data_2007086 _journal_name_full 'Acta Crystallographica' _journal_year 1998 _journal_volume C54 _journal_page_first 295 _journal_page_last 298 _publ_section_title ; Macrocyclic Thioether Complexes of Palladium with Dibromoiodide Anions ; loop_ _publ_author_name 'Blake, Alexander J.' 'Gilby, Liam M.' 'Gould, Robert O.' 'Lippolis, Vito' 'Parsons, Simon' 'Schr\"oder, Martin' _chemical_formula_moiety 'C10 H20 Pd S4 2+, 2I Br2 -' _chemical_formula_sum 'C10 H20 Br4 I2 Pd S4' _chemical_formula_iupac '[Pd (C10 H20 S4)] [I Br2]2' _chemical_formula_weight 948.34 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'I 2/a' 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' _cell_length_a 14.651(2) _cell_length_b 9.3117(7) _cell_length_c 16.7648(11) _cell_angle_alpha 90.00 _cell_angle_beta 93.468(10) _cell_angle_gamma 90.00 _cell_volume 2282.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 2.759 _diffrn_ambient_temperature 293(2) _refine_ls_R_factor_obs .0392 _refine_ls_wR_factor_obs .0903 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_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_ _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