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_7703373
_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         'C14 H14 Cl8 S4 W2'
_chemical_formula_sum            'C14 H14 Cl8 S4 W2'
_chemical_formula_weight         961.79
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 96.368(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5790(2)
_cell_length_b                   13.9272(3)
_cell_length_c                   17.2182(4)
_cell_measurement_reflns_used    7424
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.1850
_cell_measurement_theta_min      3.4920
_cell_volume                     2521.21(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 0.983
_diffrn_measured_fraction_theta_max 0.828
_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   -101.00  18.00   1.00   12.04    --  -12.10 -60.00 -60.00  119
  2  \w    -36.00  60.00   1.00   12.04    --  -12.10  38.00 -90.00   96
  3  \w   -100.00   7.00   1.00   12.04    --  -12.10 -60.00 120.00  107
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0113027000
_diffrn_orient_matrix_UB_12      -0.0097979000
_diffrn_orient_matrix_UB_13      0.0405867000
_diffrn_orient_matrix_UB_21      0.0305686000
_diffrn_orient_matrix_UB_22      0.0451204000
_diffrn_orient_matrix_UB_23      0.0061471000
_diffrn_orient_matrix_UB_31      -0.0590741000
_diffrn_orient_matrix_UB_32      0.0214960000
_diffrn_orient_matrix_UB_33      0.0057143000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17788
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.262
_diffrn_reflns_theta_min         2.925
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.300
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.534
_exptl_crystal_description       plate
_exptl_crystal_F_000             1784
_exptl_crystal_preparation       'Vapour Diffusion from DCM and Hexane'
_exptl_crystal_recrystallization_method
'Vapour Difrfusion from DCM and Hexane'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.153
_refine_diff_density_min         -2.693
_refine_diff_density_rms         0.308
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         6811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0420
_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/[\s^2^(Fo^2^)+(0.0191P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5333
_reflns_number_total             6811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00068j2.cif
_cod_data_source_block           (wscl4)2phs(ch2)2sph)
_cod_depositor_comments
'Adding full bibliography for 7703371--7703377.cif.'
_cod_database_code               7703373
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         W2S4Cl8C8H14
_chemical_oxdiff_usercomment     'Red Plate'
_reflns_odcompleteness_completeness 94.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C1(H1), C4(H4), C14(H14), C3(H3), C10(H10), C13(H13), C11(H11),
 C2(H2), C12(H12)
;
_shelx_res_checksum              75435
_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 4.946
_oxdiff_exptl_absorpt_empirical_full_min 0.355