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_7709325
_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         'C3 H7 Cl4 N O Se W, C6 H6'
_chemical_formula_sum            'C9 H13 Cl4 N O Se W'
_chemical_formula_weight         555.81
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-11-15 deposited with the CCDC.	2022-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.559(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.8765(10)
_cell_length_b                   7.3681(3)
_cell_length_c                   22.8710(13)
_cell_measurement_reflns_used    6342
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.8960
_cell_measurement_theta_min      1.8560
_cell_volume                     3078.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9988
_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    -54.00  72.00   0.50    3.50    --  -16.90  60.00 -60.00  252
  2  \w    -54.00  72.00   0.50    3.50    --  -16.90  60.00   0.00  252
  3  \w    -54.00  72.00   0.50    3.50    --  -16.90  60.00 -90.00  252
  4  \w    -54.00  72.00   0.50    3.50    --  -16.90  60.00  60.00  252
  5  \w    -60.00  -4.00   0.50    3.50    --  -16.90 -38.00 150.00  112
;
_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       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0328513000
_diffrn_orient_matrix_UB_12      0.0510031000
_diffrn_orient_matrix_UB_13      -0.0090210000
_diffrn_orient_matrix_UB_21      -0.0200836000
_diffrn_orient_matrix_UB_22      -0.0813131000
_diffrn_orient_matrix_UB_23      -0.0082465000
_diffrn_orient_matrix_UB_31      -0.0050413000
_diffrn_orient_matrix_UB_32      -0.0075916000
_diffrn_orient_matrix_UB_33      0.0296043000
_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     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20205
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.692
_diffrn_reflns_theta_min         2.229
_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 FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    10.546
_exptl_absorpt_correction_T_max  0.71760
_exptl_absorpt_correction_T_min  0.70917
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.398
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene'
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.066
_exptl_crystal_size_rad          0.043
_refine_diff_density_max         2.890
_refine_diff_density_min         -5.022
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3969
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0323P)^2^+34.6107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3300
_reflns_number_total             3969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03980f3.cif
_cod_data_source_block           vg9177-88a4
_cod_database_code               7709325
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'W Se Cl4 C9 H13 N O'
_chemical_oxdiff_usercomment     'dusky/dirty purple crystals '
_shelx_estimated_absorpt_t_max   0.543
_shelx_estimated_absorpt_t_min   0.457
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-C1 \\sim O1A-C1A
 with sigma of 0.02
 N1-C1 \\sim N1-C1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(O1A)
Uanis(C1) = Uanis(C1A)
Uanis(Cl1) = Uanis(Cl1A)
Uanis(Cl4) = Uanis(Cl4A)
Uanis(Cl3) = Uanis(Cl3A)
Uanis(Se1) = Uanis(Se1A)
Uanis(Cl2) = Uanis(Cl2A)
Uanis(W1) = Uanis(W1A)
4. Rigid body (RIGU) restrains
 W1A, Se1A, Cl1A, Cl2A, Cl3A, Cl4A, O1A, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: W1(0.95) Se1(0.95) Cl1(0.95) Cl2(0.95) Cl3(0.95) Cl4(0.95)
 O1(0.95) C1(0.95) H1(0.95) W1A(0.05) Se1A(0.05) Cl1A(0.05) Cl2A(0.05)
 Cl3A(0.05) Cl4A(0.05) O1A(0.05) C1A(0.05) H1A(0.05)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C1A(H1A), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9)
6.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              21952
_shelx_hkl_checksum              21525
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_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 2.696
_oxdiff_exptl_absorpt_empirical_full_min 0.264