#------------------------------------------------------------------------------ #$Date: 2013-08-29 18:37:19 +0300 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/25/2012538.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_2012538 loop_ _publ_author_name 'Johansson, Maria H.' 'Oskarsson, \%Ake' _publ_section_title ; Tetrakis(dimethyl sulfide)palladium(II) bis(tetrafluoroborate) and tetrakis(1,4-oxathiane-\kS)palladium(II) bis(tetrafluoroborate) ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m102 _journal_page_last m104 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Pd (C4 H8 O S)4] (B F4)2' _chemical_formula_moiety 'C16 H32 O4 Pd S4 2+ , 2B F4 -' _chemical_formula_sum 'C16 H32 B2 F8 O4 Pd S4' _chemical_formula_weight 696.68 _chemical_name_systematic ; tetrakis(1,4-oxathiane-S)palladium(II) bis(tetrafluoroborate) ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 94.11(3) _cell_angle_beta 114.12(3) _cell_angle_gamma 111.79(3) _cell_formula_units_Z 1 _cell_length_a 8.8804(18) _cell_length_b 9.5397(19) _cell_length_c 9.6999(19) _cell_measurement_reflns_used 2469 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26 _cell_measurement_theta_min 4 _cell_volume 671.8(4) _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction SAINT _computing_molecular_graphics 'DIAMOND (Brandenburg, 2000)' _computing_publication_material 'SHELXTL (Sheldrick, 1997b)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997a)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 512 _diffrn_measured_fraction_theta_full .989 _diffrn_measured_fraction_theta_max .989 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .050 _diffrn_reflns_av_sigmaI/netI .109 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 4856 _diffrn_reflns_theta_full 27.87 _diffrn_reflns_theta_max 27.87 _diffrn_reflns_theta_min 2.38 _diffrn_standards_decay_% .00 _exptl_absorpt_coefficient_mu 1.079 _exptl_absorpt_correction_T_max .882 _exptl_absorpt_correction_T_min .813 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 352 _exptl_crystal_size_max .20 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .12 _refine_diff_density_max 2.56 _refine_diff_density_min -2.61 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .960 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 188 _refine_ls_number_reflns 3185 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .960 _refine_ls_R_factor_all .109 _refine_ls_R_factor_gt .080 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.1175P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .188 _refine_ls_wR_factor_ref .203 _reflns_number_gt 2080 _reflns_number_total 3185 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file tr1008.cif _[local]_cod_data_source_block II _[local]_cod_cif_authors_sg_H-M P-1 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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 ; _cod_original_cell_volume 671.8(2) _cod_database_code 2012538 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 .0000 .0000 .0000 .0389(3) Uani d S 1 . . Pd S1 .1223(3) -.12129(19) .18864(18) .0434(4) Uani d . 1 . . S S2 -.0004(3) .1677(2) .18654(18) .0453(5) Uani d . 1 . . S O1 .1913(9) -.4185(7) .2135(7) .0646(15) Uani d . 1 . . O O2 .0678(9) .2047(7) .5288(6) .0673(17) Uani d . 1 . . O C1 .3008(11) -.1557(11) .1718(11) .061(2) Uani d . 1 . . C H1A .2616 -.1989 .0627 .074 Uiso calc R 1 . . H H1B .4106 -.0577 .2104 .074 Uiso calc R 1 . . H C2 .3429(14) -.2699(13) .2665(12) .076(3) Uani d . 1 . . C H2A .4438 -.2831 .2612 .091 Uiso calc R 1 . . H H2B .3825 -.2252 .3753 .091 Uiso calc R 1 . . H C3 -.0429(10) -.3229(8) .1328(8) .0461(16) Uani d . 1 . . C H3A -.1473 -.3286 .1462 .055 Uiso calc R 1 . . H H3B -.0868 -.3692 .0233 .055 Uiso calc R 1 . . H C4 .0455(13) -.4120(9) .2328(9) .057(2) Uani d . 1 . . C H4A .0908 -.3632 .3419 .069 Uiso calc R 1 . . H H4B -.0471 -.5179 .2077 .069 Uiso calc R 1 . . H C5 -.1404(11) .0437(9) .2626(8) .0507(18) Uani d . 1 . . C H5A -.2687 -.0030 .1842 .061 Uiso calc R 1 . . H H5B -.1054 -.0400 .2873 .061 Uiso calc R 1 . . H C6 -.1142(12) .1405(12) .4094(9) .063(2) Uani d . 1 . . C H6A -.1485 .2244 .3839 .076 Uiso calc R 1 . . H H6B -.1947 .0749 .4463 .076 Uiso calc R 1 . . H C7 .2141(12) .2538(10) .3612(9) .060(2) Uani d . 1 . . C H7A .2585 .1757 .3878 .072 Uiso calc R 1 . . H H7B .3040 .3369 .3449 .072 Uiso calc R 1 . . H C8 .1905(13) .3200(10) .4944(9) .066(2) Uani d . 1 . . C H8A .3092 .3717 .5874 .079 Uiso calc R 1 . . H H8B .1460 .3979 .4666 .079 Uiso calc R 1 . . H B1 -.4746(15) .2873(13) .1682(14) .070(3) Uani d . 1 . . B F1 -.4548(13) .2388(15) .3108(11) .157(4) Uani d . 1 . . F F2 -.646(2) .251(3) .094(2) .108(8) Uani d P .51(2) . . F F2' -.543(4) .398(3) .174(2) .134(10) Uani d P .49(2) . . F F3 -.447(3) .172(3) .0910(16) .121(8) Uani d P .51(2) . . F F3' -.607(5) .172(3) .069(4) .23(2) Uani d P .49(2) . . F F4 -.348(4) .412(3) .216(3) .191(18) Uani d P .51(2) . . F F4' -.325(4) .350(6) .168(6) .24(2) Uani d P .49(2) . . F 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 .0707(6) .0420(4) .0305(4) .0368(4) .0350(4) .0191(3) S1 .0724(12) .0431(9) .0329(8) .0363(9) .0297(8) .0181(7) S2 .0823(13) .0502(10) .0344(8) .0455(10) .0384(9) .0216(7) O1 .093(4) .071(4) .067(4) .062(4) .045(3) .031(3) O2 .118(5) .083(4) .034(3) .066(4) .043(3) .029(3) C1 .059(5) .079(6) .061(5) .040(4) .029(4) .030(4) C2 .079(6) .102(8) .074(6) .067(6) .034(5) .039(6) C3 .069(5) .045(4) .049(4) .034(4) .040(4) .021(3) C4 .101(6) .053(4) .058(5) .052(4) .054(5) .031(4) C5 .063(5) .070(5) .038(4) .038(4) .033(3) .016(3) C6 .090(6) .095(6) .046(4) .059(5) .050(4) .033(4) C7 .077(5) .050(5) .054(5) .028(4) .032(4) .004(3) C8 .095(6) .059(5) .039(4) .045(5) .020(4) -.001(4) B1 .055(7) .059(7) .077(7) .010(6) .031(5) -.004(5) F1 .179(8) .258(12) .120(7) .149(8) .093(6) .088(7) F2 .063(10) .16(2) .114(14) .055(14) .045(10) .038(15) F2' .17(2) .15(2) .112(14) .111(19) .053(13) .038(13) F3 .183(19) .18(2) .065(8) .128(17) .070(10) .032(9) F3' .21(4) .12(2) .22(3) -.02(2) .07(2) -.09(2) F4 .15(2) .119(16) .19(2) -.073(16) .117(18) -.086(15) F4' .19(3) .32(5) .44(6) .18(3) .26(4) .27(5) 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 . 2.3406(17) yes Pd S1 2 2.3406(17) ? Pd S2 2 2.3293(17) ? Pd S2 . 2.3293(17) yes S1 C1 . 1.799(9) yes S1 C3 . 1.803(7) yes S2 C5 . 1.809(7) yes S2 C7 . 1.782(8) yes O1 C2 . 1.414(12) yes O1 C4 . 1.403(10) yes O2 C6 . 1.401(10) yes O2 C8 . 1.403(11) yes C1 C2 . 1.529(12) ? C3 C4 . 1.507(10) ? C5 C6 . 1.523(10) ? C7 C8 . 1.522(11) ? B1 F4 . 1.180(19) ? B1 F3' . 1.22(2) ? B1 F4' . 1.24(2) ? B1 F2 . 1.278(18) ? B1 F2' . 1.41(2) ? B1 F3 . 1.436(19) ? B1 F1 . 1.453(14) ? F2 F3' . .99(4) ? F2 F2' . 1.31(3) ? F2' F4 . 1.56(3) ? F3 F3' . 1.35(4) ? F3 F4' . 1.55(5) ? F4 F4' . .86(4) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -.9988 1.0072 '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 S2 Pd S2 2 . 180.00(8) ? S1 Pd S2 2 . 89.48(6) yes S1 Pd S2 . . 90.52(6) yes S1 Pd S2 2 2 90.52(6) ? S2 Pd S1 . 2 89.48(6) ? S1 Pd S1 . 2 180.00(9) ? Pd S1 C1 . . 111.3(3) yes Pd S1 C3 . . 108.4(2) yes Pd S2 C5 . . 106.2(3) yes Pd S2 C7 . . 111.7(3) yes C1 S1 C3 . . 97.7(4) yes C5 S2 C7 . . 98.7(4) yes C2 O1 C4 . . 112.6(7) yes C6 O2 C8 . . 113.0(6) yes C2 C1 S1 . . 109.7(6) ? O1 C2 C1 . . 113.4(7) ? C4 C3 S1 . . 109.6(6) ? O1 C4 C3 . . 113.8(6) ? C6 C5 S2 . . 109.6(6) ? O2 C6 C5 . . 111.8(7) ? C8 C7 S2 . . 109.7(6) ? O2 C8 C7 . . 112.7(7) ? F4 B1 F3' . . 156(2) ? F4 B1 F4' . . 42(2) ? F3' B1 F4' . . 124(3) ? F4 B1 F2 . . 129(2) ? F3' B1 F2 . . 47(2) ? F4' B1 F2 . . 145(2) ? F4 B1 F2' . . 73(2) ? F3' B1 F2' . . 104(2) ? F4' B1 F2' . . 110(2) ? F2 B1 F2' . . 58.1(13) ? F4 B1 F3 . . 111.8(18) ? F3' B1 F3 . . 61(2) ? F4' B1 F3 . . 70(2) ? F2 B1 F3 . . 106.2(16) ? F2' B1 F3 . . 154.8(14) ? F4 B1 F1 . . 102.6(16) ? F3' B1 F1 . . 102(2) ? F4' B1 F1 . . 112(2) ? F2 B1 F1 . . 103.2(11) ? F2' B1 F1 . . 102.6(12) ? F3 B1 F1 . . 100.3(12) ? F3' F2 B1 . . 64(2) ? F3' F2 F2' . . 128(3) ? B1 F2 F2' . . 65.9(13) ? F2 F2' B1 . . 56.0(11) ? F2 F2' F4 . . 101.1(16) ? B1 F2' F4 . . 46.6(11) ? F3' F3 B1 . . 51.7(11) ? F3' F3 F4' . . 96.8(17) ? B1 F3 F4' . . 48.9(11) ? F2 F3' B1 . . 69.9(17) ? F2 F3' F3 . . 136(3) ? B1 F3' F3 . . 68(2) ? F4' F4 B1 . . 73(3) ? F4' F4 F2' . . 126(4) ? B1 F4 F2' . . 60.0(14) ? F4 F4' B1 . . 65.5(19) ? F4 F4' F3 . . 126(3) ? B1 F4' F3 . . 60.8(18) ? _cod_database_fobs_code 2012538