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_7703374
_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         'C5 H12 Cl3 O S2 W'
_chemical_formula_sum            'C5 H12 Cl3 O S2 W'
_chemical_formula_weight         442.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-08-19
_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                78.514(4)
_cell_angle_beta                 81.724(4)
_cell_angle_gamma                72.508(5)
_cell_formula_units_Z            2
_cell_length_a                   6.7576(4)
_cell_length_b                   7.3941(4)
_cell_length_c                   12.4200(5)
_cell_measurement_reflns_used    6925
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.9440
_cell_measurement_theta_min      3.6040
_cell_volume                     577.68(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.911
_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    -19.00  94.00   1.00    1.00    --    5.00  38.00  60.00  113
  2  \w   -101.00  18.00   1.00    1.00    --  -12.10 -60.00 -30.00  119
  3  \w   -101.00  17.00   1.00    1.00    --  -12.10 -57.00  90.00  118
  4  \w    -36.00  77.00   1.00    1.00    --  -12.10  38.00 -90.00  113
  5  \w   -101.00  18.00   1.00    1.00    --  -12.10 -60.00-180.00  119
  6  \w    -42.00  34.00   1.00    1.00    --  -12.10  60.00   0.00   76
  7  \w    -42.00  77.00   1.00    1.00    --  -12.10  60.00  90.00  119
;
_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      -0.0921703000
_diffrn_orient_matrix_UB_12      0.0651523000
_diffrn_orient_matrix_UB_13      0.0197839000
_diffrn_orient_matrix_UB_21      -0.0453624000
_diffrn_orient_matrix_UB_22      -0.0768566000
_diffrn_orient_matrix_UB_23      0.0190060000
_diffrn_orient_matrix_UB_31      0.0407075000
_diffrn_orient_matrix_UB_32      -0.0157420000
_diffrn_orient_matrix_UB_33      0.0516840000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15495
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.368
_diffrn_reflns_theta_min         2.929
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.008
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.47a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.544
_exptl_crystal_description       plate
_exptl_crystal_F_000             414
_exptl_crystal_preparation       'Slow Evporation from 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         4.933
_refine_diff_density_min         -3.100
_refine_diff_density_rms         0.380
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         3459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0684P)^2^+0.0903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3219
_reflns_number_total             3459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00068j2.cif
_cod_data_source_block           wocl3-mes(ch2)3sme
_cod_depositor_comments
'Adding full bibliography for 7703371--7703377.cif.'
_cod_database_code               7703374
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         WS3Cl3C5H12
_chemical_oxdiff_usercomment     'Yellow Plate'
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.734
_reflns_odcompleteness_completeness 99.97
_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:
 C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              91783
_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 1.904
_oxdiff_exptl_absorpt_empirical_full_min 0.563