.587(3) 0.7255(10) 0.067(5) Uani 1 1 d . . . H4A H 0.4768 0.4460 0.7221 0.080 Uiso 1 1 calc R . . H4B H 0.4598 0.6477 0.7510 0.080 Uiso 1 1 calc R . . C5 C 0.4798(7) 0.667(2) 0.6374(13) 0.090(7) Uani 1 1 d . . . H5A H 0.5052 0.6200 0.6167 0.108 Uiso 1 1 calc R . . H5B H 0.4821 0.8092 0.6416 0.108 Uiso 1 1 calc R . . C6 C 0.4387(9) 0.617(4) 0.5706(16) 0.109(8) Uani 1 1 d . . . C7 C 0.3884(9) 0.322(6) 0.5158(16) 0.204(19) Uani 1 1 d . . . H7A H 0.3787 0.2297 0.5546 0.244 Uiso 1 1 calc R . . H7B H 0.3648 0.4120 0.4914 0.244 Uiso 1 1 calc R . . C8 C 0.4042(12) 0.246(7) 0.4649(19) 0.25(2) Uani 1 1 d . . . H8A H 0.4259 0.3327 0.4495 0.370 Uiso 1 1 calc R . . H8B H 0.3819 0.2176 0.4148 0.370 Uiso 1 1 calc R . . H8C H 0.4183 0.1264 0.4881 0.370 Uiso 1 1 calc R . . C9 C 0.5443(9) 0.197(3) 0.6785(16) 0.117(10) Uani 1 1 d . . . H9A H 0.5214 0.1540 0.7076 0.140 Uiso 1 1 calc R . . H9B H 0.5336 0.2220 0.6176 0.140 Uiso 1 1 calc R . . C10 C 0.5833(11) 0.106(3) 0.7005(16) 0.116(9) Uani 1 1 d . . . H10 H 0.5855 0.0032 0.7446 0.139 Uiso 1 1 calc R . . C11 C 0.6212(7) 0.176(3) 0.6863(14) 0.091(7) Uani 1 1 d . . . H11A H 0.6227 0.1965 0.6267 0.109 Uiso 1 1 calc R . . H11B H 0.6480 0.1189 0.7206 0.109 Uiso 1 1 calc R . . C12 C 0.6975(5) 0.539(2) 0.7273(8) 0.051 Uani 1 1 d . . . H12A H 0.6996 0.3970 0.7242 0.062 Uiso 1 1 calc R . . H12B H 0.6864 0.5885 0.6696 0.062 Uiso 1 1 calc R . . C13 C 0.7428(5) 0.624(2) 0.7624(11) 0.068(5) Uani 1 1 d . . . H13A H 0.7556 0.5627 0.8169 0.082 Uiso 1 1 calc R . . H13B H 0.7403 0.7645 0.7722 0.082 Uiso 1 1 calc R . . C14 C 0.7732(7) 0.589(2) 0.6969(14) 0.070(5) Uani 1 1 d . . . C15 C 0.8471(6) 0.569(2) 0.6853(12) 0.072(5) Uani 1 1 d . . . H15A H 0.8479 0.6838 0.6496 0.086 Uiso 1 1 calc R . . H15B H 0.8388 0.4556 0.6480 0.086 Uiso 1 1 calc R . . C16 C 0.8919(6) 0.535(3) 0.7436(12) 0.097(7) Uani 1 1 d . . . H16A H 0.8975 0.6365 0.7866 0.146 Uiso 1 1 calc R . . H16B H 0.9143 0.5384 0.7102 0.146 Uiso 1 1 calc R . . H16C H 0.8922 0.4091 0.7711 0.146 Uiso 1 1 calc R . . C17 C 0.7114(7) 0.175(3) 0.8963(11) 0.097(7) Uani 1 1 d . . . H17A H 0.6983 0.0777 0.8536 0.117 Uiso 1 1 calc R . . H17B H 0.7401 0.2202 0.8896 0.117 Uiso 1 1 calc R . . C18 C 0.7070(9) 0.143(3) 0.9724(16) 0.112 Uani 1 1 d . . . H18 H 0.7338 0.2058 1.0056 0.134 Uiso 1 1 calc R . . C19 C 0.6818(7) 0.161(3) 1.0214(14) 0.103(7) Uani 1 1 d . . . H19A H 0.6949 0.2007 1.0798 0.124 Uiso 1 1 calc R . . H19B H 0.6594 0.0600 1.0181 0.124 Uiso 1 1 calc R . . C20 C 0.6294(6) 0.533(3) 1.1151(10) 0.076(5) Uani 1 1 d . . . H20A H 0.6060 0.5871 1.1399 0.091 Uiso 1 1 calc R . . H20B H 0.6287 0.3905 1.1209 0.091 Uiso 1 1 calc R . . C21 C 0.6729(5) 0.608(2) 1.1635(9) 0.054(4) Uani 1 1 d . . . H21A H 0.6755 0.7466 1.1501 0.064 Uiso 1 1 calc R . . H21B H 0.6965 0.5384 1.1446 0.064 Uiso 1 1 calc R . . C22 C 0.6788(6) 0.585(2) 1.2606(13) 0.061(5) Uani 1 1 d . . . C23 C 0.7304(5) 0.584(2) 1.3946(9) 0.060(5) Uani 1 1 d . . . H23A H 0.7175 0.4643 1.4120 0.072 Uiso 1 1 calc R . . H23B H 0.7183 0.6958 1.4196 0.072 Uiso 1 1 calc R . . C24 C 0.7795(5) 0.579(3) 1.4228(10) 0.088(6) Uani 1 1 d . . . H24A H 0.7915 0.7029 1.4099 0.132 Uiso 1 1 calc R . . H24B H 0.7912 0.4756 1.3930 0.132 Uiso 1 1 calc R . . H24C H 0.7874 0.5555 1.4837 0.132 Uiso 1 1 calc R . . O1 O 0.4085(6) 0.726(3) 0.5479(11) 0.135(7) Uani 1 1 d . . . O2 O 0.4353(6) 0.433(3) 0.5583(13) 0.177(10) Uani 1 1 d . . . O3 O 0.7606(4) 0.5773(19) 0.6231(8) 0.083(4) Uani 1 1 d . . . O4 O 0.8148(4) 0.5976(15) 0.7412(7) 0.070(3) Uani 1 1 d . . . O5 O 0.6493(4) 0.5524(17) 1.2949(7) 0.075(4) Uani 1 1 d . . . O6 O 0.7213(4) 0.6001(15) 1.2993(7) 0.069(3) Uani 1 1 d . . . Se1 Se 0.54092(5) 0.6375(2) 0.79803(12) 0.0591(5) Uani 1 1 d . . . Se2 Se 0.65588(6) 0.6105(2) 0.80157(11) 0.0547(5) Uani 1 1 d . . . Se3 Se 0.61898(5) 0.6023(2) 0.99209(10) 0.0516(5) Uani 1 1 d . . . Pd1 Pd 0.55274(4) 0.41616(17) 0.92279(8) 0.0542(4) Uani 1 1 d . . . Pd2 Pd 0.59065(4) 0.40384(17) 0.74600(8) 0.0547(4) Uani 1 1 d . . . Pd3 Pd 0.66802(4) 0.39158(17) 0.92761(8) 0.0526(4) 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 C1 0.097(15) 0.088(14) 0.064(13) 0.022(11) -0.004(12) -0.048(12) C2 0.090 0.094 0.108 0.023 -0.013 -0.030 C3 0.059(11) 0.105(15) 0.081 0.019(12) -0.017(11) -0.031 C4 0.024(8) 0.107(14) 0.064(12) 0.016(11) -0.003(8) 0.018(10) C5 0.105(17) 0.050(11) 0.095(16) 0.003(11) -0.021(14) 0.009(11) C6 0.12(2) 0.10(2) 0.094(18) 0.007(17) -0.014(16) 0.008(19) C7 0.075(19) 0.45(6) 0.07(2) -0.07(3) -0.022(16) 0.03(3) C8 0.19(4) 0.45(6) 0.10(3) -0.10(3) 0.02(2) 0.05(4) C9 0.13(2) 0.046(13) 0.16(2) -0.036(13) -0.006(18) 0.023(14) C10 0.17(3) 0.067(16) 0.13(2) -0.041(15) 0.07(2) -0.043(18) C11 0.082(16) 0.061(13) 0.128(19) -0.017(12) 0.018(15) 0.000(12) C12 0.067 0.046 0.027 -0.004 -0.020 -0.021 C13 0.050(11) 0.082(13) 0.063(12) -0.010(10) -0.009(10) -0.005(10) C14 0.078(15) 0.052(11) 0.077(15) 0.006(12) 0.009(13) -0.025(11) C15 0.068(13) 0.068(12) 0.090(14) -0.007(10) 0.041(12) -0.002(10) C16 0.057(13) 0.135(19) 0.095(16) -0.032(14) 0.006(12) -0.014(13) C17 0.133(19) 0.102(15) 0.051(12) 0.006(11) 0.006(12) 0.075(14) C18 0.147 0.095 0.104 0.038 0.050 0.087 C19 0.115(19) 0.083(15) 0.128(19) 0.031(13) 0.064(16) 0.029(13) C20 0.061(11) 0.090(13) 0.084 -0.028(10) 0.034(10) -0.025 C21 0.051(10) 0.055(10) 0.052(11) 0.006(9) 0.005(8) 0.002(9) C22 0.039(10) 0.035(9) 0.105(16) 0.014(10) 0.008(11) -0.005(9) C23 0.085(14) 0.058(11) 0.040(10) 0.010(9) 0.019(9) 0.013(10) C24 0.059(12) 0.17(2) 0.045(11) -0.002(12) 0.026(10) 0.019(13) O1 0.117(14) 0.140(15) 0.121(14) 0.021(11) -0.036(11) 0.030(12) O2 0.137(16) 0.119(15) 0.22(2) -0.038(14) -0.086(15) -0.012(13) O3 0.081(9) 0.118(11) 0.053(8) 0.001(9) 0.018(7) -0.008(8) O4 0.070(8) 0.065(8) 0.080(9) -0.004(7) 0.024(8) -0.028(7) O5 0.069(9) 0.093(10) 0.063(8) -0.005(7) 0.012(7) -0.027(8) O6 0.069(8) 0.080(8) 0.061(8) -0.004(7) 0.020(7) 0.001(7) Se1 0.0539(11) 0.0475(11) 0.0717(12) 0.0042(9) 0.0034(9) -0.0010(8) Se2 0.0563(10) 0.0510(10) 0.0569(11) 0.0026(9) 0.0125(9) -0.0064(9) Se3 0.0516(10) 0.0487(10) 0.0545(10) -0.0018(9) 0.0112(8) -0.0077(8) Pd1 0.0525(8) 0.0478(8) 0.0617(9) 0.0000(7) 0.0110(7) -0.0095(7) Pd2 0.0560(8) 0.0435(7) 0.0646(9) 0.0024(7) 0.0127(7) -0.0080(7) Pd3 0.0531(8) 0.0438(7) 0.0593(8) 0.0022(7) 0.0085(6) -0.0011(7) _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 C1 C2 1.27(2) . ? C1 Pd1 2.169(15) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.26(2) . ? C2 Pd1 2.057(19) . ? C2 H2 0.9800 . ? C3 Pd1 2.150(16) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.49(2) . ? C4 Se1 1.966(13) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.51(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O1 1.19(2) . ? C6 O2 1.27(2) . ? C7 C8 1.15(3) . ? C7 O2 1.65(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.34(3) . ? C9 Pd2 2.13(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.33(3) . ? C10 Pd2 2.15(2) . ? C10 H10 0.9800 . ? C11 Pd2 2.141(19) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.512(18) . ? C12 Se2 1.982(15) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.56(2) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O3 1.159(19) . ? C14 O4 1.33(2) . ? C15 O4 1.484(18) . ? C15 C16 1.52(2) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.26(2) . ? C17 Pd3 2.123(17) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.22(2) . ? C18 Pd3 2.109(17) . ? C18 H18 0.9800 . ? C19 Pd3 2.143(18) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.50(2) . ? C20 Se3 1.972(17) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.52(2) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 O5 1.181(19) . ? C22 O6 1.334(18) . ? C23 O6 1.486(16) . ? C23 C24 1.49(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? Se1 Pd1 2.455(2) . ? Se1 Pd2 2.472(2) . ? Se2 Pd3 2.460(2) . ? Se2 Pd2 2.466(2) . ? Se3 Pd3 2.462(2) . ? Se3 Pd1 2.464(2) . ? 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 C1 Pd1 67.7(11) . . ? C2 C1 H1A 116.9 . . ? Pd1 C1 H1A 116.9 . . ? C2 C1 H1B 116.9 . . ? Pd1 C1 H1B 116.9 . . ? H1A C1 H1B 113.9 . . ? C3 C2 C1 139(3) . . ? C3 C2 Pd1 76.7(12) . . ? C1 C2 Pd1 77.3(12) . . ? C3 C2 H2 109.3 . . ? C1 C2 H2 109.3 . . ? Pd1 C2 H2 109.3 . . ? C2 C3 Pd1 68.6(11) . . ? 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 . . ? C5 C4 Se1 110.2(12) . . ? C5 C4 H4A 109.6 . . ? Se1 C4 H4A 109.6 . . ? C5 C4 H4B 109.6 . . ? Se1 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 116.6(18) . . ? C4 C5 H5A 108.2 . . ? C6 C5 H5A 108.2 . . ? C4 C5 H5B 108.2 . . ? C6 C5 H5B 108.2 . . ? H5A C5 H5B 107.3 . . ? O1 C6 O2 122(3) . . ? O1 C6 C5 124(2) . . ? O2 C6 C5 111(2) . . ? C8 C7 O2 91(3) . . ? C8 C7 H7A 113.4 . . ? O2 C7 H7A 113.4 . . ? C8 C7 H7B 113.4 . . ? O2 C7 H7B 113.4 . . ? H7A C7 H7B 110.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 Pd2 72.6(14) . . ? C10 C9 H9A 116.3 . . ? Pd2 C9 H9A 116.3 . . ? C10 C9 H9B 116.3 . . ? Pd2 C9 H9B 116.3 . . ? H9A C9 H9B 113.3 . . ? C11 C10 C9 125(3) . . ? C11 C10 Pd2 71.6(12) . . ? C9 C10 Pd2 71.0(14) . . ? C11 C10 H10 116.3 . . ? C9 C10 H10 116.3 . . ? Pd2 C10 H10 116.3 . . ? C10 C11 Pd2 72.2(13) . . ? C10 C11 H11A 116.4 . . ? Pd2 C11 H11A 116.4 . . ? C10 C11 H11B 116.4 . . ? Pd2 C11 H11B 116.4 . . ? H11A C11 H11B 113.3 . . ? C13 C12 Se2 110.8(10) . . ? C13 C12 H12A 109.5 . . ? Se2 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? Se2 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C12 C13 C14 109.8(14) . . ? C12 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? C12 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? O3 C14 O4 128(2) . . ? O3 C14 C13 124.2(19) . . ? O4 C14 C13 107.1(16) . . ? O4 C15 C16 107.4(15) . . ? O4 C15 H15A 110.2 . . ? C16 C15 H15A 110.2 . . ? O4 C15 H15B 110.2 . . ? C16 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 Pd3 72.0(12) . . ? C18 C17 H17A 116.4 . . ? Pd3 C17 H17A 116.4 . . ? C18 C17 H17B 116.4 . . ? Pd3 C17 H17B 116.4 . . ? H17A C17 H17B 113.4 . . ? C19 C18 C17 144(3) . . ? C19 C18 Pd3 74.9(13) . . ? C17 C18 Pd3 73.2(12) . . ? C19 C18 H18 101.3 . . ? C17 C18 H18 101.3 . . ? Pd3 C18 H18 101.3 . . ? C18 C19 Pd3 71.8(13) . . ? C18 C19 H19A 116.4 . . ? Pd3 C19 H19A 116.4 . . ? C18 C19 H19B 116.4 . . ? Pd3 C19 H19B 116.4 . . ? H19A C19 H19B 113.4 . . ? C21 C20 Se3 111.7(11) . . ? C21 C20 H20A 109.3 . . ? Se3 C20 H20A 109.3 . . ? C21 C20 H20B 109.3 . . ? Se3 C20 H20B 109.3 . . ? H20A C20 H20B 107.9 . . ? C20 C21 C22 112.8(14) . . ? C20 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? C20 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? O5 C22 O6 125.9(18) . . ? O5 C22 C21 123.3(16) . . ? O6 C22 C21 110.8(16) . . ? O6 C23 C24 105.7(13) . . ? O6 C23 H23A 110.6 . . ? C24 C23 H23A 110.6 . . ? O6 C23 H23B 110.6 . . ? C24 C23 H23B 110.6 . . ? H23A C23 H23B 108.7 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C6 O2 C7 124(2) . . ? C14 O4 C15 112.1(15) . . ? C22 O6 C23 114.9(14) . . ? C4 Se1 Pd1 109.2(5) . . ? C4 Se1 Pd2 104.7(5) . . ? Pd1 Se1 Pd2 83.08(7) . . ? C12 Se2 Pd3 109.3(4) . . ? C12 Se2 Pd2 103.5(4) . . ? Pd3 Se2 Pd2 85.46(7) . . ? C20 Se3 Pd3 106.7(5) . . ? C20 Se3 Pd1 105.5(5) . . ? Pd3 Se3 Pd1 92.50(7) . . ? C2 Pd1 C3 34.8(6) . . ? C2 Pd1 C1 35.0(6) . . ? C3 Pd1 C1 66.6(6) . . ? C2 Pd1 Se1 133.9(6) . . ? C3 Pd1 Se1 101.8(5) . . ? C1 Pd1 Se1 168.4(5) . . ? C2 Pd1 Se3 134.1(6) . . ? C3 Pd1 Se3 166.7(5) . . ? C1 Pd1 Se3 100.7(5) . . ? Se1 Pd1 Se3 90.88(7) . . ? C9 Pd2 C11 67.2(8) . . ? C9 Pd2 C10 36.5(8) . . ? C11 Pd2 C10 36.1(7) . . ? C9 Pd2 Se2 166.0(7) . . ? C11 Pd2 Se2 99.5(6) . . ? C10 Pd2 Se2 132.8(9) . . ? C9 Pd2 Se1 101.0(7) . . ? C11 Pd2 Se1 168.1(5) . . ? C10 Pd2 Se1 133.6(8) . . ? Se2 Pd2 Se1 92.02(7) . . ? C18 Pd3 C17 34.7(7) . . ? C18 Pd3 C19 33.3(7) . . ? C17 Pd3 C19 67.1(7) . . ? C18 Pd3 Se2 137.5(7) . . ? C17 Pd3 Se2 103.0(5) . . ? C19 Pd3 Se2 169.3(6) . . ? C18 Pd3 Se3 133.1(7) . . ? C17 Pd3 Se3 167.8(5) . . ? C19 Pd3 Se3 100.7(6) . . ? Se2 Pd3 Se3 89.19(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 Pd1 C1 C2 C3 -52(3) . . . . ? C1 C2 C3 Pd1 52(3) . . . . ? Se1 C4 C5 C6 172.5(16) . . . . ? C4 C5 C6 O1 101(3) . . . . ? C4 C5 C6 O2 -62(3) . . . . ? Pd2 C9 C10 C11 -50(2) . . . . ? C9 C10 C11 Pd2 50(2) . . . . ? Se2 C12 C13 C14 -172.9(11) . . . . ? C12 C13 C14 O3 29(2) . . . . ? C12 C13 C14 O4 -157.5(13) . . . . ? Pd3 C17 C18 C19 29(4) . . . . ? C17 C18 C19 Pd3 -29(4) . . . . ? Se3 C20 C21 C22 171.0(10) . . . . ? C20 C21 C22 O5 -16(2) . . . . ? C20 C21 C22 O6 162.2(13) . . . . ? O1 C6 O2 C7 -4(5) . . . . ? C5 C6 O2 C7 159(2) . . . . ? C8 C7 O2 C6 127(4) . . . . ? O3 C14 O4 C15 -6(3) . . . . ? C13 C14 O4 C15 -179.2(12) . . . . ? C16 C15 O4 C14 -167.5(14) . . . . ? O5 C22 O6 C23 -3(2) . . . . ? C21 C22 O6 C23 178.7(11) . . . . ? C24 C23 O6 C22 173.0(14) . . . . ? C5 C4 Se1 Pd1 -161.4(11) . . . . ? C5 C4 Se1 Pd2 -73.8(13) . . . . ? C13 C12 Se2 Pd3 -79.8(11) . . . . ? C13 C12 Se2 Pd2 -169.6(10) . . . . ? C21 C20 Se3 Pd3 73.1(12) . . . . ? C21 C20 Se3 Pd1 170.6(10) . . . . ? C1 C2 Pd1 C3 -148(3) . . . . ? C3 C2 Pd1 C1 148(3) . . . . ? C3 C2 Pd1 Se1 -27(2) . . . . ? C1 C2 Pd1 Se1 -174.7(11) . . . . ? C3 C2 Pd1 Se3 168.5(11) . . . . ? C1 C2 Pd1 Se3 20.9(19) . . . . ? C2 C3 Pd1 C1 -19.5(16) . . . . ? C2 C3 Pd1 Se1 160.4(15) . . . . ? C2 C3 Pd1 Se3 -38(4) . . . . ? C2 C1 Pd1 C3 19.4(15) . . . . ? C2 C1 Pd1 Se1 19(4) . . . . ? C2 C1 Pd1 Se3 -164.9(14) . . . . ? C4 Se1 Pd1 C2 22.2(11) . . . . ? Pd2 Se1 Pd1 C2 -81.0(10) . . . . ? C4 Se1 Pd1 C3 6.8(8) . . . . ? Pd2 Se1 Pd1 C3 -96.4(6) . . . . ? C4 Se1 Pd1 C1 7(3) . . . . ? Pd2 Se1 Pd1 C1 -96(3) . . . . ? C4 Se1 Pd1 Se3 -168.9(5) . . . . ? Pd2 Se1 Pd1 Se3 87.85(7) . . . . ? C20 Se3 Pd1 C2 -30.3(12) . . . . ? Pd3 Se3 Pd1 C2 77.7(10) . . . . ? C20 Se3 Pd1 C3 -1(3) . . . . ? Pd3 Se3 Pd1 C3 107(2) . . . . ? C20 Se3 Pd1 C1 -18.3(8) . . . . ? Pd3 Se3 Pd1 C1 89.7(6) . . . . ? C20 Se3 Pd1 Se1 160.8(6) . . . . ? Pd3 Se3 Pd1 Se1 -91.10(8) . . . . ? C10 C9 Pd2 C11 25.1(16) . . . . ? C10 C9 Pd2 Se2 45(4) . . . . ? C10 C9 Pd2 Se1 -156.7(16) . . . . ? C10 C11 Pd2 C9 -25.3(17) . . . . ? C10 C11 Pd2 Se2 159.5(16) . . . . ? C10 C11 Pd2 Se1 -34(4) . . . . ? C11 C10 Pd2 C9 139(3) . . . . ? C9 C10 Pd2 C11 -139(3) . . . . ? C11 C10 Pd2 Se2 -28(2) . . . . ? C9 C10 Pd2 Se2 -166.6(14) . . . . ? C11 C10 Pd2 Se1 170.9(11) . . . . ? C9 C10 Pd2 Se1 32(2) . . . . ? C12 Se2 Pd2 C9 4(3) . . . . ? Pd3 Se2 Pd2 C9 -104(3) . . . . ? C12 Se2 Pd2 C11 22.9(7) . . . . ? Pd3 Se2 Pd2 C11 -85.9(6) . . . . ? C12 Se2 Pd2 C10 39.2(10) . . . . ? Pd3 Se2 Pd2 C10 -69.6(9) . . . . ? C12 Se2 Pd2 Se1 -154.4(4) . . . . ? Pd3 Se2 Pd2 Se1 96.78(7) . . . . ? C4 Se1 Pd2 C9 -18.3(9) . . . . ? Pd1 Se1 Pd2 C9 89.8(7) . . . . ? C4 Se1 Pd2 C11 -10(3) . . . . ? Pd1 Se1 Pd2 C11 98(3) . . . . ? C4 Se1 Pd2 C10 -37.2(12) . . . . ? Pd1 Se1 Pd2 C10 70.9(10) . . . . ? C4 Se1 Pd2 Se2 156.6(5) . . . . ? Pd1 Se1 Pd2 Se2 -95.32(7) . . . . ? C19 C18 Pd3 C17 -163(3) . . . . ? C17 C18 Pd3 C19 163(3) . . . . ? C19 C18 Pd3 Se2 -171.2(12) . . . . ? C17 C18 Pd3 Se2 -9(2) . . . . ? C19 C18 Pd3 Se3 16(2) . . . . ? C17 C18 Pd3 Se3 178.2(12) . . . . ? C18 C17 Pd3 C19 -10.2(18) . . . . ? C18 C17 Pd3 Se2 174.1(17) . . . . ? C18 C17 Pd3 Se3 -6(4) . . . . ? C18 C19 Pd3 C17 10.6(19) . . . . ? C18 C19 Pd3 Se2 34(5) . . . . ? C18 C19 Pd3 Se3 -168.5(17) . . . . ? C12 Se2 Pd3 C18 -4.9(12) . . . . ? Pd2 Se2 Pd3 C18 97.9(11) . . . . ? C12 Se2 Pd3 C17 -9.8(7) . . . . ? Pd2 Se2 Pd3 C17 92.9(6) . . . . ? C12 Se2 Pd3 C19 -32(3) . . . . ? Pd2 Se2 Pd3 C19 71(3) . . . . ? C12 Se2 Pd3 Se3 170.2(4) . . . . ? Pd2 Se2 Pd3 Se3 -87.05(7) . . . . ? C20 Se3 Pd3 C18 11.1(12) . . . . ? Pd1 Se3 Pd3 C18 -95.9(11) . . . . ? C20 Se3 Pd3 C17 16(3) . . . . ? Pd1 Se3 Pd3 C17 -91(3) . . . . ? C20 Se3 Pd3 C19 19.7(8) . . . . ? Pd1 Se3 Pd3 C19 -87.3(6) . . . . ? C20 Se3 Pd3 Se2 -164.3(5) . . . . ? Pd1 Se3 Pd3 Se2 88.66(7) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.098 _refine_diff_density_min -1.190 _refine_diff_density_rms 0.207