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_7703377
_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 Cl3 S3 W'
_chemical_formula_sum            'C4 H10 Cl3 S3 W'
_chemical_formula_weight         444.50
_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
_audit_creation_date             2019-08-20
_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                 94.541(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.87580(10)
_cell_length_b                   13.2588(2)
_cell_length_c                   12.5782(2)
_cell_measurement_reflns_used    18262
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.8000
_cell_measurement_theta_min      2.2090
_cell_volume                     1143.09(3)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.894
_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   -108.00  22.00   0.50    0.50    --  -18.80 -70.00 150.00  260
  2  \w    -59.00  71.00   0.50    0.50    --  -18.80  70.00  60.00  260
  3  \w   -108.00  22.00   0.50    0.50    --  -18.80 -70.00-120.00  260
  4  \w   -108.00  71.00   0.50    0.50    --  -18.80   0.00-180.00  358
  5  \w   -108.00  42.00   0.50    0.50    --  -18.80 -38.00 -90.00  300
  6  \w   -108.00  22.00   0.50    0.50    --  -18.80 -70.00  90.00  260
  7  \w    -56.00  -6.00   0.50    0.50    --  -18.80  57.00-150.00  100
  8  \w    -56.00  71.00   0.50    0.50    --  -18.80  57.00 -90.00  254
;
_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      0.0899380000
_diffrn_orient_matrix_UB_12      0.0152260000
_diffrn_orient_matrix_UB_13      0.0266961000
_diffrn_orient_matrix_UB_21      0.0196024000
_diffrn_orient_matrix_UB_22      -0.0506887000
_diffrn_orient_matrix_UB_23      0.0154511000
_diffrn_orient_matrix_UB_31      0.0471846000
_diffrn_orient_matrix_UB_32      -0.0079018000
_diffrn_orient_matrix_UB_33      -0.0474315000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30189
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.187
_diffrn_reflns_theta_min         2.236
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.296
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54286
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.583
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_preparation
'Slow evporation from (WSCl3)(MeS(CH2)2SMe) in DCM'
_exptl_crystal_recrystallization_method 'Slow evporation from dcm.'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.820
_refine_diff_density_min         -2.811
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         3609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0091P)^2^+13.7844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3332
_reflns_number_total             3609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00068j2.cif
_cod_data_source_block           (wscl3)(mes(ch2)2sme)
_cod_depositor_comments
'Adding full bibliography for 7703371--7703377.cif.'
_cod_database_code               7703377
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C4H10S3WCl4
_chemical_oxdiff_usercomment     'Red Block'
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.728
_reflns_odcompleteness_completeness 99.94
_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. Uiso/Uaniso restraints and constraints
Uanis(W1) = Uanis(W1A)
Uanis(Cl1A) = Uanis(S1)
Uanis(Cl1) = Uanis(S1A)
3. Others
 Fixed Sof: W1(0.75) Cl1(0.75) S1(0.75) Cl1A(0.25) S1A(0.25) W1A(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              30040
_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 1.815
_oxdiff_exptl_absorpt_empirical_full_min 0.701