#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/31/4323147.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4323147
loop_
_publ_author_name
'P. Michael Boorman'
'Naomi L. Langdon'
'Vivian J. Mozol'
'Masood Parvez'
'Glenn P. A. Yap'
_publ_contact_author
;
    Masood Parvez
    Department of Chemistry
    University of Calgary
    2500 University Drive N.W.
    Calgary, Alberta, Canada T2N 1N4
;
_publ_contact_author_email       ' parvez@acs.ucalgary.ca '
_publ_contact_author_fax         ' (403)289-9488 '
_publ_contact_author_phone       ' (403)220-5348 '
_publ_section_title
;
 Syntheses, Crystal Structures, Spectroscopic Characterization, and
 Electrochemical Studies of the Ditungsten(III) Complexes
 Cl₃W(μ-L)₃WCl₃ and [Cl₃W(μ-L)₂(μ-Cl)WCl₃]⁻ (L =
 1,4-Dithiane, 1,4-Thioxane, pms = Pentamethylene Sulfide). C-S Bond
 Cleavage of the Bridging Thioether(s) in Cl₃W(μ-L)₃WCl₃
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6023
_journal_page_last               6029
_journal_paper_doi               10.1021/ic971542t
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'C33 H37 Cl10 O2 P S2 W2 '
_chemical_formula_sum            'C33 H37 Cl10 O2 P S2 W2'
_chemical_formula_weight         1282.98
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_method           'by teXsan v1.7'
_cell_angle_alpha                90
_cell_angle_beta                 115.57(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.531(4)
_cell_length_b                   25.207(5)
_cell_length_c                   14.083(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    170
_cell_measurement_theta_max      10.6
_cell_measurement_theta_min      9.1
_cell_volume                     4332.9(19)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'SHELX'76 (Sheldrick, 1976)'
_computing_structure_solution    'Patterson methods'
_diffrn_ambient_temperature      170
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       ω-2θ
_diffrn_orient_matrix_UB_11      0.04768
_diffrn_orient_matrix_UB_12      0.01976
_diffrn_orient_matrix_UB_13      -0.02587
_diffrn_orient_matrix_UB_21      0.06367
_diffrn_orient_matrix_UB_22      -0.02275
_diffrn_orient_matrix_UB_23      0.04482
_diffrn_orient_matrix_UB_31      -0.01962
_diffrn_orient_matrix_UB_32      -0.02581
_diffrn_orient_matrix_UB_33      -0.05932
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.00000
_diffrn_reflns_av_sigmaI/netI    0.130
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7873
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        -1.15
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.091
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.458
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2464.00
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_ls_extinction_method     none
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3716
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0811
_refine_ls_shift/esd_max         0.04
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00001|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0869
_reflns_number_observed          3746
_reflns_number_total             7873
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic971542t_1.cif
_cod_data_source_block           Compound_8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00001|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4333(2)
_cod_original_sg_symbol_H-M      'P 21/a '
_cod_original_formula_sum        'C33 H37 Cl10 O2 P S2 W2 '
_cod_database_code               4323147
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'1/2-x,1/2+y,   -z'
'   -x,   -y,   -z'
'1/2+x,1/2-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_occupancy
_atom_site_refinement_flags
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
W(1) 0.0174(1) 0.3537(1) 0.4567(1) 0.020(1) 1.000 . Uani d ?
W(2) 0.0323(1) 0.3537(6) 0.6396(1) 0.020(1) 1.000 . Uani d ?
Cl(1) -0.1353(8) 0.3912(4) 0.4916(7) 0.024(5) 1.000 . Uani d ?
Cl(2) 0.0009(9) 0.4309(4) 0.3532(7) 0.028(5) 1.000 . Uani d ?
Cl(3) -0.1274(9) 0.3130(4) 0.3075(7) 0.032(6) 1.000 . Uani d ?
Cl(4) 0.1554(9) 0.3186(4) 0.4125(7) 0.035(6) 1.000 . Uani d ?
Cl(5) 0.0261(9) 0.4299(4) 0.7350(7) 0.035(6) 1.000 . Uani d ?
Cl(6) 0.1871(9) 0.3177(4) 0.7879(7) 0.028(5) 1.000 . Uani d ?
Cl(7) -0.0950(8) 0.3102(3) 0.6910(7) 0.026(5) 1.000 . Uani d ?
Cl(8) 0.4677(11) 0.2981(5) 0.8962(11) 0.059(8) 1.000 . Uani d ?
Cl(9) 0.6386(15) 0.3307(5) 0.8375(11) 0.086(11) 1.000 . Uani d ?
Cl(10) 0.6956(12) 0.2786(5) 1.0355(9) 0.056(8) 1.000 . Uani d ?
S(1) 0.0292(9) 0.2734(3) 0.5497(8) 0.023(4) 1.000 . Uani d ?
S(2) 0.1588(8) 0.4013(3) 0.5945(7) 0.022(5) 1.000 . Uani d ?
P(1) -0.7104(10) 0.4374(4) 0.1503(7) 0.027(6) 1.000 . Uani d ?
O(1) 0.022(2) 0.154(1) 0.489(2) 0.043(7) 1.000 . Uiso d ?
O(2) 0.360(2) 0.473(1) 0.717(2) 0.030(6) 1.000 . Uiso d ?
C(1) -0.089(3) 0.231(1) 0.509(2) 0.014(7) 1.000 . Uiso d ?
C(2) -0.075(4) 0.184(2) 0.443(3) 0.040(10) 1.000 . Uiso d ?
C(4) 0.118(3) 0.183(2) 0.505(3) 0.032(10) 1.000 . Uiso d ?
C(5) 0.138(4) 0.225(2) 0.590(3) 0.049(13) 1.000 . Uiso d ?
C(6) 0.163(3) 0.474(1) 0.592(3) 0.020(8) 1.000 . Uiso d ?
C(7) 0.251(3) 0.492(1) 0.698(3) 0.029(9) 1.000 . Uiso d ?
C(9) 0.369(5) 0.421(2) 0.740(4) 0.065(15) 1.000 . Uiso d ?
C(10) 0.303(3) 0.383(1) 0.645(3) 0.022(8) 1.000 . Uiso d ?
C(11) -0.598(2) 0.395(1) 0.179(2) 0.026(9) 1.000 . Uiso d ?
C(12) -0.624(2) 0.343(1) 0.142(2) 0.023(8) 1.000 . Uiso d ?
C(13) -0.542(2) 0.305(1) 0.163(2) 0.056(14) 1.000 . Uiso d ?
C(14) -0.432(2) 0.320(1) 0.222(2) 0.046(12) 1.000 . Uiso d ?
C(15) -0.406(2) 0.371(1) 0.259(2) 0.049(12) 1.000 . Uiso d ?
C(16) -0.488(2) 0.409(1) 0.238(2) 0.024(8) 1.000 . Uiso d ?
C(17) -0.835(2) 0.401(1) 0.102(2) 0.039(11) 1 . Uiso d ?
C(18) -0.886(2) 0.385(1) -0.004(2) 0.012(7) 1.000 . Uiso d ?
C(19) -0.982(2) 0.355(1) -0.040(2) 0.055(13) 1.000 . Uiso d ?
C(20) -1.026(2) 0.341(1) 0.029(2) 0.042(12) 1.000 . Uiso d ?
C(21) -0.975(2) 0.356(1) 0.135(2) 0.041(11) 1.000 . Uiso d ?
C(22) -0.879(2) 0.387(1) 0.171(2) 0.032(10) 1.000 . Uiso d ?
C(23) -0.691(2) 0.475(1) 0.269(2) 0.009(7) 1.000 . Uiso d ?
C(24) -0.631(2) 0.453(1) 0.368(2) 0.038(10) 1.000 . Uiso d ?
C(25) -0.625(2) 0.480(1) 0.458(2) 0.029(9) 1.000 . Uiso d ?
C(26) -0.677(2) 0.529(1) 0.448(2) 0.057(14) 1.000 . Uiso d ?
C(27) -0.737(2) 0.551(1) 0.348(2) 0.010(7) 1.000 . Uiso d ?
C(28) -0.744(2) 0.524(1) 0.259(2) 0.052(13) 1.000 . Uiso d ?
C(29) -0.714(2) 0.488(1) 0.055(2) 0.033(10) 1.000 . Uiso d ?
C(30) -0.815(2) 0.508(1) -0.017(2) 0.056(14) 1.000 . Uiso d ?
C(31) -0.819(2) 0.549(1) -0.085(2) 0.026(9) 1.000 . Uiso d ?
C(32) -0.722(2) 0.570(1) -0.081(2) 0.042(11) 1.000 . Uiso d ?
C(33) -0.621(2) 0.550(1) -0.010(2) 0.051(13) 1.000 . Uiso d ?
C(34) -0.617(2) 0.509(1) 0.058(2) 0.059(14) 1.000 . Uiso d ?
C(35) 0.597(3) 0.281(2) 0.904(3) 0.030(9) 1.000 . Uiso d ?
H(11) -0.153 0.250 0.467 0.10 1.000 . Uiso d ?
H(12) -0.095 0.217 0.569 0.10 1.000 . Uiso d ?
H(21) -0.081 0.198 0.379 0.10 1.000 . Uiso d ?
H(22) -0.134 0.160 0.430 0.10 1.000 . Uiso d ?
H(41) 0.178 0.159 0.527 0.10 1.000 . Uiso d ?
H(42) 0.109 0.200 0.441 0.10 1.000 . Uiso d ?
H(51) 0.143 0.208 0.652 0.10 1.000 . Uiso d ?
H(52) 0.205 0.243 0.605 0.10 1.000 . Uiso d ?
H(61) 0.094 0.488 0.580 0.10 1.000 . Uiso d ?
H(62) 0.182 0.486 0.537 0.10 1.000 . Uiso d ?
H(71) 0.233 0.479 0.752 0.10 1.000 . Uiso d ?
H(72) 0.252 0.530 0.700 0.10 1.000 . Uiso d ?
H(91) 0.444 0.412 0.767 0.10 1.000 . Uiso d ?
H(92) 0.343 0.415 0.792 0.10 1.000 . Uiso d ?
H(101) 0.327 0.387 0.591 0.10 1.000 . Uiso d ?
H(102) 0.312 0.347 0.668 0.10 1.000 . Uiso d ?
H(121) -0.699 0.333 0.102 0.10 1.000 . Uiso d ?
H(131) -0.560 0.270 0.138 0.10 1.000 . Uiso d ?
H(141) -0.376 0.294 0.236 0.10 1.000 . Uiso d ?
H(151) -0.331 0.381 0.299 0.10 1.000 . Uiso d ?
H(161) -0.470 0.444 0.263 0.10 1.000 . Uiso d ?
H(181) -0.856 0.395 -0.051 0.10 1.000 . Uiso d ?
H(191) -1.017 0.344 -0.111 0.10 1.000 . Uiso d ?
H(201) -1.091 0.320 0.005 0.10 1.000 . Uiso d ?
H(211) -1.005 0.347 0.182 0.10 1.000 . Uiso d ?
H(221) -0.844 0.397 0.242 0.10 1.000 . Uiso d ?
H(241) -0.595 0.420 0.375 0.10 1.000 . Uiso d ?
H(251) -0.584 0.465 0.526 0.10 1.000 . Uiso d ?
H(261) -0.673 0.547 0.508 0.10 1.000 . Uiso d ?
H(271) -0.773 0.584 0.341 0.10 1.000 . Uiso d ?
H(281) -0.785 0.539 0.191 0.10 1.000 . Uiso d ?
H(301) -0.881 0.493 -0.019 0.10 1.000 . Uiso d ?
H(311) -0.888 0.562 -0.133 0.10 1.000 . Uiso d ?
H(321) -0.725 0.598 -0.127 0.10 1.000 . Uiso d ?
H(331) -0.555 0.564 -0.007 0.10 1.000 . Uiso d ?
H(341) -0.548 0.495 0.107 0.10 1.000 . Uiso d ?
H(351) 0.592 0.247 0.873 0.10 1.000 . Uiso d ?
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
C 0 132 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H 0 148 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O 0 8 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
P 0 4 0.102 0.094
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
S 0 8 0.125 0.123
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cl 0 40 0.148 0.159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
W 0 8 -0.849 6.872
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
3 -6 -6
1 -2 -6
4 -5 -6
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl(1) W(1) W(2) 60.3(4) . . . n
Cl(2) W(1) W(2) 125.2(5) . . . n
Cl(2) W(1) Cl(1) 86.8(7) . . . n
Cl(3) W(1) W(2) 125.2(6) . . . n
Cl(3) W(1) Cl(1) 84.4(7) . . . n
Cl(3) W(1) Cl(2) 89.3(8) . . . n
Cl(4) W(1) W(2) 123.2(5) . . . n
Cl(4) W(1) Cl(1) 176.5(7) . . . n
Cl(4) W(1) Cl(2) 91.2(8) . . . n
Cl(4) W(1) Cl(3) 92.8(8) . . . n
S(1) W(1) W(2) 58.4(5) . . . n
S(1) W(1) Cl(1) 94.5(7) . . . n
S(1) W(1) Cl(2) 176.3(7) . . . n
S(1) W(1) Cl(3) 87.4(8) . . . n
S(1) W(1) Cl(4) 87.4(8) . . . n
S(2) W(1) W(2) 58.7(5) . . . n
S(2) W(1) Cl(1) 95.2(7) . . . n
S(2) W(1) Cl(2) 85.3(7) . . . n
S(2) W(1) Cl(3) 174.6(7) . . . n
S(2) W(1) Cl(4) 87.4(8) . . . n
S(2) W(1) S(1) 98.1(7) . . . n
Cl(1) W(2) W(1) 60.1(5) . . . n
Cl(5) W(2) W(1) 125.4(5) . . . n
Cl(5) W(2) Cl(1) 85.7(7) . . . n
Cl(6) W(2) W(1) 123.2(5) . . . n
Cl(6) W(2) Cl(1) 176.6(7) . . . n
Cl(6) W(2) Cl(5) 92.5(8) . . . n
Cl(7) W(2) W(1) 124.2(5) . . . n
Cl(7) W(2) Cl(1) 85.1(7) . . . n
Cl(7) W(2) Cl(5) 89.6(7) . . . n
Cl(7) W(2) Cl(6) 92.0(8) . . . n
S(1) W(2) W(1) 58.4(5) . . . n
S(1) W(2) Cl(1) 94.4(7) . . . n
S(1) W(2) Cl(5) 175.1(8) . . . n
S(1) W(2) Cl(6) 87.1(7) . . . n
S(1) W(2) Cl(7) 85.5(7) . . . n
S(2) W(2) W(1) 58.2(5) . . . n
S(2) W(2) Cl(1) 94.8(7) . . . n
S(2) W(2) Cl(5) 87.1(7) . . . n
S(2) W(2) Cl(6) 88.0(7) . . . n
S(2) W(2) Cl(7) 176.7(7) . . . n
S(2) W(2) S(1) 97.8(7) . . . n
W(2) Cl(1) W(1) 59.7(5) . . . n
W(2) S(1) W(1) 63.3(5) . . . n
W(2) S(2) W(1) 63.1(6) . . . n
C(1) S(1) W(1) 120(2) . . . n
C(1) S(1) W(2) 119(2) . . . n
C(5) S(1) W(1) 127(3) . . . n
C(5) S(1) W(2) 126(3) . . . n
C(5) S(1) C(1) 101(4) . . . n
C(6) S(2) W(1) 121(3) . . . n
C(6) S(2) W(2) 123(3) . . . n
C(10) S(2) W(1) 122(2) . . . n
C(10) S(2) W(2) 122(3) . . . n
C(10) S(2) C(6) 103(4) . . . n
C(17) P(1) C(11) 111(2) . . . n
C(23) P(1) C(11) 110(2) . . . n
C(23) P(1) C(17) 111(3) . . . n
C(29) P(1) C(11) 110(3) . . . n
C(29) P(1) C(17) 111(2) . . . n
C(29) P(1) C(23) 105(3) . . . n
C(4) O(1) C(2) 115(7) . . . n
C(9) O(2) C(7) 110(7) . . . n
C(2) C(1) S(1) 109(6) . . . n
C(1) C(2) O(1) 117(7) . . . n
C(5) C(4) O(1) 108(7) . . . n
C(4) C(5) S(1) 112(7) . . . n
C(7) C(6) S(2) 107(5) . . . n
C(6) C(7) O(2) 112(6) . . . n
Cl(10) C(35) Cl(9) 108(5) . . . n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W(2) W(1) 2.496(4) . . n
Cl(1) W(1) 2.51(2) . . n
Cl(2) W(1) 2.38(2) . . n
Cl(3) W(1) 2.40(2) . . n
Cl(4) W(1) 2.38(2) . . n
S(1) W(1) 2.38(2) . . n
S(2) W(1) 2.38(2) . . n
Cl(1) W(2) 2.51(2) . . n
Cl(5) W(2) 2.37(2) . . n
Cl(6) W(2) 2.41(2) . . n
Cl(7) W(2) 2.40(2) . . n
S(1) W(2) 2.38(2) . . n
S(2) W(2) 2.39(2) . . n
C(1) S(1) 1.80(8) . . n
C(5) S(1) 1.81(10) . . n
C(6) S(2) 1.84(8) . . n
C(10) S(2) 1.82(8) . . n
C(11) P(1) 1.76(6) . . n
C(17) P(1) 1.78(6) . . n
C(23) P(1) 1.84(5) . . n
C(29) P(1) 1.83(6) . . n
C(2) O(1) 1.39(11) . . n
C(4) O(1) 1.41(10) . . n
C(7) O(2) 1.46(10) . . n
C(9) O(2) 1.35(12) . . n
C(2) C(1) 1.57(11) . . n
C(5) C(4) 1.54(12) . . n
C(7) C(6) 1.52(10) . . n
C(10) C(9) 1.58(13) . . n
Cl(8) C(35) 1.76(9) . . n
Cl(9) C(35) 1.80(9) . . n
Cl(10) C(35) 1.75(9) . . n
