#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/47/2004739.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2004739 loop_ _publ_author_name 'Lee, G.-H.' 'Tzeng, B.-C.' _publ_section_title ; Palladium Complexes of 1,4,7-Trithiacyclodecane ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 879 _journal_page_last 882 _journal_volume 52 _journal_year 1996 _chemical_formula_moiety '[Pd Cl2 (C7 H14 S3 )]' _chemical_formula_sum 'C7 H14 Cl2 Pd S3' _chemical_formula_weight 371.7 _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_type_scat_source 'IntTabIV Table 2.2B' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.565(1) _cell_length_b 12.046(1) _cell_length_c 13.701(1) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298 _cell_measurement_theta_max 25 _cell_measurement_theta_min 18.50 _cell_volume 1248.5(2) _diffrn_measurement_device 'Nonius CAD-4' _diffrn_measurement_method \q/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1283 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% <2 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.34 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_type '\y scan (North, Phillips & Mathews, 1968)' _exptl_crystal_colour red-brown _exptl_crystal_density_diffrn 1.977 _exptl_crystal_density_meas 1.958 _exptl_crystal_density_method flotation _exptl_crystal_description plate _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.57 _refine_diff_density_min -0.39 _refine_ls_extinction_coef 0.34(4) _refine_ls_extinction_method 'Gaussian (Zachariasen, 1967)' _refine_ls_goodness_of_fit_obs 1.16 _refine_ls_hydrogen_treatment 'H atoms fixed at calculated positions with U~H~ = U~attached~ + 0.01' _refine_ls_number_parameters 119 _refine_ls_number_reflns 1091 _refine_ls_R_factor_obs 0.026 _refine_ls_shift/esd_max 0.007 _refine_ls_weighting_scheme 1/[\s^2^(F~o~)+(0.002F~c~)^2^] _refine_ls_wR_factor_obs 0.026 _reflns_number_observed 1091 _reflns_number_total 1283 _reflns_observed_criterion I>=2\s(I) _[local]_cod_data_source_file hl1041.cif _[local]_cod_data_source_block hl1041a _[local]_cod_chemical_formula_sum_orig 'C7 H14 Cl2 Pd1 S3' _cod_original_cell_volume 1248.4(2) _cod_database_code 2004739 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z -x,1/2+y,1/2-z 1/2+x,1/2-y,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv Pd .05887(6) .16384(4) .24350(4) 2.37(2) Cl(1) .2134(3) .1525(2) .3908(1) 4.18(9) Cl(2) .2972(2) .2512(2) .1675(1) 3.85(9) S(1) -.1594(3) .0708(2) .3216(1) 3.13(8) S(2) -.1767(3) .3639(2) .2924(1) 3.35(8) S(3) -.0655(2) .1793(2) .0938(1) 2.87(7) C(1) -.2563(9) .1717(7) .4028(5) 3.5(3) C(2) -.3302(9) .2763(6) .3573(5) 3.4(3) C(3) -.2627(9) .3620(6) .1698(5) 2.8(3) C(4) -.1337(9) .3228(6) .0906(5) 2.8(3) C(5) -.2728(10) .1060(7) .0772(6) 3.8(4) C(6) -.2951(10) .0059(7) .1409(6) 3.9(4) C(7) -.3455(9) .0331(6) .2448(7) 3.9(4) H1A -.174 .192 .452 3.8 H1B -.357 .135 .438 3.8 H2A -.422 .255 .312 3.8 H2B -.386 .321 .407 3.8 H3A -.308 .435 .152 3.1 H3B -.365 .312 .166 3.1 H4A -.182 .340 .028 3.4 H4B -.029 .370 .099 3.4 H5A -.288 .085 .010 4.6 H5B -.372 .156 .092 4.6 H6A -.377 -.045 .112 4.1 H6B -.181 -.031 .143 4.1 H7A -.433 .093 .244 4.3 H7B -.409 -.031 .273 4.3 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl(1) Pd Cl(2) 91.44(7) yes Cl(1) Pd S(1) 85.86(8) yes Cl(1) Pd S(2) 98.51(6) yes Cl(1) Pd S(3) 174.41(7) yes Cl(2) Pd S(1) 176.15(7) yes Cl(2) Pd S(2) 101.06(7) yes Cl(2) Pd S(3) 83.10(7) yes S(1) Pd S(2) 82.07(6) yes S(1) Pd S(3) 99.54(7) yes S(2) Pd S(3) 83.78(6) yes Pd S(1) C(1) 104.7(3) yes Pd S(1) C(7) 114.5(3) yes C(1) S(1) C(7) 102.2(4) yes Pd S(2) C(2) 91.3(2) yes Pd S(2) C(3) 89.8(2) yes C(2) S(2) C(3) 102.7(3) yes Pd S(3) C(4) 102.7(2) yes Pd S(3) C(5) 115.6(3) yes C(4) S(3) C(5) 102.5(3) yes S(1) C(1) C(2) 117.2(5) yes S(2) C(2) C(1) 116.9(5) yes S(2) C(3) C(4) 115.7(5) yes S(3) C(4) C(3) 117.3(5) yes S(3) C(5) C(6) 114.6(5) yes C(5) C(6) C(7) 113.8(7) yes S(1) C(7) C(6) 113.9(5) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Pd Cl(1) 2.336(2) yes Pd Cl(2) 2.333(2) yes Pd S(1) 2.264(2) yes Pd S(2) 3.071(2) yes Pd S(3) 2.265(2) yes S(1) C(1) 1.804(8) yes S(1) C(7) 1.816(8) yes S(2) C(2) 1.803(8) yes S(2) C(3) 1.801(7) yes S(3) C(4) 1.805(7) yes S(3) C(5) 1.814(7) yes C(1) C(2) 1.510(10) yes C(3) C(4) 1.530(10) yes C(5) C(6) 1.500(10) yes C(6) C(7) 1.510(10) yes