Thioether complexes of WSCl<sub>4</sub>, WOCl<sub>4</sub> and WSCl<sub>3</sub> and evaluation of thiochloride complexes as CVD precursors for WS<sub>2</sub> thin films.
Smith, Danielle E.; Greenacre, Victoria K.; Hector, Andrew L.; Huang, Ruomeng; Levason, William; Reid, Gillian; Robinson, Fred; Thomas, Shibin; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2496–2504; doi:10.1039/d0dt00068j

data_7703375
_publ_section_title
;
 Thioether complexes of WSCl<sub>4</sub>, WOCl<sub>4</sub> and
 WSCl<sub>3</sub> and evaluation of thiochloride complexes as CVD
 precursors for WS<sub>2</sub> 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
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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
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_cell_angle_gamma                90
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_cell_length_b                   10.5079(3)
_cell_length_c                   11.8240(4)
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_cell_measurement_temperature    100.00(10)
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_cell_measurement_theta_min      3.2880
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_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -37.00  77.00   1.00    1.00    --  -12.30  38.00 -90.00  114
  2  \w   -102.00  17.00   1.00    1.00    --  -12.30 -57.00 -30.00  119
  3  \w   -102.00  17.00   1.00    1.00    --  -12.30 -57.00-120.00  119
  4  \w   -102.00  17.00   1.00    1.00    --  -12.30 -57.00 150.00  119
  5  \w    -43.00  28.00   1.00    1.00    --  -12.30  60.00   0.00   71
  6  \w    -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'
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_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
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_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/[\s^2^(Fo^2^)+(0.0969P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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_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