# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sk1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H44 Cl4 Pd2 Se2' _chemical_formula_weight 989.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P -1' _symmetry_cell_setting triclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5654(5) _cell_length_b 11.1973(8) _cell_length_c 11.5045(6) _cell_angle_alpha 110.442(6) _cell_angle_beta 97.754(5) _cell_angle_gamma 109.719(6) _cell_volume 932.46(12) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4119 _cell_measurement_theta_min 4.2772 _cell_measurement_theta_max 66.4884 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 12.829 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3082 _exptl_absorpt_correction_T_max 0.7834 _exptl_absorpt_process_details ; R.H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2413 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13045 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.28 _diffrn_reflns_theta_max 66.60 _reflns_number_total 3294 _reflns_number_gt 2746 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.8 (release 13-04-2012 CrysAlis171 .NET) (compiled Apr 13 2012,18:42:44) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.8 (release 13-04-2012 CrysAlis171 .NET) (compiled Apr 13 2012,18:42:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.8 (release 13-04-2012 CrysAlis171 .NET) (compiled Apr 13 2012,18:42:44) ; _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ortep 3 for windows' _computing_publication_material 'WinGX 1.70.1' _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^)+(0.0315P)^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 3294 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0676 _refine_ls_wR_factor_gt 0.0631 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 C1 C 0.0605(5) 0.3099(4) 0.4599(4) 0.0174(8) Uani 1 1 d . . . C2 C -0.0130(5) 0.3550(4) 0.5598(4) 0.0182(8) Uani 1 1 d . . . C3 C 0.0844(5) 0.4019(4) 0.6858(4) 0.0207(9) Uani 1 1 d . . . H3 H 0.0359 0.4314 0.7544 0.025 Uiso 1 1 calc R . . C4 C 0.2505(5) 0.4076(4) 0.7160(4) 0.0213(9) Uani 1 1 d . . . C5 C 0.3199(5) 0.3681(4) 0.6157(4) 0.0194(8) Uani 1 1 d . . . H5 H 0.4348 0.3748 0.6358 0.023 Uiso 1 1 calc R . . C6 C 0.2300(5) 0.3181(4) 0.4850(4) 0.0185(8) Uani 1 1 d . . . C7 C 0.3181(5) 0.2750(5) 0.3837(4) 0.0304(10) Uani 1 1 d . . . H7A H 0.4318 0.2840 0.4251 0.046 Uiso 1 1 calc R . . H7B H 0.3327 0.3354 0.3379 0.046 Uiso 1 1 calc R . . H7C H 0.2474 0.1774 0.3219 0.046 Uiso 1 1 calc R . . C8 C -0.1924(5) 0.3516(4) 0.5361(4) 0.0219(9) Uani 1 1 d . . . H8A H -0.2785 0.2555 0.5072 0.033 Uiso 1 1 calc R . . H8B H -0.2113 0.3847 0.4692 0.033 Uiso 1 1 calc R . . H8C H -0.2041 0.4125 0.6164 0.033 Uiso 1 1 calc R . . C9 C 0.3491(5) 0.4530(4) 0.8539(4) 0.0264(9) Uani 1 1 d . . . H9A H 0.3359 0.3702 0.8700 0.040 Uiso 1 1 calc R . . H9B H 0.3035 0.5100 0.9132 0.040 Uiso 1 1 calc R . . H9C H 0.4720 0.5084 0.8683 0.040 Uiso 1 1 calc R . . C10 C -0.2905(5) 0.1010(4) 0.2607(4) 0.0168(8) Uani 1 1 d . . . C11 C -0.4385(5) 0.1005(4) 0.1912(3) 0.0174(8) Uani 1 1 d . . . C12 C -0.5965(5) -0.0080(4) 0.1652(4) 0.0210(9) Uani 1 1 d . . . H12 H -0.6981 -0.0110 0.1170 0.025 Uiso 1 1 calc R . . C13 C -0.6114(5) -0.1131(4) 0.2075(4) 0.0231(9) Uani 1 1 d . . . C14 C -0.4600(5) -0.1067(4) 0.2766(4) 0.0252(9) Uani 1 1 d . . . H14 H -0.4679 -0.1770 0.3065 0.030 Uiso 1 1 calc R . . C15 C -0.2978(5) -0.0020(4) 0.3038(4) 0.0194(8) Uani 1 1 d . . . C16 C -0.4319(5) 0.2117(4) 0.1453(4) 0.0219(9) Uani 1 1 d . . . H16A H -0.5479 0.1883 0.0943 0.033 Uiso 1 1 calc R . . H16B H -0.3526 0.2173 0.0915 0.033 Uiso 1 1 calc R . . H16C H -0.3908 0.3022 0.2202 0.033 Uiso 1 1 calc R . . C17 C -0.7835(6) -0.2286(5) 0.1787(5) 0.0410(12) Uani 1 1 d . . . H17A H -0.7662 -0.3046 0.1940 0.061 Uiso 1 1 calc R . . H17B H -0.8483 -0.2640 0.0880 0.061 Uiso 1 1 calc R . . H17C H -0.8486 -0.1928 0.2351 0.061 Uiso 1 1 calc R . . C18 C -0.1424(5) -0.0058(4) 0.3795(4) 0.0244(9) Uani 1 1 d . . . H18A H -0.1123 0.0577 0.4710 0.037 Uiso 1 1 calc R . . H18B H -0.0443 0.0237 0.3455 0.037 Uiso 1 1 calc R . . H18C H -0.1700 -0.1014 0.3711 0.037 Uiso 1 1 calc R . . Cl1 Cl 0.10980(12) 0.07304(9) -0.07527(9) 0.0206(2) Uani 1 1 d . . . Cl2 Cl 0.16706(13) 0.38532(10) 0.13728(10) 0.0262(2) Uani 1 1 d . . . Se1 Se -0.07890(5) 0.25739(4) 0.28717(4) 0.01586(11) Uani 1 1 d . . . Pd1 Pd 0.02805(3) 0.16098(3) 0.11274(3) 0.01661(9) 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 0.015(2) 0.017(2) 0.0136(19) 0.0034(17) 0.0018(16) 0.0045(17) C2 0.017(2) 0.016(2) 0.021(2) 0.0063(17) 0.0084(17) 0.0062(17) C3 0.020(2) 0.019(2) 0.019(2) 0.0077(18) 0.0059(18) 0.0040(18) C4 0.021(2) 0.018(2) 0.019(2) 0.0086(18) 0.0013(18) 0.0020(18) C5 0.015(2) 0.019(2) 0.025(2) 0.0114(18) 0.0040(17) 0.0066(18) C6 0.013(2) 0.017(2) 0.020(2) 0.0064(18) 0.0021(17) 0.0031(17) C7 0.015(2) 0.049(3) 0.022(2) 0.007(2) 0.0045(18) 0.016(2) C8 0.019(2) 0.023(2) 0.020(2) 0.0043(18) 0.0058(18) 0.0095(19) C9 0.029(2) 0.028(2) 0.016(2) 0.0087(19) -0.0009(18) 0.008(2) C10 0.0111(19) 0.017(2) 0.018(2) 0.0047(17) 0.0040(16) 0.0046(17) C11 0.018(2) 0.018(2) 0.0130(19) 0.0030(17) 0.0046(16) 0.0074(18) C12 0.016(2) 0.024(2) 0.018(2) 0.0057(18) -0.0012(17) 0.0080(18) C13 0.017(2) 0.025(2) 0.023(2) 0.0092(19) 0.0055(18) 0.0061(19) C14 0.024(2) 0.022(2) 0.030(2) 0.014(2) 0.0051(19) 0.0074(19) C15 0.020(2) 0.020(2) 0.015(2) 0.0051(17) 0.0014(17) 0.0089(18) C16 0.016(2) 0.025(2) 0.024(2) 0.0108(19) 0.0010(17) 0.0080(18) C17 0.023(3) 0.041(3) 0.057(3) 0.029(3) 0.004(2) 0.005(2) C18 0.024(2) 0.022(2) 0.024(2) 0.0103(19) -0.0030(19) 0.0087(19) Cl1 0.0209(5) 0.0210(5) 0.0186(5) 0.0063(4) 0.0080(4) 0.0084(4) Cl2 0.0282(5) 0.0204(5) 0.0264(5) 0.0079(4) 0.0130(4) 0.0062(4) Se1 0.0130(2) 0.0175(2) 0.0155(2) 0.00538(18) 0.00357(17) 0.00637(18) Pd1 0.01412(16) 0.01835(17) 0.01496(16) 0.00434(13) 0.00402(12) 0.00684(13) _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 1.405(5) . ? C1 C6 1.407(5) . ? C1 Se1 1.947(4) . ? C2 C3 1.386(5) . ? C2 C8 1.509(5) . ? C3 C4 1.392(5) . ? C3 H3 0.9500 . ? C4 C5 1.374(5) . ? C4 C9 1.508(5) . ? C5 C6 1.406(5) . ? C5 H5 0.9500 . ? C6 C7 1.501(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.392(5) . ? C10 C11 1.402(5) . ? C10 Se1 1.945(4) . ? C11 C12 1.387(5) . ? C11 C16 1.501(5) . ? C12 C13 1.397(5) . ? C12 H12 0.9500 . ? C13 C14 1.392(5) . ? C13 C17 1.496(6) . ? C14 C15 1.389(6) . ? C14 H14 0.9500 . ? C15 C18 1.511(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? Cl1 Pd1 2.3307(10) 2 ? Cl1 Pd1 2.3504(9) . ? Cl2 Pd1 2.2810(10) . ? Se1 Pd1 2.3837(5) . ? Pd1 Cl1 2.3307(10) 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 C6 122.1(4) . . ? C2 C1 Se1 114.8(3) . . ? C6 C1 Se1 122.6(3) . . ? C3 C2 C1 117.6(3) . . ? C3 C2 C8 119.0(3) . . ? C1 C2 C8 123.4(3) . . ? C2 C3 C4 122.7(4) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C5 C4 C3 117.7(4) . . ? C5 C4 C9 121.3(4) . . ? C3 C4 C9 121.0(4) . . ? C4 C5 C6 123.4(4) . . ? C4 C5 H5 118.3 . . ? C6 C5 H5 118.3 . . ? C5 C6 C1 116.3(3) . . ? C5 C6 C7 118.6(3) . . ? C1 C6 C7 125.1(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 122.4(3) . . ? C15 C10 Se1 124.6(3) . . ? C11 C10 Se1 112.9(3) . . ? C12 C11 C10 117.7(3) . . ? C12 C11 C16 119.6(3) . . ? C10 C11 C16 122.7(3) . . ? C11 C12 C13 122.2(4) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C14 C13 C12 117.5(4) . . ? C14 C13 C17 121.3(4) . . ? C12 C13 C17 121.2(4) . . ? C15 C14 C13 122.9(4) . . ? C15 C14 H14 118.6 . . ? C13 C14 H14 118.6 . . ? C14 C15 C10 117.3(3) . . ? C14 C15 C18 118.2(4) . . ? C10 C15 C18 124.5(4) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Pd1 Cl1 Pd1 95.04(3) 2 . ? C10 Se1 C1 104.08(16) . . ? C10 Se1 Pd1 103.38(11) . . ? C1 Se1 Pd1 116.04(11) . . ? Cl2 Pd1 Cl1 176.37(3) . 2 ? Cl2 Pd1 Cl1 91.42(3) . . ? Cl1 Pd1 Cl1 84.96(3) 2 . ? Cl2 Pd1 Se1 86.04(3) . . ? Cl1 Pd1 Se1 97.51(3) 2 . ? Cl1 Pd1 Se1 172.57(3) . . ? 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 C6 C1 C2 C3 -3.3(6) . . . . ? Se1 C1 C2 C3 -176.2(3) . . . . ? C6 C1 C2 C8 178.1(4) . . . . ? Se1 C1 C2 C8 5.2(5) . . . . ? C1 C2 C3 C4 0.9(6) . . . . ? C8 C2 C3 C4 179.6(4) . . . . ? C2 C3 C4 C5 1.7(6) . . . . ? C2 C3 C4 C9 -177.2(4) . . . . ? C3 C4 C5 C6 -2.3(6) . . . . ? C9 C4 C5 C6 176.6(4) . . . . ? C4 C5 C6 C1 0.1(6) . . . . ? C4 C5 C6 C7 -178.6(4) . . . . ? C2 C1 C6 C5 2.8(6) . . . . ? Se1 C1 C6 C5 175.1(3) . . . . ? C2 C1 C6 C7 -178.6(4) . . . . ? Se1 C1 C6 C7 -6.3(6) . . . . ? C15 C10 C11 C12 -0.2(6) . . . . ? Se1 C10 C11 C12 179.1(3) . . . . ? C15 C10 C11 C16 179.5(4) . . . . ? Se1 C10 C11 C16 -1.2(5) . . . . ? C10 C11 C12 C13 1.0(6) . . . . ? C16 C11 C12 C13 -178.7(4) . . . . ? C11 C12 C13 C14 -0.7(6) . . . . ? C11 C12 C13 C17 179.7(4) . . . . ? C12 C13 C14 C15 -0.4(6) . . . . ? C17 C13 C14 C15 179.2(4) . . . . ? C13 C14 C15 C10 1.1(6) . . . . ? C13 C14 C15 C18 -179.9(4) . . . . ? C11 C10 C15 C14 -0.8(6) . . . . ? Se1 C10 C15 C14 -180.0(3) . . . . ? C11 C10 C15 C18 -179.7(4) . . . . ? Se1 C10 C15 C18 1.1(6) . . . . ? C15 C10 Se1 C1 -37.4(4) . . . . ? C11 C10 Se1 C1 143.4(3) . . . . ? C15 C10 Se1 Pd1 84.3(3) . . . . ? C11 C10 Se1 Pd1 -95.0(3) . . . . ? C2 C1 Se1 C10 -61.9(3) . . . . ? C6 C1 Se1 C10 125.3(3) . . . . ? C2 C1 Se1 Pd1 -174.7(2) . . . . ? C6 C1 Se1 Pd1 12.4(4) . . . . ? Pd1 Cl1 Pd1 Cl2 -179.67(4) 2 . . . ? Pd1 Cl1 Pd1 Cl1 0.0 2 . . 2 ? Pd1 Cl1 Pd1 Se1 -109.8(2) 2 . . . ? C10 Se1 Pd1 Cl2 155.48(12) . . . . ? C1 Se1 Pd1 Cl2 -91.28(13) . . . . ? C10 Se1 Pd1 Cl1 -23.75(12) . . . 2 ? C1 Se1 Pd1 Cl1 89.49(13) . . . 2 ? C10 Se1 Pd1 Cl1 85.3(2) . . . . ? C1 Se1 Pd1 Cl1 -161.5(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 66.60 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.933 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.099 _iucr_refine_instruction_details ; TITL SK1 in P-1 #2 CELL 1.54184 8.5654 11.1973 11.5045 110.442 97.754 109.719 ZERR 2.00 0.0005 0.0008 0.0006 0.006 0.005 0.006 LATT 1 SFAC C H CL SE PD UNIT 36 44 4 2 2 MERG 2 FMAP 2 PLAN 20 SIZE 0.02 0.05 0.12 ACTA BOND $H CONF LIST 4 L.S. 4 TEMP -173.00 WGHT 0.031500 FVAR 4.87450 C1 1 0.060458 0.309921 0.459910 11.00000 0.01549 0.01739 = 0.01358 0.00338 0.00175 0.00454 C2 1 -0.013029 0.354975 0.559772 11.00000 0.01688 0.01625 = 0.02059 0.00630 0.00840 0.00617 C3 1 0.084398 0.401894 0.685812 11.00000 0.01988 0.01926 = 0.01916 0.00771 0.00595 0.00398 AFIX 43 H3 2 0.035910 0.431378 0.754364 11.00000 -1.20000 AFIX 0 C4 1 0.250457 0.407569 0.716032 11.00000 0.02092 0.01803 = 0.01895 0.00858 0.00126 0.00199 C5 1 0.319926 0.368060 0.615738 11.00000 0.01488 0.01944 = 0.02486 0.01142 0.00402 0.00662 AFIX 43 H5 2 0.434760 0.374845 0.635757 11.00000 -1.20000 AFIX 0 C6 1 0.229975 0.318105 0.485009 11.00000 0.01347 0.01741 = 0.01962 0.00640 0.00209 0.00310 C7 1 0.318123 0.274991 0.383686 11.00000 0.01516 0.04863 = 0.02220 0.00698 0.00450 0.01586 AFIX 137 H7A 2 0.431841 0.284046 0.425096 11.00000 -1.50000 H7B 2 0.332684 0.335360 0.337850 11.00000 -1.50000 H7C 2 0.247404 0.177413 0.321948 11.00000 -1.50000 AFIX 0 C8 1 -0.192449 0.351621 0.536069 11.00000 0.01932 0.02295 = 0.01976 0.00425 0.00582 0.00950 AFIX 137 H8A 2 -0.278464 0.255515 0.507183 11.00000 -1.50000 H8B 2 -0.211269 0.384654 0.469188 11.00000 -1.50000 H8C 2 -0.204103 0.412516 0.616447 11.00000 -1.50000 AFIX 0 C9 1 0.349079 0.453040 0.853944 11.00000 0.02864 0.02798 = 0.01604 0.00874 -0.00095 0.00757 AFIX 137 H9A 2 0.335881 0.370244 0.869956 11.00000 -1.50000 H9B 2 0.303495 0.510042 0.913181 11.00000 -1.50000 H9C 2 0.471955 0.508384 0.868320 11.00000 -1.50000 AFIX 0 C10 1 -0.290521 0.100972 0.260700 11.00000 0.01109 0.01731 = 0.01815 0.00466 0.00401 0.00456 C11 1 -0.438535 0.100451 0.191219 11.00000 0.01776 0.01819 = 0.01297 0.00297 0.00456 0.00739 C12 1 -0.596521 -0.008039 0.165231 11.00000 0.01640 0.02393 = 0.01754 0.00569 -0.00117 0.00799 AFIX 43 H12 2 -0.698063 -0.011014 0.117028 11.00000 -1.20000 AFIX 0 C13 1 -0.611399 -0.113073 0.207526 11.00000 0.01722 0.02516 = 0.02345 0.00920 0.00546 0.00607 C14 1 -0.459977 -0.106689 0.276624 11.00000 0.02359 0.02168 = 0.03018 0.01359 0.00509 0.00743 AFIX 43 H14 2 -0.467916 -0.177021 0.306521 11.00000 -1.20000 AFIX 0 C15 1 -0.297846 -0.002013 0.303757 11.00000 0.01990 0.02050 = 0.01497 0.00511 0.00145 0.00893 C16 1 -0.431890 0.211704 0.145334 11.00000 0.01551 0.02460 = 0.02421 0.01084 0.00102 0.00796 AFIX 137 H16A 2 -0.547919 0.188281 0.094287 11.00000 -1.50000 H16B 2 -0.352567 0.217284 0.091538 11.00000 -1.50000 H16C 2 -0.390846 0.302178 0.220220 11.00000 -1.50000 AFIX 0 C17 1 -0.783492 -0.228589 0.178681 11.00000 0.02268 0.04117 = 0.05687 0.02899 0.00431 0.00476 AFIX 137 H17A 2 -0.766246 -0.304617 0.194013 11.00000 -1.50000 H17B 2 -0.848348 -0.264000 0.087989 11.00000 -1.50000 H17C 2 -0.848629 -0.192829 0.235142 11.00000 -1.50000 AFIX 0 C18 1 -0.142435 -0.005841 0.379474 11.00000 0.02360 0.02231 = 0.02376 0.01027 -0.00303 0.00867 AFIX 137 H18A 2 -0.112321 0.057710 0.470961 11.00000 -1.50000 H18B 2 -0.044255 0.023653 0.345506 11.00000 -1.50000 H18C 2 -0.169960 -0.101370 0.371052 11.00000 -1.50000 AFIX 0 CL1 3 0.109796 0.073038 -0.075273 11.00000 0.02090 0.02096 = 0.01855 0.00628 0.00800 0.00839 CL2 3 0.167062 0.385318 0.137278 11.00000 0.02819 0.02042 = 0.02645 0.00786 0.01298 0.00619 SE1 4 -0.078903 0.257389 0.287175 11.00000 0.01301 0.01751 = 0.01547 0.00538 0.00357 0.00637 PD1 5 0.028053 0.160982 0.112741 11.00000 0.01412 0.01835 = 0.01496 0.00434 0.00402 0.00684 HKLF 4 REM SK1 in P-1 #2 REM R1 = 0.0291 for 2746 Fo > 4sig(Fo) and 0.0407 for all 3294 data REM 205 parameters refined using 0 restraints END WGHT 0.0317 0.0000 REM Highest difference peak 0.933, deepest hole -0.512, 1-sigma level 0.099 Q1 1 -0.0240 0.0844 0.1404 11.00000 0.05 0.93 Q2 1 0.0967 0.2430 0.0964 11.00000 0.05 0.69 Q3 1 -0.1224 0.1836 0.3014 11.00000 0.05 0.56 Q4 1 -0.0754 0.1801 0.3441 11.00000 0.05 0.55 Q5 1 -0.0063 0.3464 0.2734 11.00000 0.05 0.48 Q6 1 0.1859 0.2495 0.1964 11.00000 0.05 0.47 Q7 1 -0.0306 0.2722 0.1863 11.00000 0.05 0.46 Q8 1 0.1483 0.1447 -0.0823 11.00000 0.05 0.45 Q9 1 -0.0753 0.1504 0.0884 11.00000 0.05 0.44 Q10 1 0.0651 0.0550 0.0162 11.00000 0.05 0.39 Q11 1 0.0959 0.3195 0.1887 11.00000 0.05 0.39 Q12 1 -0.4514 0.1453 0.1504 11.00000 0.05 0.38 Q13 1 0.0941 0.3991 0.2582 11.00000 0.05 0.37 Q14 1 -0.0982 0.3503 0.5471 11.00000 0.05 0.36 Q15 1 -0.1303 0.0524 0.0211 11.00000 0.05 0.35 Q16 1 0.2321 0.1014 -0.0176 11.00000 0.05 0.34 Q17 1 0.1133 0.0459 0.0571 11.00000 0.05 0.34 Q18 1 0.0751 0.3639 0.3805 11.00000 0.05 0.34 Q19 1 -0.6788 -0.3036 0.1416 11.00000 0.05 0.33 Q20 1 0.1907 0.3381 0.3141 11.00000 0.05 0.33 ; _database_code_depnum_ccdc_archive 'CCDC 901678' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sk2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H42 Cl2 Pd2 Se2' _chemical_formula_weight 916.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_cell_setting monoclinic 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 15.1293(5) _cell_length_b 15.0902(5) _cell_length_c 15.1702(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.287(3) _cell_angle_gamma 90.00 _cell_volume 3435.45(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2219 _cell_measurement_theta_min 4.1459 _cell_measurement_theta_max 66.4852 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.772 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 12.475 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.7060 _exptl_absorpt_correction_T_max 0.8854 _exptl_absorpt_process_details ; ABSORPTION CORRECTION (NUMERICAL) - (a) W. R. Busing and H. A. Levy, Acta Crystallogr. 1957, 10, 180-182. (b) P. Coppens, L. Leiserowitz and D. Rabinovich, Acta Crystallogr. 1965, 18, 1035-1038. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2413 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10027 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.15 _diffrn_reflns_theta_max 66.63 _reflns_number_total 5986 _reflns_number_gt 4265 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.8 (release 13-04-2012 CrysAlis171 .NET) (compiled Apr 13 2012,18:42:44) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.8 (release 13-04-2012 CrysAlis171 .NET) (compiled Apr 13 2012,18:42:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.8 (release 13-04-2012 CrysAlis171 .NET) (compiled Apr 13 2012,18:42:44) ; _computing_structure_solution SIR-92 _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^)+(0.0285P)^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 5990 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 C1 C 0.7252(4) 0.8652(5) 0.5877(4) 0.0203(14) Uani 1 1 d . . . C2 C 0.7387(5) 0.8323(5) 0.5050(5) 0.0254(15) Uani 1 1 d . . . C3 C 0.6730(4) 0.7742(5) 0.4643(4) 0.0246(15) Uani 1 1 d . . . H3 H 0.6796 0.7506 0.4075 0.030 Uiso 1 1 calc R . . C4 C 0.5991(5) 0.7503(5) 0.5042(5) 0.0273(16) Uani 1 1 d . . . C5 C 0.5912(5) 0.7848(6) 0.5888(5) 0.0311(18) Uani 1 1 d . . . H5 H 0.5417 0.7674 0.6175 0.037 Uiso 1 1 calc R . . C6 C 0.6525(5) 0.8427(5) 0.6318(5) 0.0294(17) Uani 1 1 d . . . C7 C 0.8206(5) 0.8530(5) 0.4627(4) 0.0257(15) Uani 1 1 d . . . H7A H 0.8016 0.8716 0.4006 0.031 Uiso 1 1 calc R . . H7B H 0.8552 0.7976 0.4604 0.031 Uiso 1 1 calc R . . C8 C 0.5269(5) 0.6927(6) 0.4586(5) 0.0345(18) Uani 1 1 d . . . H8A H 0.4738 0.7287 0.4403 0.052 Uiso 1 1 calc R . . H8B H 0.5123 0.6462 0.4995 0.052 Uiso 1 1 calc R . . H8C H 0.5472 0.6654 0.4061 0.052 Uiso 1 1 calc R . . C9 C 0.6419(5) 0.8799(6) 0.7214(5) 0.0350(19) Uani 1 1 d . . . H9A H 0.6352 0.9444 0.7171 0.053 Uiso 1 1 calc R . . H9B H 0.6947 0.8655 0.7633 0.053 Uiso 1 1 calc R . . H9C H 0.5889 0.8542 0.7424 0.053 Uiso 1 1 calc R . . C10 C 0.8707(4) 0.9088(5) 0.7407(4) 0.0197(14) Uani 1 1 d . . . C11 C 0.8865(4) 0.9705(5) 0.8099(4) 0.0218(14) Uani 1 1 d . . . C12 C 0.9343(4) 0.9421(5) 0.8890(4) 0.0236(15) Uani 1 1 d . . . H12 H 0.9449 0.9827 0.9370 0.028 Uiso 1 1 calc R . . C13 C 0.9672(4) 0.8565(5) 0.9004(4) 0.0205(14) Uani 1 1 d . . . C14 C 0.9488(4) 0.7978(5) 0.8301(5) 0.0239(15) Uani 1 1 d . . . H14 H 0.9695 0.7384 0.8373 0.029 Uiso 1 1 calc R . . C15 C 0.9018(5) 0.8222(5) 0.7502(4) 0.0227(14) Uani 1 1 d . . . C16 C 0.8553(5) 1.0660(5) 0.8015(5) 0.0337(18) Uani 1 1 d . . . H16A H 0.8675 1.0955 0.8593 0.051 Uiso 1 1 calc R . . H16B H 0.7911 1.0675 0.7815 0.051 Uiso 1 1 calc R . . H16C H 0.8871 1.0968 0.7581 0.051 Uiso 1 1 calc R . . C17 C 1.0228(5) 0.8274(5) 0.9842(5) 0.0288(16) Uani 1 1 d . . . H17A H 1.0186 0.7629 0.9902 0.043 Uiso 1 1 calc R . . H17B H 1.0011 0.8561 1.0353 0.043 Uiso 1 1 calc R . . H17C H 1.0851 0.8441 0.9820 0.043 Uiso 1 1 calc R . . C18 C 0.8876(5) 0.7534(5) 0.6775(5) 0.0314(17) Uani 1 1 d . . . H18A H 0.8257 0.7328 0.6712 0.047 Uiso 1 1 calc R . . H18B H 0.9277 0.7031 0.6927 0.047 Uiso 1 1 calc R . . H18C H 0.9003 0.7795 0.6213 0.047 Uiso 1 1 calc R . . C19 C 0.2542(4) 0.5510(5) 0.1804(4) 0.0238(15) Uani 1 1 d . . . C20 C 0.3099(4) 0.4878(5) 0.2228(4) 0.0232(15) Uani 1 1 d . . . C21 C 0.2858(5) 0.4511(5) 0.3007(4) 0.0246(15) Uani 1 1 d . . . H21 H 0.3227 0.4071 0.3312 0.030 Uiso 1 1 calc R . . C22 C 0.2089(5) 0.4775(5) 0.3347(5) 0.0284(16) Uani 1 1 d . . . C23 C 0.1553(5) 0.5422(5) 0.2886(5) 0.0292(17) Uani 1 1 d . . . H23 H 0.1030 0.5612 0.3117 0.035 Uiso 1 1 calc R . . C24 C 0.1761(5) 0.5799(5) 0.2094(5) 0.0307(17) Uani 1 1 d . . . C25 C 0.3957(5) 0.4616(5) 0.1893(5) 0.0282(16) Uani 1 1 d . . . H25A H 0.3972 0.3962 0.1856 0.034 Uiso 1 1 calc R . . H25B H 0.4456 0.4799 0.2343 0.034 Uiso 1 1 calc R . . C26 C 0.1830(6) 0.4409(6) 0.4199(5) 0.042(2) Uani 1 1 d . . . H26A H 0.2214 0.3904 0.4393 0.063 Uiso 1 1 calc R . . H26B H 0.1207 0.4214 0.4103 0.063 Uiso 1 1 calc R . . H26C H 0.1900 0.4870 0.4658 0.063 Uiso 1 1 calc R . . C27 C 0.1164(5) 0.6484(6) 0.1617(5) 0.0349(18) Uani 1 1 d . . . H27A H 0.1394 0.7076 0.1783 0.052 Uiso 1 1 calc R . . H27B H 0.0562 0.6422 0.1782 0.052 Uiso 1 1 calc R . . H27C H 0.1146 0.6403 0.0974 0.052 Uiso 1 1 calc R . . C28 C 0.3089(4) 0.7119(5) 0.0744(4) 0.0220(14) Uani 1 1 d . . . C29 C 0.2800(4) 0.7598(5) -0.0022(5) 0.0236(15) Uani 1 1 d . . . C30 C 0.3000(5) 0.8506(5) -0.0019(5) 0.0287(16) Uani 1 1 d . . . H30 H 0.2819 0.8847 -0.0537 0.034 Uiso 1 1 calc R . . C31 C 0.3459(5) 0.8922(5) 0.0726(5) 0.0317(17) Uani 1 1 d . . . C32 C 0.3712(5) 0.8409(5) 0.1473(5) 0.0299(17) Uani 1 1 d . . . H32 H 0.4014 0.8690 0.1986 0.036 Uiso 1 1 calc R . . C33 C 0.3548(4) 0.7512(5) 0.1510(5) 0.0244(15) Uani 1 1 d . . . C34 C 0.2308(5) 0.7186(5) -0.0849(5) 0.0307(17) Uani 1 1 d . . . H34A H 0.2142 0.7649 -0.1292 0.046 Uiso 1 1 calc R . . H34B H 0.1769 0.6891 -0.0700 0.046 Uiso 1 1 calc R . . H34C H 0.2694 0.6752 -0.1091 0.046 Uiso 1 1 calc R . . C35 C 0.3694(7) 0.9886(6) 0.0698(6) 0.052(3) Uani 1 1 d . . . H35A H 0.3194 1.0242 0.0850 0.079 Uiso 1 1 calc R . . H35B H 0.3820 1.0041 0.0099 0.079 Uiso 1 1 calc R . . H35C H 0.4222 1.0003 0.1126 0.079 Uiso 1 1 calc R . . C36 C 0.3900(5) 0.7021(5) 0.2345(5) 0.0306(17) Uani 1 1 d . . . H36A H 0.4314 0.7403 0.2722 0.046 Uiso 1 1 calc R . . H36B H 0.4213 0.6486 0.2189 0.046 Uiso 1 1 calc R . . H36C H 0.3404 0.6855 0.2667 0.046 Uiso 1 1 calc R . . Cl1 Cl 1.00428(12) 1.06294(12) 0.59307(11) 0.0282(4) Uani 1 1 d . . . Cl2 Cl 0.44631(12) 0.57079(12) -0.07735(11) 0.0295(4) Uani 1 1 d . . . Se1 Se 0.80719(5) 0.95631(5) 0.63114(4) 0.02115(16) Uani 1 1 d . . . Se2 Se 0.28345(5) 0.58552(5) 0.06542(5) 0.02130(16) Uani 1 1 d . . . Pd1 Pd 0.90312(3) 0.94722(3) 0.52168(3) 0.02122(12) Uani 1 1 d . . . Pd2 Pd 0.41928(3) 0.51131(4) 0.06950(3) 0.02280(12) 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 0.020(3) 0.025(4) 0.016(3) 0.002(3) 0.004(3) 0.005(3) C2 0.026(4) 0.023(4) 0.028(4) 0.002(3) 0.005(3) 0.008(3) C3 0.026(4) 0.031(4) 0.017(3) -0.001(3) 0.001(3) 0.005(3) C4 0.025(4) 0.027(4) 0.028(4) -0.004(3) -0.003(3) 0.001(3) C5 0.021(4) 0.045(5) 0.026(4) -0.004(3) 0.001(3) 0.001(3) C6 0.027(4) 0.038(5) 0.023(4) -0.003(3) 0.002(3) 0.005(3) C7 0.028(4) 0.027(4) 0.023(3) -0.003(3) 0.005(3) -0.002(3) C8 0.024(4) 0.046(5) 0.034(4) -0.009(4) 0.006(3) -0.006(3) C9 0.027(4) 0.053(6) 0.026(4) -0.006(4) 0.007(3) -0.001(4) C10 0.015(3) 0.025(4) 0.020(3) 0.003(3) 0.007(3) -0.002(3) C11 0.019(3) 0.023(4) 0.024(3) 0.005(3) 0.004(3) 0.004(3) C12 0.020(3) 0.033(4) 0.017(3) -0.001(3) 0.001(3) 0.000(3) C13 0.016(3) 0.026(4) 0.021(3) 0.003(3) 0.008(3) -0.004(3) C14 0.023(3) 0.020(4) 0.030(4) 0.007(3) 0.009(3) 0.002(3) C15 0.025(4) 0.023(4) 0.021(3) 0.004(3) 0.007(3) -0.004(3) C16 0.048(5) 0.025(4) 0.024(4) -0.001(3) -0.012(3) 0.011(3) C17 0.026(4) 0.032(4) 0.029(4) 0.007(3) 0.005(3) 0.007(3) C18 0.036(4) 0.022(4) 0.036(4) -0.001(3) 0.001(3) 0.003(3) C19 0.019(3) 0.028(4) 0.025(3) -0.008(3) 0.006(3) -0.001(3) C20 0.020(3) 0.024(4) 0.026(3) -0.010(3) 0.004(3) 0.001(3) C21 0.027(4) 0.025(4) 0.022(3) 0.001(3) 0.007(3) -0.005(3) C22 0.042(4) 0.021(4) 0.022(3) -0.004(3) 0.005(3) -0.009(3) C23 0.026(4) 0.036(5) 0.029(4) -0.010(3) 0.016(3) -0.007(3) C24 0.026(4) 0.033(4) 0.032(4) -0.003(3) 0.003(3) -0.005(3) C25 0.029(4) 0.027(4) 0.031(4) -0.004(3) 0.013(3) 0.005(3) C26 0.059(5) 0.044(6) 0.028(4) -0.005(4) 0.020(4) -0.017(4) C27 0.021(4) 0.040(5) 0.046(5) 0.003(4) 0.013(3) 0.010(3) C28 0.017(3) 0.026(4) 0.024(3) -0.004(3) 0.007(3) 0.001(3) C29 0.019(3) 0.024(4) 0.029(4) -0.001(3) 0.006(3) 0.003(3) C30 0.034(4) 0.022(4) 0.029(4) 0.006(3) 0.000(3) 0.008(3) C31 0.029(4) 0.027(4) 0.038(4) 0.004(3) -0.001(3) -0.002(3) C32 0.036(4) 0.024(4) 0.028(4) -0.004(3) 0.000(3) -0.005(3) C33 0.018(3) 0.028(4) 0.027(4) -0.005(3) 0.004(3) 0.003(3) C34 0.031(4) 0.034(5) 0.026(4) 0.005(3) 0.002(3) 0.004(3) C35 0.068(6) 0.035(5) 0.051(5) -0.002(4) -0.006(5) -0.011(5) C36 0.028(4) 0.038(5) 0.024(4) 0.000(3) -0.002(3) 0.000(3) Cl1 0.0364(9) 0.0270(9) 0.0244(8) -0.0073(7) 0.0158(7) -0.0086(7) Cl2 0.0315(9) 0.0300(10) 0.0300(8) 0.0072(7) 0.0157(7) 0.0111(7) Se1 0.0242(4) 0.0235(4) 0.0161(3) -0.0005(3) 0.0037(3) 0.0032(3) Se2 0.0206(3) 0.0241(4) 0.0201(3) -0.0019(3) 0.0061(3) 0.0003(3) Pd1 0.0273(3) 0.0202(3) 0.0172(2) 0.00028(19) 0.00703(19) -0.0013(2) Pd2 0.0240(3) 0.0225(3) 0.0241(2) -0.0003(2) 0.01149(19) 0.0038(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 C1 C2 1.388(10) . ? C1 C6 1.398(10) . ? C1 Se1 1.912(7) . ? C2 C3 1.408(10) . ? C2 C7 1.499(10) . ? C3 C4 1.384(10) . ? C3 H3 0.9500 . ? C4 C5 1.404(10) . ? C4 C8 1.496(10) . ? C5 C6 1.378(10) . ? C5 H5 0.9500 . ? C6 C9 1.498(10) . ? C7 Pd1 2.024(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.390(10) . ? C10 C11 1.401(10) . ? C10 Se1 1.948(6) . ? C11 C12 1.388(9) . ? C11 C16 1.517(9) . ? C12 C13 1.387(10) . ? C12 H12 0.9500 . ? C13 C14 1.388(10) . ? C13 C17 1.499(9) . ? C14 C15 1.375(9) . ? C14 H14 0.9500 . ? C15 C18 1.512(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.376(10) . ? C19 C24 1.383(10) . ? C19 Se2 1.925(7) . ? C20 C21 1.395(10) . ? C20 C25 1.506(9) . ? C21 C22 1.389(10) . ? C21 H21 0.9500 . ? C22 C23 1.400(11) . ? C22 C26 1.503(10) . ? C23 C24 1.401(10) . ? C23 H23 0.9500 . ? C24 C27 1.497(10) . ? C25 Pd2 2.039(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.392(10) . ? C28 C33 1.406(9) . ? C28 Se2 1.946(7) . ? C29 C30 1.404(10) . ? C29 C34 1.509(9) . ? C30 C31 1.398(10) . ? C30 H30 0.9500 . ? C31 C32 1.385(10) . ? C31 C35 1.498(11) . ? C32 C33 1.379(10) . ? C32 H32 0.9500 . ? C33 C36 1.506(9) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? Cl1 Pd1 2.3739(16) 3_776 ? Cl1 Pd1 2.4786(17) . ? Cl2 Pd2 2.3713(17) 3_665 ? Cl2 Pd2 2.4833(17) . ? Se1 Pd1 2.3438(8) . ? Se2 Pd2 2.3342(9) . ? Pd1 Cl1 2.3739(16) 3_776 ? Pd2 Cl2 2.3713(17) 3_665 ? 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 C6 124.0(7) . . ? C2 C1 Se1 113.9(5) . . ? C6 C1 Se1 121.6(5) . . ? C1 C2 C3 116.3(7) . . ? C1 C2 C7 122.5(7) . . ? C3 C2 C7 121.2(6) . . ? C4 C3 C2 122.3(7) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C3 C4 C5 118.0(7) . . ? C3 C4 C8 122.2(7) . . ? C5 C4 C8 119.7(7) . . ? C6 C5 C4 122.5(7) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C1 116.8(7) . . ? C5 C6 C9 121.6(7) . . ? C1 C6 C9 121.6(7) . . ? C2 C7 Pd1 117.0(5) . . ? C2 C7 H7A 108.0 . . ? Pd1 C7 H7A 108.0 . . ? C2 C7 H7B 108.0 . . ? Pd1 C7 H7B 108.0 . . ? H7A C7 H7B 107.3 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 121.6(6) . . ? C15 C10 Se1 123.9(5) . . ? C11 C10 Se1 114.4(5) . . ? C12 C11 C10 117.6(7) . . ? C12 C11 C16 119.3(6) . . ? C10 C11 C16 123.1(6) . . ? C13 C12 C11 122.3(7) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C12 C13 C14 117.7(6) . . ? C12 C13 C17 122.2(6) . . ? C14 C13 C17 120.1(7) . . ? C15 C14 C13 122.4(7) . . ? C15 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? C14 C15 C10 118.3(7) . . ? C14 C15 C18 117.9(7) . . ? C10 C15 C18 123.8(6) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 124.5(7) . . ? C20 C19 Se2 114.4(5) . . ? C24 C19 Se2 120.4(6) . . ? C19 C20 C21 117.4(6) . . ? C19 C20 C25 121.8(7) . . ? C21 C20 C25 120.7(7) . . ? C22 C21 C20 121.5(7) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 118.3(7) . . ? C21 C22 C26 122.4(7) . . ? C23 C22 C26 119.3(7) . . ? C22 C23 C24 122.2(7) . . ? C22 C23 H23 118.9 . . ? C24 C23 H23 118.9 . . ? C19 C24 C23 116.0(7) . . ? C19 C24 C27 123.5(7) . . ? C23 C24 C27 120.5(7) . . ? C20 C25 Pd2 117.4(5) . . ? C20 C25 H25A 108.0 . . ? Pd2 C25 H25A 108.0 . . ? C20 C25 H25B 108.0 . . ? Pd2 C25 H25B 108.0 . . ? H25A C25 H25B 107.2 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 122.7(7) . . ? C29 C28 Se2 114.3(5) . . ? C33 C28 Se2 123.0(5) . . ? C28 C29 C30 117.4(7) . . ? C28 C29 C34 123.4(7) . . ? C30 C29 C34 119.2(6) . . ? C31 C30 C29 121.7(7) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C32 C31 C30 117.8(7) . . ? C32 C31 C35 121.6(7) . . ? C30 C31 C35 120.5(7) . . ? C33 C32 C31 123.3(7) . . ? C33 C32 H32 118.3 . . ? C31 C32 H32 118.3 . . ? C32 C33 C28 117.0(7) . . ? C32 C33 C36 118.1(7) . . ? C28 C33 C36 124.9(7) . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Pd1 Cl1 Pd1 91.33(6) 3_776 . ? Pd2 Cl2 Pd2 90.22(6) 3_665 . ? C1 Se1 C10 104.9(3) . . ? C1 Se1 Pd1 98.5(2) . . ? C10 Se1 Pd1 107.49(19) . . ? C19 Se2 C28 105.5(3) . . ? C19 Se2 Pd2 98.6(2) . . ? C28 Se2 Pd2 107.62(19) . . ? C7 Pd1 Se1 87.22(19) . . ? C7 Pd1 Cl1 91.1(2) . 3_776 ? Se1 Pd1 Cl1 177.92(5) . 3_776 ? C7 Pd1 Cl1 179.7(2) . . ? Se1 Pd1 Cl1 93.02(4) . . ? Cl1 Pd1 Cl1 88.67(6) 3_776 . ? C25 Pd2 Se2 87.0(2) . . ? C25 Pd2 Cl2 90.5(2) . 3_665 ? Se2 Pd2 Cl2 176.84(5) . 3_665 ? C25 Pd2 Cl2 179.3(2) . . ? Se2 Pd2 Cl2 92.72(5) . . ? Cl2 Pd2 Cl2 89.78(6) 3_665 . ? 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 C6 C1 C2 C3 1.1(11) . . . . ? Se1 C1 C2 C3 -171.4(5) . . . . ? C6 C1 C2 C7 -175.7(7) . . . . ? Se1 C1 C2 C7 11.8(9) . . . . ? C1 C2 C3 C4 -0.4(10) . . . . ? C7 C2 C3 C4 176.4(7) . . . . ? C2 C3 C4 C5 -1.0(11) . . . . ? C2 C3 C4 C8 176.5(7) . . . . ? C3 C4 C5 C6 1.8(12) . . . . ? C8 C4 C5 C6 -175.8(7) . . . . ? C4 C5 C6 C1 -1.1(12) . . . . ? C4 C5 C6 C9 178.9(8) . . . . ? C2 C1 C6 C5 -0.4(11) . . . . ? Se1 C1 C6 C5 171.6(6) . . . . ? C2 C1 C6 C9 179.6(7) . . . . ? Se1 C1 C6 C9 -8.5(10) . . . . ? C1 C2 C7 Pd1 -9.6(9) . . . . ? C3 C2 C7 Pd1 173.7(5) . . . . ? C15 C10 C11 C12 -0.2(10) . . . . ? Se1 C10 C11 C12 -177.7(5) . . . . ? C15 C10 C11 C16 178.7(7) . . . . ? Se1 C10 C11 C16 1.2(9) . . . . ? C10 C11 C12 C13 1.0(10) . . . . ? C16 C11 C12 C13 -178.0(7) . . . . ? C11 C12 C13 C14 -1.7(10) . . . . ? C11 C12 C13 C17 176.8(6) . . . . ? C12 C13 C14 C15 1.7(10) . . . . ? C17 C13 C14 C15 -176.9(6) . . . . ? C13 C14 C15 C10 -0.9(10) . . . . ? C13 C14 C15 C18 178.5(6) . . . . ? C11 C10 C15 C14 0.2(10) . . . . ? Se1 C10 C15 C14 177.4(5) . . . . ? C11 C10 C15 C18 -179.2(6) . . . . ? Se1 C10 C15 C18 -2.0(10) . . . . ? C24 C19 C20 C21 -0.4(11) . . . . ? Se2 C19 C20 C21 -171.6(5) . . . . ? C24 C19 C20 C25 -177.8(7) . . . . ? Se2 C19 C20 C25 10.9(9) . . . . ? C19 C20 C21 C22 -0.4(10) . . . . ? C25 C20 C21 C22 177.0(7) . . . . ? C20 C21 C22 C23 0.2(11) . . . . ? C20 C21 C22 C26 -178.1(7) . . . . ? C21 C22 C23 C24 0.8(11) . . . . ? C26 C22 C23 C24 179.2(7) . . . . ? C20 C19 C24 C23 1.4(11) . . . . ? Se2 C19 C24 C23 172.1(5) . . . . ? C20 C19 C24 C27 -179.7(7) . . . . ? Se2 C19 C24 C27 -9.0(10) . . . . ? C22 C23 C24 C19 -1.6(11) . . . . ? C22 C23 C24 C27 179.5(7) . . . . ? C19 C20 C25 Pd2 -7.7(9) . . . . ? C21 C20 C25 Pd2 174.9(5) . . . . ? C33 C28 C29 C30 1.3(10) . . . . ? Se2 C28 C29 C30 -176.9(5) . . . . ? C33 C28 C29 C34 179.9(6) . . . . ? Se2 C28 C29 C34 1.7(9) . . . . ? C28 C29 C30 C31 -0.9(11) . . . . ? C34 C29 C30 C31 -179.6(7) . . . . ? C29 C30 C31 C32 -0.3(12) . . . . ? C29 C30 C31 C35 177.6(8) . . . . ? C30 C31 C32 C33 1.3(12) . . . . ? C35 C31 C32 C33 -176.7(8) . . . . ? C31 C32 C33 C28 -0.9(11) . . . . ? C31 C32 C33 C36 176.8(7) . . . . ? C29 C28 C33 C32 -0.4(10) . . . . ? Se2 C28 C33 C32 177.7(5) . . . . ? C29 C28 C33 C36 -177.9(7) . . . . ? Se2 C28 C33 C36 0.2(10) . . . . ? C2 C1 Se1 C10 -118.6(5) . . . . ? C6 C1 Se1 C10 68.7(6) . . . . ? C2 C1 Se1 Pd1 -7.9(5) . . . . ? C6 C1 Se1 Pd1 179.4(5) . . . . ? C15 C10 Se1 C1 42.9(6) . . . . ? C11 C10 Se1 C1 -139.7(5) . . . . ? C15 C10 Se1 Pd1 -61.2(6) . . . . ? C11 C10 Se1 Pd1 116.2(5) . . . . ? C20 C19 Se2 C28 -119.4(5) . . . . ? C24 C19 Se2 C28 69.0(6) . . . . ? C20 C19 Se2 Pd2 -8.3(5) . . . . ? C24 C19 Se2 Pd2 -179.9(6) . . . . ? C29 C28 Se2 C19 -143.3(5) . . . . ? C33 C28 Se2 C19 38.5(6) . . . . ? C29 C28 Se2 Pd2 112.2(5) . . . . ? C33 C28 Se2 Pd2 -66.0(6) . . . . ? C2 C7 Pd1 Se1 2.6(5) . . . . ? C2 C7 Pd1 Cl1 -176.2(5) . . . 3_776 ? C2 C7 Pd1 Cl1 -139(41) . . . . ? C1 Se1 Pd1 C7 2.5(3) . . . . ? C10 Se1 Pd1 C7 111.1(3) . . . . ? C1 Se1 Pd1 Cl1 37.8(15) . . . 3_776 ? C10 Se1 Pd1 Cl1 146.4(15) . . . 3_776 ? C1 Se1 Pd1 Cl1 -177.7(2) . . . . ? C10 Se1 Pd1 Cl1 -69.1(2) . . . . ? Pd1 Cl1 Pd1 C7 -37(42) 3_776 . . . ? Pd1 Cl1 Pd1 Se1 -178.79(5) 3_776 . . . ? Pd1 Cl1 Pd1 Cl1 0.0 3_776 . . 3_776 ? C20 C25 Pd2 Se2 1.0(5) . . . . ? C20 C25 Pd2 Cl2 -177.1(5) . . . 3_665 ? C20 C25 Pd2 Cl2 -63(18) . . . . ? C19 Se2 Pd2 C25 3.4(3) . . . . ? C28 Se2 Pd2 C25 112.8(3) . . . . ? C19 Se2 Pd2 Cl2 40.6(10) . . . 3_665 ? C28 Se2 Pd2 Cl2 150.0(10) . . . 3_665 ? C19 Se2 Pd2 Cl2 -177.2(2) . . . . ? C28 Se2 Pd2 Cl2 -67.9(2) . . . . ? Pd2 Cl2 Pd2 C25 -114(18) 3_665 . . . ? Pd2 Cl2 Pd2 Se2 -178.06(6) 3_665 . . . ? Pd2 Cl2 Pd2 Cl2 0.0 3_665 . . 3_665 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 66.63 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.893 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.140 _iucr_refine_instructions_details ; TITL SK2 in P21/c #14 CELL 1.54184 15.1293 15.0902 15.1702 90.000 97.287 90.000 ZERR 4.00 0.0005 0.0005 0.0004 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H CL SE PD UNIT 144 168 8 8 8 MERG 2 FMAP 2 PLAN 20 SIZE 0.03 0.03 0.11 ACTA BOND $H CONF LIST 4 L.S. 4 TEMP -173.00 WGHT 0.028500 FVAR 1.66297 C1 1 0.725183 0.865164 0.587736 11.00000 0.02044 0.02454 = 0.01625 0.00161 0.00373 0.00516 C2 1 0.738660 0.832312 0.505000 11.00000 0.02610 0.02265 = 0.02783 0.00238 0.00486 0.00804 C3 1 0.672964 0.774232 0.464300 11.00000 0.02551 0.03071 = 0.01733 -0.00077 0.00148 0.00492 AFIX 43 H3 2 0.679558 0.750595 0.407461 11.00000 -1.20000 AFIX 0 C4 1 0.599104 0.750343 0.504156 11.00000 0.02471 0.02746 = 0.02834 -0.00409 -0.00256 0.00129 C5 1 0.591192 0.784774 0.588754 11.00000 0.02135 0.04488 = 0.02643 -0.00369 0.00073 0.00100 AFIX 43 H5 2 0.541653 0.767444 0.617455 11.00000 -1.20000 AFIX 0 C6 1 0.652529 0.842745 0.631762 11.00000 0.02694 0.03757 = 0.02331 -0.00286 0.00224 0.00525 C7 1 0.820601 0.852978 0.462720 11.00000 0.02805 0.02706 = 0.02257 -0.00264 0.00533 -0.00167 AFIX 23 H7A 2 0.801582 0.871582 0.400628 11.00000 -1.20000 H7B 2 0.855237 0.797552 0.460387 11.00000 -1.20000 AFIX 0 C8 1 0.526863 0.692691 0.458596 11.00000 0.02420 0.04574 = 0.03423 -0.00918 0.00600 -0.00562 AFIX 137 H8A 2 0.473764 0.728661 0.440312 11.00000 -1.50000 H8B 2 0.512288 0.646227 0.499521 11.00000 -1.50000 H8C 2 0.547208 0.665414 0.406107 11.00000 -1.50000 AFIX 0 C9 1 0.641923 0.879945 0.721400 11.00000 0.02687 0.05286 = 0.02618 -0.00610 0.00677 -0.00109 AFIX 137 H9A 2 0.635197 0.944447 0.717065 11.00000 -1.50000 H9B 2 0.694697 0.865516 0.763313 11.00000 -1.50000 H9C 2 0.588937 0.854201 0.742447 11.00000 -1.50000 AFIX 0 C10 1 0.870668 0.908836 0.740736 11.00000 0.01537 0.02515 = 0.01989 0.00293 0.00670 -0.00167 C11 1 0.886473 0.970550 0.809915 11.00000 0.01899 0.02275 = 0.02387 0.00549 0.00400 0.00406 C12 1 0.934302 0.942119 0.888984 11.00000 0.01983 0.03343 = 0.01725 -0.00147 0.00100 0.00024 AFIX 43 H12 2 0.944875 0.982723 0.937021 11.00000 -1.20000 AFIX 0 C13 1 0.967216 0.856524 0.900367 11.00000 0.01635 0.02600 = 0.02073 0.00320 0.00828 -0.00429 C14 1 0.948849 0.797755 0.830057 11.00000 0.02299 0.02016 = 0.03001 0.00667 0.00948 0.00186 AFIX 43 H14 2 0.969550 0.738446 0.837337 11.00000 -1.20000 AFIX 0 C15 1 0.901782 0.822237 0.750239 11.00000 0.02461 0.02320 = 0.02149 0.00410 0.00719 -0.00447 C16 1 0.855302 1.066043 0.801459 11.00000 0.04788 0.02475 = 0.02433 -0.00108 -0.01205 0.01149 AFIX 137 H16A 2 0.867495 1.095452 0.859321 11.00000 -1.50000 H16B 2 0.791131 1.067542 0.781463 11.00000 -1.50000 H16C 2 0.887138 1.096842 0.758128 11.00000 -1.50000 AFIX 0 C17 1 1.022813 0.827400 0.984242 11.00000 0.02586 0.03224 = 0.02880 0.00737 0.00484 0.00690 AFIX 137 H17A 2 1.018582 0.762926 0.990220 11.00000 -1.50000 H17B 2 1.001118 0.856108 1.035322 11.00000 -1.50000 H17C 2 1.085077 0.844131 0.982004 11.00000 -1.50000 AFIX 0 C18 1 0.887605 0.753355 0.677478 11.00000 0.03556 0.02186 = 0.03587 -0.00110 0.00100 0.00276 AFIX 137 H18A 2 0.825669 0.732835 0.671227 11.00000 -1.50000 H18B 2 0.927657 0.703098 0.692749 11.00000 -1.50000 H18C 2 0.900297 0.779472 0.621286 11.00000 -1.50000 AFIX 0 C19 1 0.254194 0.550958 0.180385 11.00000 0.01924 0.02838 = 0.02452 -0.00830 0.00603 -0.00091 C20 1 0.309875 0.487832 0.222812 11.00000 0.02029 0.02358 = 0.02600 -0.01046 0.00379 0.00106 C21 1 0.285759 0.451120 0.300699 11.00000 0.02742 0.02517 = 0.02211 0.00064 0.00669 -0.00510 AFIX 43 H21 2 0.322746 0.407100 0.331174 11.00000 -1.20000 AFIX 0 C22 1 0.208899 0.477467 0.334701 11.00000 0.04223 0.02102 = 0.02239 -0.00437 0.00526 -0.00875 C23 1 0.155258 0.542204 0.288550 11.00000 0.02644 0.03579 = 0.02857 -0.01047 0.01596 -0.00709 AFIX 43 H23 2 0.102968 0.561237 0.311724 11.00000 -1.20000 AFIX 0 C24 1 0.176075 0.579870 0.209358 11.00000 0.02642 0.03308 = 0.03246 -0.00301 0.00282 -0.00474 C25 1 0.395718 0.461637 0.189328 11.00000 0.02927 0.02708 = 0.03078 -0.00402 0.01343 0.00530 AFIX 23 H25A 2 0.397236 0.396166 0.185621 11.00000 -1.20000 H25B 2 0.445559 0.479916 0.234327 11.00000 -1.20000 AFIX 0 C26 1 0.182999 0.440912 0.419921 11.00000 0.05854 0.04388 = 0.02774 -0.00498 0.02037 -0.01747 AFIX 137 H26A 2 0.221407 0.390445 0.439253 11.00000 -1.50000 H26B 2 0.120734 0.421409 0.410341 11.00000 -1.50000 H26C 2 0.189963 0.487039 0.465751 11.00000 -1.50000 AFIX 0 C27 1 0.116430 0.648412 0.161722 11.00000 0.02063 0.04013 = 0.04623 0.00313 0.01309 0.01001 AFIX 137 H27A 2 0.139415 0.707619 0.178324 11.00000 -1.50000 H27B 2 0.056183 0.642158 0.178234 11.00000 -1.50000 H27C 2 0.114645 0.640330 0.097422 11.00000 -1.50000 AFIX 0 C28 1 0.308856 0.711857 0.074447 11.00000 0.01709 0.02576 = 0.02436 -0.00388 0.00740 0.00056 C29 1 0.280015 0.759793 -0.002186 11.00000 0.01856 0.02416 = 0.02885 -0.00088 0.00584 0.00315 C30 1 0.300017 0.850627 -0.001877 11.00000 0.03414 0.02228 = 0.02883 0.00611 0.00037 0.00753 AFIX 43 H30 2 0.281865 0.884735 -0.053651 11.00000 -1.20000 AFIX 0 C31 1 0.345937 0.892235 0.072589 11.00000 0.02931 0.02676 = 0.03786 0.00444 -0.00055 -0.00163 C32 1 0.371191 0.840922 0.147276 11.00000 0.03646 0.02433 = 0.02770 -0.00423 -0.00018 -0.00478 AFIX 43 H32 2 0.401352 0.868971 0.198557 11.00000 -1.20000 AFIX 0 C33 1 0.354769 0.751217 0.150950 11.00000 0.01792 0.02828 = 0.02747 -0.00514 0.00426 0.00263 C34 1 0.230823 0.718640 -0.084870 11.00000 0.03108 0.03431 = 0.02632 0.00501 0.00232 0.00441 AFIX 137 H34A 2 0.214197 0.764947 -0.129174 11.00000 -1.50000 H34B 2 0.176948 0.689089 -0.070035 11.00000 -1.50000 H34C 2 0.269370 0.675152 -0.109110 11.00000 -1.50000 AFIX 0 C35 1 0.369420 0.988551 0.069792 11.00000 0.06815 0.03496 = 0.05095 -0.00187 -0.00569 -0.01118 AFIX 137 H35A 2 0.319396 1.024231 0.085019 11.00000 -1.50000 H35B 2 0.381991 1.004112 0.009908 11.00000 -1.50000 H35C 2 0.422236 1.000316 0.112617 11.00000 -1.50000 AFIX 0 C36 1 0.390045 0.702127 0.234493 11.00000 0.02831 0.03846 = 0.02353 0.00045 -0.00240 0.00039 AFIX 137 H36A 2 0.431442 0.740334 0.272159 11.00000 -1.50000 H36B 2 0.421291 0.648576 0.218946 11.00000 -1.50000 H36C 2 0.340357 0.685527 0.266736 11.00000 -1.50000 AFIX 0 CL1 3 1.004277 1.062938 0.593066 11.00000 0.03638 0.02703 = 0.02442 -0.00732 0.01577 -0.00857 CL2 3 0.446309 0.570794 -0.077350 11.00000 0.03145 0.02996 = 0.03003 0.00717 0.01575 0.01107 SE1 4 0.807193 0.956308 0.631142 11.00000 0.02417 0.02347 = 0.01611 -0.00054 0.00370 0.00322 SE2 4 0.283453 0.585521 0.065416 11.00000 0.02056 0.02410 = 0.02012 -0.00193 0.00606 0.00028 PD1 5 0.903120 0.947220 0.521685 11.00000 0.02728 0.02025 = 0.01723 0.00028 0.00703 -0.00129 PD2 5 0.419279 0.511314 0.069497 11.00000 0.02399 0.02245 = 0.02413 -0.00030 0.01149 0.00376 HKLF 4 REM SK2 in P21/c #14 REM R1 = 0.0446 for 4269 Fo > 4sig(Fo) and 0.0723 for all 5990 data REM 389 parameters refined using 0 restraints END WGHT 0.0285 0.0000 REM Highest difference peak 0.893, deepest hole -0.826, 1-sigma level 0.140 Q1 1 0.8807 0.9484 0.6126 11.00000 0.05 0.89 Q2 1 0.9025 1.1347 0.7656 11.00000 0.05 0.80 Q3 1 1.0846 1.0512 0.5705 11.00000 0.05 0.77 Q4 1 0.8314 0.9436 0.5499 11.00000 0.05 0.75 Q5 1 0.5021 0.5094 -0.0514 11.00000 0.05 0.71 Q6 1 0.8460 0.9322 0.4633 11.00000 0.05 0.67 Q7 1 0.8512 0.9636 0.6868 11.00000 0.05 0.66 Q8 1 0.4081 0.5650 -0.0002 11.00000 0.05 0.66 Q9 1 0.9527 0.9501 0.5783 11.00000 0.05 0.65 Q10 1 0.4656 0.5007 0.1322 11.00000 0.05 0.63 Q11 1 0.3449 0.5612 0.0542 11.00000 0.05 0.62 Q12 1 0.9674 0.9363 0.4969 11.00000 0.05 0.60 Q13 1 0.9541 1.0054 0.5563 11.00000 0.05 0.59 Q14 1 0.8443 1.0223 0.6472 11.00000 0.05 0.59 Q15 1 0.7527 0.9980 0.6385 11.00000 0.05 0.58 Q16 1 0.2865 0.5828 -0.0268 11.00000 0.05 0.57 Q17 1 0.3852 0.5817 0.1281 11.00000 0.05 0.57 Q18 1 0.2191 0.5609 0.0019 11.00000 0.05 0.57 Q19 1 0.7823 0.9677 0.7212 11.00000 0.05 0.56 Q20 1 0.7526 0.9579 0.5676 11.00000 0.05 0.56 ; _database_code_depnum_ccdc_archive 'CCDC 901679' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ups1554ddsk_1_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H50 N2 Pd2 S2 Se2' _chemical_formula_weight 1065.72 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' S S 0.1246 0.1234 '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 8.735(5) _cell_length_b 10.919(5) _cell_length_c 23.272(5) _cell_angle_alpha 98.092(5) _cell_angle_beta 93.574(5) _cell_angle_gamma 96.018(5) _cell_volume 2178.7(17) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9887 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 26.48 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 2.626 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5598 _exptl_absorpt_correction_T_max 0.6941 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33744 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.89 _diffrn_reflns_theta_max 26.50 _reflns_number_total 8908 _reflns_number_gt 7318 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0447P)^2^+0.2485P] 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 0.0043(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8908 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.003 _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 0.3966(3) 0.2020(2) 0.72797(11) 0.0386(6) Uani 1 1 d . . . C2 C 0.2663(3) 0.2575(3) 0.71239(13) 0.0492(7) Uani 1 1 d . . . H2 H 0.1748 0.2080 0.6985 0.059 Uiso 1 1 calc R . . C3 C 0.2724(4) 0.3844(3) 0.71743(14) 0.0579(8) Uani 1 1 d . . . H3 H 0.1847 0.4215 0.7084 0.069 Uiso 1 1 calc R . . C4 C 0.4093(4) 0.4557(3) 0.73591(15) 0.0592(8) Uani 1 1 d . . . H4 H 0.4167 0.5421 0.7393 0.071 Uiso 1 1 calc R . . C5 C 0.5347(4) 0.3978(3) 0.74924(14) 0.0540(8) Uani 1 1 d . . . H5 H 0.6280 0.4467 0.7609 0.065 Uiso 1 1 calc R . . C6 C 0.5920(3) -0.1495(3) 0.74792(14) 0.0498(7) Uani 1 1 d . . . H6A H 0.5679 -0.1076 0.7853 0.060 Uiso 1 1 calc R . . H6B H 0.5042 -0.2101 0.7332 0.060 Uiso 1 1 calc R . . C7 C 0.7273(4) -0.2189(2) 0.75825(13) 0.0473(7) Uani 1 1 d . . . C8 C 0.8495(4) -0.2192(2) 0.72281(13) 0.0485(7) Uani 1 1 d . . . C9 C 0.9713(4) -0.2899(3) 0.72932(15) 0.0581(8) Uani 1 1 d . . . C10 C 0.9672(5) -0.3625(3) 0.77400(17) 0.0694(11) Uani 1 1 d . . . H10 H 1.0459 -0.4122 0.7788 0.083 Uiso 1 1 calc R . . C11 C 0.8508(5) -0.3634(3) 0.81124(16) 0.0665(10) Uani 1 1 d . . . C12 C 0.7321(4) -0.2911(3) 0.80331(14) 0.0573(8) Uani 1 1 d . . . H12 H 0.6537 -0.2905 0.8286 0.069 Uiso 1 1 calc R . . C13 C 1.1068(4) -0.2838(4) 0.69228(19) 0.0815(12) Uani 1 1 d . . . H13A H 1.0715 -0.3113 0.6522 0.122 Uiso 1 1 calc R . . H13B H 1.1800 -0.3366 0.7044 0.122 Uiso 1 1 calc R . . H13C H 1.1553 -0.1996 0.6967 0.122 Uiso 1 1 calc R . . C14 C 0.8540(6) -0.4404(4) 0.86075(19) 0.0984(15) Uani 1 1 d . . . H14A H 0.8876 -0.5197 0.8473 0.148 Uiso 1 1 calc R . . H14B H 0.7523 -0.4529 0.8739 0.148 Uiso 1 1 calc R . . H14C H 0.9241 -0.3974 0.8923 0.148 Uiso 1 1 calc R . . C15 C 0.8403(3) -0.2052(3) 0.59409(13) 0.0476(7) Uani 1 1 d . . . C16 C 0.7333(3) -0.3110(3) 0.57862(13) 0.0520(7) Uani 1 1 d . . . C17 C 0.7465(4) -0.3839(3) 0.52498(14) 0.0604(8) Uani 1 1 d . . . H17 H 0.6780 -0.4559 0.5142 0.072 Uiso 1 1 calc R . . C18 C 0.8553(4) -0.3546(4) 0.48763(15) 0.0693(9) Uani 1 1 d . . . C19 C 0.9537(4) -0.2473(4) 0.50375(16) 0.0707(10) Uani 1 1 d . . . H19 H 1.0256 -0.2244 0.4782 0.085 Uiso 1 1 calc R . . C20 C 0.9505(4) -0.1711(3) 0.55699(15) 0.0589(8) Uani 1 1 d . . . C21 C 0.6066(4) -0.3492(3) 0.61551(16) 0.0729(10) Uani 1 1 d . . . H21A H 0.6505 -0.3773 0.6495 0.109 Uiso 1 1 calc R . . H21B H 0.5367 -0.4153 0.5935 0.109 Uiso 1 1 calc R . . H21C H 0.5516 -0.2792 0.6271 0.109 Uiso 1 1 calc R . . C22 C 0.8635(6) -0.4390(5) 0.43029(18) 0.1080(16) Uani 1 1 d . . . H22A H 0.9652 -0.4642 0.4282 0.162 Uiso 1 1 calc R . . H22B H 0.8410 -0.3948 0.3985 0.162 Uiso 1 1 calc R . . H22C H 0.7894 -0.5113 0.4280 0.162 Uiso 1 1 calc R . . C23 C 1.0647(5) -0.0550(4) 0.57193(18) 0.0864(12) Uani 1 1 d . . . H23A H 1.0097 0.0166 0.5789 0.130 Uiso 1 1 calc R . . H23B H 1.1281 -0.0471 0.5401 0.130 Uiso 1 1 calc R . . H23C H 1.1287 -0.0610 0.6063 0.130 Uiso 1 1 calc R . . C24 C 0.7030(3) 0.2141(3) 0.63110(12) 0.0414(6) Uani 1 1 d . . . C25 C 0.6867(4) 0.2890(3) 0.58745(14) 0.0582(8) Uani 1 1 d . . . H25 H 0.7531 0.3619 0.5887 0.070 Uiso 1 1 calc R . . C26 C 0.5730(4) 0.2554(4) 0.54284(15) 0.0721(10) Uani 1 1 d . . . H26 H 0.5633 0.3043 0.5135 0.087 Uiso 1 1 calc R . . C27 C 0.4746(4) 0.1496(3) 0.54200(15) 0.0717(10) Uani 1 1 d . . . H27 H 0.3944 0.1264 0.5130 0.086 Uiso 1 1 calc R . . C28 C 0.4972(4) 0.0783(3) 0.58520(13) 0.0567(8) Uani 1 1 d . . . H28 H 0.4311 0.0054 0.5843 0.068 Uiso 1 1 calc R . . C29 C 0.9547(3) 0.1510(3) 0.79258(13) 0.0466(7) Uani 1 1 d . . . H29A H 0.9978 0.1170 0.7572 0.056 Uiso 1 1 calc R . . H29B H 1.0226 0.2249 0.8097 0.056 Uiso 1 1 calc R . . C30 C 0.9582(3) 0.0581(2) 0.83365(12) 0.0415(6) Uani 1 1 d . . . C31 C 0.8455(3) 0.0448(2) 0.87250(12) 0.0414(6) Uani 1 1 d . . . C32 C 0.8553(4) -0.0332(3) 0.91516(13) 0.0491(7) Uani 1 1 d . . . C33 C 0.9829(4) -0.0967(3) 0.91781(14) 0.0561(8) Uani 1 1 d . . . H33 H 0.9932 -0.1469 0.9467 0.067 Uiso 1 1 calc R . . C34 C 1.0966(4) -0.0888(3) 0.87915(14) 0.0528(8) Uani 1 1 d . . . C35 C 1.0814(3) -0.0125(3) 0.83715(13) 0.0479(7) Uani 1 1 d . . . H35 H 1.1557 -0.0081 0.8104 0.057 Uiso 1 1 calc R . . C36 C 0.7284(4) -0.0497(3) 0.95546(15) 0.0692(10) Uani 1 1 d . . . H36A H 0.6357 -0.0897 0.9333 0.104 Uiso 1 1 calc R . . H36B H 0.7097 0.0303 0.9749 0.104 Uiso 1 1 calc R . . H36C H 0.7589 -0.1002 0.9838 0.104 Uiso 1 1 calc R . . C37 C 1.2325(4) -0.1621(4) 0.88185(18) 0.0771(11) Uani 1 1 d . . . H37A H 1.2877 -0.1406 0.9195 0.116 Uiso 1 1 calc R . . H37B H 1.2998 -0.1429 0.8525 0.116 Uiso 1 1 calc R . . H37C H 1.1969 -0.2494 0.8753 0.116 Uiso 1 1 calc R . . C38 C 0.6648(3) 0.2468(2) 0.92820(12) 0.0435(6) Uani 1 1 d . . . C39 C 0.5172(4) 0.2613(3) 0.94613(14) 0.0524(7) Uani 1 1 d . . . C40 C 0.5052(4) 0.3331(3) 0.99988(15) 0.0616(9) Uani 1 1 d . . . H40 H 0.4077 0.3423 1.0126 0.074 Uiso 1 1 calc R . . C41 C 0.6338(5) 0.3909(3) 1.03498(14) 0.0625(9) Uani 1 1 d . . . C42 C 0.7752(4) 0.3796(3) 1.01430(14) 0.0609(9) Uani 1 1 d . . . H42 H 0.8619 0.4209 1.0369 0.073 Uiso 1 1 calc R . . C43 C 0.7968(4) 0.3094(3) 0.96115(13) 0.0500(7) Uani 1 1 d . . . C44 C 0.3734(4) 0.2006(4) 0.91053(17) 0.0725(10) Uani 1 1 d . . . H44A H 0.3745 0.2225 0.8720 0.109 Uiso 1 1 calc R . . H44B H 0.2847 0.2287 0.9284 0.109 Uiso 1 1 calc R . . H44C H 0.3689 0.1119 0.9084 0.109 Uiso 1 1 calc R . . C45 C 0.6180(6) 0.4623(4) 1.09447(17) 0.0927(13) Uani 1 1 d . . . H45A H 0.6000 0.4048 1.1216 0.139 Uiso 1 1 calc R . . H45B H 0.5327 0.5106 1.0924 0.139 Uiso 1 1 calc R . . H45C H 0.7112 0.5166 1.1071 0.139 Uiso 1 1 calc R . . C46 C 0.9575(4) 0.3034(3) 0.94284(16) 0.0641(9) Uani 1 1 d . . . H46A H 0.9892 0.2235 0.9473 0.096 Uiso 1 1 calc R . . H46B H 1.0264 0.3676 0.9666 0.096 Uiso 1 1 calc R . . H46C H 0.9597 0.3152 0.9028 0.096 Uiso 1 1 calc R . . N1 N 0.5309(2) 0.2733(2) 0.74639(10) 0.0397(5) Uani 1 1 d . . . N2 N 0.6096(3) 0.1077(2) 0.62890(10) 0.0421(5) Uani 1 1 d . . . S1 S 0.38149(8) 0.04095(6) 0.72466(3) 0.04803(18) Uani 1 1 d . . . S2 S 0.84919(8) 0.25996(8) 0.68662(3) 0.05121(19) Uani 1 1 d . . . Se1 Se 0.84937(3) -0.09978(3) 0.669424(14) 0.04669(9) Uani 1 1 d . . . Se2 Se 0.66723(3) 0.12776(3) 0.857578(12) 0.04231(9) Uani 1 1 d . . . Pd1 Pd 0.61100(2) -0.020562(18) 0.692650(9) 0.04000(8) Uani 1 1 d . . . Pd2 Pd 0.74670(2) 0.204511(19) 0.770242(9) 0.03893(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 C1 0.0337(13) 0.0445(14) 0.0389(15) 0.0085(12) 0.0038(11) 0.0068(12) C2 0.0316(14) 0.0586(18) 0.0591(18) 0.0141(15) 0.0003(13) 0.0072(13) C3 0.0483(18) 0.063(2) 0.068(2) 0.0167(16) 0.0007(15) 0.0257(16) C4 0.061(2) 0.0402(16) 0.077(2) 0.0061(15) -0.0012(17) 0.0154(15) C5 0.0536(18) 0.0433(16) 0.063(2) 0.0066(14) -0.0062(15) 0.0046(14) C6 0.0553(18) 0.0417(15) 0.0566(18) 0.0176(14) 0.0082(14) 0.0094(14) C7 0.0588(18) 0.0317(14) 0.0487(17) 0.0021(12) -0.0083(14) 0.0059(13) C8 0.0578(18) 0.0338(14) 0.0517(18) 0.0013(13) -0.0117(15) 0.0111(13) C9 0.065(2) 0.0362(15) 0.069(2) -0.0056(15) -0.0165(17) 0.0153(15) C10 0.080(3) 0.0417(17) 0.079(3) -0.0034(17) -0.037(2) 0.0175(17) C11 0.088(3) 0.0407(17) 0.066(2) 0.0090(15) -0.029(2) 0.0049(17) C12 0.077(2) 0.0410(16) 0.0519(19) 0.0109(14) -0.0139(16) 0.0009(15) C13 0.072(2) 0.073(2) 0.102(3) 0.001(2) -0.008(2) 0.041(2) C14 0.124(4) 0.078(3) 0.092(3) 0.037(2) -0.043(3) 0.005(3) C15 0.0445(16) 0.0469(16) 0.0524(17) 0.0108(13) -0.0003(13) 0.0083(13) C16 0.0497(17) 0.0535(17) 0.0531(19) 0.0098(15) 0.0000(14) 0.0069(14) C17 0.067(2) 0.0553(19) 0.055(2) 0.0017(16) -0.0068(17) 0.0052(16) C18 0.072(2) 0.083(3) 0.053(2) 0.0050(18) -0.0010(18) 0.016(2) C19 0.060(2) 0.097(3) 0.059(2) 0.017(2) 0.0117(17) 0.013(2) C20 0.0499(18) 0.067(2) 0.062(2) 0.0185(17) 0.0012(16) 0.0086(16) C21 0.069(2) 0.072(2) 0.069(2) 0.0005(18) 0.0072(18) -0.0200(19) C22 0.121(4) 0.131(4) 0.063(3) -0.015(3) 0.016(3) 0.010(3) C23 0.068(2) 0.097(3) 0.090(3) 0.021(2) 0.016(2) -0.021(2) C24 0.0364(14) 0.0493(16) 0.0423(15) 0.0144(12) 0.0046(12) 0.0113(12) C25 0.0582(19) 0.0607(19) 0.059(2) 0.0278(16) -0.0042(15) 0.0013(15) C26 0.082(3) 0.081(2) 0.057(2) 0.0332(19) -0.0157(19) 0.005(2) C27 0.073(2) 0.084(3) 0.056(2) 0.0163(19) -0.0204(18) 0.005(2) C28 0.0600(19) 0.0557(19) 0.0508(19) 0.0055(15) -0.0073(15) 0.0003(15) C29 0.0343(14) 0.0634(18) 0.0453(16) 0.0188(14) -0.0011(12) 0.0085(13) C30 0.0406(15) 0.0431(15) 0.0391(15) 0.0046(12) -0.0061(12) 0.0041(12) C31 0.0447(15) 0.0413(14) 0.0371(15) 0.0054(12) -0.0039(12) 0.0048(12) C32 0.0595(19) 0.0430(15) 0.0423(16) 0.0058(13) -0.0036(14) 0.0001(14) C33 0.074(2) 0.0425(16) 0.0513(19) 0.0134(14) -0.0140(17) 0.0062(16) C34 0.0569(19) 0.0425(16) 0.0575(19) 0.0052(14) -0.0106(15) 0.0104(14) C35 0.0441(16) 0.0503(17) 0.0489(17) 0.0054(14) -0.0046(13) 0.0109(13) C36 0.087(3) 0.070(2) 0.055(2) 0.0266(17) 0.0121(18) 0.0016(19) C37 0.077(2) 0.069(2) 0.090(3) 0.018(2) -0.011(2) 0.029(2) C38 0.0474(16) 0.0413(15) 0.0426(16) 0.0102(12) 0.0020(13) 0.0045(13) C39 0.0524(18) 0.0506(17) 0.0554(19) 0.0087(14) 0.0047(15) 0.0101(14) C40 0.073(2) 0.0559(19) 0.062(2) 0.0138(16) 0.0175(18) 0.0217(17) C41 0.094(3) 0.0434(17) 0.053(2) 0.0068(15) 0.0009(19) 0.0237(18) C42 0.079(2) 0.0456(17) 0.055(2) 0.0051(15) -0.0117(18) 0.0079(17) C43 0.0554(18) 0.0409(15) 0.0523(18) 0.0092(13) -0.0080(14) 0.0040(13) C44 0.0482(19) 0.081(2) 0.085(3) -0.002(2) 0.0039(18) 0.0093(18) C45 0.146(4) 0.074(2) 0.060(2) -0.0008(19) 0.001(2) 0.041(3) C46 0.0518(19) 0.0564(19) 0.078(2) 0.0056(17) -0.0083(17) -0.0055(15) N1 0.0355(12) 0.0408(12) 0.0421(13) 0.0053(10) -0.0027(10) 0.0061(10) N2 0.0405(12) 0.0445(13) 0.0433(13) 0.0106(10) 0.0010(10) 0.0100(11) S1 0.0378(4) 0.0417(4) 0.0662(5) 0.0134(3) 0.0070(3) 0.0029(3) S2 0.0354(4) 0.0665(5) 0.0542(4) 0.0273(4) -0.0038(3) -0.0032(3) Se1 0.04315(17) 0.03735(15) 0.0602(2) 0.00698(13) 0.00244(13) 0.00861(12) Se2 0.03689(15) 0.04937(17) 0.04020(16) 0.00813(12) -0.00015(11) 0.00262(12) Pd1 0.04014(13) 0.03398(12) 0.04768(14) 0.01070(9) 0.00247(9) 0.00701(9) Pd2 0.03286(12) 0.04481(13) 0.03990(13) 0.01156(9) -0.00381(9) 0.00486(9) _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 N1 1.348(3) . ? C1 C2 1.396(4) . ? C1 S1 1.740(3) . ? C2 C3 1.369(4) . ? C2 H2 0.9300 . ? C3 C4 1.366(4) . ? C3 H3 0.9300 . ? C4 C5 1.362(4) . ? C4 H4 0.9300 . ? C5 N1 1.348(3) . ? C5 H5 0.9300 . ? C6 C7 1.495(4) . ? C6 Pd1 2.037(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.389(4) . ? C7 C12 1.399(4) . ? C8 C9 1.391(4) . ? C8 Se1 1.924(3) . ? C9 C10 1.394(5) . ? C9 C13 1.509(5) . ? C10 C11 1.376(5) . ? C10 H10 0.9300 . ? C11 C12 1.387(5) . ? C11 C14 1.519(5) . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C20 1.390(4) . ? C15 C16 1.397(4) . ? C15 Se1 1.950(3) . ? C16 C17 1.401(4) . ? C16 C21 1.502(4) . ? C17 C18 1.371(5) . ? C17 H17 0.9300 . ? C18 C19 1.370(5) . ? C18 C22 1.522(5) . ? C19 C20 1.396(5) . ? C19 H19 0.9300 . ? C20 C23 1.513(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N2 1.340(3) . ? C24 C25 1.401(4) . ? C24 S2 1.741(3) . ? C25 C26 1.374(5) . ? C25 H25 0.9300 . ? C26 C27 1.362(5) . ? C26 H26 0.9300 . ? C27 C28 1.372(4) . ? C27 H27 0.9300 . ? C28 N2 1.349(4) . ? C28 H28 0.9300 . ? C29 C30 1.490(4) . ? C29 Pd2 2.025(3) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.388(4) . ? C30 C35 1.393(4) . ? C31 C32 1.400(4) . ? C31 Se2 1.919(3) . ? C32 C33 1.376(5) . ? C32 C36 1.509(4) . ? C33 C34 1.385(5) . ? C33 H33 0.9300 . ? C34 C35 1.379(4) . ? C34 C37 1.503(5) . ? C35 H35 0.9300 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.398(4) . ? C38 C43 1.401(4) . ? C38 Se2 1.949(3) . ? C39 C40 1.395(5) . ? C39 C44 1.498(4) . ? C40 C41 1.385(5) . ? C40 H40 0.9300 . ? C41 C42 1.365(5) . ? C41 C45 1.512(5) . ? C42 C43 1.395(4) . ? C42 H42 0.9300 . ? C43 C46 1.497(4) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? N1 Pd2 2.171(2) . ? N2 Pd1 2.179(2) . ? S1 Pd1 2.3136(13) . ? S2 Pd2 2.3218(9) . ? Se1 Pd1 2.4005(12) . ? Se2 Pd2 2.4184(6) . ? Pd1 Pd2 2.9289(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 119.9(2) . . ? N1 C1 S1 120.96(19) . . ? C2 C1 S1 119.1(2) . . ? C3 C2 C1 120.5(3) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 119.0(3) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C5 C4 C3 118.7(3) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 123.6(3) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C7 C6 Pd1 118.1(2) . . ? C7 C6 H6A 107.8 . . ? Pd1 C6 H6A 107.8 . . ? C7 C6 H6B 107.8 . . ? Pd1 C6 H6B 107.8 . . ? H6A C6 H6B 107.1 . . ? C8 C7 C12 117.2(3) . . ? C8 C7 C6 122.2(3) . . ? C12 C7 C6 120.5(3) . . ? C7 C8 C9 123.1(3) . . ? C7 C8 Se1 114.5(2) . . ? C9 C8 Se1 122.1(3) . . ? C8 C9 C10 116.9(3) . . ? C8 C9 C13 122.2(3) . . ? C10 C9 C13 120.8(3) . . ? C11 C10 C9 122.4(3) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C10 C11 C12 118.7(3) . . ? C10 C11 C14 120.6(4) . . ? C12 C11 C14 120.7(4) . . ? C11 C12 C7 121.7(3) . . ? C11 C12 H12 119.2 . . ? C7 C12 H12 119.2 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 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 . . ? C20 C15 C16 121.6(3) . . ? C20 C15 Se1 115.8(2) . . ? C16 C15 Se1 122.6(2) . . ? C15 C16 C17 116.8(3) . . ? C15 C16 C21 124.1(3) . . ? C17 C16 C21 119.1(3) . . ? C18 C17 C16 123.3(3) . . ? C18 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? C19 C18 C17 117.7(3) . . ? C19 C18 C22 122.0(4) . . ? C17 C18 C22 120.3(4) . . ? C18 C19 C20 122.6(3) . . ? C18 C19 H19 118.7 . . ? C20 C19 H19 118.7 . . ? C15 C20 C19 118.0(3) . . ? C15 C20 C23 122.7(3) . . ? C19 C20 C23 119.4(3) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C24 C25 120.1(3) . . ? N2 C24 S2 121.2(2) . . ? C25 C24 S2 118.7(2) . . ? C26 C25 C24 120.3(3) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 119.4(3) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C28 118.0(3) . . ? C26 C27 H27 121.0 . . ? C28 C27 H27 121.0 . . ? N2 C28 C27 123.9(3) . . ? N2 C28 H28 118.1 . . ? C27 C28 H28 118.1 . . ? C30 C29 Pd2 117.28(19) . . ? C30 C29 H29A 108.0 . . ? Pd2 C29 H29A 108.0 . . ? C30 C29 H29B 108.0 . . ? Pd2 C29 H29B 108.0 . . ? H29A C29 H29B 107.2 . . ? C31 C30 C35 117.5(3) . . ? C31 C30 C29 121.6(2) . . ? C35 C30 C29 120.7(3) . . ? C30 C31 C32 122.2(3) . . ? C30 C31 Se2 114.4(2) . . ? C32 C31 Se2 123.1(2) . . ? C33 C32 C31 117.4(3) . . ? C33 C32 C36 121.4(3) . . ? C31 C32 C36 121.2(3) . . ? C32 C33 C34 122.5(3) . . ? C32 C33 H33 118.8 . . ? C34 C33 H33 118.8 . . ? C35 C34 C33 118.3(3) . . ? C35 C34 C37 120.3(3) . . ? C33 C34 C37 121.5(3) . . ? C34 C35 C30 122.0(3) . . ? C34 C35 H35 119.0 . . ? C30 C35 H35 119.0 . . ? C32 C36 H36A 109.5 . . ? C32 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C32 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C43 121.1(3) . . ? C39 C38 Se2 114.2(2) . . ? C43 C38 Se2 124.7(2) . . ? C40 C39 C38 118.1(3) . . ? C40 C39 C44 119.5(3) . . ? C38 C39 C44 122.5(3) . . ? C41 C40 C39 122.2(3) . . ? C41 C40 H40 118.9 . . ? C39 C40 H40 118.9 . . ? C42 C41 C40 117.6(3) . . ? C42 C41 C45 121.2(4) . . ? C40 C41 C45 121.1(4) . . ? C41 C42 C43 123.6(3) . . ? C41 C42 H42 118.2 . . ? C43 C42 H42 118.2 . . ? C42 C43 C38 117.2(3) . . ? C42 C43 C46 119.0(3) . . ? C38 C43 C46 123.8(3) . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C41 C45 H45A 109.5 . . ? C41 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C41 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C5 N1 C1 118.3(2) . . ? C5 N1 Pd2 116.28(18) . . ? C1 N1 Pd2 125.41(17) . . ? C24 N2 C28 118.3(2) . . ? C24 N2 Pd1 126.32(18) . . ? C28 N2 Pd1 115.32(19) . . ? C1 S1 Pd1 106.55(9) . . ? C24 S2 Pd2 105.59(9) . . ? C8 Se1 C15 102.35(12) . . ? C8 Se1 Pd1 97.89(10) . . ? C15 Se1 Pd1 114.57(9) . . ? C31 Se2 C38 103.39(12) . . ? C31 Se2 Pd2 97.09(9) . . ? C38 Se2 Pd2 118.57(8) . . ? C6 Pd1 N2 174.19(11) . . ? C6 Pd1 S1 86.89(9) . . ? N2 Pd1 S1 90.40(6) . . ? C6 Pd1 Se1 85.94(9) . . ? N2 Pd1 Se1 96.86(6) . . ? S1 Pd1 Se1 172.71(2) . . ? C6 Pd1 Pd2 102.38(10) . . ? N2 Pd1 Pd2 82.38(7) . . ? S1 Pd1 Pd2 83.27(3) . . ? Se1 Pd1 Pd2 96.95(3) . . ? C29 Pd2 N1 176.47(10) . . ? C29 Pd2 S2 87.70(8) . . ? N1 Pd2 S2 90.55(7) . . ? C29 Pd2 Se2 85.05(8) . . ? N1 Pd2 Se2 96.85(6) . . ? S2 Pd2 Se2 172.12(2) . . ? C29 Pd2 Pd1 99.58(9) . . ? N1 Pd2 Pd1 83.28(6) . . ? S2 Pd2 Pd1 84.02(3) . . ? Se2 Pd2 Pd1 94.12(2) . . ? 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 N1 C1 C2 C3 -2.1(4) . . . . ? S1 C1 C2 C3 176.6(2) . . . . ? C1 C2 C3 C4 2.4(5) . . . . ? C2 C3 C4 C5 -0.6(5) . . . . ? C3 C4 C5 N1 -1.4(5) . . . . ? Pd1 C6 C7 C8 -14.5(4) . . . . ? Pd1 C6 C7 C12 168.2(2) . . . . ? C12 C7 C8 C9 1.9(4) . . . . ? C6 C7 C8 C9 -175.6(3) . . . . ? C12 C7 C8 Se1 -171.4(2) . . . . ? C6 C7 C8 Se1 11.2(4) . . . . ? C7 C8 C9 C10 -0.1(4) . . . . ? Se1 C8 C9 C10 172.7(2) . . . . ? C7 C8 C9 C13 -176.8(3) . . . . ? Se1 C8 C9 C13 -4.0(4) . . . . ? C8 C9 C10 C11 -1.4(5) . . . . ? C13 C9 C10 C11 175.3(3) . . . . ? C9 C10 C11 C12 1.2(5) . . . . ? C9 C10 C11 C14 -177.7(3) . . . . ? C10 C11 C12 C7 0.7(5) . . . . ? C14 C11 C12 C7 179.6(3) . . . . ? C8 C7 C12 C11 -2.2(4) . . . . ? C6 C7 C12 C11 175.3(3) . . . . ? C20 C15 C16 C17 2.6(4) . . . . ? Se1 C15 C16 C17 -175.3(2) . . . . ? C20 C15 C16 C21 -176.8(3) . . . . ? Se1 C15 C16 C21 5.3(4) . . . . ? C15 C16 C17 C18 -1.5(5) . . . . ? C21 C16 C17 C18 178.0(3) . . . . ? C16 C17 C18 C19 -1.0(5) . . . . ? C16 C17 C18 C22 179.5(4) . . . . ? C17 C18 C19 C20 2.5(6) . . . . ? C22 C18 C19 C20 -178.0(4) . . . . ? C16 C15 C20 C19 -1.2(5) . . . . ? Se1 C15 C20 C19 176.8(2) . . . . ? C16 C15 C20 C23 178.2(3) . . . . ? Se1 C15 C20 C23 -3.8(4) . . . . ? C18 C19 C20 C15 -1.4(5) . . . . ? C18 C19 C20 C23 179.1(3) . . . . ? N2 C24 C25 C26 1.3(5) . . . . ? S2 C24 C25 C26 179.7(3) . . . . ? C24 C25 C26 C27 1.2(6) . . . . ? C25 C26 C27 C28 -2.3(6) . . . . ? C26 C27 C28 N2 1.1(6) . . . . ? Pd2 C29 C30 C31 -25.1(4) . . . . ? Pd2 C29 C30 C35 159.5(2) . . . . ? C35 C30 C31 C32 1.9(4) . . . . ? C29 C30 C31 C32 -173.6(3) . . . . ? C35 C30 C31 Se2 -171.9(2) . . . . ? C29 C30 C31 Se2 12.6(3) . . . . ? C30 C31 C32 C33 0.5(4) . . . . ? Se2 C31 C32 C33 173.8(2) . . . . ? C30 C31 C32 C36 -177.7(3) . . . . ? Se2 C31 C32 C36 -4.4(4) . . . . ? C31 C32 C33 C34 -2.1(5) . . . . ? C36 C32 C33 C34 176.2(3) . . . . ? C32 C33 C34 C35 1.0(5) . . . . ? C32 C33 C34 C37 -178.2(3) . . . . ? C33 C34 C35 C30 1.6(4) . . . . ? C37 C34 C35 C30 -179.2(3) . . . . ? C31 C30 C35 C34 -3.0(4) . . . . ? C29 C30 C35 C34 172.5(3) . . . . ? C43 C38 C39 C40 -4.4(4) . . . . ? Se2 C38 C39 C40 172.4(2) . . . . ? C43 C38 C39 C44 177.0(3) . . . . ? Se2 C38 C39 C44 -6.1(4) . . . . ? C38 C39 C40 C41 1.0(5) . . . . ? C44 C39 C40 C41 179.6(3) . . . . ? C39 C40 C41 C42 2.4(5) . . . . ? C39 C40 C41 C45 -176.6(3) . . . . ? C40 C41 C42 C43 -2.5(5) . . . . ? C45 C41 C42 C43 176.5(3) . . . . ? C41 C42 C43 C38 -0.8(4) . . . . ? C41 C42 C43 C46 -179.9(3) . . . . ? C39 C38 C43 C42 4.3(4) . . . . ? Se2 C38 C43 C42 -172.2(2) . . . . ? C39 C38 C43 C46 -176.6(3) . . . . ? Se2 C38 C43 C46 6.9(4) . . . . ? C4 C5 N1 C1 1.7(5) . . . . ? C4 C5 N1 Pd2 -179.8(3) . . . . ? C2 C1 N1 C5 0.1(4) . . . . ? S1 C1 N1 C5 -178.6(2) . . . . ? C2 C1 N1 Pd2 -178.26(19) . . . . ? S1 C1 N1 Pd2 3.1(3) . . . . ? C25 C24 N2 C28 -2.6(4) . . . . ? S2 C24 N2 C28 179.1(2) . . . . ? C25 C24 N2 Pd1 -178.6(2) . . . . ? S2 C24 N2 Pd1 3.0(3) . . . . ? C27 C28 N2 C24 1.4(5) . . . . ? C27 C28 N2 Pd1 177.9(3) . . . . ? N1 C1 S1 Pd1 -38.5(2) . . . . ? C2 C1 S1 Pd1 142.9(2) . . . . ? N2 C24 S2 Pd2 -38.2(2) . . . . ? C25 C24 S2 Pd2 143.4(2) . . . . ? C7 C8 Se1 C15 -120.8(2) . . . . ? C9 C8 Se1 C15 65.8(3) . . . . ? C7 C8 Se1 Pd1 -3.4(2) . . . . ? C9 C8 Se1 Pd1 -176.8(2) . . . . ? C20 C15 Se1 C8 -128.9(2) . . . . ? C16 C15 Se1 C8 49.1(3) . . . . ? C20 C15 Se1 Pd1 126.4(2) . . . . ? C16 C15 Se1 Pd1 -55.6(3) . . . . ? C30 C31 Se2 C38 -119.1(2) . . . . ? C32 C31 Se2 C38 67.2(3) . . . . ? C30 C31 Se2 Pd2 2.6(2) . . . . ? C32 C31 Se2 Pd2 -171.1(2) . . . . ? C39 C38 Se2 C31 -141.7(2) . . . . ? C43 C38 Se2 C31 35.1(3) . . . . ? C39 C38 Se2 Pd2 112.4(2) . . . . ? C43 C38 Se2 Pd2 -70.8(2) . . . . ? C7 C6 Pd1 N2 127.7(9) . . . . ? C7 C6 Pd1 S1 -169.9(2) . . . . ? C7 C6 Pd1 Se1 8.7(2) . . . . ? C7 C6 Pd1 Pd2 -87.5(2) . . . . ? C24 N2 Pd1 C6 170.3(10) . . . . ? C28 N2 Pd1 C6 -5.9(11) . . . . ? C24 N2 Pd1 S1 108.1(2) . . . . ? C28 N2 Pd1 S1 -68.1(2) . . . . ? C24 N2 Pd1 Se1 -71.2(2) . . . . ? C28 N2 Pd1 Se1 112.7(2) . . . . ? C24 N2 Pd1 Pd2 25.0(2) . . . . ? C28 N2 Pd1 Pd2 -151.2(2) . . . . ? C1 S1 Pd1 C6 143.15(13) . . . . ? C1 S1 Pd1 N2 -41.99(11) . . . . ? C1 S1 Pd1 Se1 132.40(17) . . . . ? C1 S1 Pd1 Pd2 40.29(10) . . . . ? C8 Se1 Pd1 C6 -2.69(12) . . . . ? C15 Se1 Pd1 C6 104.81(13) . . . . ? C8 Se1 Pd1 N2 -177.58(10) . . . . ? C15 Se1 Pd1 N2 -70.08(11) . . . . ? C8 Se1 Pd1 S1 8.07(19) . . . . ? C15 Se1 Pd1 S1 115.57(19) . . . . ? C8 Se1 Pd1 Pd2 99.30(9) . . . . ? C15 Se1 Pd1 Pd2 -153.20(9) . . . . ? C30 C29 Pd2 N1 142.7(15) . . . . ? C30 C29 Pd2 S2 -156.9(2) . . . . ? C30 C29 Pd2 Se2 20.0(2) . . . . ? C30 C29 Pd2 Pd1 -73.4(2) . . . . ? C5 N1 Pd2 C29 -9.4(17) . . . . ? C1 N1 Pd2 C29 169.0(16) . . . . ? C5 N1 Pd2 S2 -69.7(2) . . . . ? C1 N1 Pd2 S2 108.7(2) . . . . ? C5 N1 Pd2 Se2 113.0(2) . . . . ? C1 N1 Pd2 Se2 -68.6(2) . . . . ? C5 N1 Pd2 Pd1 -153.6(2) . . . . ? C1 N1 Pd2 Pd1 24.8(2) . . . . ? C24 S2 Pd2 C29 140.08(13) . . . . ? C24 S2 Pd2 N1 -42.99(12) . . . . ? C24 S2 Pd2 Se2 116.87(17) . . . . ? C24 S2 Pd2 Pd1 40.19(10) . . . . ? C31 Se2 Pd2 C29 -11.16(12) . . . . ? C38 Se2 Pd2 C29 98.32(13) . . . . ? C31 Se2 Pd2 N1 171.83(10) . . . . ? C38 Se2 Pd2 N1 -78.69(11) . . . . ? C31 Se2 Pd2 S2 12.12(18) . . . . ? C38 Se2 Pd2 S2 121.61(18) . . . . ? C31 Se2 Pd2 Pd1 88.12(9) . . . . ? C38 Se2 Pd2 Pd1 -162.39(9) . . . . ? C6 Pd1 Pd2 C29 65.27(12) . . . . ? N2 Pd1 Pd2 C29 -118.11(10) . . . . ? S1 Pd1 Pd2 C29 150.58(8) . . . . ? Se1 Pd1 Pd2 C29 -22.08(8) . . . . ? C6 Pd1 Pd2 N1 -116.82(10) . . . . ? N2 Pd1 Pd2 N1 59.80(8) . . . . ? S1 Pd1 Pd2 N1 -31.51(6) . . . . ? Se1 Pd1 Pd2 N1 155.83(6) . . . . ? C6 Pd1 Pd2 S2 151.91(9) . . . . ? N2 Pd1 Pd2 S2 -31.46(6) . . . . ? S1 Pd1 Pd2 S2 -122.78(3) . . . . ? Se1 Pd1 Pd2 S2 64.57(3) . . . . ? C6 Pd1 Pd2 Se2 -20.40(9) . . . . ? N2 Pd1 Pd2 Se2 156.22(6) . . . . ? S1 Pd1 Pd2 Se2 64.91(2) . . . . ? Se1 Pd1 Pd2 Se2 -107.749(19) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.756 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.184 _iucr_refine_instructions_details ; TITL ups1554DDsk_1_0m in P-1 CELL 0.71073 8.7350 10.9190 23.2720 98.092 93.574 96.018 ZERR 2.00 0.0050 0.0050 0.0050 0.005 0.005 0.005 LATT 1 SFAC C H N S SE PD UNIT 92 100 4 4 4 4 MERG 2 FMAP 2 PLAN 25 SIZE 0.15 0.15 0.25 ACTA BOND $H CONF LIST 4 L.S. 4 TEMP 25.00 WGHT 0.044700 0.248500 EXTI 0.004266 FVAR 0.07970 C1 1 0.396565 0.201953 0.727972 11.00000 0.03372 0.04453 = 0.03890 0.00845 0.00381 0.00676 C2 1 0.266342 0.257541 0.712390 11.00000 0.03160 0.05864 = 0.05906 0.01413 0.00030 0.00721 AFIX 43 H2 2 0.174773 0.207995 0.698482 11.00000 -1.20000 AFIX 0 C3 1 0.272412 0.384422 0.717429 11.00000 0.04833 0.06269 = 0.06830 0.01672 0.00071 0.02571 AFIX 43 H3 2 0.184668 0.421546 0.708405 11.00000 -1.20000 AFIX 0 C4 1 0.409273 0.455705 0.735908 11.00000 0.06114 0.04019 = 0.07665 0.00606 -0.00124 0.01541 AFIX 43 H4 2 0.416650 0.542051 0.739316 11.00000 -1.20000 AFIX 0 C5 1 0.534671 0.397762 0.749236 11.00000 0.05356 0.04334 = 0.06316 0.00659 -0.00619 0.00462 AFIX 43 H5 2 0.628028 0.446723 0.760942 11.00000 -1.20000 AFIX 0 C6 1 0.592014 -0.149468 0.747921 11.00000 0.05532 0.04169 = 0.05659 0.01756 0.00815 0.00944 AFIX 23 H6A 2 0.567917 -0.107641 0.785305 11.00000 -1.20000 H6B 2 0.504246 -0.210130 0.733184 11.00000 -1.20000 AFIX 0 C7 1 0.727334 -0.218903 0.758254 11.00000 0.05880 0.03173 = 0.04873 0.00210 -0.00828 0.00594 C8 1 0.849480 -0.219206 0.722806 11.00000 0.05782 0.03378 = 0.05171 0.00128 -0.01174 0.01109 C9 1 0.971328 -0.289862 0.729322 11.00000 0.06456 0.03619 = 0.06892 -0.00559 -0.01655 0.01529 C10 1 0.967181 -0.362503 0.774000 11.00000 0.08049 0.04170 = 0.07924 -0.00338 -0.03683 0.01746 AFIX 43 H10 2 1.045890 -0.412157 0.778821 11.00000 -1.20000 AFIX 0 C11 1 0.850847 -0.363430 0.811245 11.00000 0.08829 0.04066 = 0.06576 0.00903 -0.02943 0.00492 C12 1 0.732133 -0.291059 0.803308 11.00000 0.07656 0.04099 = 0.05189 0.01093 -0.01385 0.00090 AFIX 43 H12 2 0.653740 -0.290491 0.828580 11.00000 -1.20000 AFIX 0 C13 1 1.106839 -0.283800 0.692277 11.00000 0.07176 0.07255 = 0.10213 0.00103 -0.00751 0.04147 AFIX 137 H13A 2 1.071484 -0.311305 0.652191 11.00000 -1.50000 H13B 2 1.179985 -0.336648 0.704408 11.00000 -1.50000 H13C 2 1.155286 -0.199589 0.696656 11.00000 -1.50000 AFIX 0 C14 1 0.853991 -0.440430 0.860748 11.00000 0.12406 0.07817 = 0.09192 0.03675 -0.04347 0.00528 AFIX 137 H14A 2 0.887599 -0.519689 0.847297 11.00000 -1.50000 H14B 2 0.752300 -0.452860 0.873909 11.00000 -1.50000 H14C 2 0.924061 -0.397392 0.892316 11.00000 -1.50000 AFIX 0 C15 1 0.840263 -0.205218 0.594089 11.00000 0.04449 0.04689 = 0.05241 0.01078 -0.00029 0.00831 C16 1 0.733274 -0.311011 0.578624 11.00000 0.04968 0.05351 = 0.05312 0.00982 -0.00003 0.00687 C17 1 0.746466 -0.383946 0.524984 11.00000 0.06722 0.05527 = 0.05484 0.00172 -0.00681 0.00525 AFIX 43 H17 2 0.678005 -0.455879 0.514182 11.00000 -1.20000 AFIX 0 C18 1 0.855274 -0.354556 0.487625 11.00000 0.07185 0.08284 = 0.05270 0.00504 -0.00095 0.01641 C19 1 0.953738 -0.247305 0.503747 11.00000 0.06010 0.09660 = 0.05854 0.01667 0.01166 0.01295 AFIX 43 H19 2 1.025551 -0.224391 0.478204 11.00000 -1.20000 AFIX 0 C20 1 0.950530 -0.171077 0.556989 11.00000 0.04992 0.06714 = 0.06225 0.01854 0.00121 0.00864 C21 1 0.606591 -0.349183 0.615505 11.00000 0.06885 0.07171 = 0.06946 0.00046 0.00723 -0.02004 AFIX 137 H21A 2 0.650491 -0.377350 0.649465 11.00000 -1.50000 H21B 2 0.536693 -0.415340 0.593479 11.00000 -1.50000 H21C 2 0.551644 -0.279248 0.627137 11.00000 -1.50000 AFIX 0 C22 1 0.863459 -0.439005 0.430288 11.00000 0.12140 0.13108 = 0.06315 -0.01458 0.01630 0.00957 AFIX 137 H22A 2 0.965239 -0.464226 0.428185 11.00000 -1.50000 H22B 2 0.840951 -0.394780 0.398495 11.00000 -1.50000 H22C 2 0.789352 -0.511290 0.428007 11.00000 -1.50000 AFIX 0 C23 1 1.064697 -0.055043 0.571932 11.00000 0.06839 0.09741 = 0.09005 0.02078 0.01611 -0.02073 AFIX 137 H23A 2 1.009746 0.016617 0.578887 11.00000 -1.50000 H23B 2 1.128127 -0.047103 0.540124 11.00000 -1.50000 H23C 2 1.128667 -0.061007 0.606268 11.00000 -1.50000 AFIX 0 C24 1 0.702987 0.214078 0.631096 11.00000 0.03638 0.04927 = 0.04230 0.01445 0.00456 0.01134 C25 1 0.686698 0.289045 0.587455 11.00000 0.05821 0.06065 = 0.05888 0.02779 -0.00415 0.00127 AFIX 43 H25 2 0.753118 0.361895 0.588689 11.00000 -1.20000 AFIX 0 C26 1 0.572992 0.255368 0.542842 11.00000 0.08178 0.08073 = 0.05682 0.03321 -0.01567 0.00481 AFIX 43 H26 2 0.563287 0.304310 0.513476 11.00000 -1.20000 AFIX 0 C27 1 0.474566 0.149624 0.542002 11.00000 0.07329 0.08363 = 0.05580 0.01627 -0.02043 0.00523 AFIX 43 H27 2 0.394431 0.126449 0.513019 11.00000 -1.20000 AFIX 0 C28 1 0.497177 0.078310 0.585198 11.00000 0.05999 0.05566 = 0.05083 0.00549 -0.00731 0.00033 AFIX 43 H28 2 0.431089 0.005392 0.584277 11.00000 -1.20000 AFIX 0 C29 1 0.954700 0.151044 0.792577 11.00000 0.03427 0.06336 = 0.04534 0.01884 -0.00112 0.00849 AFIX 23 H29A 2 0.997752 0.116981 0.757156 11.00000 -1.20000 H29B 2 1.022610 0.224894 0.809720 11.00000 -1.20000 AFIX 0 C30 1 0.958183 0.058064 0.833652 11.00000 0.04057 0.04306 = 0.03907 0.00464 -0.00611 0.00410 C31 1 0.845457 0.044811 0.872505 11.00000 0.04472 0.04127 = 0.03715 0.00544 -0.00390 0.00477 C32 1 0.855255 -0.033163 0.915164 11.00000 0.05952 0.04302 = 0.04228 0.00581 -0.00358 0.00005 C33 1 0.982907 -0.096708 0.917812 11.00000 0.07389 0.04254 = 0.05129 0.01344 -0.01403 0.00620 AFIX 43 H33 2 0.993221 -0.146870 0.946653 11.00000 -1.20000 AFIX 0 C34 1 1.096593 -0.088777 0.879151 11.00000 0.05689 0.04248 = 0.05747 0.00523 -0.01060 0.01041 C35 1 1.081431 -0.012549 0.837151 11.00000 0.04413 0.05026 = 0.04892 0.00542 -0.00458 0.01091 AFIX 43 H35 2 1.155731 -0.008145 0.810350 11.00000 -1.20000 AFIX 0 C36 1 0.728357 -0.049685 0.955456 11.00000 0.08667 0.06977 = 0.05534 0.02660 0.01213 0.00158 AFIX 137 H36A 2 0.635721 -0.089686 0.933314 11.00000 -1.50000 H36B 2 0.709689 0.030291 0.974892 11.00000 -1.50000 H36C 2 0.758905 -0.100174 0.983803 11.00000 -1.50000 AFIX 0 C37 1 1.232507 -0.162050 0.881852 11.00000 0.07680 0.06929 = 0.08951 0.01845 -0.01057 0.02933 AFIX 137 H37A 2 1.287680 -0.140577 0.919524 11.00000 -1.50000 H37B 2 1.299807 -0.142945 0.852459 11.00000 -1.50000 H37C 2 1.196873 -0.249446 0.875298 11.00000 -1.50000 AFIX 0 C38 1 0.664809 0.246797 0.928201 11.00000 0.04738 0.04131 = 0.04265 0.01017 0.00204 0.00448 C39 1 0.517183 0.261315 0.946133 11.00000 0.05240 0.05057 = 0.05543 0.00867 0.00465 0.01011 C40 1 0.505233 0.333055 0.999882 11.00000 0.07308 0.05587 = 0.06206 0.01382 0.01755 0.02173 AFIX 43 H40 2 0.407666 0.342335 1.012574 11.00000 -1.20000 AFIX 0 C41 1 0.633774 0.390919 1.034975 11.00000 0.09358 0.04339 = 0.05332 0.00682 0.00094 0.02371 C42 1 0.775201 0.379573 1.014298 11.00000 0.07939 0.04563 = 0.05508 0.00514 -0.01166 0.00791 AFIX 43 H42 2 0.861886 0.420870 1.036879 11.00000 -1.20000 AFIX 0 C43 1 0.796808 0.309421 0.961150 11.00000 0.05539 0.04094 = 0.05230 0.00921 -0.00805 0.00398 C44 1 0.373388 0.200642 0.910532 11.00000 0.04823 0.08054 = 0.08500 -0.00152 0.00390 0.00934 AFIX 137 H44A 2 0.374461 0.222511 0.872011 11.00000 -1.50000 H44B 2 0.284666 0.228664 0.928420 11.00000 -1.50000 H44C 2 0.368890 0.111869 0.908353 11.00000 -1.50000 AFIX 0 C45 1 0.617964 0.462252 1.094468 11.00000 0.14555 0.07431 = 0.06026 -0.00080 0.00110 0.04140 AFIX 137 H45A 2 0.600001 0.404770 1.121632 11.00000 -1.50000 H45B 2 0.532680 0.510648 1.092442 11.00000 -1.50000 H45C 2 0.711171 0.516635 1.107109 11.00000 -1.50000 AFIX 0 C46 1 0.957458 0.303389 0.942835 11.00000 0.05178 0.05642 = 0.07845 0.00555 -0.00834 -0.00555 AFIX 137 H46A 2 0.989213 0.223506 0.947342 11.00000 -1.50000 H46B 2 1.026438 0.367573 0.966637 11.00000 -1.50000 H46C 2 0.959741 0.315219 0.902782 11.00000 -1.50000 AFIX 0 N1 3 0.530850 0.273313 0.746386 11.00000 0.03546 0.04082 = 0.04208 0.00526 -0.00272 0.00607 N2 3 0.609562 0.107729 0.628898 11.00000 0.04048 0.04451 = 0.04331 0.01058 0.00104 0.01005 S1 4 0.381486 0.040946 0.724656 11.00000 0.03777 0.04172 = 0.06619 0.01345 0.00704 0.00287 S2 4 0.849191 0.259957 0.686619 11.00000 0.03538 0.06648 = 0.05421 0.02728 -0.00378 -0.00318 SE1 5 0.849374 -0.099779 0.669424 11.00000 0.04315 0.03735 = 0.06016 0.00698 0.00244 0.00861 SE2 5 0.667229 0.127758 0.857578 11.00000 0.03689 0.04937 = 0.04020 0.00813 -0.00015 0.00262 PD1 6 0.610995 -0.020562 0.692650 11.00000 0.04014 0.03398 = 0.04768 0.01070 0.00247 0.00701 PD2 6 0.746698 0.204511 0.770242 11.00000 0.03286 0.04481 = 0.03990 0.01156 -0.00381 0.00486 HKLF 4 REM ups1554DDsk_1_0m in P-1 REM R1 = 0.0277 for 7318 Fo > 4sig(Fo) and 0.0393 for all 8908 data REM 498 parameters refined using 0 restraints END WGHT 0.0447 0.2485 REM Highest difference peak 0.756, deepest hole -0.502, 1-sigma level 0.184 Q1 1 0.6758 0.1829 0.7884 11.00000 0.05 0.76 Q2 1 0.7514 -0.3450 0.5567 11.00000 0.05 0.61 Q3 1 0.7917 0.3630 0.9808 11.00000 0.05 0.59 Q4 1 0.8647 -0.4006 0.4765 11.00000 0.05 0.54 Q5 1 0.7275 0.2996 0.9492 11.00000 0.05 0.54 Q6 1 0.4244 0.5428 1.0414 11.00000 0.05 0.54 Q7 1 0.8009 -0.3410 0.4835 11.00000 0.05 0.54 Q8 1 0.5581 0.3937 1.0016 11.00000 0.05 0.52 Q9 1 0.8555 0.3350 0.9417 11.00000 0.05 0.52 Q10 1 0.9155 -0.3393 0.5001 11.00000 0.05 0.52 Q11 1 0.8279 0.2841 0.9627 11.00000 0.05 0.51 Q12 1 0.8598 -0.2771 0.4903 11.00000 0.05 0.50 Q13 1 0.6815 0.0594 0.6049 11.00000 0.05 0.50 Q14 1 0.7573 0.3344 0.9397 11.00000 0.05 0.50 Q15 1 0.5792 0.4718 1.0020 11.00000 0.05 0.50 Q16 1 0.5982 0.3425 1.0287 11.00000 0.05 0.49 Q17 1 0.8130 -0.4400 0.4986 11.00000 0.05 0.49 Q18 1 0.5757 0.4276 1.0478 11.00000 0.05 0.49 Q19 1 0.6912 -0.3203 0.5897 11.00000 0.05 0.48 Q20 1 0.9145 -0.5430 0.4501 11.00000 0.05 0.48 Q21 1 0.8467 -0.1646 0.6225 11.00000 0.05 0.48 Q22 1 0.7144 0.4380 1.0195 11.00000 0.05 0.48 Q23 1 0.7922 -0.1463 0.6692 11.00000 0.05 0.47 Q24 1 0.7787 -0.0320 0.9276 11.00000 0.05 0.47 Q25 1 0.7227 -0.3426 0.5076 11.00000 0.05 0.46 ; _database_code_depnum_ccdc_archive 'CCDC 901680' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ups1743sk_6_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H50 N2 Pd2 Se4' _chemical_formula_weight 1159.52 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' 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' 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 24.997(5) _cell_length_b 9.941(5) _cell_length_c 18.149(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.153(5) _cell_angle_gamma 90.00 _cell_volume 4475(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9892 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 26.76 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 4.090 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4951 _exptl_absorpt_correction_T_max 0.6852 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35379 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.34 _reflns_number_total 5558 _reflns_number_gt 3544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0511P)^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 5558 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.1013 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 C1 C 0.99913(18) 0.3724(4) 0.1425(2) 0.0557(11) Uani 1 1 d . . . C2 C 1.0003(2) 0.4871(6) 0.0998(3) 0.100(2) Uani 1 1 d . . . H2 H 1.0278 0.4995 0.0703 0.120 Uiso 1 1 calc R . . C3 C 0.9609(3) 0.5824(6) 0.1010(5) 0.136(3) Uani 1 1 d . . . H3 H 0.9608 0.6580 0.0708 0.163 Uiso 1 1 calc R . . C4 C 0.9223(3) 0.5672(6) 0.1454(4) 0.114(2) Uani 1 1 d . . . H4 H 0.8963 0.6332 0.1481 0.137 Uiso 1 1 calc R . . C5 C 0.92223(19) 0.4529(4) 0.1865(3) 0.0717(14) Uani 1 1 d . . . H5 H 0.8956 0.4425 0.2176 0.086 Uiso 1 1 calc R . . C8 C 0.86865(15) -0.0664(4) 0.1313(2) 0.0448(9) Uani 1 1 d . . . C7 C 0.86560(16) -0.0813(4) 0.2069(2) 0.0504(10) Uani 1 1 d . . . C12 C 0.82619(19) -0.1682(4) 0.2277(3) 0.0616(12) Uani 1 1 d . . . H12 H 0.8224 -0.1778 0.2778 0.074 Uiso 1 1 calc R . . C11 C 0.79252(19) -0.2405(5) 0.1753(3) 0.0628(12) Uani 1 1 d . . . C10 C 0.79980(17) -0.2271(4) 0.1027(3) 0.0580(11) Uani 1 1 d . . . H10 H 0.7784 -0.2788 0.0679 0.070 Uiso 1 1 calc R . . C9 C 0.83739(15) -0.1407(4) 0.0769(2) 0.0486(10) Uani 1 1 d . . . C6 C 0.9049(2) -0.0109(5) 0.2639(2) 0.0659(13) Uani 1 1 d . . . H6A H 0.9342 -0.0724 0.2799 0.079 Uiso 1 1 calc R . . H6B H 0.8867 0.0093 0.3068 0.079 Uiso 1 1 calc R . . C14 C 0.7493(2) -0.3322(6) 0.1983(3) 0.100(2) Uani 1 1 d . . . H14A H 0.7145 -0.2972 0.1798 0.151 Uiso 1 1 calc R . . H14B H 0.7527 -0.3373 0.2515 0.151 Uiso 1 1 calc R . . H14C H 0.7534 -0.4205 0.1783 0.151 Uiso 1 1 calc R . . C13 C 0.84411(18) -0.1288(5) -0.0035(2) 0.0682(13) Uani 1 1 d . . . H13A H 0.8219 -0.1947 -0.0314 0.102 Uiso 1 1 calc R . . H13B H 0.8812 -0.1438 -0.0099 0.102 Uiso 1 1 calc R . . H13C H 0.8335 -0.0404 -0.0209 0.102 Uiso 1 1 calc R . . C15 C 0.88502(15) 0.1872(3) 0.0402(2) 0.0408(9) Uani 1 1 d . . . C16 C 0.90795(16) 0.2107(4) -0.0248(2) 0.0478(10) Uani 1 1 d . . . C17 C 0.88473(19) 0.3096(4) -0.0725(2) 0.0601(12) Uani 1 1 d . . . H17 H 0.8996 0.3270 -0.1160 0.072 Uiso 1 1 calc R . . C18 C 0.84100(19) 0.3824(5) -0.0582(3) 0.0616(12) Uani 1 1 d . . . C19 C 0.81872(18) 0.3540(4) 0.0053(3) 0.0589(11) Uani 1 1 d . . . H19 H 0.7884 0.4018 0.0150 0.071 Uiso 1 1 calc R . . C20 C 0.83965(17) 0.2564(4) 0.0561(2) 0.0503(10) Uani 1 1 d . . . C21 C 0.95729(17) 0.1365(5) -0.0443(2) 0.0609(12) Uani 1 1 d . . . H21A H 0.9659 0.1673 -0.0915 0.091 Uiso 1 1 calc R . . H21B H 0.9500 0.0417 -0.0468 0.091 Uiso 1 1 calc R . . H21C H 0.9872 0.1536 -0.0069 0.091 Uiso 1 1 calc R . . C22 C 0.8187(2) 0.4951(5) -0.1105(3) 0.0899(17) Uani 1 1 d . . . H22A H 0.8427 0.5708 -0.1048 0.135 Uiso 1 1 calc R . . H22B H 0.7839 0.5217 -0.0986 0.135 Uiso 1 1 calc R . . H22C H 0.8155 0.4637 -0.1609 0.135 Uiso 1 1 calc R . . C23 C 0.81242(18) 0.2317(5) 0.1242(3) 0.0652(13) Uani 1 1 d . . . H23A H 0.7969 0.1433 0.1218 0.098 Uiso 1 1 calc R . . H23B H 0.7846 0.2974 0.1268 0.098 Uiso 1 1 calc R . . H23C H 0.8385 0.2386 0.1677 0.098 Uiso 1 1 calc R . . N1 N 0.95874(14) 0.3539(3) 0.18433(18) 0.0503(8) Uani 1 1 d . . . Se1 Se 1.054219(19) 0.24053(5) 0.14374(2) 0.05892(15) Uani 1 1 d . . . Se2 Se 0.923733(15) 0.05773(4) 0.10812(2) 0.04319(12) Uani 1 1 d . . . Pd1 Pd 0.937095(11) 0.16340(3) 0.228873(15) 0.04255(11) 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 0.058(3) 0.055(2) 0.049(3) 0.013(2) -0.010(2) -0.014(2) C2 0.074(4) 0.105(4) 0.118(5) 0.062(4) -0.004(3) -0.021(3) C3 0.099(6) 0.085(5) 0.209(9) 0.087(5) -0.040(5) -0.019(4) C4 0.077(5) 0.063(4) 0.194(8) 0.041(4) -0.018(5) 0.007(3) C5 0.060(3) 0.054(3) 0.096(4) 0.004(3) -0.009(3) 0.007(2) C8 0.041(2) 0.048(2) 0.045(2) 0.0038(18) 0.0032(18) 0.0023(17) C7 0.051(3) 0.048(2) 0.049(3) 0.0108(19) -0.004(2) -0.0041(19) C12 0.066(3) 0.065(3) 0.053(3) 0.016(2) 0.005(2) -0.008(2) C11 0.058(3) 0.068(3) 0.061(3) 0.018(2) 0.001(2) -0.010(2) C10 0.046(3) 0.055(3) 0.070(3) -0.002(2) -0.006(2) -0.009(2) C9 0.041(2) 0.055(2) 0.049(3) -0.003(2) 0.0002(19) -0.0023(19) C6 0.082(4) 0.065(3) 0.047(3) 0.012(2) -0.004(2) -0.022(3) C14 0.095(4) 0.115(5) 0.088(4) 0.027(4) -0.002(3) -0.050(4) C13 0.065(3) 0.081(3) 0.058(3) -0.021(2) 0.003(2) -0.019(3) C15 0.043(2) 0.043(2) 0.035(2) 0.0033(16) -0.0022(17) -0.0015(17) C16 0.047(2) 0.057(2) 0.037(2) -0.0020(19) -0.0042(19) -0.0069(19) C17 0.066(3) 0.072(3) 0.040(2) 0.012(2) -0.005(2) -0.015(2) C18 0.057(3) 0.057(3) 0.064(3) 0.013(2) -0.019(2) -0.009(2) C19 0.048(3) 0.059(3) 0.065(3) 0.004(2) -0.009(2) 0.007(2) C20 0.045(3) 0.057(3) 0.047(2) 0.0012(19) -0.002(2) -0.0021(19) C21 0.061(3) 0.083(3) 0.039(2) 0.000(2) 0.009(2) -0.004(2) C22 0.084(4) 0.080(3) 0.096(4) 0.035(3) -0.027(3) -0.007(3) C23 0.042(3) 0.086(3) 0.069(3) 0.001(3) 0.010(2) 0.011(2) N1 0.053(2) 0.0425(19) 0.051(2) 0.0048(16) -0.0095(17) -0.0007(16) Se1 0.0563(3) 0.0805(3) 0.0403(3) 0.0026(2) 0.0074(2) -0.0045(2) Se2 0.0410(2) 0.0478(2) 0.0395(2) 0.00341(17) 0.00005(18) -0.00124(17) Pd1 0.0421(2) 0.04840(19) 0.03566(18) 0.00476(13) -0.00125(13) -0.00168(13) _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 N1 1.349(5) . ? C1 C2 1.381(6) . ? C1 Se1 1.900(5) . ? C2 C3 1.369(9) . ? C2 H2 0.9300 . ? C3 C4 1.340(9) . ? C3 H3 0.9300 . ? C4 C5 1.359(7) . ? C4 H4 0.9300 . ? C5 N1 1.346(5) . ? C5 H5 0.9300 . ? C8 C7 1.392(5) . ? C8 C9 1.392(5) . ? C8 Se2 1.934(4) . ? C7 C12 1.397(5) . ? C7 C6 1.507(6) . ? C12 C11 1.389(6) . ? C12 H12 0.9300 . ? C11 C10 1.360(6) . ? C11 C14 1.511(6) . ? C10 C9 1.396(5) . ? C10 H10 0.9300 . ? C9 C13 1.496(5) . ? C6 Pd1 2.045(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C15 C20 1.387(5) . ? C15 C16 1.395(5) . ? C15 Se2 1.953(4) . ? C16 C17 1.389(6) . ? C16 C21 1.516(5) . ? C17 C18 1.362(6) . ? C17 H17 0.9300 . ? C18 C19 1.370(6) . ? C18 C22 1.528(6) . ? C19 C20 1.394(6) . ? C19 H19 0.9300 . ? C20 C23 1.505(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? N1 Pd1 2.154(3) . ? Se1 Pd1 2.4197(8) 2_755 ? Se2 Pd1 2.4156(8) . ? Pd1 Se1 2.4197(8) 2_755 ? Pd1 Pd1 3.1429(8) 2_755 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 119.9(5) . . ? N1 C1 Se1 119.4(3) . . ? C2 C1 Se1 120.7(4) . . ? C3 C2 C1 119.8(6) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C4 C3 C2 120.3(6) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 118.4(6) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 123.2(5) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? C7 C8 C9 123.2(4) . . ? C7 C8 Se2 114.2(3) . . ? C9 C8 Se2 122.4(3) . . ? C8 C7 C12 117.4(4) . . ? C8 C7 C6 121.0(4) . . ? C12 C7 C6 121.6(4) . . ? C11 C12 C7 121.5(4) . . ? C11 C12 H12 119.3 . . ? C7 C12 H12 119.3 . . ? C10 C11 C12 118.0(4) . . ? C10 C11 C14 120.9(4) . . ? C12 C11 C14 121.1(4) . . ? C11 C10 C9 124.2(4) . . ? C11 C10 H10 117.9 . . ? C9 C10 H10 117.9 . . ? C8 C9 C10 115.5(4) . . ? C8 C9 C13 122.0(4) . . ? C10 C9 C13 122.5(4) . . ? C7 C6 Pd1 115.4(3) . . ? C7 C6 H6A 108.4 . . ? Pd1 C6 H6A 108.4 . . ? C7 C6 H6B 108.4 . . ? Pd1 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? 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 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C20 C15 C16 121.7(4) . . ? C20 C15 Se2 123.4(3) . . ? C16 C15 Se2 114.9(3) . . ? C17 C16 C15 117.5(4) . . ? C17 C16 C21 119.2(4) . . ? C15 C16 C21 123.2(4) . . ? C18 C17 C16 122.7(4) . . ? C18 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C17 C18 C19 118.1(4) . . ? C17 C18 C22 120.6(5) . . ? C19 C18 C22 121.2(5) . . ? C18 C19 C20 122.7(4) . . ? C18 C19 H19 118.6 . . ? C20 C19 H19 118.6 . . ? C15 C20 C19 117.2(4) . . ? C15 C20 C23 123.7(4) . . ? C19 C20 C23 119.1(4) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C5 N1 C1 118.3(4) . . ? C5 N1 Pd1 115.4(3) . . ? C1 N1 Pd1 124.9(3) . . ? C1 Se1 Pd1 102.04(13) . 2_755 ? C8 Se2 C15 104.33(16) . . ? C8 Se2 Pd1 95.84(12) . . ? C15 Se2 Pd1 106.71(11) . . ? C6 Pd1 N1 171.26(16) . . ? C6 Pd1 Se2 84.15(13) . . ? N1 Pd1 Se2 93.13(9) . . ? C6 Pd1 Se1 87.92(12) . 2_755 ? N1 Pd1 Se1 94.77(9) . 2_755 ? Se2 Pd1 Se1 172.059(19) . 2_755 ? C6 Pd1 Pd1 110.18(14) . 2_755 ? N1 Pd1 Pd1 78.53(9) . 2_755 ? Se2 Pd1 Pd1 104.033(16) . 2_755 ? Se1 Pd1 Pd1 78.396(16) 2_755 2_755 ? 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 N1 C1 C2 C3 1.0(9) . . . . ? Se1 C1 C2 C3 -178.5(5) . . . . ? C1 C2 C3 C4 2.5(11) . . . . ? C2 C3 C4 C5 -2.7(12) . . . . ? C3 C4 C5 N1 -0.4(10) . . . . ? C9 C8 C7 C12 -5.0(6) . . . . ? Se2 C8 C7 C12 179.2(3) . . . . ? C9 C8 C7 C6 172.5(4) . . . . ? Se2 C8 C7 C6 -3.3(5) . . . . ? C8 C7 C12 C11 2.2(6) . . . . ? C6 C7 C12 C11 -175.3(4) . . . . ? C7 C12 C11 C10 1.6(7) . . . . ? C7 C12 C11 C14 -178.9(4) . . . . ? C12 C11 C10 C9 -3.0(7) . . . . ? C14 C11 C10 C9 177.5(5) . . . . ? C7 C8 C9 C10 3.7(6) . . . . ? Se2 C8 C9 C10 179.2(3) . . . . ? C7 C8 C9 C13 -175.9(4) . . . . ? Se2 C8 C9 C13 -0.4(6) . . . . ? C11 C10 C9 C8 0.4(6) . . . . ? C11 C10 C9 C13 -180.0(4) . . . . ? C8 C7 C6 Pd1 26.9(5) . . . . ? C12 C7 C6 Pd1 -155.7(3) . . . . ? C20 C15 C16 C17 2.1(6) . . . . ? Se2 C15 C16 C17 -175.0(3) . . . . ? C20 C15 C16 C21 -179.6(4) . . . . ? Se2 C15 C16 C21 3.3(5) . . . . ? C15 C16 C17 C18 -0.4(6) . . . . ? C21 C16 C17 C18 -178.7(4) . . . . ? C16 C17 C18 C19 -1.3(7) . . . . ? C16 C17 C18 C22 176.8(4) . . . . ? C17 C18 C19 C20 1.4(7) . . . . ? C22 C18 C19 C20 -176.8(4) . . . . ? C16 C15 C20 C19 -2.0(6) . . . . ? Se2 C15 C20 C19 174.8(3) . . . . ? C16 C15 C20 C23 178.0(4) . . . . ? Se2 C15 C20 C23 -5.2(6) . . . . ? C18 C19 C20 C15 0.2(7) . . . . ? C18 C19 C20 C23 -179.8(4) . . . . ? C4 C5 N1 C1 3.8(7) . . . . ? C4 C5 N1 Pd1 -163.2(5) . . . . ? C2 C1 N1 C5 -4.0(6) . . . . ? Se1 C1 N1 C5 175.5(3) . . . . ? C2 C1 N1 Pd1 161.7(4) . . . . ? Se1 C1 N1 Pd1 -18.8(5) . . . . ? N1 C1 Se1 Pd1 -34.9(3) . . . 2_755 ? C2 C1 Se1 Pd1 144.6(4) . . . 2_755 ? C7 C8 Se2 C15 -125.0(3) . . . . ? C9 C8 Se2 C15 59.1(4) . . . . ? C7 C8 Se2 Pd1 -16.1(3) . . . . ? C9 C8 Se2 Pd1 168.0(3) . . . . ? C20 C15 Se2 C8 53.0(4) . . . . ? C16 C15 Se2 C8 -130.0(3) . . . . ? C20 C15 Se2 Pd1 -47.8(3) . . . . ? C16 C15 Se2 Pd1 129.2(3) . . . . ? C7 C6 Pd1 N1 43.2(12) . . . . ? C7 C6 Pd1 Se2 -29.1(3) . . . . ? C7 C6 Pd1 Se1 151.3(3) . . . 2_755 ? C7 C6 Pd1 Pd1 -131.9(3) . . . 2_755 ? C5 N1 Pd1 C6 38.1(11) . . . . ? C1 N1 Pd1 C6 -128.0(10) . . . . ? C5 N1 Pd1 Se2 109.6(3) . . . . ? C1 N1 Pd1 Se2 -56.4(3) . . . . ? C5 N1 Pd1 Se1 -69.5(3) . . . 2_755 ? C1 N1 Pd1 Se1 124.4(3) . . . 2_755 ? C5 N1 Pd1 Pd1 -146.7(3) . . . 2_755 ? C1 N1 Pd1 Pd1 47.3(3) . . . 2_755 ? C8 Se2 Pd1 C6 22.17(18) . . . . ? C15 Se2 Pd1 C6 129.06(18) . . . . ? C8 Se2 Pd1 N1 -149.49(15) . . . . ? C15 Se2 Pd1 N1 -42.61(14) . . . . ? C8 Se2 Pd1 Se1 24.64(18) . . . 2_755 ? C15 Se2 Pd1 Se1 131.52(18) . . . 2_755 ? C8 Se2 Pd1 Pd1 131.56(11) . . . 2_755 ? C15 Se2 Pd1 Pd1 -121.56(11) . . . 2_755 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.539 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.202 _iucr_refine_instructions_details ; TITL ups1743sk_6_0m in C2/c CELL 0.71073 24.9970 9.9410 18.1490 90.000 97.153 90.000 ZERR 4.00 0.0050 0.0050 0.0050 0.000 0.005 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N SE PD UNIT 184 200 8 16 8 MERG 2 FMAP 2 PLAN 25 SIZE 0.10 0.15 0.20 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 50 TEMP 25.00 WGHT 0.051100 FVAR 0.04267 C1 1 0.999125 0.372438 0.142511 11.00000 0.05849 0.05496 = 0.04933 0.01331 -0.01000 -0.01379 C2 1 1.000299 0.487099 0.099774 11.00000 0.07352 0.10533 = 0.11780 0.06215 -0.00445 -0.02147 AFIX 43 H2 2 1.027774 0.499546 0.070288 11.00000 -1.20000 AFIX 0 C3 1 0.960870 0.582369 0.100975 11.00000 0.09950 0.08517 = 0.20908 0.08678 -0.03953 -0.01856 AFIX 43 H3 2 0.960833 0.657982 0.070795 11.00000 -1.20000 AFIX 0 C4 1 0.922323 0.567175 0.145442 11.00000 0.07735 0.06289 = 0.19433 0.04109 -0.01800 0.00690 AFIX 43 H4 2 0.896287 0.633216 0.148135 11.00000 -1.20000 AFIX 0 C5 1 0.922227 0.452864 0.186501 11.00000 0.05960 0.05443 = 0.09618 0.00378 -0.00935 0.00690 AFIX 43 H5 2 0.895631 0.442525 0.217615 11.00000 -1.20000 AFIX 0 C8 1 0.868648 -0.066369 0.131318 11.00000 0.04056 0.04790 = 0.04528 0.00384 0.00324 0.00232 C7 1 0.865601 -0.081322 0.206939 11.00000 0.05140 0.04834 = 0.04902 0.01082 -0.00396 -0.00406 C12 1 0.826190 -0.168189 0.227736 11.00000 0.06631 0.06512 = 0.05257 0.01591 0.00478 -0.00842 AFIX 43 H12 2 0.822399 -0.177821 0.277792 11.00000 -1.20000 AFIX 0 C11 1 0.792522 -0.240528 0.175332 11.00000 0.05809 0.06771 = 0.06085 0.01837 0.00056 -0.01021 C10 1 0.799800 -0.227113 0.102687 11.00000 0.04571 0.05545 = 0.06970 -0.00204 -0.00565 -0.00927 AFIX 43 H10 2 0.778363 -0.278810 0.067935 11.00000 -1.20000 AFIX 0 C9 1 0.837394 -0.140695 0.076936 11.00000 0.04055 0.05507 = 0.04890 -0.00332 0.00018 -0.00229 C6 1 0.904886 -0.010874 0.263871 11.00000 0.08234 0.06509 = 0.04720 0.01194 -0.00385 -0.02158 AFIX 23 H6A 2 0.934152 -0.072373 0.279944 11.00000 -1.20000 H6B 2 0.886704 0.009307 0.306764 11.00000 -1.20000 AFIX 0 C14 1 0.749350 -0.332234 0.198319 11.00000 0.09460 0.11523 = 0.08780 0.02699 -0.00207 -0.05025 AFIX 137 H14A 2 0.714468 -0.297242 0.179761 11.00000 -1.50000 H14B 2 0.752698 -0.337256 0.251519 11.00000 -1.50000 H14C 2 0.753447 -0.420484 0.178286 11.00000 -1.50000 AFIX 0 C13 1 0.844109 -0.128846 -0.003546 11.00000 0.06474 0.08098 = 0.05773 -0.02074 0.00293 -0.01913 AFIX 137 H13A 2 0.821932 -0.194671 -0.031421 11.00000 -1.50000 H13B 2 0.881189 -0.143840 -0.009941 11.00000 -1.50000 H13C 2 0.833517 -0.040422 -0.020937 11.00000 -1.50000 AFIX 0 C15 1 0.885017 0.187228 0.040213 11.00000 0.04289 0.04285 = 0.03499 0.00331 -0.00216 -0.00154 C16 1 0.907946 0.210681 -0.024849 11.00000 0.04746 0.05689 = 0.03655 -0.00195 -0.00421 -0.00690 C17 1 0.884731 0.309633 -0.072540 11.00000 0.06574 0.07185 = 0.03966 0.01226 -0.00497 -0.01471 AFIX 43 H17 2 0.899635 0.326958 -0.116037 11.00000 -1.20000 AFIX 0 C18 1 0.841005 0.382357 -0.058186 11.00000 0.05692 0.05693 = 0.06434 0.01254 -0.01914 -0.00859 C19 1 0.818722 0.354002 0.005326 11.00000 0.04811 0.05933 = 0.06533 0.00416 -0.00858 0.00722 AFIX 43 H19 2 0.788386 0.401844 0.014968 11.00000 -1.20000 AFIX 0 C20 1 0.839649 0.256436 0.056054 11.00000 0.04501 0.05734 = 0.04683 0.00121 -0.00154 -0.00211 C21 1 0.957285 0.136548 -0.044277 11.00000 0.06148 0.08275 = 0.03920 0.00009 0.00913 -0.00351 AFIX 137 H21A 2 0.965947 0.167327 -0.091511 11.00000 -1.50000 H21B 2 0.950000 0.041732 -0.046774 11.00000 -1.50000 H21C 2 0.987163 0.153627 -0.006853 11.00000 -1.50000 AFIX 0 C22 1 0.818714 0.495099 -0.110482 11.00000 0.08389 0.08014 = 0.09580 0.03497 -0.02735 -0.00732 AFIX 137 H22A 2 0.842731 0.570777 -0.104811 11.00000 -1.50000 H22B 2 0.783862 0.521654 -0.098628 11.00000 -1.50000 H22C 2 0.815546 0.463686 -0.160856 11.00000 -1.50000 AFIX 0 C23 1 0.812419 0.231695 0.124239 11.00000 0.04174 0.08589 = 0.06877 0.00129 0.00996 0.01109 AFIX 137 H23A 2 0.796855 0.143277 0.121766 11.00000 -1.50000 H23B 2 0.784572 0.297419 0.126790 11.00000 -1.50000 H23C 2 0.838459 0.238607 0.167655 11.00000 -1.50000 AFIX 0 N1 3 0.958743 0.353877 0.184334 11.00000 0.05323 0.04249 = 0.05104 0.00484 -0.00947 -0.00069 SE1 4 1.054219 0.240528 0.143741 11.00000 0.05629 0.08046 = 0.04033 0.00264 0.00735 -0.00454 SE2 4 0.923733 0.057734 0.108122 11.00000 0.04099 0.04782 = 0.03950 0.00341 0.00005 -0.00124 PD1 5 0.937095 0.163397 0.228873 11.00000 0.04205 0.04840 = 0.03566 0.00476 -0.00125 -0.00168 HKLF 4 REM ups1743sk_6_0m in C2/c REM R1 = 0.0336 for 3544 Fo > 4sig(Fo) and 0.0804 for all 5558 data REM 249 parameters refined using 0 restraints END WGHT 0.0479 0.0000 REM Highest difference peak 0.539, deepest hole -0.568, 1-sigma level 0.202 Q1 1 0.8211 0.4137 -0.0744 11.00000 0.05 0.54 Q2 1 0.7575 0.5730 -0.0420 11.00000 0.05 0.53 Q3 1 0.7986 -0.2697 0.0821 11.00000 0.05 0.52 Q4 1 0.8009 0.6122 -0.0723 11.00000 0.05 0.52 Q5 1 0.7976 0.0571 0.0660 11.00000 0.05 0.52 Q6 1 0.7762 -0.3194 -0.0223 11.00000 0.05 0.51 Q7 1 0.7844 -0.1188 0.0664 11.00000 0.05 0.51 Q8 1 0.7305 0.2072 0.1347 11.00000 0.05 0.51 Q9 1 0.7397 -0.3530 0.0648 11.00000 0.05 0.50 Q10 1 0.7874 0.5082 -0.1368 11.00000 0.05 0.50 Q11 1 0.8017 0.3613 -0.1148 11.00000 0.05 0.50 Q12 1 0.7190 0.3395 0.0540 11.00000 0.05 0.50 Q13 1 0.8010 0.3270 -0.0048 11.00000 0.05 0.50 Q14 1 0.7770 -0.3887 0.2146 11.00000 0.05 0.49 Q15 1 0.7827 -0.3456 0.0777 11.00000 0.05 0.49 Q16 1 0.8104 -0.0296 0.0232 11.00000 0.05 0.49 Q17 1 0.7777 -0.3340 0.0259 11.00000 0.05 0.48 Q18 1 0.7393 0.2969 0.1015 11.00000 0.05 0.48 Q19 1 0.7995 0.5571 -0.0445 11.00000 0.05 0.48 Q20 1 0.7539 0.4013 0.0672 11.00000 0.05 0.48 Q21 1 0.7612 -0.4349 0.2383 11.00000 0.05 0.48 Q22 1 0.7793 -0.2202 0.0325 11.00000 0.05 0.47 Q23 1 0.7491 0.5966 -0.0273 11.00000 0.05 0.47 Q24 1 0.7912 -0.4073 0.0197 11.00000 0.05 0.47 Q25 1 0.7792 -0.2402 0.0648 11.00000 0.05 0.47 ; _database_code_depnum_ccdc_archive 'CCDC 930643'