#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/72/7027297.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7027297
loop_
_publ_author_name
'Leung, Kelvin Sze-Yin'
'Wong, Wing-Tak'
_publ_contact_author
;
    ENTER NAME
 ENTER ADDRESS
;
_publ_section_title
;
 Synthesis, structural characterization and reactivities of hexaosmium
 carbonyl clusters with six-membered cyclic thioether and thioxane ligands
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2077
_journal_paper_doi               10.1039/a900808j
_journal_year                    1999
_chemical_formula_moiety         'C20 H8 O16 Os6 S2 '
_chemical_formula_sum            'C20 H8 O16 Os6 S2'
_chemical_formula_weight         1709.59
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Fri Apr 23 16:41:04 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90.43(2)
_cell_angle_beta                 90.44(2)
_cell_angle_gamma                87.36(2)
_cell_formula_units_Z            2
_cell_length_a                   11.976(3)
_cell_length_b                   13.059(4)
_cell_length_c                   9.823(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298.2
_cell_measurement_theta_max      18.5
_cell_measurement_theta_min      12.5
_cell_volume                     1534.5(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      298.2
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.00069
_diffrn_orient_matrix_UB_12      -0.04749
_diffrn_orient_matrix_UB_13      0.07941
_diffrn_orient_matrix_UB_21      0.07238
_diffrn_orient_matrix_UB_22      -0.03278
_diffrn_orient_matrix_UB_23      -0.03180
_diffrn_orient_matrix_UB_31      0.04182
_diffrn_orient_matrix_UB_32      0.05046
_diffrn_orient_matrix_UB_33      0.05520
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4245
_diffrn_reflns_theta_max         22.50
_diffrn_standards_decay_%        -4.91
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    24.932
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.449
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    3.700
_exptl_crystal_description       block
_exptl_crystal_F_000             1488.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.79
_refine_diff_density_min         -3.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.708
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         2535
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0665
_refine_ls_shift/esd_max         0.0140
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0665
_reflns_number_observed          2535
_reflns_number_total             4013
_reflns_observed_criterion       1.50
_cod_data_source_file            900808jsup1.cif
_cod_data_source_block           9
_cod_original_cell_volume        1534.6(6)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C20 H8 O16 Os6 S2 '
_cod_database_code               7027297
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_thermal_displace_type
Os(1) 0.9843(1) 0.3314(1) 0.2809(2) 0.0414(6) Uij
Os(2) 0.8927(1) 0.1608(1) 0.1781(2) 0.0399(5) Uij
Os(3) 0.7699(1) 0.2791(1) 0.3785(2) 0.0355(5) Uij
Os(4) 0.7890(1) 0.3489(1) 0.1161(2) 0.0374(5) Uij
Os(5) 0.6709(1) 0.1752(1) 0.1550(2) 0.0368(5) Uij
Os(6) 0.5733(1) 0.3556(1) 0.2414(2) 0.0367(5) Uij
S(1) 0.7747(9) 0.0312(9) 0.205(1) 0.046(3) Uij
S(2) 0.639(1) -0.136(1) 0.101(2) 0.093(6) Uij
O(1) 1.140(3) 0.271(3) 0.516(3) 0.09(2) Uij
O(2) 1.183(4) 0.343(3) 0.094(4) 0.12(2) Uij
O(3) 0.992(3) 0.557(3) 0.362(4) 0.09(1) Uij
O(4) 1.110(3) 0.070(3) 0.300(3) 0.08(1) Uij
O(5) 0.968(3) 0.124(4) -0.103(5) 0.12(2) Uij
O(6) 0.921(3) 0.159(3) 0.582(4) 0.09(1) Uij
O(7) 0.580(3) 0.176(3) 0.523(3) 0.08(1) Uij
O(8) 0.753(3) 0.477(3) 0.543(4) 0.10(2) Uij
O(9) 0.658(3) 0.382(3) -0.147(3) 0.09(1) Uij
O(10) 0.773(2) 0.577(3) 0.198(4) 0.08(1) Uij
O(11) 0.982(3) 0.377(4) -0.084(4) 0.10(2) Uij
O(12) 0.633(3) 0.133(3) -0.146(3) 0.09(1) Uij
O(13) 0.446(4) 0.109(3) 0.236(3) 0.09(2) Uij
O(14) 0.372(3) 0.307(3) 0.402(4) 0.08(1) Uij
O(15) 0.427(3) 0.395(2) 0.000(3) 0.06(1) Uij
O(16) 0.547(3) 0.572(3) 0.349(3) 0.06(1) Uij
C(1) 1.087(5) 0.288(5) 0.434(6) 0.08(2) Uij
C(2) 1.115(4) 0.335(2) 0.180(5) 0.0568 Uij
C(3) 0.992(3) 0.474(4) 0.337(4) 0.05(1) Uij
C(4) 1.030(3) 0.103(3) 0.252(4) 0.04(1) Uij
C(5) 0.939(3) 0.133(4) 0.006(5) 0.06(2) Uij
C(6) 0.877(4) 0.209(4) 0.497(6) 0.07(2) Uij
C(7) 0.649(4) 0.213(5) 0.465(5) 0.12(2) Uij
C(8) 0.761(4) 0.404(4) 0.480(5) 0.06(2) Uij
C(9) 0.701(4) 0.362(3) -0.051(4) 0.05(1) Uij
C(10) 0.771(3) 0.495(4) 0.166(5) 0.05(2) Uij
C(11) 0.914(5) 0.366(3) -0.003(7) 0.0896 Uij
C(12) 0.645(4) 0.146(4) -0.029(5) 0.07(2) Uij
C(13) 0.552(8) 0.145(3) 0.203(3) 0.14(3) Uij
C(14) 0.447(5) 0.328(3) 0.327(6) 0.0762 Uij
C(15) 0.485(3) 0.378(3) 0.096(4) 0.04(1) Uij
C(16) 0.557(4) 0.482(4) 0.302(6) 0.09(2) Uij
C(17) 0.767(4) -0.038(3) 0.363(4) 0.06(2) Uij
C(18) 0.647(3) -0.088(2) 0.387(4) 0.0327 Uij
C(19) 0.652(4) -0.175(3) 0.275(5) 0.07(2) Uij
C(20) 0.768(3) -0.078(3) 0.090(4) 0.05(1) Uij
H(1) 0.8232 -0.0918 0.3619 0.0687 Uij
H(2) 0.7810 0.0079 0.4356 0.0687 Uij
H(3) 0.6412 -0.1147 0.4763 0.0392 Uij
H(4) 0.5862 -0.0392 0.3717 0.0392 Uij
H(5) 0.5933 -0.2194 0.2922 0.0782 Uij
H(6) 0.7219 -0.2117 0.2845 0.0782 Uij
H(7) 0.8257 -0.1268 0.1134 0.0581 Uij
H(8) 0.7778 -0.0552 -0.0002 0.0581 Uij
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Os 0 12 -1.216 7.603 'International Tables'
C 0 40 0.003 0.002 'International Tables'
H 0 16 0.000 0.000 'International Tables'
S 0 4 0.125 0.123 'International Tables'
O 0 32 0.011 0.006 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
4 3 2
4 2 1
0 4 2
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
Os(2) Os(1) Os(3) 61.81(6) yes
Os(2) Os(1) Os(4) 59.87(6) yes
Os(2) Os(1) C(1) 107(1) yes
Os(2) Os(1) C(2) 101(1) yes
Os(2) Os(1) C(3) 157(1) yes
Os(3) Os(1) Os(4) 57.86(6) yes
Os(3) Os(1) C(1) 102(1) yes
Os(3) Os(1) C(2) 162(1) yes
Os(3) Os(1) C(3) 102(1) yes
Os(4) Os(1) C(1) 159(1) yes
Os(4) Os(1) C(2) 112(1) yes
Os(4) Os(1) C(3) 98(1) yes
C(1) Os(1) C(2) 84(2) yes
C(1) Os(1) C(3) 90(1) yes
C(2) Os(1) C(3) 92(1) yes
Os(1) Os(2) Os(3) 61.63(6) yes
Os(1) Os(2) Os(4) 62.27(6) yes
Os(1) Os(2) Os(5) 114.22(8) yes
Os(1) Os(2) S(1) 148.6(3) yes
Os(1) Os(2) C(4) 79(1) yes
Os(1) Os(2) C(5) 111(1) yes
Os(3) Os(2) Os(4) 58.51(6) yes
Os(3) Os(2) Os(5) 61.99(6) yes
Os(3) Os(2) S(1) 89.6(3) yes
Os(3) Os(2) C(4) 111(1) yes
Os(3) Os(2) C(5) 153(1) yes
Os(4) Os(2) Os(5) 60.99(6) yes
Os(4) Os(2) S(1) 114.9(3) yes
Os(4) Os(2) C(4) 140(1) yes
Os(4) Os(2) C(5) 95(1) yes
Os(5) Os(2) S(1) 53.9(3) yes
Os(5) Os(2) C(4) 153(1) yes
Os(5) Os(2) C(5) 103(1) yes
S(1) Os(2) C(4) 102(1) yes
S(1) Os(2) C(5) 99(1) yes
C(4) Os(2) C(5) 91(1) yes
Os(1) Os(3) Os(2) 56.55(6) yes
Os(1) Os(3) Os(4) 60.62(6) yes
Os(1) Os(3) Os(5) 104.39(7) yes
Os(1) Os(3) Os(6) 119.42(8) yes
Os(1) Os(3) C(6) 74(1) yes
Os(1) Os(3) C(7) 164(2) yes
Os(1) Os(3) C(8) 89(1) yes
Os(2) Os(3) Os(4) 59.03(6) yes
Os(2) Os(3) Os(5) 55.50(6) yes
Os(2) Os(3) Os(6) 105.19(7) yes
Os(2) Os(3) C(6) 81(1) yes
Os(2) Os(3) C(7) 116(1) yes
Os(2) Os(3) C(8) 145(1) yes
Os(4) Os(3) Os(5) 58.91(6) yes
Os(4) Os(3) Os(6) 61.51(6) yes
Os(4) Os(3) C(6) 131(1) yes
Os(4) Os(3) C(7) 130(1) yes
Os(4) Os(3) C(8) 101(1) yes
Os(5) Os(3) Os(6) 56.87(6) yes
Os(5) Os(3) C(6) 120(1) yes
Os(5) Os(3) C(7) 78(1) yes
Os(5) Os(3) C(8) 142(1) yes
Os(6) Os(3) C(6) 165(1) yes
Os(6) Os(3) C(7) 75(2) yes
Os(6) Os(3) C(8) 85(1) yes
C(6) Os(3) C(7) 90(2) yes
C(6) Os(3) C(8) 96(2) yes
C(7) Os(3) C(8) 97(2) yes
Os(1) Os(4) Os(2) 57.85(6) yes
Os(1) Os(4) Os(3) 61.52(6) yes
Os(1) Os(4) Os(5) 107.55(8) yes
Os(1) Os(4) Os(6) 119.65(7) yes
Os(1) Os(4) C(9) 157(1) yes
Os(1) Os(4) C(10) 89(1) yes
Os(1) Os(4) C(11) 73(1) yes
Os(2) Os(4) Os(3) 62.46(6) yes
Os(2) Os(4) Os(5) 57.56(6) yes
Os(2) Os(4) Os(6) 107.23(7) yes
Os(2) Os(4) C(9) 119(1) yes
Os(2) Os(4) C(10) 145(1) yes
Os(2) Os(4) C(11) 85(1) yes
Os(3) Os(4) Os(5) 62.29(6) yes
Os(3) Os(4) Os(6) 60.85(6) yes
Os(3) Os(4) C(9) 139(1) yes
Os(3) Os(4) C(10) 94(1) yes
Os(3) Os(4) C(11) 133(1) yes
Os(5) Os(4) Os(6) 57.66(6) yes
Os(5) Os(4) C(9) 84(1) yes
Os(5) Os(4) C(10) 136(1) yes
Os(5) Os(4) C(11) 128.2(10) yes
Os(6) Os(4) C(9) 83(1) yes
Os(6) Os(4) C(10) 78(1) yes
Os(6) Os(4) C(11) 165(1) yes
C(9) Os(4) C(10) 94(1) yes
C(9) Os(4) C(11) 84(2) yes
C(10) Os(4) C(11) 94(1) yes
Os(2) Os(5) Os(3) 62.51(6) yes
Os(2) Os(5) Os(4) 61.45(6) yes
Os(2) Os(5) Os(6) 115.17(8) yes
Os(2) Os(5) S(1) 54.3(3) yes
Os(2) Os(5) C(12) 103(1) yes
Os(2) Os(5) C(13) 150(1) yes
Os(3) Os(5) Os(4) 58.80(6) yes
Os(3) Os(5) Os(6) 61.51(6) yes
Os(3) Os(5) S(1) 90.2(3) yes
Os(3) Os(5) C(12) 155(1) yes
Os(3) Os(5) C(13) 106(1) yes
Os(4) Os(5) Os(6) 63.17(6) yes
Os(4) Os(5) S(1) 115.7(3) yes
Os(4) Os(5) C(12) 96(1) yes
Os(4) Os(5) C(13) 139(1) yes
Os(6) Os(5) S(1) 148.4(3) yes
Os(6) Os(5) C(12) 113(1) yes
Os(6) Os(5) C(13) 76(1) yes
S(1) Os(5) C(12) 97(1) yes
S(1) Os(5) C(13) 101(1) yes
C(12) Os(5) C(13) 95(2) yes
Os(3) Os(6) Os(4) 57.64(5) yes
Os(3) Os(6) Os(5) 61.62(6) yes
Os(3) Os(6) C(14) 113(1) yes
Os(3) Os(6) C(15) 154(1) yes
Os(3) Os(6) C(16) 103(1) yes
Os(4) Os(6) Os(5) 59.17(6) yes
Os(4) Os(6) C(14) 166(1) yes
Os(4) Os(6) C(15) 100(1) yes
Os(4) Os(6) C(16) 103(1) yes
Os(5) Os(6) C(14) 108(1) yes
Os(5) Os(6) C(15) 97(1) yes
Os(5) Os(6) C(16) 160(1) yes
C(14) Os(6) C(15) 84(2) yes
C(14) Os(6) C(16) 88(1) yes
C(15) Os(6) C(16) 94(2) yes
Os(2) S(1) Os(5) 71.9(3) yes
Os(2) S(1) C(17) 122(1) yes
Os(2) S(1) C(20) 123(1) yes
Os(5) S(1) C(17) 124(1) yes
Os(5) S(1) C(20) 118(1) yes
C(17) S(1) C(20) 97(1) yes
C(19) S(2) C(20) 97(2) yes
Os(1) C(1) O(1) 175(5) yes
Os(1) C(2) O(2) 166(4) yes
Os(1) C(3) O(3) 176(3) yes
Os(2) C(4) O(4) 177(3) yes
Os(2) C(5) O(5) 174(5) yes
Os(3) C(6) O(6) 165(4) yes
Os(3) C(7) O(7) 176(4) yes
Os(3) C(8) O(8) 177(4) yes
Os(4) C(9) O(9) 170(4) yes
Os(4) C(10) O(10) 172(4) yes
Os(4) C(11) O(11) 173(5) yes
Os(5) C(12) O(12) 176(4) yes
Os(5) C(13) O(13) 173(3) yes
Os(6) C(14) O(14) 170(4) yes
Os(6) C(15) O(15) 178(3) yes
Os(6) C(16) O(16) 178(4) yes
S(1) C(17) C(18) 113(2) yes
S(1) C(17) H(1) 108.4 no
S(1) C(17) H(2) 108.4 no
C(18) C(17) H(1) 108.4 no
C(18) C(17) H(2) 108.4 no
H(1) C(17) H(2) 109.5 no
C(17) C(18) C(19) 99(3) yes
C(17) C(18) H(3) 111.9 no
C(17) C(18) H(4) 111.8 no
C(19) C(18) H(3) 111.9 no
C(19) C(18) H(4) 111.8 no
H(3) C(18) H(4) 109.5 no
S(2) C(19) C(18) 117(2) yes
S(2) C(19) H(5) 107.6 no
S(2) C(19) H(6) 107.5 no
C(18) C(19) H(5) 107.6 no
C(18) C(19) H(6) 107.5 no
H(5) C(19) H(6) 109.5 no
S(1) C(20) S(2) 111(2) yes
S(1) C(20) H(7) 108.9 no
S(1) C(20) H(8) 108.9 no
S(2) C(20) H(7) 108.9 no
S(2) C(20) H(8) 108.9 no
H(7) C(20) H(8) 109.5 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Os(1) Os(2) 2.713(2) yes
Os(1) Os(3) 2.861(2) yes
Os(1) Os(4) 2.836(2) yes
Os(1) C(1) 2.00(6) yes
Os(1) C(2) 1.86(5) yes
Os(1) C(3) 1.94(5) yes
Os(2) Os(3) 2.865(2) yes
Os(2) Os(4) 2.771(3) yes
Os(2) Os(5) 2.662(2) yes
Os(2) S(1) 2.27(1) yes
Os(2) C(4) 1.92(4) yes
Os(2) C(5) 1.82(5) yes
Os(3) Os(4) 2.755(2) yes
Os(3) Os(5) 2.852(2) yes
Os(3) Os(6) 2.849(2) yes
Os(3) C(6) 1.93(6) yes
Os(3) C(7) 1.93(3) yes
Os(3) C(8) 1.91(6) yes
Os(4) Os(5) 2.759(2) yes
Os(4) Os(6) 2.867(2) yes
Os(4) C(9) 1.95(4) yes
Os(4) C(10) 1.97(6) yes
Os(4) C(11) 1.93(6) yes
Os(5) Os(6) 2.714(2) yes
Os(5) S(1) 2.26(1) yes
Os(5) C(12) 1.87(5) yes
Os(5) C(13) 1.57(9) yes
Os(6) C(14) 1.78(7) yes
Os(6) C(15) 1.79(4) yes
Os(6) C(16) 1.76(6) yes
S(1) C(17) 1.80(4) yes
S(1) C(20) 1.81(4) yes
S(2) C(19) 1.79(5) yes
S(2) C(20) 1.75(4) yes
O(1) C(1) 1.04(6) yes
O(2) C(2) 1.19(5) yes
O(3) C(3) 1.12(6) yes
O(4) C(4) 1.13(5) yes
O(5) C(5) 1.13(5) yes
O(6) C(6) 1.16(6) yes
O(7) C(7) 1.13(4) yes
O(8) C(8) 1.14(5) yes
O(9) C(9) 1.10(4) yes
O(10) C(10) 1.11(5) yes
O(11) C(11) 1.16(6) yes
O(12) C(12) 1.16(5) yes
O(13) C(13) 1.42(9) yes
O(14) C(14) 1.21(6) yes
O(15) C(15) 1.19(4) yes
O(16) C(16) 1.25(6) yes
C(17) C(18) 1.63(5) yes
C(17) H(1) 0.950 no
C(17) H(2) 0.950 no
C(18) C(19) 1.58(5) yes
C(18) H(3) 0.950 no
C(18) H(4) 0.950 no
C(19) H(5) 0.950 no
C(19) H(6) 0.950 no
C(20) H(7) 0.950 no
C(20) H(8) 0.950 no
