#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/70/2007085.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_2007085 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_volume 54 _journal_year 1998 _chemical_formula_iupac '[Pd (C6 H12 S3)2] [I Br2]2' _chemical_formula_moiety 'C12 H24 Pd S6 2+, 2I Br2 -' _chemical_formula_sum 'C12 H24 Br4 I2 Pd S6' _chemical_formula_weight 1040.51 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 109.69(7) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.253(8) _cell_length_b 12.88(2) _cell_length_c 12.455(10) _cell_measurement_reflns_used 36 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 16.0 _cell_measurement_theta_min 15.5 _cell_volume 1398(3) _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 'SHELXL97 (Sheldrick, 1993)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Stoe Stadi-4 four-circle' _diffrn_measurement_method \w/2\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 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2478 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.82 _diffrn_standards_decay_% 'variation +-2' _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 9.039 _exptl_absorpt_correction_T_max 0.062 _exptl_absorpt_correction_T_min 0.010 _exptl_absorpt_correction_type ; \y scans (North, Phillips & Mathews, 1968), and then refdelf (Walker & Stuart, 1983) ; _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 2.473 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 968 _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.28 _refine_diff_density_max '3.46 (0.30\%A from Br2)' _refine_diff_density_min '-3.56 (0.89\%A from I1)' _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment 'riding model' _refine_ls_matrix_type full _refine_ls_number_parameters 116 _refine_ls_number_reflns 2435 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.1236 _refine_ls_R_factor_gt 0.0935 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.192P)^2^+20.95P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_ref 0.2882 _reflns_number_gt 1740 _reflns_number_total 2435 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ha1202.cif _[local]_cod_data_source_block 1 _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_depositor_comments ; The following automatic conversions were performed: '_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 (5 times). Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 2007085 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Pd -.5000 1.0000 .0000 .0380(6) Uani d S 1 . . Pd S1 -.6845(6) .8360(4) -.1544(4) .0488(13) Uani d . 1 . . S C2 -.822(2) .9362(16) -.2246(18) .046(5) Uani d . 1 . . C H2A -.8954 .9059 -.2926 .055 Uiso calc R 1 . . H H2B -.8789 .9543 -.1742 .055 Uiso calc R 1 . . H C3 -.763(2) 1.0372(18) -.2598(17) .052(6) Uani d . 1 . . C H3A -.8508 1.0795 -.3021 .063 Uiso calc R 1 . . H H3B -.7072 1.0204 -.3107 .063 Uiso calc R 1 . . H S4 -.6387(6) 1.1139(4) -.1405(4) .0438(12) Uani d . 1 . . S C5 -.487(2) 1.1545(14) -.1948(16) .040(4) Uani d . 1 . . C H5A -.5317 1.1957 -.2632 .048 Uiso calc R 1 . . H H5B -.4145 1.1982 -.1384 .048 Uiso calc R 1 . . H C6 -.400(2) 1.0621(17) -.2225(16) .047(5) Uani d . 1 . . C H6A -.3131 1.0875 -.2411 .056 Uiso calc R 1 . . H H6B -.4678 1.0255 -.2885 .056 Uiso calc R 1 . . H S7 -.3342(5) .9729(4) -.1019(4) .0413(11) Uani d . 1 . . S C8 -.395(3) .8444(16) -.1726(17) .050(5) Uani d . 1 . . C H8A -.3363 .8327 -.2232 .059 Uiso calc R 1 . . H H8B -.3634 .7915 -.1138 .059 Uiso calc R 1 . . H C9 -.556(3) .827(2) -.238(2) .059(6) Uani d . 1 . . C H9A -.5664 .7580 -.2722 .071 Uiso calc R 1 . . H H9B -.5880 .8768 -.2997 .071 Uiso calc R 1 . . H I1 .18218(15) .61898(12) .03933(11) .0504(6) Uani d . 1 . . I Br1 .3212(2) .42217(17) .05488(18) .0491(6) Uani d . 1 . . Br Br2 .0353(2) .81623(16) .01655(17) .0434(6) 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 .0371(11) .0412(12) .0336(10) .0064(9) .0092(8) .0028(9) S1 .052(3) .047(3) .047(3) -.009(2) .016(2) .001(2) C2 .031(10) .045(11) .055(12) -.008(9) .005(8) .006(10) C3 .030(9) .074(15) .037(9) -.003(10) -.008(7) .019(10) S4 .042(3) .042(3) .043(2) .008(2) .008(2) .004(2) C5 .032(9) .035(10) .044(10) .007(8) .000(8) .006(9) C6 .038(10) .060(13) .039(10) .004(10) .010(8) .013(10) S7 .036(2) .045(3) .043(2) .000(2) .0130(19) .001(2) C8 .072(14) .036(10) .037(10) .015(10) .014(9) .007(9) C9 .057(13) .058(14) .053(12) -.002(11) .007(10) .003(11) I1 .0477(9) .0606(10) .0420(8) -.0136(6) .0142(6) .0006(6) Br1 .0412(11) .0457(12) .0529(12) -.0016(9) .0061(9) .0074(9) Br2 .0333(10) .0460(11) .0535(11) -.0054(8) .0179(8) .0072(9) 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 . 2.997(6) yes Pd S4 . 2.313(5) yes Pd S7 . 2.323(5) yes Pd S4 3_475 2.313(5) ? Pd S7 3_475 2.323(5) ? S1 C2 . 1.82(2) ? S1 C9 . 1.83(3) ? C2 C3 . 1.53(3) ? C3 S4 . 1.83(2) ? S4 C5 . 1.83(2) ? C5 C6 . 1.54(3) ? C6 S7 . 1.825(19) ? S7 C8 . 1.87(2) ? C8 C9 . 1.46(3) ? I1 Br1 . 2.819(4) yes I1 Br2 . 2.850(4) yes 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' Br Br -0.2901 2.4595 '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' Pd Pd -0.9988 1.0072 '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' 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 S4 Pd S4 . 3_475 180.0 ? S4 Pd S7 . 3_475 91.05(19) ? S4 Pd S7 3_475 3_475 88.95(19) ? S1 Pd S4 . . 84.8(2) ? S1 Pd S7 . . 83.2(2) ? S4 Pd S7 . . 88.95(19) ? S4 Pd S7 3_475 . 91.05(19) ? S7 Pd S7 3_475 . 180.0 ? C2 S1 C9 . . 105.0(11) ? C3 C2 S1 . . 118.7(14) ? C2 C3 S4 . . 114.5(14) ? C5 S4 C3 . . 102.0(10) ? C5 S4 Pd . . 99.3(6) ? C3 S4 Pd . . 108.0(7) ? C6 C5 S4 . . 112.6(13) ? C5 C6 S7 . . 111.0(13) ? C6 S7 C8 . . 101.9(10) ? C6 S7 Pd . . 104.7(7) ? C8 S7 Pd . . 104.0(8) ? C9 C8 S7 . . 119.4(16) ? C8 C9 S1 . . 114.2(17) ? Br1 I1 Br2 . . 178.18(7) 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 S1 C2 C3 S4 -64(2) C2 C3 S4 C5 137.4(16) C3 S4 C5 C6 -60.4(15) S4 C5 C6 S7 -51.6(16) C5 C6 S7 C8 132.9(15) C6 S7 C8 C9 -57(2) S7 C8 C9 S1 -61(2) C8 C9 S1 C2 122.4(17) C9 S1 C2 C3 -45.5(19) _journal_paper_doi 10.1107/S0108270197014212