#------------------------------------------------------------------------------ #$Date: 2017-02-17 18:23:55 +0200 (Fri, 17 Feb 2017) $ #$Revision: 192233 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/32/40/4324065.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4324065 loop_ _publ_author_name 'Raymond J. Batchelor' 'Frederick W. B. Einstein' 'Ian D. Gay' 'Jian Gu' 'B. Mario Pinto' 'Xuemin Zhou' _publ_contact_author ; Prof. Frederick W.B. Einstein Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; _publ_contact_author_email einstein@sfu.ca _publ_contact_author_fax '604 291 3765' _publ_contact_author_phone '604 291 4878' _publ_section_title ; Stereochemical Analysis of Palladium(II) Complexes of the Selenium Coronands 1,5,9,13-Tetraselenacyclohexadecane and 1,5,9,13,17,21-Hexaselenacyclotetracosane ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3667 _journal_page_last 3674 _journal_paper_doi 10.1021/ic951151j _journal_volume 35 _journal_year 1996 _chemical_formula_moiety 'Pd Se4 Cl F4 C12 B1 H24 ' _chemical_formula_sum 'C12 H24 B Cl F4 Pd Se4' _chemical_formula_weight 712.8 _chemical_name_systematic ? _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 76.607(6) _cell_angle_beta 86.020(6) _cell_angle_gamma 85.186(5) _cell_formula_units_Z 2 _cell_length_a 7.2377(4) _cell_length_b 10.7784(7) _cell_length_c 12.9523(9) _cell_measurement_reflns_used 25 _cell_measurement_temperature 295 _cell_measurement_theta_max 21.00 _cell_measurement_theta_min 16.00 _cell_volume 978.17(11) _computing_data_reduction 'NRCVAX DATRD2' _computing_molecular_graphics NRCVAX _computing_publication_material 'NRCVAX TABLES and CRYSTALS' _computing_structure_refinement CRYSTALS _computing_structure_solution 'NRCVAX SOLVER' _diffrn_ambient_temperature 295 _diffrn_measurement_device 'Nonius CAD-4 ' _diffrn_measurement_method 'Theta/2theta scan b/P/b ' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'xray tube' _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_wavelength 0.70930 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 2864 _diffrn_reflns_theta_max 23.5 _diffrn_reflns_theta_min 2 _diffrn_standards_decay_% 0.0 _diffrn_standards_interval_time 60 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 8.474 _exptl_absorpt_correction_T_max 0.575 _exptl_absorpt_correction_T_min 0.218 _exptl_absorpt_correction_type integration _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.420 _exptl_crystal_description plate _exptl_crystal_F_000 671.88 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.6(1) _refine_diff_density_min -0.6(1) _refine_ls_goodness_of_fit_obs 1.55 _refine_ls_matrix_type full _refine_ls_number_parameters 214 _refine_ls_number_reflns 2134 _refine_ls_number_restraints 31 _refine_ls_R_factor_obs 0.022 _refine_ls_shift/esd_max 0.13 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/(\s^2^(F)+0.0001F^2^)' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.027 _reflns_number_observed 2134 _reflns_number_total 2864 _reflns_observed_criterion 'Inet > 2.5\s(Inet)' _cod_data_source_file ic951151j_3.cif _cod_data_source_block rpdse4 _cod_depositor_comments ; Changing the occupancy of atoms 'F5', 'F6', 'F7', 'B2' from '0.030(1)' to '0.30(1)' after consulting the supplementary data of the original publication. Antanas Vaitkus, 2017-02-17 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '1/(\s^2^(F)+0.0001F^2^)' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/(\s^2^(F)+0.0001F^2^)'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_formula_sum 'Pd Se4 Cl F4 C12 B1 H24 ' _cod_database_code 4324065 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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 _atom_site_aniso_type_symbol Pd 0.03821(24) 0.02942(24) 0.0327(3) -0.00971(19) -0.00294(17) -0.00166(17) Pd Se3 0.0396(3) 0.0373(3) 0.0451(4) -0.0113(3) -0.0026(3) -0.00558(24) Se Se7 0.0383(3) 0.0401(4) 0.0465(4) -0.0167(3) -0.0038(3) 0.00400(24) Se Se11 0.0518(4) 0.0334(3) 0.0398(4) -0.0046(3) -0.0046(3) -0.0052(3) Se Se15 0.0528(3) 0.0397(4) 0.0320(3) -0.0110(3) -0.0016(3) -0.0014(3) Se Cl 0.0426(8) 0.0474(9) 0.0460(9) -0.0068(7) -0.0046(7) 0.0032(6) Cl C1 0.060(4) 0.032(4) 0.062(4) -0.009(3) -0.002(3) 0.004(3) C C2 0.063(4) 0.036(4) 0.058(4) -0.014(3) 0.003(3) -0.006(3) C C4 0.046(3) 0.042(4) 0.043(4) 0.001(3) -0.003(3) 0.001(3) C C5 0.044(3) 0.059(4) 0.041(4) -0.011(3) -0.001(3) 0.001(3) C C6 0.048(3) 0.059(4) 0.041(4) -0.023(3) -0.003(3) 0.001(3) C C8 0.066(4) 0.044(4) 0.061(4) -0.029(3) -0.001(3) 0.000(3) C C9 0.066(4) 0.043(4) 0.062(4) -0.025(3) -0.013(3) -0.006(3) C C10 0.072(4) 0.034(4) 0.078(5) -0.019(4) -0.004(4) -0.013(3) C C12 0.043(3) 0.059(4) 0.059(4) -0.014(4) 0.003(3) -0.011(3) C C13 0.037(3) 0.071(5) 0.056(4) -0.010(4) -0.001(3) -0.004(3) C C14 0.045(3) 0.060(4) 0.049(4) -0.016(3) 0.005(3) 0.000(3) C C16 0.073(4) 0.041(4) 0.054(4) -0.021(3) 0.005(3) -0.002(3) C F1 0.079(3) 0.126(4) 0.089(3) -0.027(3) -0.0345(24) -0.003(3) F loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol _atom_site_occupancy Pd1 0.35455(5) 0.30863(4) 0.24867(3) 0.03301(24) Uij ? . Pd . Se3 0.17559(7) 0.12251(5) 0.32612(5) 0.0402(3) Uij ? . Se . Se7 0.14335(7) 0.41919(5) 0.36056(5) 0.0408(3) Uij ? . Se . Se11 0.49486(8) 0.50055(5) 0.14692(5) 0.0421(3) Uij ? . Se . Se15 0.51439(8) 0.22009(6) 0.10660(4) 0.0411(3) Uij ? . Se . Cl1 0.65304(18) 0.24643(14) 0.41372(11) 0.0462(8) Uij ? . Cl . C1 0.5044(8) -0.0270(5) 0.2581(5) 0.052(4) Uij ? . C . C2 0.3107(8) -0.0380(5) 0.3070(5) 0.052(4) Uij ? . C . C4 0.2219(7) 0.0918(5) 0.4775(4) 0.045(3) Uij ? . C . C5 0.1157(8) 0.1902(6) 0.5308(5) 0.049(4) Uij ? . C . C6 0.1958(8) 0.3201(6) 0.5037(4) 0.048(4) Uij ? . C . C8 0.2470(8) 0.5755(6) 0.3779(5) 0.055(4) Uij ? . C . C9 0.4453(8) 0.5933(6) 0.3440(5) 0.054(4) Uij ? . C . C10 0.4851(9) 0.6338(6) 0.2262(5) 0.060(4) Uij ? . C . C12 0.7607(7) 0.4538(6) 0.1640(5) 0.053(4) Uij ? . C . C13 0.8419(8) 0.3583(6) 0.1022(5) 0.055(4) Uij ? . C . C14 0.7743(8) 0.2257(6) 0.1391(5) 0.051(4) Uij ? . C . C16 0.5127(9) 0.0347(6) 0.1403(5) 0.055(4) Uij ? . C . F1 0.8545(5) 0.8084(4) 0.0531(3) 0.096(3) Uij ? . F . F2 1.0778(14) 0.6659(9) 0.1315(10) 0.0821(12) Uiso ? . F 0.39(1) F3 0.8912(14) 0.7797(15) 0.2274(6) 0.0821(12) Uiso ? . F 0.39(1) F4 1.1121(14) 0.8745(10) 0.1050(10) 0.0821(12) Uiso ? . F 0.39(1) F5 0.9354(17) 0.9262(11) 0.1660(10) 0.0821(12) Uiso ? . F 0.30(1) F6 0.9242(19) 0.7134(12) 0.2216(8) 0.0821(12) Uiso ? . F 0.30(1) F7 1.1503(11) 0.7964(14) 0.1059(11) 0.0821(12) Uiso ? . F 0.30(1) F8 1.0327(20) 0.6714(10) 0.1667(12) 0.0821(12) Uiso ? . F 0.31(1) F9 1.1484(14) 0.8543(16) 0.0768(11) 0.0821(12) Uiso ? . F 0.31(1) F10 0.9210(17) 0.8596(18) 0.2046(10) 0.0821(12) Uiso ? . F 0.31(1) B1 0.9837(8) 0.7830(8) 0.1301(5) 0.0587(23) Uiso ? . B 0.39(1) B2 0.9643(10) 0.8113(9) 0.1354(5) 0.0587(23) Uiso ? . B 0.30(1) B3 0.9895(9) 0.7996(9) 0.1252(6) 0.0587(23) Uiso ? . B 0.31(1) H11 0.5687(8) 0.0228(5) 0.2937(5) 0.060(4) Uiso ? . H . H12 0.5642(8) -0.1104(5) 0.2679(5) 0.060(4) Uiso ? . H . H21 0.3174(8) -0.0948(5) 0.3750(5) 0.062(4) Uiso ? . H . H22 0.2409(8) -0.0734(5) 0.2628(5) 0.062(4) Uiso ? . H . H41 0.3509(7) 0.0953(5) 0.4847(4) 0.054(4) Uiso ? . H . H42 0.1848(7) 0.0093(5) 0.5120(4) 0.054(4) Uiso ? . H . H51 0.1164(8) 0.1583(6) 0.6056(5) 0.059(4) Uiso ? . H . H52 -0.0085(8) 0.2007(6) 0.5093(5) 0.059(4) Uiso ? . H . H61 0.1444(8) 0.3673(6) 0.5535(4) 0.060(4) Uiso ? . H . H62 0.3266(8) 0.3079(6) 0.5090(4) 0.060(4) Uiso ? . H . H81 0.2331(8) 0.5763(6) 0.4512(5) 0.068(4) Uiso ? . H . H82 0.1754(8) 0.6462(6) 0.3381(5) 0.068(4) Uiso ? . H . H91 0.4858(8) 0.6567(6) 0.3759(5) 0.067(4) Uiso ? . H . H92 0.5144(8) 0.5144(6) 0.3692(5) 0.067(4) Uiso ? . H . H01 0.6018(9) 0.6704(6) 0.2148(5) 0.070(4) Uiso ? . H . H02 0.3907(9) 0.6969(6) 0.1982(5) 0.070(4) Uiso ? . H . H21 0.8255(7) 0.5293(6) 0.1412(5) 0.064(4) Uiso ? . H . H22 0.7786(7) 0.4186(6) 0.2372(5) 0.064(4) Uiso ? . H . H31 0.9729(8) 0.3519(6) 0.1068(5) 0.064(4) Uiso ? . H . H32 0.8118(8) 0.3897(6) 0.0301(5) 0.064(4) Uiso ? . H . H41 0.7850(8) 0.1986(6) 0.2138(5) 0.062(4) Uiso ? . H . H42 0.8497(8) 0.1693(6) 0.1047(5) 0.062(4) Uiso ? . H . H61 0.6226(9) 0.0013(6) 0.1089(5) 0.066(4) Uiso ? . H . H62 0.4074(9) 0.0127(6) 0.1103(5) 0.066(4) Uiso ? . H . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd ? -1.177 1.007 'International Tables Vol. IV Table 2.2B' Se ? -0.178 2.223 'International Tables Vol. IV Table 2.2B' Cl ? 0.132 0.159 'International Tables Vol. IV Table 2.2B' F ? 0.014 0.010 'International Tables Vol. IV Table 2.2B' C ? 0.002 0.002 'International Tables Vol. IV Table 2.2B' B ? 0.000 0.001 'International Tables Vol. IV Table 2.2B' H ? 0.000 0.000 'International Tables Vol. IV Table 2.2B' 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se3 Pd1 Se7 84.89(2) ? ? ? ? Se3 Pd1 Se11 170.03(3) ? ? ? ? Se3 Pd1 Se15 96.14(2) ? ? ? ? Se7 Pd1 Se11 95.63(2) ? ? ? ? Se7 Pd1 Se15 166.97(2) ? ? ? ? Se11 Pd1 Se15 81.12(2) ? ? ? ? Pd1 Se3 C2 111.6(2) ? ? ? ? Pd1 Se3 C4 102.4(2) ? ? ? ? C2 Se3 C4 94.5(3) ? ? ? ? Pd1 Se7 C6 102.0(2) ? ? ? ? Pd1 Se7 C8 110.9(2) ? ? ? ? C6 Se7 C8 95.1(3) ? ? ? ? Pd1 Se11 C10 112.2(2) ? ? ? ? Pd1 Se11 C12 102.2(2) ? ? ? ? C10 Se11 C12 94.6(3) ? ? ? ? Pd1 Se15 C14 100.5(2) ? ? ? ? Pd1 Se15 C16 110.8(2) ? ? ? ? C14 Se15 C16 96.1(3) ? ? ? ? C2 C1 C16 113.8(5) ? ? ? ? Se3 C2 C1 116.2(4) ? ? ? ? Se3 C4 C5 112.4(4) ? ? ? ? C4 C5 C6 114.0(5) ? ? ? ? Se7 C6 C5 113.5(4) ? ? ? ? Se7 C8 C9 117.7(4) ? ? ? ? C8 C9 C10 115.2(5) ? ? ? ? Se11 C10 C9 116.5(4) ? ? ? ? Se11 C12 C13 114.5(4) ? ? ? ? C12 C13 C14 115.3(5) ? ? ? ? Se15 C14 C13 112.1(4) ? ? ? ? Se15 C16 C1 114.7(4) ? ? ? ? F1 B1 F2 109.7 ? ? ? ? F1 B1 F3 108.4 ? ? ? ? F1 B1 F4 109.1 ? ? ? ? F2 B1 F3 109.3 ? ? ? ? F2 B1 F4 107.6 ? ? ? ? F3 B1 F4 112.8 ? ? ? ? F1 B2 F5 111.3 ? ? ? ? F1 B2 F6 109.7 ? ? ? ? F1 B2 F7 111.1 ? ? ? ? F5 B2 F6 108.9 ? ? ? ? F5 B2 F7 107.4 ? ? ? ? F6 B2 F7 108.3 ? ? ? ? F1 B3 F8 107.4 ? ? ? ? F1 B3 F9 111.4 ? ? ? ? F1 B3 F10 109.2 ? ? ? ? F8 B3 F9 108.6 ? ? ? ? F8 B3 F10 110.4 ? ? ? ? F9 B3 F10 109.8 ? ? ? ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Se3 2.4560(7) ? ? ? Pd1 Se7 2.4583(7) ? ? ? Pd1 Se11 2.4395(7) ? ? ? Pd1 Se15 2.4430(7) ? ? ? Se3 C2 1.973(6) ? ? ? Se3 C4 1.959(5) ? ? ? Se7 C6 1.958(6) ? ? ? Se7 C8 1.965(5) ? ? ? Se11 C10 1.944(6) ? ? ? Se11 C12 1.962(5) ? ? ? Se15 C14 1.965(5) ? ? ? Se15 C16 1.944(6) ? ? ? C1 C2 1.500(8) ? ? ? C1 C16 1.516(8) ? ? ? C4 C5 1.523(7) ? ? ? C5 C6 1.517(8) ? ? ? C8 C9 1.487(8) ? ? ? C9 C10 1.502(8) ? ? ? C12 C13 1.504(8) ? ? ? C13 C14 1.510(8) ? ? ? F1 B1 1.38 ? ? ? F1 B2 1.38 ? ? ? F1 B3 1.38 ? ? ? F2 B1 1.38 ? ? ? F3 B1 1.38 ? ? ? F4 B1 1.38 ? ? ? F5 B2 1.38 ? ? ? F6 B2 1.38 ? ? ? F7 B2 1.38 ? ? ? F8 B3 1.38 ? ? ? F9 B3 1.38 ? ? ? F10 B3 1.38 ? ? ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 C16 C1 C2 Se3 -72.6(5) ? ? ? ? C2 Se3 C4 C5 -172.5(5) ? ? ? ? C4 C5 C6 Se7 75.0(4) ? ? ? ? C6 Se7 C8 C9 92.5(5) ? ? ? ? C8 C9 C10 Se11 -78.9(5) ? ? ? ? C10 Se11 C12 C13 -173.3(6) ? ? ? ? C12 C13 C14 Se15 70.6(5) ? ? ? ? C14 Se15 C16 C1 75.6(4) ? ? ? ? C4 Se3 C2 C1 -100.3(5) ? ? ? ? Se3 C4 C5 C6 -74.7(4) ? ? ? ? C8 Se7 C6 C5 173.4(5) ? ? ? ? Se7 C8 C9 C10 76.4(5) ? ? ? ? C12 Se11 C10 C9 -88.9(5) ? ? ? ? Se11 C12 C13 C14 -67.7(5) ? ? ? ? C16 Se15 C14 C13 169.0(6) ? ? ? ? C2 C1 C16 Se15 88.3(5) ? ? ? ? Se7 Pd1 Se3 C2 -162.3(2) ? ? ? ? Se15 Pd1 Se3 C2 30.8(2) ? ? ? ? Se3 Pd1 Se7 C6 61.7(2) ? ? ? ? Se11 Pd1 Se7 C6 -128.3(2) ? ? ? ? Se7 Pd1 Se11 C10 26.5(2) ? ? ? ? Se15 Pd1 Se11 C10 -166.3(2) ? ? ? ? Se3 Pd1 Se15 C14 -121.3(2) ? ? ? ? Se11 Pd1 Se15 C14 68.3(2) ? ? ? ? Se7 Pd1 Se3 C4 -62.3(2) ? ? ? ? Se15 Pd1 Se3 C4 130.7(2) ? ? ? ? Se3 Pd1 Se7 C8 162.0(2) ? ? ? ? Se11 Pd1 Se7 C8 -28.0(2) ? ? ? ? Se7 Pd1 Se11 C12 126.7(2) ? ? ? ? Se15 Pd1 Se11 C12 -66.1(2) ? ? ? ? Se3 Pd1 Se15 C16 -20.6(2) ? ? ? ? Se11 Pd1 Se15 C16 169.1(2) ? ? ? ? Pd1 Se3 C2 C1 5.0(3) ? ? ? ? Pd1 Se3 C4 C5 74.2(3) ? ? ? ? Pd1 Se7 C6 C5 -73.9(4) ? ? ? ? Pd1 Se7 C8 C9 -12.5(3) ? ? ? ? Pd1 Se11 C10 C9 16.3(3) ? ? ? ? Pd1 Se11 C12 C13 72.8(4) ? ? ? ? Pd1 Se15 C14 C13 -78.4(4) ? ? ? ? Pd1 Se15 C16 C1 -28.1(3) ? ? ? ?