#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/70/2007086.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_2007086 loop_ _publ_author_name 'Blake, Alexander J.' 'Gilby, Liam M.' 'Gould, Robert O.' 'Lippolis, Vito' 'Parsons, Simon' 'Schr\"oder, Martin' _publ_section_title ; Macrocyclic Thioether Complexes of Palladium with Dibromoiodide Anions ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 295 _journal_page_last 298 _journal_paper_doi 10.1107/S0108270197014212 _journal_volume 54 _journal_year 1998 _chemical_formula_iupac '[Pd (C10 H20 S4)] [I Br2]2' _chemical_formula_moiety 'C10 H20 Pd S4 2+, 2I Br2 -' _chemical_formula_sum 'C10 H20 Br4 I2 Pd S4' _chemical_formula_weight 948.34 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-I 2ya' _symmetry_space_group_name_H-M 'I 1 2/a 1' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 93.468(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.651(2) _cell_length_b 9.3117(7) _cell_length_c 16.7648(11) _cell_measurement_reflns_used 48 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 14 _cell_measurement_theta_min 13 _cell_volume 2283.0(4) _computing_cell_refinement DIF4 _computing_data_collection 'DIF4 (Stoe & Cie, 1992a)' _computing_data_reduction 'REDU4 (Stoe & Cie, 1992b)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1995)' _computing_publication_material 'SHELXL93 (Sheldrick, 1993)' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Stoe Stadi-4 four-circle' _diffrn_measurement_method \w/\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 2523 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.50 _diffrn_standards_decay_% none _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 10.877 _exptl_absorpt_correction_T_max 0.694 _exptl_absorpt_correction_T_min 0.176 _exptl_absorpt_correction_type '\y scans (North, Phillips & Matthews, 1968)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.759 _exptl_crystal_density_meas ? _exptl_crystal_description plate _exptl_crystal_F_000 1744 _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.04 _refine_diff_density_max '1.12 (0.89\%A from Br2)' _refine_diff_density_min '-1.07 (0.84\%A from Br2)' _refine_ls_extinction_coef 0.00123(10) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_all 1.055 _refine_ls_goodness_of_fit_obs 1.053 _refine_ls_hydrogen_treatment 'constr with U~iso~(H) = 1.2U~eq~(C)' _refine_ls_matrix_type full _refine_ls_number_parameters 98 _refine_ls_number_reflns 1878 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.164 _refine_ls_restrained_S_obs 1.053 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_obs .0392 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.041P)^2^+29.01P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1102 _refine_ls_wR_factor_obs .0903 _reflns_number_observed 1564 _reflns_number_total 1894 _reflns_observed_criterion I>2\s(I) _[local]_cod_data_source_file ha1202.cif _[local]_cod_data_source_block 2 _[local]_cod_cif_authors_sg_H-M 'I 2/a' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (6 times). Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.041P)^2^+29.01P] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.041P)^2^+29.01P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 2282.9(4) _cod_database_code 2007086 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd .0290(5) .0310(4) .0295(4) -.0002(3) -.0043(4) -.0004(3) S1 .0319(11) .0402(11) .0352(10) -.0039(9) -.0033(9) .0012(9) C2 .039(5) .058(5) .039(5) -.006(4) -.008(4) .003(4) C3 .025(4) .057(5) .050(5) .012(4) -.005(4) .012(4) C4 .040(5) .035(4) .047(5) .004(4) .002(4) .008(4) S5 .0339(12) .0367(11) .0384(11) .0024(8) -.0001(9) -.0017(9) C6 .056(6) .030(4) .046(5) -.015(4) -.008(5) -.002(4) C7 .035(5) .043(4) .040(4) -.008(4) -.006(4) -.001(4) I .0344(4) .0629(4) .0353(3) .0060(3) -.0001(2) .0021(3) Br1 .0611(7) .0657(7) .0619(7) -.0117(5) .0107(6) -.0086(5) Br2 .0638(8) .0762(8) .1002(10) -.0092(6) .0175(7) -.0329(7) 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_occupancy _atom_site_disorder_group _atom_site_type_symbol Pd 1.0000 .0000 1.0000 .0301(3) Uani d S 1 . Pd S1 1.12982(15) .0841(2) 1.06734(12) .0360(5) Uani d . 1 . S C2 1.1464(7) -.0446(10) 1.1487(5) .046(2) Uani d . 1 . C H2A 1.1913(7) -.0075(10) 1.1884(5) .055 Uiso calc R 1 . H H2B 1.0893(7) -.0577(10) 1.1742(5) .055 Uiso calc R 1 . H C3 1.1785(6) -.1873(10) 1.1181(5) .044(2) Uani d . 1 . C H3A 1.2272(6) -.1690(10) 1.0828(5) .053 Uiso calc R 1 . H H3B 1.2048(6) -.2413(10) 1.1633(5) .053 Uiso calc R 1 . H C4 1.1085(6) -.2806(9) 1.0744(5) .041(2) Uani d . 1 . C H4A 1.0552(6) -.2883(9) 1.1058(5) .049 Uiso calc R 1 . H H4B 1.1336(6) -.3763(9) 1.0689(5) .049 Uiso calc R 1 . H S5 1.07356(15) -.2114(2) .97581(12) .0364(5) Uani d . 1 . S C6 .9752(7) -.3233(9) .9444(5) .045(2) Uani d . 1 . C H6A .9961(7) -.4114(9) .9206(5) .054 Uiso calc R 1 . H H6B .9416(7) -.3485(9) .9905(5) .054 Uiso calc R 1 . H C7 .9133(6) -.2433(9) .8844(5) .040(2) Uani d . 1 . C H7A .8627(6) -.3043(9) .8658(5) .048 Uiso calc R 1 . H H7B .9469(6) -.2157(9) .8388(5) .048 Uiso calc R 1 . H I .86256(4) -.20923(7) 1.16481(3) .0443(2) Uani d . 1 . I Br1 .90772(8) .04889(12) 1.22879(7) .0626(3) Uani d . 1 . Br Br2 .81742(9) -.47120(14) 1.10871(9) .0796(4) Uani d . 1 . Br 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 Pd S1 . 5_757 180.0 ? S1 Pd S5 . 5_757 90.26(8) ? S1 Pd S5 5_757 5_757 89.74(8) ? S1 Pd S5 . . 89.74(8) yes S1 Pd S5 5_757 . 90.26(8) ? S5 Pd S5 5_757 . 180.0 ? C7 S1 C2 5_757 . 103.7(4) ? C7 S1 Pd 5_757 . 101.4(3) ? C2 S1 Pd . . 102.3(3) ? C7 S1 I 5_757 6_655 83.5(3) ? C2 S1 I . 6_655 78.9(3) ? Pd S1 I . 6_655 174.37(9) ? C7 S1 I 5_757 5_757 102.8(3) ? C2 S1 I . 5_757 153.5(3) ? Pd S1 I . 5_757 72.34(5) ? I S1 I 6_655 5_757 104.07(5) ? C3 C2 S1 . . 110.8(6) ? C4 C3 C2 . . 117.2(7) ? C3 C4 S5 . . 112.6(6) ? C4 S5 C6 . . 103.5(4) ? C4 S5 Pd . . 104.7(3) ? C6 S5 Pd . . 99.8(3) ? C4 S5 Br2 . 5_747 87.7(3) ? C6 S5 Br2 . 5_747 77.6(3) ? Pd S5 Br2 . 5_747 167.59(9) ? C4 S5 Br1 . 5_757 159.4(3) ? C6 S5 Br1 . 5_757 93.8(3) ? Pd S5 Br1 . 5_757 82.95(6) ? Br2 S5 Br1 5_747 5_757 85.13(5) ? C7 C6 S5 . . 110.0(6) ? C6 C7 S1 . 5_757 108.5(6) ? Br1 I Br2 . . 177.10(5) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd S1 . 2.290(2) yes Pd S1 5_757 2.290(2) ? Pd S5 5_757 2.292(2) ? Pd S5 . 2.292(2) yes S1 C7 5_757 1.819(9) ? S1 C2 . 1.821(9) ? S1 I 6_655 3.870(2) yes S1 I 5_757 4.071(2) ? C2 C3 . 1.510(12) ? C3 C4 . 1.501(12) ? C4 S5 . 1.819(8) ? S5 C6 . 1.830(8) ? S5 Br2 5_747 3.684(2) yes S5 Br1 5_757 3.774(2) ? C6 C7 . 1.509(12) ? C7 S1 5_757 1.819(9) ? I Br1 . 2.6981(12) yes I Br2 . 2.6827(13) yes 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_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion C7 S1 C2 C3 5_757 . 177.5(6) I S1 C2 C3 6_655 . -102.1(6) I S1 C2 C3 5_757 . -2.8(12) S1 C2 C3 C4 . . -75.8(9) C2 C3 C4 S5 . . 71.8(10) C3 C4 S5 C6 . . -169.8(7) C3 C4 S5 Br2 . 5_747 113.6(6) C3 C4 S5 Br1 . 5_757 43.9(12) C4 S5 C6 C7 . . 154.6(6) Br2 S5 C6 C7 5_747 . -120.9(7) Br1 S5 C6 C7 5_757 . -36.7(6) S5 C6 C7 S1 . 5_757 -62.5(7)