#------------------------------------------------------------------------------
#$Date: 2018-07-31 16:03:28 +0300 (Tue, 31 Jul 2018) $
#$Revision: 209315 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/01/81/2018155.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_2018155
loop_
_publ_author_name
'Benjamin, Sophie L.'
'Hyslop, Alison'
'Levason, William'
'Webster, Michael'
_publ_section_title
;
 [Cl₅Ta(μ-O)TaCl₃{ⁱPrS(CH₂)₂SⁱPr}] and
 [(TaCl₄)₂(μ-O)(μ-Me₂Se₂)]: two chalcogenoether complexes of
 Ta₂OCl₈ with very different geometries
;
_journal_coeditor_code           SK3411
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m221
_journal_page_last               m223
_journal_paper_doi               10.1107/S0108270111022037
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ta2 Cl8 O (C8 H18 S2)]'
_chemical_formula_moiety         'C8 H18 Cl8 O S2 Ta2'
_chemical_formula_sum            'C8 H18 Cl8 O S2 Ta2'
_chemical_formula_weight         839.84
_chemical_name_systematic
;
[1,2-bis(isopropylsulfanyl)ethane-2κ²S,S']octachlorido-
1κ⁵Cl,2κ³Cl-μ-oxido-ditantalum(V)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.684(3)
_cell_length_b                   13.007(2)
_cell_length_c                   21.981(4)
_cell_measurement_reflns_used    100483
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     4484.2(14)
_computing_cell_refinement
;
COLLECT (Nonius, 1998) and DENZO (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Nonius, 1998) and DENZO (Otwinowski & Minor, 1997)
;
_computing_data_reduction
;
COLLECT (Nonius, 1998) and DENZO (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Bruker Nonius APEXII CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36044
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         3.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.886
_exptl_absorpt_correction_T_max  0.8968
_exptl_absorpt_correction_T_min  0.4252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.264
_refine_diff_density_min         -1.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         5139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+47.4498P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                4364
_reflns_number_total             5139
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sk3411.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-07-31
;
_cod_original_cell_volume        4484.4(14)
_cod_database_code               2018155
_cod_database_fobs_code          2018155
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 '-x, y+1/2, -z+1/2'
4 'x+1/2, -y+1/2, -z'
5 '-x, -y, -z'
6 'x-1/2, y, -z-1/2'
7 'x, -y-1/2, z-1/2'
8 '-x-1/2, y-1/2, z'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta Ta1 0.122173(17) 0.67937(2) 0.450206(12) 0.02203(7) Uani d . 1 1 . .
Ta Ta2 0.028140(18) 0.85299(2) 0.327462(12) 0.02434(8) Uani d . 1 1 . .
Cl Cl1 0.15077(11) 0.54250(13) 0.38585(8) 0.0309(4) Uani d . 1 1 . .
Cl Cl2 0.13947(11) 0.79462(12) 0.53118(8) 0.0288(3) Uani d . 1 1 . .
Cl Cl3 -0.00818(10) 0.62581(12) 0.48379(8) 0.0293(4) Uani d . 1 1 . .
Cl Cl4 0.06825(12) 0.72523(13) 0.25984(8) 0.0333(4) Uani d . 1 1 . .
Cl Cl5 -0.09426(11) 0.75863(14) 0.35272(8) 0.0334(4) Uani d . 1 1 . .
Cl Cl6 0.00228(11) 0.96675(13) 0.40917(8) 0.0320(4) Uani d . 1 1 . .
Cl Cl7 0.15599(11) 0.93887(13) 0.30790(8) 0.0326(4) Uani d . 1 1 . .
Cl Cl8 -0.04585(12) 0.94923(14) 0.25791(8) 0.0367(4) Uani d . 1 1 . .
O O1 0.0917(3) 0.7684(3) 0.3922(2) 0.0273(10) Uani d . 1 1 . .
S S1 0.28316(11) 0.73779(12) 0.43775(7) 0.0252(3) Uani d . 1 1 . .
S S2 0.19843(10) 0.53807(12) 0.52560(7) 0.0238(3) Uani d . 1 1 . .
C C1 0.2940(5) 0.7191(7) 0.3132(3) 0.0386(18) Uani d . 1 1 . .
H H1A 0.2359 0.6912 0.3132 0.058 Uiso calc R 1 1 . .
H H1B 0.3249 0.6932 0.2777 0.058 Uiso calc R 1 1 . .
H H1C 0.2916 0.7943 0.3116 0.058 Uiso calc R 1 1 . .
C C2 0.3397(5) 0.6857(6) 0.3710(3) 0.0308(15) Uani d . 1 1 . .
H H2 0.3403 0.6089 0.3732 0.037 Uiso calc R 1 1 . .
C C3 0.4306(4) 0.7255(6) 0.3725(4) 0.0377(17) Uani d . 1 1 . .
H H3A 0.4583 0.7031 0.4102 0.057 Uiso calc R 1 1 . .
H H3B 0.4301 0.8008 0.3708 0.057 Uiso calc R 1 1 . .
H H3C 0.4621 0.6984 0.3375 0.057 Uiso calc R 1 1 . .
C C4 0.3349(5) 0.6676(5) 0.4989(3) 0.0312(15) Uani d . 1 1 . .
H H4A 0.3974 0.6713 0.4931 0.037 Uiso calc R 1 1 . .
H H4B 0.3213 0.7016 0.5381 0.037 Uiso calc R 1 1 . .
C C5 0.3088(4) 0.5558(5) 0.5029(3) 0.0272(14) Uani d . 1 1 . .
H H5A 0.3462 0.5204 0.5325 0.033 Uiso calc R 1 1 . .
H H5B 0.3177 0.5231 0.4627 0.033 Uiso calc R 1 1 . .
C C6 0.1081(5) 0.5689(6) 0.6289(3) 0.0364(17) Uani d . 1 1 . .
H H6A 0.0738 0.6178 0.6055 0.055 Uiso calc R 1 1 . .
H H6B 0.1058 0.5868 0.6721 0.055 Uiso calc R 1 1 . .
H H6C 0.0856 0.4993 0.6230 0.055 Uiso calc R 1 1 . .
C C7 0.2003(4) 0.5730(6) 0.6070(3) 0.0286(15) Uani d . 1 1 . .
H H7 0.2228 0.6446 0.6117 0.034 Uiso calc R 1 1 . .
C C8 0.2563(5) 0.4987(6) 0.6428(3) 0.0383(17) Uani d . 1 1 . .
H H8A 0.3148 0.5020 0.6274 0.057 Uiso calc R 1 1 . .
H H8B 0.2343 0.4286 0.6381 0.057 Uiso calc R 1 1 . .
H H8C 0.2556 0.5178 0.6859 0.057 Uiso calc R 1 1 . .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
O1 Ta1 Cl3 . . 100.88(16) ?
O1 Ta1 Cl1 . . 96.58(15) ?
Cl3 Ta1 Cl1 . . 97.83(6) ?
O1 Ta1 Cl2 . . 99.07(15) ?
Cl3 Ta1 Cl2 . . 93.06(6) ?
Cl1 Ta1 Cl2 . . 158.87(6) ?
O1 Ta1 S1 . . 89.74(15) y
Cl3 Ta1 S1 . . 166.90(6) ?
Cl1 Ta1 S1 . . 88.44(6) ?
Cl2 Ta1 S1 . . 77.57(6) ?
O1 Ta1 S2 . . 168.44(15) y
Cl3 Ta1 S2 . . 89.47(6) ?
Cl1 Ta1 S2 . . 76.71(6) ?
Cl2 Ta1 S2 . . 85.38(5) ?
S1 Ta1 S2 . . 80.76(5) y
O1 Ta2 Cl8 . . 177.98(14) ?
O1 Ta2 Cl4 . . 85.94(13) ?
Cl8 Ta2 Cl4 . . 95.81(6) ?
O1 Ta2 Cl7 . . 88.12(14) ?
Cl8 Ta2 Cl7 . . 92.91(7) ?
Cl4 Ta2 Cl7 . . 89.53(6) ?
O1 Ta2 Cl5 . . 87.30(14) ?
Cl8 Ta2 Cl5 . . 91.68(7) ?
Cl4 Ta2 Cl5 . . 89.93(7) ?
Cl7 Ta2 Cl5 . . 175.41(6) ?
O1 Ta2 Cl6 . . 83.78(13) ?
Cl8 Ta2 Cl6 . . 94.48(7) ?
Cl4 Ta2 Cl6 . . 169.68(6) ?
Cl7 Ta2 Cl6 . . 89.30(6) ?
Cl5 Ta2 Cl6 . . 90.42(6) ?
Ta1 O1 Ta2 . . 165.9(3) y
C4 S1 C2 . . 100.9(3) ?
C4 S1 Ta1 . . 101.8(2) ?
C2 S1 Ta1 . . 115.8(2) ?
C5 S2 C7 . . 102.7(3) ?
C5 S2 Ta1 . . 99.4(2) ?
C7 S2 Ta1 . . 115.3(2) ?
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
C3 C2 C1 . . 111.3(6) ?
C3 C2 S1 . . 108.0(5) ?
C1 C2 S1 . . 109.4(5) ?
C3 C2 H2 . . 109.4 ?
C1 C2 H2 . . 109.4 ?
S1 C2 H2 . . 109.4 ?
C2 C3 H3A . . 109.5 ?
C2 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C2 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
C5 C4 S1 . . 113.8(5) ?
C5 C4 H4A . . 108.8 ?
S1 C4 H4A . . 108.8 ?
C5 C4 H4B . . 108.8 ?
S1 C4 H4B . . 108.8 ?
H4A C4 H4B . . 107.7 ?
C4 C5 S2 . . 113.3(5) ?
C4 C5 H5A . . 108.9 ?
S2 C5 H5A . . 108.9 ?
C4 C5 H5B . . 108.9 ?
S2 C5 H5B . . 108.9 ?
H5A C5 H5B . . 107.7 ?
C7 C6 H6A . . 109.5 ?
C7 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
C7 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
C6 C7 C8 . . 111.1(6) ?
C6 C7 S2 . . 106.4(5) ?
C8 C7 S2 . . 110.7(5) ?
C6 C7 H7 . . 109.5 ?
C8 C7 H7 . . 109.5 ?
S2 C7 H7 . . 109.5 ?
C7 C8 H8A . . 109.5 ?
C7 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C7 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
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
Ta1 O1 . 1.787(4) y
Ta1 Cl3 . 2.2826(17) y
Ta1 Cl1 . 2.3177(16) y
Ta1 Cl2 . 2.3429(17) y
Ta1 S1 . 2.6511(17) y
Ta1 S2 . 2.7486(16) y
Ta2 O1 . 2.057(4) y
Ta2 Cl8 . 2.2916(17) y
Ta2 Cl4 . 2.3166(17) y
Ta2 Cl7 . 2.3354(17) y
Ta2 Cl5 . 2.3452(17) y
Ta2 Cl6 . 2.3622(17) y
S1 C4 . 1.817(7) ?
S1 C2 . 1.844(7) ?
S2 C5 . 1.817(7) ?
S2 C7 . 1.846(7) ?
C1 C2 . 1.521(10) ?
C1 H1A . 0.9800 ?
C1 H1B . 0.9800 ?
C1 H1C . 0.9800 ?
C2 C3 . 1.518(10) ?
C2 H2 . 1.0000 ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C3 H3C . 0.9800 ?
C4 C5 . 1.513(9) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 C7 . 1.525(10) ?
C6 H6A . 0.9800 ?
C6 H6B . 0.9800 ?
C6 H6C . 0.9800 ?
C7 C8 . 1.524(10) ?
C7 H7 . 1.0000 ?
C8 H8A . 0.9800 ?
C8 H8B . 0.9800 ?
C8 H8C . 0.9800 ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
S1 C4 C5 S2 . . . . -67.7(6) ?
