# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Risto Laitinen' 'Tristram Chivers' 'Aino Eironen' 'Elisa Mannisto' 'Raija Oilunkaniemi' 'Maarit Risto' _publ_contact_author_name 'Risto Laitinen' _publ_contact_author_email RISTO.LAITINEN@OULU.FI _publ_section_title ; Palladium Complexes Containing Novel Cyclic Selenium Imides ; # Attachment 'cmpd1.cif' data_cmpd1 _database_code_depnum_ccdc_archive 'CCDC 733388' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (tert-butyl selenium dimide)dichloridopalladium ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H18 Cl2 N2 Pd Se' _chemical_formula_weight 398.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.399(3) _cell_length_b 11.096(2) _cell_length_c 18.280(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2717.8(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2660 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 25.99 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.948 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 4.406 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3515 _exptl_absorpt_correction_T_max 0.8792 _exptl_absorpt_process_details '(SHELXTL; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Nonius Kappaccd' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15052 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2660 _reflns_number_gt 2150 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (Altonare, et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Branderburg & Berndt, 1999)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0251P)^2^+4.5551P] 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 SHELXL _refine_ls_extinction_coef 0.00180(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2660 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0740 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 Pd1 Pd 0.19758(3) 0.25978(3) 0.40069(2) 0.01380(13) Uani 1 1 d . . . Se1 Se 0.37142(3) 0.40304(4) 0.43100(3) 0.01490(15) Uani 1 1 d . . . Cl1 Cl 0.04173(9) 0.23550(11) 0.45010(7) 0.0235(3) Uani 1 1 d . . . Cl2 Cl 0.15603(9) 0.12270(11) 0.31316(7) 0.0214(3) Uani 1 1 d . . . N1 N 0.2575(3) 0.3807(4) 0.4735(2) 0.0169(9) Uani 1 1 d . . . N2 N 0.3395(3) 0.2963(3) 0.3656(2) 0.0170(9) Uani 1 1 d . . . C11 C 0.2299(4) 0.4456(4) 0.5413(3) 0.0177(11) Uani 1 1 d . . . C12 C 0.1910(4) 0.3504(5) 0.5943(3) 0.0259(12) Uani 1 1 d . . . H12A H 0.2451 0.2945 0.6067 0.039 Uiso 1 1 calc R . . H12B H 0.1363 0.3057 0.5712 0.039 Uiso 1 1 calc R . . H12C H 0.1668 0.3896 0.6389 0.039 Uiso 1 1 calc R . . C13 C 0.3196(4) 0.5100(4) 0.5744(3) 0.0221(12) Uani 1 1 d . . . H13A H 0.3437 0.5714 0.5401 0.033 Uiso 1 1 calc R . . H13B H 0.3728 0.4514 0.5839 0.033 Uiso 1 1 calc R . . H13C H 0.2999 0.5486 0.6204 0.033 Uiso 1 1 calc R . . C14 C 0.1464(4) 0.5342(5) 0.5212(3) 0.0260(13) Uani 1 1 d . . . H14A H 0.1724 0.5948 0.4872 0.039 Uiso 1 1 calc R . . H14B H 0.1221 0.5741 0.5656 0.039 Uiso 1 1 calc R . . H14C H 0.0914 0.4903 0.4980 0.039 Uiso 1 1 calc R . . C21 C 0.4066(4) 0.2669(4) 0.3042(3) 0.0189(11) Uani 1 1 d . . . C22 C 0.3528(4) 0.3026(5) 0.2334(3) 0.0311(14) Uani 1 1 d . . . H22A H 0.2899 0.2580 0.2297 0.047 Uiso 1 1 calc R . . H22B H 0.3952 0.2831 0.1914 0.047 Uiso 1 1 calc R . . H22C H 0.3391 0.3893 0.2340 0.047 Uiso 1 1 calc R . . C23 C 0.5045(4) 0.3357(4) 0.3109(3) 0.0207(12) Uani 1 1 d . . . H23A H 0.5384 0.3121 0.3561 0.031 Uiso 1 1 calc R . . H23B H 0.4910 0.4225 0.3118 0.031 Uiso 1 1 calc R . . H23C H 0.5473 0.3167 0.2689 0.031 Uiso 1 1 calc R . . C24 C 0.4253(5) 0.1307(4) 0.3075(4) 0.0342(15) Uani 1 1 d . . . H24A H 0.3617 0.0878 0.3031 0.051 Uiso 1 1 calc R . . H24B H 0.4568 0.1102 0.3543 0.051 Uiso 1 1 calc R . . H24C H 0.4694 0.1070 0.2672 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0130(2) 0.0137(2) 0.0147(2) 0.00087(15) -0.00179(15) -0.00155(15) Se1 0.0140(2) 0.0154(3) 0.0153(3) -0.0014(2) -0.0002(2) -0.0017(2) Cl1 0.0146(6) 0.0280(7) 0.0279(7) 0.0018(5) 0.0021(5) -0.0034(5) Cl2 0.0244(7) 0.0205(7) 0.0194(7) -0.0020(5) -0.0047(5) -0.0068(5) N1 0.013(2) 0.018(2) 0.019(2) 0.0004(17) 0.0002(17) 0.0005(17) N2 0.019(2) 0.017(2) 0.016(2) 0.0027(17) 0.0000(18) 0.0002(17) C11 0.020(3) 0.011(2) 0.021(3) 0.000(2) 0.006(2) 0.005(2) C12 0.038(3) 0.024(3) 0.016(3) 0.001(2) 0.002(3) -0.009(2) C13 0.028(3) 0.018(3) 0.020(3) -0.005(2) 0.001(2) -0.005(2) C14 0.025(3) 0.022(3) 0.031(3) -0.002(2) 0.003(3) 0.003(2) C21 0.022(3) 0.020(3) 0.015(3) -0.002(2) 0.002(2) -0.002(2) C22 0.036(4) 0.043(3) 0.013(3) -0.003(2) 0.001(3) -0.014(3) C23 0.019(3) 0.019(3) 0.025(3) -0.001(2) 0.006(2) 0.003(2) C24 0.035(3) 0.016(3) 0.052(4) -0.012(3) 0.011(3) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 2.047(4) . ? Pd1 N1 2.053(4) . ? Pd1 Cl2 2.2767(13) . ? Pd1 Cl1 2.2912(13) . ? Pd1 Se1 2.8739(7) . ? Se1 N1 1.731(4) . ? Se1 N2 1.736(4) . ? N1 C11 1.480(6) . ? N2 C21 1.475(6) . ? C11 C12 1.524(7) . ? C11 C13 1.524(7) . ? C11 C14 1.534(7) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C21 C23 1.523(7) . ? C21 C22 1.532(7) . ? C21 C24 1.534(7) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 N2 Pd1 N1 73.18(16) . . ? N2 Pd1 Cl2 98.01(12) . . ? N1 Pd1 Cl2 171.01(11) . . ? N2 Pd1 Cl1 173.38(12) . . ? N1 Pd1 Cl1 100.23(11) . . ? Cl2 Pd1 Cl1 88.60(5) . . ? N2 Pd1 Se1 36.69(11) . . ? N1 Pd1 Se1 36.56(11) . . ? Cl2 Pd1 Se1 134.68(4) . . ? Cl1 Pd1 Se1 136.70(4) . . ? N1 Se1 N2 89.64(18) . . ? N1 Se1 Pd1 44.96(13) . . ? N2 Se1 Pd1 44.77(13) . . ? C11 N1 Se1 121.8(3) . . ? C11 N1 Pd1 139.7(3) . . ? Se1 N1 Pd1 98.47(18) . . ? C21 N2 Se1 121.6(3) . . ? C21 N2 Pd1 139.5(3) . . ? Se1 N2 Pd1 98.54(19) . . ? N1 C11 C12 106.3(4) . . ? N1 C11 C13 111.3(4) . . ? C12 C11 C13 110.0(4) . . ? N1 C11 C14 107.0(4) . . ? C12 C11 C14 110.4(4) . . ? C13 C11 C14 111.7(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C21 C23 110.7(4) . . ? N2 C21 C22 107.4(4) . . ? C23 C21 C22 110.1(4) . . ? N2 C21 C24 106.7(4) . . ? C23 C21 C24 110.4(4) . . ? C22 C21 C24 111.4(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? 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 N2 Pd1 Se1 N1 -175.4(3) . . . . ? Cl2 Pd1 Se1 N1 -176.85(19) . . . . ? Cl1 Pd1 Se1 N1 4.96(19) . . . . ? N1 Pd1 Se1 N2 175.4(3) . . . . ? Cl2 Pd1 Se1 N2 -1.48(19) . . . . ? Cl1 Pd1 Se1 N2 -179.67(19) . . . . ? N2 Se1 N1 C11 178.3(4) . . . . ? Pd1 Se1 N1 C11 -178.4(5) . . . . ? N2 Se1 N1 Pd1 -3.26(18) . . . . ? N2 Pd1 N1 C11 -179.2(5) . . . . ? Cl2 Pd1 N1 C11 -167.6(5) . . . . ? Cl1 Pd1 N1 C11 1.4(5) . . . . ? Se1 Pd1 N1 C11 177.9(6) . . . . ? N2 Pd1 N1 Se1 2.89(16) . . . . ? Cl2 Pd1 N1 Se1 14.5(9) . . . . ? Cl1 Pd1 N1 Se1 -176.55(13) . . . . ? N1 Se1 N2 C21 178.2(4) . . . . ? Pd1 Se1 N2 C21 174.9(4) . . . . ? N1 Se1 N2 Pd1 3.27(18) . . . . ? N1 Pd1 N2 C21 -176.2(5) . . . . ? Cl2 Pd1 N2 C21 5.6(5) . . . . ? Cl1 Pd1 N2 C21 -171.4(7) . . . . ? Se1 Pd1 N2 C21 -173.3(6) . . . . ? N1 Pd1 N2 Se1 -2.88(16) . . . . ? Cl2 Pd1 N2 Se1 178.94(13) . . . . ? Cl1 Pd1 N2 Se1 2.0(11) . . . . ? Se1 N1 C11 C12 -131.2(4) . . . . ? Pd1 N1 C11 C12 51.2(6) . . . . ? Se1 N1 C11 C13 -11.4(5) . . . . ? Pd1 N1 C11 C13 171.0(4) . . . . ? Se1 N1 C11 C14 110.9(4) . . . . ? Pd1 N1 C11 C14 -66.7(6) . . . . ? Se1 N2 C21 C23 3.7(5) . . . . ? Pd1 N2 C21 C23 175.9(4) . . . . ? Se1 N2 C21 C22 -116.6(4) . . . . ? Pd1 N2 C21 C22 55.7(6) . . . . ? Se1 N2 C21 C24 123.9(4) . . . . ? Pd1 N2 C21 C24 -63.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.667 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.145 # Attachment 'cmpd2.cif' data_cmpd2 _database_code_depnum_ccdc_archive 'CCDC 733389' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [tris(tert-butylimido)tetraselane)dichlorido- palladium-benzonitrile(1/1) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H27 Cl2 N3 Pd Se4, C7 H5 N' _chemical_formula_sum 'C19 H32 Cl2 N4 Pd Se4' _chemical_formula_weight 809.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.174(2) _cell_length_b 11.088(2) _cell_length_c 12.827(3) _cell_angle_alpha 71.65(3) _cell_angle_beta 86.40(3) _cell_angle_gamma 75.21(3) _cell_volume 1327.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5100 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.025 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 6.398 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2947 _exptl_absorpt_correction_T_max 0.5274 _exptl_absorpt_process_details '(SHELXTL; Bruker 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Nonius Kappaccd' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19036 _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5100 _reflns_number_gt 4127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (Altonare, et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Branderburg & Berndt, 1999)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0370P)^2^+8.5036P] 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 SHELXL _refine_ls_extinction_coef 0.0045(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5100 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 -0.01963(4) 0.13957(5) 0.90139(4) 0.02067(15) Uani 1 1 d . . . Se1 Se 0.21053(6) 0.14203(6) 0.89314(5) 0.02162(17) Uani 1 1 d . . . Se2 Se 0.06003(6) 0.04327(6) 0.76001(5) 0.02252(17) Uani 1 1 d . . . Se3 Se 0.10336(6) 0.30802(7) 0.58246(5) 0.02638(18) Uani 1 1 d . . . Se4 Se 0.04709(6) 0.40110(6) 0.72393(5) 0.02570(18) Uani 1 1 d . . . Cl1 Cl -0.04811(16) 0.22724(16) 1.04808(13) 0.0277(3) Uani 1 1 d . . . Cl2 Cl -0.24513(15) 0.12430(16) 0.90278(13) 0.0280(4) Uani 1 1 d . . . N1 N 0.2288(5) 0.0591(5) 0.7841(5) 0.0256(12) Uani 1 1 d . . . N2 N 0.0204(5) 0.1700(5) 0.6188(4) 0.0269(12) Uani 1 1 d . . . N3 N 0.1925(5) 0.3174(5) 0.8235(4) 0.0250(12) Uani 1 1 d . . . C1 C 0.3571(6) -0.0311(6) 0.7596(6) 0.0269(14) Uani 1 1 d . . . C2 C -0.1272(6) 0.2018(7) 0.5788(5) 0.0266(14) Uani 1 1 d . . . C3 C 0.3098(6) 0.3788(7) 0.8126(6) 0.0265(14) Uani 1 1 d . . . C11 C 0.4789(7) -0.0064(8) 0.8060(7) 0.0418(19) Uani 1 1 d . . . H11A H 0.4761 0.0873 0.7783 0.063 Uiso 1 1 calc R . . H11B H 0.5633 -0.0566 0.7831 0.063 Uiso 1 1 calc R . . H11C H 0.4756 -0.0340 0.8864 0.063 Uiso 1 1 calc R . . C12 C 0.3682(8) 0.0025(8) 0.6352(6) 0.0424(19) Uani 1 1 d . . . H12A H 0.2847 -0.0023 0.6043 0.064 Uiso 1 1 calc R . . H12B H 0.4460 -0.0601 0.6171 0.064 Uiso 1 1 calc R . . H12C H 0.3809 0.0915 0.6043 0.064 Uiso 1 1 calc R . . C13 C 0.3525(7) -0.1727(7) 0.8124(6) 0.0364(17) Uani 1 1 d . . . H13A H 0.3413 -0.1902 0.8918 0.055 Uiso 1 1 calc R . . H13B H 0.4375 -0.2305 0.7983 0.055 Uiso 1 1 calc R . . H13C H 0.2758 -0.1893 0.7812 0.055 Uiso 1 1 calc R . . C21 C -0.1237(7) 0.2369(7) 0.4541(6) 0.0340(16) Uani 1 1 d . . . H21A H -0.0914 0.3167 0.4235 0.051 Uiso 1 1 calc R . . H21B H -0.2153 0.2517 0.4251 0.051 Uiso 1 1 calc R . . H21C H -0.0621 0.1647 0.4334 0.051 Uiso 1 1 calc R . . C22 C -0.1816(7) 0.0792(7) 0.6259(6) 0.0307(15) Uani 1 1 d . . . H22A H -0.1213 0.0059 0.6058 0.046 Uiso 1 1 calc R . . H22B H -0.2731 0.0963 0.5960 0.046 Uiso 1 1 calc R . . H22C H -0.1850 0.0570 0.7061 0.046 Uiso 1 1 calc R . . C23 C -0.2184(6) 0.3168(7) 0.6130(6) 0.0287(15) Uani 1 1 d . . . H23A H -0.2182 0.2938 0.6933 0.043 Uiso 1 1 calc R . . H23B H -0.3115 0.3347 0.5857 0.043 Uiso 1 1 calc R . . H23C H -0.1835 0.3951 0.5817 0.043 Uiso 1 1 calc R . . C31 C 0.2532(7) 0.5163(7) 0.8229(6) 0.0345(16) Uani 1 1 d . . . H31A H 0.1928 0.5706 0.7599 0.052 Uiso 1 1 calc R . . H31B H 0.3285 0.5561 0.8244 0.052 Uiso 1 1 calc R . . H31C H 0.2021 0.5103 0.8909 0.052 Uiso 1 1 calc R . . C32 C 0.4096(7) 0.2994(7) 0.9092(6) 0.0299(15) Uani 1 1 d . . . H32A H 0.3612 0.2926 0.9785 0.045 Uiso 1 1 calc R . . H32B H 0.4822 0.3436 0.9071 0.045 Uiso 1 1 calc R . . H32C H 0.4492 0.2113 0.9035 0.045 Uiso 1 1 calc R . . C33 C 0.3801(7) 0.3879(8) 0.7021(6) 0.0352(17) Uani 1 1 d . . . H33A H 0.4189 0.2994 0.6972 0.053 Uiso 1 1 calc R . . H33B H 0.4528 0.4329 0.6963 0.053 Uiso 1 1 calc R . . H33C H 0.3135 0.4372 0.6421 0.053 Uiso 1 1 calc R . . N5 N 0.4926(7) 0.2995(7) 0.4780(5) 0.0437(16) Uani 1 1 d . . . C51 C 0.4179(7) 0.3218(7) 0.4060(6) 0.0333(16) Uani 1 1 d . . . C52 C 0.3282(6) 0.3464(7) 0.3156(5) 0.0266(14) Uani 1 1 d . . . C53 C 0.2524(7) 0.2571(7) 0.3184(6) 0.0316(15) Uani 1 1 d . . . H53 H 0.2567 0.1820 0.3809 0.038 Uiso 1 1 calc R . . C54 C 0.1711(7) 0.2796(7) 0.2286(6) 0.0352(16) Uani 1 1 d . . . H54 H 0.1196 0.2189 0.2295 0.042 Uiso 1 1 calc R . . C55 C 0.1633(7) 0.3885(7) 0.1378(6) 0.0324(16) Uani 1 1 d . . . H55 H 0.1065 0.4025 0.0769 0.039 Uiso 1 1 calc R . . C56 C 0.2388(7) 0.4784(7) 0.1353(6) 0.0318(16) Uani 1 1 d . . . H56 H 0.2342 0.5535 0.0728 0.038 Uiso 1 1 calc R . . C57 C 0.3206(6) 0.4563(7) 0.2253(6) 0.0275(15) Uani 1 1 d . . . H57 H 0.3718 0.5171 0.2248 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0164(2) 0.0201(3) 0.0234(3) -0.0041(2) 0.00174(18) -0.00434(18) Se1 0.0169(3) 0.0216(3) 0.0244(3) -0.0038(3) 0.0002(2) -0.0054(2) Se2 0.0222(3) 0.0199(3) 0.0239(3) -0.0042(3) -0.0006(2) -0.0056(2) Se3 0.0264(3) 0.0264(4) 0.0252(4) -0.0046(3) 0.0017(3) -0.0092(3) Se4 0.0224(3) 0.0241(4) 0.0287(4) -0.0066(3) -0.0014(3) -0.0041(3) Cl1 0.0304(8) 0.0256(8) 0.0250(8) -0.0068(7) 0.0030(6) -0.0052(7) Cl2 0.0166(7) 0.0326(9) 0.0306(9) -0.0040(7) 0.0019(6) -0.0064(6) N1 0.019(3) 0.028(3) 0.032(3) -0.014(3) 0.002(2) -0.005(2) N2 0.023(3) 0.029(3) 0.025(3) -0.003(2) -0.002(2) -0.006(2) N3 0.019(3) 0.026(3) 0.028(3) -0.005(2) 0.001(2) -0.007(2) C1 0.021(3) 0.023(3) 0.034(4) -0.011(3) 0.005(3) 0.002(3) C2 0.021(3) 0.031(4) 0.028(4) -0.007(3) -0.004(3) -0.007(3) C3 0.020(3) 0.030(4) 0.032(4) -0.009(3) -0.001(3) -0.011(3) C11 0.023(4) 0.040(5) 0.064(6) -0.022(4) 0.001(3) -0.002(3) C12 0.034(4) 0.046(5) 0.033(4) -0.008(4) 0.010(3) 0.008(3) C13 0.033(4) 0.025(4) 0.043(4) -0.009(3) 0.011(3) 0.001(3) C21 0.038(4) 0.038(4) 0.026(4) -0.008(3) -0.004(3) -0.011(3) C22 0.027(3) 0.032(4) 0.036(4) -0.013(3) -0.002(3) -0.009(3) C23 0.023(3) 0.028(4) 0.035(4) -0.010(3) -0.003(3) -0.004(3) C31 0.043(4) 0.033(4) 0.032(4) -0.013(3) 0.002(3) -0.013(3) C32 0.028(3) 0.031(4) 0.033(4) -0.009(3) -0.002(3) -0.012(3) C33 0.030(4) 0.053(5) 0.028(4) -0.013(4) 0.007(3) -0.023(3) N5 0.039(4) 0.059(5) 0.035(4) -0.015(3) -0.002(3) -0.014(3) C51 0.028(4) 0.041(4) 0.033(4) -0.012(3) 0.007(3) -0.014(3) C52 0.022(3) 0.032(4) 0.024(3) -0.007(3) 0.000(3) -0.007(3) C53 0.039(4) 0.032(4) 0.023(4) -0.006(3) -0.002(3) -0.011(3) C54 0.034(4) 0.035(4) 0.039(4) -0.012(3) 0.005(3) -0.011(3) C55 0.024(3) 0.043(4) 0.029(4) -0.012(3) -0.003(3) -0.004(3) C56 0.028(4) 0.025(4) 0.034(4) -0.001(3) 0.003(3) -0.002(3) C57 0.020(3) 0.027(4) 0.036(4) -0.010(3) 0.001(3) -0.008(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 Cl2 2.3417(16) . ? Pd1 Se1 2.3439(8) . ? Pd1 Cl1 2.3471(17) . ? Pd1 Se2 2.3830(10) . ? Se1 N3 1.833(5) . ? Se1 N1 1.879(5) . ? Se2 N1 1.825(5) . ? Se2 N2 1.902(6) . ? Se3 N2 1.853(6) . ? Se3 Se4 2.3307(11) . ? Se4 N3 1.863(5) . ? N1 C1 1.510(8) . ? N2 C2 1.535(8) . ? N3 C3 1.497(8) . ? C1 C13 1.514(10) . ? C1 C12 1.523(10) . ? C1 C11 1.529(9) . ? C2 C21 1.523(9) . ? C2 C22 1.530(9) . ? C2 C23 1.542(9) . ? C3 C31 1.531(9) . ? C3 C33 1.533(9) . ? C3 C32 1.534(9) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? N5 C51 1.158(9) . ? C51 C52 1.435(9) . ? C52 C57 1.381(10) . ? C52 C53 1.393(9) . ? C53 C54 1.380(10) . ? C53 H53 0.9500 . ? C54 C55 1.378(11) . ? C54 H54 0.9500 . ? C55 C56 1.397(10) . ? C55 H55 0.9500 . ? C56 C57 1.387(10) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? 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 Cl2 Pd1 Se1 175.48(5) . . ? Cl2 Pd1 Cl1 94.06(6) . . ? Se1 Pd1 Cl1 90.10(5) . . ? Cl2 Pd1 Se2 97.91(5) . . ? Se1 Pd1 Se2 77.85(4) . . ? Cl1 Pd1 Se2 167.66(5) . . ? N3 Se1 N1 107.4(2) . . ? N3 Se1 Pd1 99.06(16) . . ? N1 Se1 Pd1 87.69(16) . . ? N1 Se2 N2 99.5(2) . . ? N1 Se2 Pd1 87.76(16) . . ? N2 Se2 Pd1 110.95(17) . . ? N2 Se3 Se4 104.57(17) . . ? N3 Se4 Se3 103.93(17) . . ? C1 N1 Se2 122.1(4) . . ? C1 N1 Se1 125.9(4) . . ? Se2 N1 Se1 106.6(3) . . ? C2 N2 Se3 116.8(4) . . ? C2 N2 Se2 114.5(4) . . ? Se3 N2 Se2 117.6(3) . . ? C3 N3 Se1 121.8(4) . . ? C3 N3 Se4 118.4(4) . . ? Se1 N3 Se4 116.0(3) . . ? N1 C1 C13 110.1(5) . . ? N1 C1 C12 107.8(5) . . ? C13 C1 C12 111.4(6) . . ? N1 C1 C11 108.7(5) . . ? C13 C1 C11 109.4(6) . . ? C12 C1 C11 109.3(6) . . ? C21 C2 C22 109.2(5) . . ? C21 C2 N2 106.6(5) . . ? C22 C2 N2 108.9(5) . . ? C21 C2 C23 110.3(6) . . ? C22 C2 C23 110.1(5) . . ? N2 C2 C23 111.8(5) . . ? N3 C3 C31 107.1(5) . . ? N3 C3 C33 111.9(5) . . ? C31 C3 C33 109.9(6) . . ? N3 C3 C32 108.7(5) . . ? C31 C3 C32 107.8(5) . . ? C33 C3 C32 111.3(5) . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C12 H12A 109.5 . . ? C1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C2 C22 H22A 109.5 . . ? C2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C2 C23 H23A 109.5 . . ? C2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C3 C31 H31A 109.5 . . ? C3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C3 C32 H32A 109.5 . . ? C3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C3 C33 H33A 109.5 . . ? C3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N5 C51 C52 178.2(8) . . ? C57 C52 C53 120.6(6) . . ? C57 C52 C51 119.8(6) . . ? C53 C52 C51 119.6(6) . . ? C54 C53 C52 118.8(7) . . ? C54 C53 H53 120.6 . . ? C52 C53 H53 120.6 . . ? C55 C54 C53 121.2(7) . . ? C55 C54 H54 119.4 . . ? C53 C54 H54 119.4 . . ? C54 C55 C56 120.0(6) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C57 C56 C55 119.0(7) . . ? C57 C56 H56 120.5 . . ? C55 C56 H56 120.5 . . ? C52 C57 C56 120.4(6) . . ? C52 C57 H57 119.8 . . ? C56 C57 H57 119.8 . . ? 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 Cl2 Pd1 Se1 N3 125.7(6) . . . . ? Cl1 Pd1 Se1 N3 -77.12(18) . . . . ? Se2 Pd1 Se1 N3 105.57(17) . . . . ? Cl2 Pd1 Se1 N1 18.4(7) . . . . ? Cl1 Pd1 Se1 N1 175.63(18) . . . . ? Se2 Pd1 Se1 N1 -1.68(18) . . . . ? Cl2 Pd1 Se2 N1 -176.70(18) . . . . ? Se1 Pd1 Se2 N1 1.73(18) . . . . ? Cl1 Pd1 Se2 N1 -10.9(3) . . . . ? Cl2 Pd1 Se2 N2 83.97(18) . . . . ? Se1 Pd1 Se2 N2 -97.60(17) . . . . ? Cl1 Pd1 Se2 N2 -110.3(3) . . . . ? N2 Se3 Se4 N3 93.2(2) . . . . ? N2 Se2 N1 C1 -95.9(5) . . . . ? Pd1 Se2 N1 C1 153.2(5) . . . . ? N2 Se2 N1 Se1 108.7(3) . . . . ? Pd1 Se2 N1 Se1 -2.2(2) . . . . ? N3 Se1 N1 C1 109.2(5) . . . . ? Pd1 Se1 N1 C1 -152.0(5) . . . . ? N3 Se1 N1 Se2 -96.5(3) . . . . ? Pd1 Se1 N1 Se2 2.2(2) . . . . ? Se4 Se3 N2 C2 87.5(4) . . . . ? Se4 Se3 N2 Se2 -54.6(3) . . . . ? N1 Se2 N2 C2 -170.0(4) . . . . ? Pd1 Se2 N2 C2 -78.7(4) . . . . ? N1 Se2 N2 Se3 -27.0(3) . . . . ? Pd1 Se2 N2 Se3 64.2(3) . . . . ? N1 Se1 N3 C3 -99.6(5) . . . . ? Pd1 Se1 N3 C3 170.0(4) . . . . ? N1 Se1 N3 Se4 58.2(3) . . . . ? Pd1 Se1 N3 Se4 -32.2(3) . . . . ? Se3 Se4 N3 C3 91.2(4) . . . . ? Se3 Se4 N3 Se1 -67.3(3) . . . . ? Se2 N1 C1 C13 -51.0(7) . . . . ? Se1 N1 C1 C13 99.6(6) . . . . ? Se2 N1 C1 C12 70.8(7) . . . . ? Se1 N1 C1 C12 -138.7(5) . . . . ? Se2 N1 C1 C11 -170.8(5) . . . . ? Se1 N1 C1 C11 -20.3(8) . . . . ? Se3 N2 C2 C21 67.7(6) . . . . ? Se2 N2 C2 C21 -149.1(5) . . . . ? Se3 N2 C2 C22 -174.6(4) . . . . ? Se2 N2 C2 C22 -31.4(6) . . . . ? Se3 N2 C2 C23 -52.9(6) . . . . ? Se2 N2 C2 C23 90.4(6) . . . . ? Se1 N3 C3 C31 -144.1(5) . . . . ? Se4 N3 C3 C31 58.7(6) . . . . ? Se1 N3 C3 C33 95.5(6) . . . . ? Se4 N3 C3 C33 -61.7(7) . . . . ? Se1 N3 C3 C32 -27.9(7) . . . . ? Se4 N3 C3 C32 174.9(4) . . . . ? N5 C51 C52 C57 -104(27) . . . . ? N5 C51 C52 C53 74(27) . . . . ? C57 C52 C53 C54 0.8(10) . . . . ? C51 C52 C53 C54 -177.3(7) . . . . ? C52 C53 C54 C55 -0.5(11) . . . . ? C53 C54 C55 C56 0.2(11) . . . . ? C54 C55 C56 C57 -0.3(10) . . . . ? C53 C52 C57 C56 -0.9(10) . . . . ? C51 C52 C57 C56 177.2(6) . . . . ? C55 C56 C57 C52 0.6(10) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.950 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.163 # Attachment 'cmpd3.cif' data_cmpd3 _database_code_depnum_ccdc_archive 'CCDC 733390' _audit_creation_method SHELXL-97 _chemical_name_systematic ; {tetrakis(tert-butylimido)tetraselane}dichlorido- palladium ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H36 Cl2 N4 Pd Se4' _chemical_formula_sum 'C16 H36 Cl2 N4 Pd Se4' _chemical_formula_weight 777.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 26.816(5) _cell_length_b 9.7383(19) _cell_length_c 20.082(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.16(3) _cell_angle_gamma 90.00 _cell_volume 5106.4(18) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4892 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 25.99 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 6.649 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.477 _exptl_absorpt_correction_T_max 0.587 _exptl_absorpt_process_details '(SHELXTL (Bruker 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Nonius Kappaccd' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14480 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4892 _reflns_number_gt 4186 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (Altonare, et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Branderburg & Berndt, 1999)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0579P)^2^+5.6758P] 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 SHELXL _refine_ls_extinction_coef 0.00230(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4892 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1111 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _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 0.212543(14) 0.69882(4) 0.07527(2) 0.01504(14) Uani 1 1 d . . . Se1 Se 0.127517(19) 0.78748(5) 0.03846(3) 0.01668(16) Uani 1 1 d . . . Se2 Se 0.153595(19) 0.60361(5) -0.07134(3) 0.01686(16) Uani 1 1 d . . . Se3 Se 0.195613(19) 0.45802(5) 0.06475(3) 0.01530(16) Uani 1 1 d . . . Se4 Se 0.085097(19) 0.51371(6) 0.08964(3) 0.01781(16) Uani 1 1 d . . . Cl1 Cl 0.23230(5) 0.93306(13) 0.08958(7) 0.0212(3) Uani 1 1 d . . . Cl2 Cl 0.29570(5) 0.62237(13) 0.12569(7) 0.0214(3) Uani 1 1 d . . . N1 N 0.10074(17) 0.6915(5) -0.0407(2) 0.0193(10) Uani 1 1 d . . . N2 N 0.15415(17) 0.4433(4) -0.0218(2) 0.0183(9) Uani 1 1 d . . . N3 N 0.14658(17) 0.4197(5) 0.1154(2) 0.0199(10) Uani 1 1 d . . . N4 N 0.09126(17) 0.7020(5) 0.0973(2) 0.0204(10) Uani 1 1 d . . . C1 C 0.0541(2) 0.7508(6) -0.0898(3) 0.0211(12) Uani 1 1 d . . . C2 C 0.1435(2) 0.3046(5) -0.0556(3) 0.0192(11) Uani 1 1 d . . . C4 C 0.0883(2) 0.7881(6) 0.1594(3) 0.0246(13) Uani 1 1 d . . . C3 C 0.1680(2) 0.3679(6) 0.1881(3) 0.0211(12) Uani 1 1 d . . . C11 C 0.0338(2) 0.6417(7) -0.1427(3) 0.0272(13) Uani 1 1 d . . . H11A H 0.0598 0.6202 -0.1684 0.041 Uiso 1 1 calc R . . H11B H 0.0028 0.6756 -0.1742 0.041 Uiso 1 1 calc R . . H11C H 0.0256 0.5586 -0.1198 0.041 Uiso 1 1 calc R . . C12 C 0.0136(2) 0.7830(6) -0.0503(3) 0.0263(13) Uani 1 1 d . . . H12A H 0.0054 0.6995 -0.0277 0.039 Uiso 1 1 calc R . . H12B H -0.0174 0.8168 -0.0819 0.039 Uiso 1 1 calc R . . H12C H 0.0265 0.8533 -0.0158 0.039 Uiso 1 1 calc R . . C13 C 0.0683(2) 0.8792(7) -0.1245(3) 0.0319(14) Uani 1 1 d . . . H13A H 0.0805 0.9501 -0.0900 0.048 Uiso 1 1 calc R . . H13B H 0.0381 0.9132 -0.1576 0.048 Uiso 1 1 calc R . . H13C H 0.0954 0.8572 -0.1484 0.048 Uiso 1 1 calc R . . C21 C 0.1797(3) 0.2824(7) -0.1027(4) 0.0406(17) Uani 1 1 d . . . H21A H 0.1734 0.3526 -0.1387 0.061 Uiso 1 1 calc R . . H21B H 0.1739 0.1911 -0.1236 0.061 Uiso 1 1 calc R . . H21C H 0.2152 0.2893 -0.0764 0.061 Uiso 1 1 calc R . . C22 C 0.1506(3) 0.1923(6) -0.0024(4) 0.0415(17) Uani 1 1 d . . . H22A H 0.1862 0.1918 0.0239 0.062 Uiso 1 1 calc R . . H22B H 0.1424 0.1033 -0.0251 0.062 Uiso 1 1 calc R . . H22C H 0.1277 0.2088 0.0285 0.062 Uiso 1 1 calc R . . C23 C 0.0881(2) 0.3052(7) -0.0961(4) 0.0350(15) Uani 1 1 d . . . H23A H 0.0655 0.3284 -0.0657 0.052 Uiso 1 1 calc R . . H23B H 0.0792 0.2141 -0.1160 0.052 Uiso 1 1 calc R . . H23C H 0.0840 0.3735 -0.1328 0.052 Uiso 1 1 calc R . . C31 C 0.2076(3) 0.2569(8) 0.1862(4) 0.0449(19) Uani 1 1 d . . . H31A H 0.2147 0.2061 0.2295 0.067 Uiso 1 1 calc R . . H31B H 0.2393 0.2995 0.1797 0.067 Uiso 1 1 calc R . . H31C H 0.1944 0.1937 0.1484 0.067 Uiso 1 1 calc R . . C32 C 0.1245(3) 0.3049(8) 0.2136(4) 0.0445(19) Uani 1 1 d . . . H32A H 0.1379 0.2625 0.2584 0.067 Uiso 1 1 calc R . . H32B H 0.1076 0.2349 0.1812 0.067 Uiso 1 1 calc R . . H32C H 0.0997 0.3765 0.2179 0.067 Uiso 1 1 calc R . . C33 C 0.1929(3) 0.4831(8) 0.2347(4) 0.0447(18) Uani 1 1 d . . . H33A H 0.1666 0.5482 0.2413 0.067 Uiso 1 1 calc R . . H33B H 0.2178 0.5305 0.2139 0.067 Uiso 1 1 calc R . . H33C H 0.2104 0.4449 0.2790 0.067 Uiso 1 1 calc R . . C41 C 0.0616(3) 0.7060(7) 0.2051(3) 0.0347(15) Uani 1 1 d . . . H41A H 0.0284 0.6736 0.1784 0.052 Uiso 1 1 calc R . . H41B H 0.0562 0.7644 0.2426 0.052 Uiso 1 1 calc R . . H41C H 0.0828 0.6271 0.2240 0.052 Uiso 1 1 calc R . . C42 C 0.0543(3) 0.9128(7) 0.1319(3) 0.0353(15) Uani 1 1 d . . . H42A H 0.0703 0.9658 0.1009 0.053 Uiso 1 1 calc R . . H42B H 0.0506 0.9711 0.1702 0.053 Uiso 1 1 calc R . . H42C H 0.0205 0.8808 0.1072 0.053 Uiso 1 1 calc R . . C43 C 0.1407(2) 0.8390(7) 0.1984(3) 0.0320(14) Uani 1 1 d . . . H43A H 0.1636 0.7603 0.2120 0.048 Uiso 1 1 calc R . . H43B H 0.1370 0.8892 0.2392 0.048 Uiso 1 1 calc R . . H43C H 0.1553 0.9000 0.1689 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0120(2) 0.0141(2) 0.0182(2) -0.00027(15) 0.00179(17) 0.00011(14) Se1 0.0136(3) 0.0152(3) 0.0205(3) 0.0000(2) 0.0024(2) 0.00164(19) Se2 0.0170(3) 0.0164(3) 0.0175(3) 0.0022(2) 0.0047(2) 0.0017(2) Se3 0.0134(3) 0.0143(3) 0.0176(3) 0.0007(2) 0.0022(2) 0.00061(19) Se4 0.0135(3) 0.0196(3) 0.0199(3) 0.0017(2) 0.0029(2) -0.0004(2) Cl1 0.0180(6) 0.0152(6) 0.0291(7) -0.0022(5) 0.0024(5) -0.0003(5) Cl2 0.0133(6) 0.0203(7) 0.0283(7) 0.0006(6) -0.0004(5) 0.0006(5) N1 0.015(2) 0.021(2) 0.020(2) -0.0002(19) 0.0005(19) 0.0023(18) N2 0.027(2) 0.012(2) 0.013(2) -0.0005(18) -0.0018(19) 0.0009(18) N3 0.021(2) 0.021(2) 0.018(2) 0.0052(19) 0.0035(19) 0.0030(19) N4 0.021(2) 0.017(2) 0.023(3) 0.0025(19) 0.005(2) 0.0041(18) C1 0.015(3) 0.024(3) 0.024(3) 0.004(2) 0.003(2) 0.007(2) C2 0.024(3) 0.014(3) 0.018(3) -0.003(2) 0.002(2) 0.000(2) C4 0.025(3) 0.028(3) 0.021(3) -0.005(2) 0.006(2) 0.005(2) C3 0.022(3) 0.025(3) 0.015(3) 0.002(2) 0.002(2) 0.002(2) C11 0.022(3) 0.034(3) 0.023(3) 0.001(3) -0.002(2) 0.001(3) C12 0.016(3) 0.034(3) 0.027(3) 0.004(3) 0.001(2) 0.004(2) C13 0.024(3) 0.032(3) 0.034(4) 0.012(3) -0.004(3) -0.001(3) C21 0.052(4) 0.027(3) 0.049(4) -0.015(3) 0.023(4) -0.001(3) C22 0.064(5) 0.021(3) 0.029(4) -0.004(3) -0.010(3) -0.002(3) C23 0.030(3) 0.030(4) 0.039(4) -0.007(3) -0.004(3) -0.003(3) C31 0.056(5) 0.054(5) 0.025(3) 0.012(3) 0.012(3) 0.031(4) C32 0.035(4) 0.063(5) 0.038(4) 0.029(4) 0.013(3) 0.000(3) C33 0.058(5) 0.038(4) 0.028(4) 0.003(3) -0.011(3) -0.002(3) C41 0.043(4) 0.036(4) 0.030(4) -0.008(3) 0.020(3) -0.003(3) C42 0.039(4) 0.032(4) 0.035(4) -0.003(3) 0.009(3) 0.019(3) C43 0.030(3) 0.034(4) 0.029(3) -0.013(3) 0.000(3) 0.001(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 Cl1 2.3446(14) . ? Pd1 Cl2 2.3502(14) . ? Pd1 Se3 2.3887(8) . ? Pd1 Se1 2.3923(8) . ? Se1 N1 1.842(5) . ? Se1 N4 1.886(4) . ? Se2 N2 1.849(4) . ? Se2 N1 1.876(4) . ? Se3 N2 1.844(4) . ? Se3 N3 1.873(4) . ? Se4 N4 1.845(5) . ? Se4 N3 1.853(4) . ? N1 C1 1.519(7) . ? N2 C2 1.509(7) . ? N3 C3 1.528(7) . ? N4 C4 1.519(7) . ? C1 C11 1.514(8) . ? C1 C12 1.519(8) . ? C1 C13 1.522(8) . ? C2 C22 1.509(8) . ? C2 C21 1.517(8) . ? C2 C23 1.524(8) . ? C4 C41 1.516(8) . ? C4 C43 1.527(8) . ? C4 C42 1.543(8) . ? C3 C32 1.508(8) . ? C3 C33 1.515(9) . ? C3 C31 1.522(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pd1 Cl2 95.14(5) . . ? Cl1 Pd1 Se3 177.45(4) . . ? Cl2 Pd1 Se3 82.51(4) . . ? Cl1 Pd1 Se1 81.93(4) . . ? Cl2 Pd1 Se1 172.51(4) . . ? Se3 Pd1 Se1 100.28(2) . . ? N1 Se1 N4 99.3(2) . . ? N1 Se1 Pd1 103.89(14) . . ? N4 Se1 Pd1 103.78(14) . . ? N2 Se2 N1 97.0(2) . . ? N2 Se3 N3 98.6(2) . . ? N2 Se3 Pd1 102.78(14) . . ? N3 Se3 Pd1 106.87(14) . . ? N4 Se4 N3 114.2(2) . . ? C1 N1 Se1 118.0(3) . . ? C1 N1 Se2 122.1(3) . . ? Se1 N1 Se2 109.8(2) . . ? C2 N2 Se3 120.3(3) . . ? C2 N2 Se2 122.5(3) . . ? Se3 N2 Se2 111.8(2) . . ? C3 N3 Se4 123.2(3) . . ? C3 N3 Se3 115.2(3) . . ? Se4 N3 Se3 116.1(2) . . ? C4 N4 Se4 126.6(4) . . ? C4 N4 Se1 113.6(3) . . ? Se4 N4 Se1 115.8(2) . . ? C11 C1 C12 108.9(5) . . ? C11 C1 N1 107.5(4) . . ? C12 C1 N1 108.7(4) . . ? C11 C1 C13 110.1(5) . . ? C12 C1 C13 110.7(5) . . ? N1 C1 C13 110.9(4) . . ? N2 C2 C22 110.5(5) . . ? N2 C2 C21 109.0(4) . . ? C22 C2 C21 110.1(5) . . ? N2 C2 C23 107.3(4) . . ? C22 C2 C23 109.3(5) . . ? C21 C2 C23 110.5(5) . . ? C41 C4 N4 109.1(5) . . ? C41 C4 C43 111.5(5) . . ? N4 C4 C43 112.7(4) . . ? C41 C4 C42 108.0(5) . . ? N4 C4 C42 106.1(5) . . ? C43 C4 C42 109.1(5) . . ? C32 C3 C33 110.9(6) . . ? C32 C3 C31 108.5(6) . . ? C33 C3 C31 109.2(6) . . ? C32 C3 N3 107.9(5) . . ? C33 C3 N3 111.3(5) . . ? C31 C3 N3 108.9(4) . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C12 H12A 109.5 . . ? C1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C2 C22 H22A 109.5 . . ? C2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C2 C23 H23A 109.5 . . ? C2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C3 C31 H31A 109.5 . . ? C3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C3 C32 H32A 109.5 . . ? C3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C3 C33 H33A 109.5 . . ? C3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 C42 H42A 109.5 . . ? C4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C4 C43 H43A 109.5 . . ? C4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? 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 Cl1 Pd1 Se1 N1 133.85(15) . . . . ? Cl2 Pd1 Se1 N1 -158.7(3) . . . . ? Se3 Pd1 Se1 N1 -47.44(15) . . . . ? Cl1 Pd1 Se1 N4 -122.76(15) . . . . ? Cl2 Pd1 Se1 N4 -55.4(3) . . . . ? Se3 Pd1 Se1 N4 55.95(15) . . . . ? Cl1 Pd1 Se3 N2 -161.2(9) . . . . ? Cl2 Pd1 Se3 N2 -138.11(15) . . . . ? Se1 Pd1 Se3 N2 48.93(14) . . . . ? Cl1 Pd1 Se3 N3 95.6(9) . . . . ? Cl2 Pd1 Se3 N3 118.68(15) . . . . ? Se1 Pd1 Se3 N3 -54.28(15) . . . . ? N4 Se1 N1 C1 92.2(4) . . . . ? Pd1 Se1 N1 C1 -161.0(3) . . . . ? N4 Se1 N1 Se2 -121.5(2) . . . . ? Pd1 Se1 N1 Se2 -14.7(2) . . . . ? N2 Se2 N1 C1 -127.3(4) . . . . ? N2 Se2 N1 Se1 88.1(2) . . . . ? N3 Se3 N2 C2 -83.7(4) . . . . ? Pd1 Se3 N2 C2 166.7(3) . . . . ? N3 Se3 N2 Se2 121.8(2) . . . . ? Pd1 Se3 N2 Se2 12.2(2) . . . . ? N1 Se2 N2 C2 119.4(4) . . . . ? N1 Se2 N2 Se3 -86.8(3) . . . . ? N4 Se4 N3 C3 91.3(4) . . . . ? N4 Se4 N3 Se3 -61.2(3) . . . . ? N2 Se3 N3 C3 157.6(4) . . . . ? Pd1 Se3 N3 C3 -96.2(4) . . . . ? N2 Se3 N3 Se4 -47.7(3) . . . . ? Pd1 Se3 N3 Se4 58.5(3) . . . . ? N3 Se4 N4 C4 -90.6(5) . . . . ? N3 Se4 N4 Se1 65.6(3) . . . . ? N1 Se1 N4 C4 -158.4(4) . . . . ? Pd1 Se1 N4 C4 94.8(3) . . . . ? N1 Se1 N4 Se4 42.4(3) . . . . ? Pd1 Se1 N4 Se4 -64.5(3) . . . . ? Se1 N1 C1 C11 -169.3(3) . . . . ? Se2 N1 C1 C11 48.8(5) . . . . ? Se1 N1 C1 C12 -51.5(5) . . . . ? Se2 N1 C1 C12 166.6(4) . . . . ? Se1 N1 C1 C13 70.3(5) . . . . ? Se2 N1 C1 C13 -71.5(6) . . . . ? Se3 N2 C2 C22 24.0(6) . . . . ? Se2 N2 C2 C22 175.7(4) . . . . ? Se3 N2 C2 C21 -97.2(5) . . . . ? Se2 N2 C2 C21 54.6(6) . . . . ? Se3 N2 C2 C23 143.1(4) . . . . ? Se2 N2 C2 C23 -65.2(5) . . . . ? Se4 N4 C4 C41 -19.7(7) . . . . ? Se1 N4 C4 C41 -176.3(4) . . . . ? Se4 N4 C4 C43 104.8(5) . . . . ? Se1 N4 C4 C43 -51.8(6) . . . . ? Se4 N4 C4 C42 -135.8(4) . . . . ? Se1 N4 C4 C42 67.6(5) . . . . ? Se4 N3 C3 C32 43.2(6) . . . . ? Se3 N3 C3 C32 -164.1(4) . . . . ? Se4 N3 C3 C33 -78.7(6) . . . . ? Se3 N3 C3 C33 74.0(5) . . . . ? Se4 N3 C3 C31 160.9(5) . . . . ? Se3 N3 C3 C31 -46.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.202 _refine_diff_density_min -1.157 _refine_diff_density_rms 0.307