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_7709329
_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         '2(C5 H4 Cl4 N Se W), 3(C6 H6)'
_chemical_formula_sum            'C28 H26 Cl8 N2 Se2 W2'
_chemical_formula_weight         1199.73
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-30
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2021-11-15 deposited with the CCDC.	2022-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                103.815(2)
_cell_angle_beta                 94.9132(17)
_cell_angle_gamma                98.3755(17)
_cell_formula_units_Z            2
_cell_length_a                   6.03153(11)
_cell_length_b                   15.4384(4)
_cell_length_c                   20.1476(5)
_cell_measurement_reflns_used    26196
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.5240
_cell_measurement_theta_min      1.9320
_cell_volume                     1788.17(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -98.00  22.00   0.50    8.00    --   -9.10 -57.00  30.00  240
  2  \w    -98.00  52.00   0.50    8.00    --   -9.10 -19.00 -60.00  300
  3  \w    -98.00  22.00   0.50    8.00    --   -9.10 -57.00  60.00  240
  4  \w    -98.00  23.00   0.50    8.00    --   -9.10 -60.00-180.00  242
  5  \w    -98.00  23.00   0.50    8.00    --   -9.10 -60.00-120.00  242
  6  \w    -98.00  22.00   0.50    8.00    --   -9.10 -57.00 -60.00  240
  7  \w    -44.00  -9.00   0.50    8.00    --   -9.10  38.00 -90.00   70
  8  \w    -44.00  80.00   0.50    8.00    --   -9.10  38.00  60.00  248
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0371346000
_diffrn_orient_matrix_UB_12      0.0229430000
_diffrn_orient_matrix_UB_13      -0.0246864000
_diffrn_orient_matrix_UB_21      -0.1104714000
_diffrn_orient_matrix_UB_22      -0.0114433000
_diffrn_orient_matrix_UB_23      -0.0182505000
_diffrn_orient_matrix_UB_31      -0.0277824000
_diffrn_orient_matrix_UB_32      0.0406094000
_diffrn_orient_matrix_UB_33      0.0198197000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            52666
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.934
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    9.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.106a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.228
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.651
_refine_diff_density_min         -1.311
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         8594
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0518P)^2^+7.9181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7517
_reflns_number_total             8594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03980f3.cif
_cod_data_source_block           vg9177_862_auto
_cod_original_cell_volume        1788.18(7)
_cod_database_code               7709329
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C28H26Cl8N2Se2W2
_chemical_oxdiff_usercomment     'running higher scan time'
_shelx_estimated_absorpt_t_max   0.612
_shelx_estimated_absorpt_t_min   0.495
_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) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C100(H100),
 C101(H101), C102(H102), C103(H103), C104(H104), C105(H105), C106(H106),
 C107(H107), C108(H108), C109(H109), C110(H110), C111(H111), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116), C117(H117)
;
_shelx_res_checksum              89893
_shelx_hkl_checksum              40275
_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 4.449
_oxdiff_exptl_absorpt_empirical_full_min 0.234