Tungsten(vi) selenide tetrachloride, WSeCl4 – synthesis, properties, coordination complexes and application of [WSeCl4(SenBu2)] for CVD growth of WSe2 thin films
Greenacre, Victoria K.; Hector, Andrew L.; Huang, Ruomeng; Levason, William; Sethi, Vikesh; Reid, Gillian; Dalton Transactions  (2022) –; doi:10.1039/D1DT03980F

data_7709328
_publ_section_title
;
 Tungsten(vi) selenide tetrachloride, WSeCl4 -- synthesis, properties,
 coordination complexes and application of [WSeCl4(SenBu2)] for CVD growth
 of WSe2 thin films
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03980F
_journal_year                    2022
_chemical_formula_moiety         'C4 H12 Cl6 S2 Se3 W2'
_chemical_formula_sum            'C4 H12 Cl6 S2 Se3 W2'
_chemical_formula_weight         941.54
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-15 deposited with the CCDC.	2022-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.58820(13)
_cell_length_b                   19.5279(2)
_cell_length_c                   6.69716(7)
_cell_measurement_reflns_used    21668
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.2240
_cell_measurement_theta_min      6.4880
_cell_volume                     1777.08(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_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   -157.00 -35.00   0.50    0.75    --  -90.00  59.00-106.64  244
  2  \w   -179.00  -1.00   0.50    0.75    --  -90.00  59.00  60.63  356
  3  \w   -179.00  -1.00   0.50    0.75    --  -90.00  59.00 169.17  356
  4  \w   -179.00  -1.00   0.50    0.75    --  -90.00  55.00-171.79  356
  5  \w   -179.00  -1.00   0.50    0.75    --  -90.00  52.00-136.98  356
  6  \w   -179.00  -1.00   0.50    0.75    --  -90.00  59.00 -19.37  356
  7  \w   -179.00  -1.00   0.50    0.75    --  -90.00  59.00 130.00  356
  8  \w   -179.00  -1.00   0.50    0.75    --  -90.00  56.00 -66.40  356
  9  \w   -157.00 -35.00   0.50    0.75    --  -90.00  59.00-106.64  244
 10  \w   -127.00 -36.00   0.50    0.75    --  -90.00  10.00  60.00  182
 11  \w   -178.00-152.00   0.50    0.75    --  -90.00  59.00  82.86   52
 12  \w   -142.00-116.00   0.50    0.75    --  -90.00  59.00  82.86   52
 13  \w    -55.00  -1.00   0.50    0.75    --  -90.00  59.00  82.86  108
 14  \w   -179.00-127.00   0.50    0.75    --  -90.00  10.00   0.00  104
 15  \w    -56.00 -19.00   0.50    0.75    --  -90.00  10.00   0.00   74
 16  \w   -174.00-148.00   0.50    0.75    --  -90.00  39.00 -30.00   52
 17  \w   -170.00-139.00   0.50    0.75    --  -90.00  10.00  60.00   62
 18  \w    -89.00  89.00   0.50    0.50    --    0.00  59.00  60.00  356
 19  \w    -89.00  89.00   0.50    0.50    --    0.00   0.00-180.00  356
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0401948000
_diffrn_orient_matrix_UB_12      -0.0418192000
_diffrn_orient_matrix_UB_13      0.1772477000
_diffrn_orient_matrix_UB_21      -0.1043428000
_diffrn_orient_matrix_UB_22      0.0040833000
_diffrn_orient_matrix_UB_23      -0.0891072000
_diffrn_orient_matrix_UB_31      0.0189100000
_diffrn_orient_matrix_UB_32      -0.0667646000
_diffrn_orient_matrix_UB_33      -0.1163429000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            30236
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.442
_diffrn_reflns_theta_min         6.515
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    40.932
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'brownish black'
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.519
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.427
_refine_diff_density_min         -1.872
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+31.1694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1738
_reflns_number_total             1743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03980f3.cif
_cod_data_source_block           vg9177_90_auto
_cod_original_cell_volume        1777.09(3)
_cod_database_code               7709328
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'W Se Cl4 O S C2 H6'
_chemical_oxdiff_usercomment     'black chunk'
_shelx_estimated_absorpt_t_max   0.234
_shelx_estimated_absorpt_t_min   0.162
_diffrn_oxdiff_digest_frames
;
0175c9ee5bd0ec4854b0da1fe731646670000380e3a
;
_diffrn_oxdiff_digest_hkl
;
01144455af219bbf68ee5918001bff7bf0aba1
;
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              69404
_shelx_hkl_checksum              24981
_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 2.578
_oxdiff_exptl_absorpt_empirical_full_min 0.604