#------------------------------------------------------------------------------
#$Date: 2020-03-05 01:01:06 +0100 (jue 05 de mar de 2020) $
#$Revision: 248909 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/33/7703375.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_7703375
loop_
_publ_author_name
'Smith, Danielle E.'
'Greenacre, Victoria K.'
'Hector, Andrew L.'
'Huang, Ruomeng'
'Levason, William'
'Reid, Gillian'
'Robinson, Fred'
'Thomas, Shibin'
_publ_section_title
;
 Thioether complexes of WSCl₄, WOCl₄ and
 WSCl₃ and evaluation of thiochloride complexes as CVD
 precursors for WS₂ thin films.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2496
_journal_page_last               2504
_journal_paper_doi               10.1039/d0dt00068j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C4 H10 Cl8 S4 W2'
_chemical_formula_sum            'C4 H10 Cl8 S4 W2'
_chemical_formula_weight         837.66
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-28 deposited with the CCDC.	2020-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.882(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.6849(2)
_cell_length_b                   10.5079(3)
_cell_length_c                   11.8240(4)
_cell_measurement_reflns_used    7344
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.1650
_cell_measurement_theta_min      3.2880
_cell_volume                     954.30(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -37.00  77.00   1.00    1.00    --  -12.30  38.00 -90.00  114
  2  ω   -102.00  17.00   1.00    1.00    --  -12.30 -57.00 -30.00  119
  3  ω   -102.00  17.00   1.00    1.00    --  -12.30 -57.00-120.00  119
  4  ω   -102.00  17.00   1.00    1.00    --  -12.30 -57.00 150.00  119
  5  ω    -43.00  28.00   1.00    1.00    --  -12.30  60.00   0.00   71
  6  ω    -42.00  77.00   1.00    1.00    --  -12.30  57.00  90.00  119
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0769411000
_diffrn_orient_matrix_UB_12      -0.0160792000
_diffrn_orient_matrix_UB_13      -0.0316001000
_diffrn_orient_matrix_UB_21      -0.0349005000
_diffrn_orient_matrix_UB_22      -0.0279082000
_diffrn_orient_matrix_UB_23      0.0489127000
_diffrn_orient_matrix_UB_31      -0.0373271000
_diffrn_orient_matrix_UB_32      0.0593180000
_diffrn_orient_matrix_UB_33      0.0145066000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1412
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13938
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.981
_diffrn_reflns_theta_min         3.956
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    13.581
_exptl_absorpt_correction_T_max  0.00827
_exptl_absorpt_correction_T_min  0.00090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.915
_exptl_crystal_description       plate
_exptl_crystal_F_000             764
_exptl_crystal_preparation       'Slow evporation from DCM'
_exptl_crystal_recrystallization_method 'Slow evporation from DCM'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.356
_refine_diff_density_min         -1.347
_refine_diff_density_rms         0.431
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0969P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1697
_reflns_number_total             1864
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt00068j2.cif
_cod_data_source_block           dsex94rdb
_cod_depositor_comments
'Adding full bibliography for 7703371--7703377.cif.'
_cod_database_code               7703375
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'W2 S4 Cl8 C4 H10'
_chemical_oxdiff_usercomment     'Red Block'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.773
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_shelx_res_file
;
TITL dsex94rdb_a.res in P2(1)/c
    dsex94rdb.res
    created by SHELXL-2018/3 at 14:18:29 on 01-Jul-2019
REM Old TITL DS EX94 rdb in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.073, Rweak 0.011, Alpha 0.026, Orientation as input
REM Formula found by SHELXT: C2 S Cl3 W
CELL 0.71073 7.684899 10.507902 11.824044 90 91.8823 90
ZERR 2 0.000226 0.0003 0.000413 0 0.0029 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl S W
UNIT 8 20 16 8 4

L.S. 10 0 0
PLAN  20
SIZE 0.02 0.02 0.01
LIST 6
fmap 2 53
acta
OMIT -4 52
OMIT 0 2 0
OMIT 0 2 1
OMIT 0 0 2
OMIT 1 1 0
OMIT 1 1 1
OMIT -1 1 1
REM <olex2.extras>
REM <HklSrc "%.\\DS%20EX94%20rdb.hkl">
REM </olex2.extras>

WGHT    0.096900
FVAR       2.26767
W1    5    0.267129    0.423559    0.668375    11.00000    0.04347    0.04198 =
         0.04580    0.00098    0.00483    0.00014
CL4   3    0.550206    0.429950    0.740308    11.00000    0.04212    0.05414 =
         0.05517   -0.00051    0.00576   -0.00010
CL2   3   -0.032338    0.426920    0.658791    11.00000    0.04402    0.06559 =
         0.05509   -0.00172    0.00224    0.00213
S2    4    0.236655    0.465680    0.903709    11.00000    0.04671    0.04922 =
         0.04745    0.00037    0.00711    0.00219
CL1   3    0.245500    0.218319    0.735697    11.00000    0.06210    0.04408 =
         0.05483    0.00210    0.00108   -0.00480
CL3   3    0.260916    0.641732    0.659885    11.00000    0.06737    0.04603 =
         0.05863    0.00373    0.00552   -0.00071
S1    4    0.322844    0.382772    0.499980    11.00000    0.05772    0.05855 =
         0.04872   -0.00136    0.00684   -0.00090
C2    1    0.326155    0.620657    0.934604    11.00000    0.05662    0.04779 =
         0.06576   -0.00986    0.00575   -0.00949
AFIX 137
H2A   2    0.440665    0.626600    0.904940    11.00000   -1.50000
H2B   2    0.332816    0.633257    1.015045    11.00000   -1.50000
H2C   2    0.252703    0.684744    0.900301    11.00000   -1.50000
AFIX   0
C1    1    0.010837    0.488343    0.937963    11.00000    0.04217    0.05915 =
         0.05422   -0.00101    0.01526    0.00752
AFIX  23
H1A   2   -0.035981    0.560216    0.895426    11.00000   -1.20000
H1B   2   -0.055240    0.413396    0.915305    11.00000   -1.20000
AFIX   0
HKLF 4




REM  dsex94rdb_a.res in P2(1)/c
REM wR2 = 0.1519, GooF = S = 1.113, Restrained GooF = 1.113 for all data
REM R1 = 0.0572 for 1697 Fo > 4sig(Fo) and 0.0597 for all 1864 data
REM 83 parameters refined using 0 restraints

END

WGHT      0.0969      0.0000

REM Highest difference peak  3.356,  deepest hole -1.347,  1-sigma level  0.431
Q1    1   0.1545  0.4176  0.6686  11.00000  0.05    3.36
Q2    1   0.3806  0.4172  0.6683  11.00000  0.05    3.24
Q3    1   0.3173  0.3605  0.6555  11.00000  0.05    2.77
Q4    1   0.2379  0.4975  0.6726  11.00000  0.05    2.62
Q5    1   0.2822  0.4974  0.6589  11.00000  0.05    2.59
Q6    1   0.2542  0.3469  0.6777  11.00000  0.05    2.52
Q7    1   0.2937  0.4182  0.5884  11.00000  0.05    2.50
Q8    1   0.2616  0.4267  0.7404  11.00000  0.05    1.99
Q9    1   0.2712  0.7174  0.6679  11.00000  0.05    1.36
Q10   1   0.1155  0.4715  0.9209  11.00000  0.05    0.97
Q11   1   0.2720  0.1635  0.6818  11.00000  0.05    0.95
Q12   1   0.2028  0.4360  0.9945  11.00000  0.05    0.93
Q13   1   0.5396  0.4251  0.6644  11.00000  0.05    0.93
Q14   1   0.2424  0.2158  0.6668  11.00000  0.05    0.91
Q15   1   0.1672  0.1964  0.7426  11.00000  0.05    0.91
Q16   1   0.2911  0.6623  0.5857  11.00000  0.05    0.90
Q17   1   0.1898  0.1548  0.6640  11.00000  0.05    0.86
Q18   1   0.2737  0.6662  0.9181  11.00000  0.05    0.81
Q19   1   0.2001  0.6827  0.5986  11.00000  0.05    0.81
Q20   1   0.1388  0.6560  0.6659  11.00000  0.05    0.76
;
_shelx_res_checksum              84528
_olex2_exptl_crystal_mounting_method Mounted
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.229
_oxdiff_exptl_absorpt_empirical_full_min 0.088
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
W1 W 0.26713(4) 0.42356(3) 0.66838(3) 0.0437(3) Uani 1 1 d .
Cl4 Cl 0.5502(3) 0.42995(19) 0.7403(3) 0.0504(6) Uani 1 1 d .
Cl2 Cl -0.0323(3) 0.4269(2) 0.6588(3) 0.0549(6) Uani 1 1 d .
S2 S 0.2367(3) 0.4657(2) 0.9037(2) 0.0477(5) Uani 1 1 d .
Cl1 Cl 0.2455(3) 0.2183(2) 0.7357(2) 0.0537(6) Uani 1 1 d .
Cl3 Cl 0.2609(3) 0.6417(3) 0.6599(2) 0.0573(7) Uani 1 1 d .
S1 S 0.3228(3) 0.3828(3) 0.5000(2) 0.0549(6) Uani 1 1 d .
C2 C 0.3262(13) 0.6207(9) 0.9346(9) 0.057(2) Uani 1 1 d .
H2A H 0.440665 0.626600 0.904940 0.085 Uiso 1 1 calc GR
H2B H 0.332816 0.633257 1.015045 0.085 Uiso 1 1 calc GR
H2C H 0.252703 0.684744 0.900301 0.085 Uiso 1 1 calc GR
C1 C 0.0108(12) 0.4883(10) 0.9380(9) 0.052(2) Uani 1 1 d .
H1A H -0.035981 0.560216 0.895426 0.062 Uiso 1 1 calc R
H1B H -0.055240 0.413396 0.915305 0.062 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.0435(3) 0.0420(4) 0.0458(4) 0.00098(12) 0.0048(2) 0.00014(11)
Cl4 0.0421(12) 0.0541(13) 0.0552(15) -0.0005(9) 0.0058(11) -0.0001(8)
Cl2 0.0440(13) 0.0656(15) 0.0551(16) -0.0017(10) 0.0022(11) 0.0021(8)
S2 0.0467(12) 0.0492(12) 0.0475(13) 0.0004(10) 0.0071(9) 0.0022(9)
Cl1 0.0621(13) 0.0441(11) 0.0548(13) 0.0021(9) 0.0011(10) -0.0048(9)
Cl3 0.0674(16) 0.0460(15) 0.0586(16) 0.0037(9) 0.0055(12) -0.0007(8)
S1 0.0577(14) 0.0585(13) 0.0487(13) -0.0014(11) 0.0068(10) -0.0009(10)
C2 0.057(5) 0.048(5) 0.066(6) -0.010(5) 0.006(4) -0.009(4)
C1 0.042(4) 0.059(5) 0.054(5) -0.001(4) 0.015(4) 0.008(4)
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'
Cl Cl 0.1484 0.1585 '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'
W W -0.8490 6.8722 '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
_geom_angle_site_symmetry_1
Cl4 W1 S2 75.01(9) .
Cl2 W1 Cl4 161.06(12) .
Cl2 W1 S2 86.05(9) .
Cl2 W1 Cl1 87.02(9) .
Cl1 W1 Cl4 88.73(8) .
Cl1 W1 S2 78.35(8) .
Cl3 W1 Cl4 90.29(8) .
Cl3 W1 Cl2 87.89(8) .
Cl3 W1 S2 83.38(8) .
Cl3 W1 Cl1 161.32(8) .
S1 W1 Cl4 97.84(10) .
S1 W1 Cl2 101.05(10) .
S1 W1 S2 172.33(8) .
S1 W1 Cl1 98.98(10) .
S1 W1 Cl3 99.64(10) .
C2 S2 W1 107.3(4) .
C2 S2 C1 101.4(5) .
C1 S2 W1 110.5(3) .
C1 C1 S2 112.2(9) 3_567
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 Cl4 2.311(3) .
W1 Cl2 2.301(3) .
W1 S2 2.835(2) .
W1 Cl1 2.307(2) .
W1 Cl3 2.295(3) .
W1 S1 2.095(2) .
S2 C2 1.801(10) .
S2 C1 1.811(9) .
C1 C1 1.50(2) 3_567
