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_7703372
_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 O S2 W'
_chemical_formula_sum            'C4 H10 Cl3 O S2 W'
_chemical_formula_weight         428.44
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
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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.
;
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_diffrn_ambient_environment      N~2~
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_diffrn_measured_fraction_theta_max 0.909
_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  16.00   1.00    1.00    --  -19.10 -57.00 -60.00  124
  2  \w   -108.00  16.00   1.00    1.00    --  -19.10 -57.00  30.00  124
  3  \w   -108.00  16.00   1.00    1.00    --  -19.10 -57.00-120.00  124
  4  \w   -108.00  16.00   1.00    1.00    --  -19.10 -57.00 150.00  124
  5  \w    -55.00  70.00   1.00    1.00    --  -19.10  60.00  60.00  125
  6  \w    -55.00  16.00   1.00    1.00    --  -19.10  60.00 150.00   71
  7  \w    -55.00  70.00   1.00    1.00    --  -19.10  60.00-120.00  125
;
_diffrn_measurement_device       'four-circle diffractometer'
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'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0560061000
_diffrn_orient_matrix_UB_12      -0.1219409000
_diffrn_orient_matrix_UB_13      -0.0287687000
_diffrn_orient_matrix_UB_21      0.0631138000
_diffrn_orient_matrix_UB_22      0.0213866000
_diffrn_orient_matrix_UB_23      0.0998944000
_diffrn_orient_matrix_UB_31      -0.0890535000
_diffrn_orient_matrix_UB_32      0.0073677000
_diffrn_orient_matrix_UB_33      0.0379704000
_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5239
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.669
_diffrn_reflns_theta_min         3.179
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.619
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33969
_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            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.601
_exptl_crystal_description       plate
_exptl_crystal_F_000             199
_exptl_crystal_preparation       'Slow evporation from DCM'
_exptl_crystal_recrystallization_method 'Slow evporation from DCM'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.758
_refine_diff_density_min         -2.629
_refine_diff_density_rms         0.290
_refine_ls_abs_structure_details
;
 Flack x determined using 1267 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.029(14)
_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     3
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0699P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                2854
_reflns_number_total             2880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00068j2.cif
_cod_data_source_block           wocl3(mes(ch2)2sme)
_cod_depositor_comments
'Adding full bibliography for 7703371--7703377.cif.'
_cod_original_cell_volume        273.54(2)
_cod_database_code               7703372
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         S2OWCl4C4H10
_chemical_oxdiff_usercomment     'Green Block'
_shelx_estimated_absorpt_t_max   0.205
_shelx_estimated_absorpt_t_min   0.205
_reflns_odcompleteness_completeness 99.58
_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:
 C2(H2A,H2B), C3(H3A,H3B)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              86325
_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 5.417
_oxdiff_exptl_absorpt_empirical_full_min 0.145