#------------------------------------------------------------------------------
#$Date: 2022-01-20 01:52:26 +0200 (Thu, 20 Jan 2022) $
#$Revision: 272142 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/93/7709323.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7709323
loop_
_publ_author_name
'Greenacre, Victoria K.'
'Hector, Andrew L.'
'Huang, Ruomeng'
'Levason, William'
'Sethi, Vikesh'
'Reid, Gillian'
_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         'Cl4 Se W'
_chemical_formula_sum            'Cl4 Se W'
_chemical_formula_weight         404.61
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_audit_creation_date             2021-01-05
_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                 111.125(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.8639(2)
_cell_length_b                   12.4149(2)
_cell_length_c                   12.1003(3)
_cell_measurement_reflns_used    13638
_cell_measurement_temperature    120
_cell_measurement_theta_max      75.7850
_cell_measurement_theta_min      5.2510
_cell_volume                     1242.08(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  27.00   0.50    4.00    --  -46.06  77.00-180.00  192
  2  ω    -37.00  27.00   0.50    4.00    --  -46.06  37.00 -90.00  128
  3  ω    -16.00  29.00   0.50    4.00    --  -46.06  19.00-120.00   90
  4  ω   -118.00 -31.00   0.50    4.00    --  -46.06 -57.00  30.00  174
  5  ω    -37.00  27.00   0.50    4.00    --  -46.06  37.00 150.00  128
  6  ω     23.00  94.00   0.50    4.00    --   46.06-125.00  60.00  142
  7  ω     29.00 125.00   0.50    8.00    --  101.75 -77.00 -60.00  192
  8  ω     29.00  76.00   0.50    8.00    --  101.75 -61.00  90.00   94
  9  ω     29.00 106.00   0.50    8.00    --  101.75 -94.00  60.00  154
 10  ω     30.00 174.00   0.50    8.00    --  101.75   0.00  60.00  288
 11  ω     29.00  76.00   0.50    8.00    --  101.75 -61.00   0.00   94
 12  ω     82.00 175.00   0.50    8.00    --  101.75 125.00 -60.00  186
 13  ω     29.00 106.00   0.50    8.00    --  101.75 -94.00 -60.00  154
 14  ω     29.00  76.00   0.50    8.00    --  101.75 -61.00-150.00   94
 15  ω     29.00 106.00   0.50    8.00    --  101.75 -99.00 106.12  154
 16  ω     29.00  76.00   0.50    8.00    --  101.75 -61.00  30.00   94
 17  ω     29.00 112.00   0.50    8.00    --  101.75-125.00-150.00  166
 18  ω     30.00 174.00   0.50    8.00    --  101.75   0.00 -90.00  288
 19  ω     29.00 106.00   0.50    8.00    --  101.75 -94.00-150.00  154
 20  ω     89.00 174.00   0.50    8.00    --  101.75  45.00   0.00  170
 21  ω    -70.00 -30.00   0.50    8.00    -- -103.00  61.00 -90.00   80
 22  ω    -70.00 -30.00   0.50    8.00    -- -103.00  61.00 -60.00   80
 23  ω   -174.00 -90.00   0.50    8.00    -- -103.00 -49.00-159.25  168
 24  ω   -174.00 -90.00   0.50    8.00    -- -103.00 -30.00 -60.00  168
 25  ω   -174.00 -90.00   0.50    8.00    -- -103.00 -45.00 -30.00  168
 26  ω   -118.00 -33.00   0.50    4.00    --  -46.06 -46.00  96.78  170
 27  ω     24.00 119.00   0.50    4.00    --   46.06  77.00 -60.00  190
 28  ω     24.00 119.00   0.50    4.00    --   46.06  77.00-150.00  190
 29  ω     24.00 119.00   0.50    4.00    --   46.06  77.00   0.00  190
 30  ω     24.00 119.00   0.50    4.00    --   46.06  77.00 120.00  190
 31  ω    108.00 174.00   0.50    8.00    --  101.75   0.00 120.00  132
 32  ω   -174.00 -86.00   0.50    8.00    -- -103.00 -61.00 153.13  176
 33  ω   -174.00 -78.00   0.50    8.00    -- -103.00 -81.00 -94.75  192
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0579774000
_diffrn_orient_matrix_UB_12      0.0071433000
_diffrn_orient_matrix_UB_13      0.1360845000
_diffrn_orient_matrix_UB_21      0.1144670000
_diffrn_orient_matrix_UB_22      -0.0960364000
_diffrn_orient_matrix_UB_23      0.0105429000
_diffrn_orient_matrix_UB_31      0.1351741000
_diffrn_orient_matrix_UB_32      0.0782022000
_diffrn_orient_matrix_UB_33      0.0005516000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18376
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.002
_diffrn_reflns_theta_max         67.002
_diffrn_reflns_theta_min         5.296
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    55.880
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    4.327
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0162
_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/[σ²(Fo²)+(0.0259P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0392
_refine_ls_wR_factor_ref         0.0398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2069
_reflns_number_total             2207
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt03980f3.cif
_cod_data_source_block           2020vkwsecl4_2b
_cod_database_code               7709323
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         WSeCl4
_chemical_oxdiff_usercomment     'very small green crystal'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.401
_shelx_estimated_absorpt_t_min   0.401
_reflns_odcompleteness_completeness 99.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
;
_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 6.604
_oxdiff_exptl_absorpt_empirical_full_min 0.477
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W2 W 0.62837(2) 0.86244(2) 0.57196(2) 0.01076(7) Uani 1 1 d . . . . .
W1 W 0.29484(2) 0.59346(2) 0.65841(2) 0.01108(6) Uani 1 1 d . . . . .
Se1 Se 0.23976(5) 0.44775(3) 0.74179(3) 0.01694(10) Uani 1 1 d . . . . .
Se2 Se 0.75296(5) 0.78567(3) 0.74624(3) 0.01634(10) Uani 1 1 d . . . . .
Cl3 Cl 0.53720(10) 0.54714(7) 0.64322(7) 0.01512(18) Uani 1 1 d . . . . .
Cl5 Cl 0.36473(10) 0.80563(6) 0.54246(7) 0.01358(18) Uani 1 1 d . . . . .
Cl7 Cl 0.83597(10) 0.95397(7) 0.54650(7) 0.01548(18) Uani 1 1 d . . . . .
Cl6 Cl 0.55214(10) 1.02614(7) 0.64268(7) 0.01354(17) Uani 1 1 d . . . . .
Cl8 Cl 0.64284(10) 0.73069(7) 0.44621(7) 0.01581(18) Uani 1 1 d . . . . .
Cl2 Cl 0.43905(11) 0.69382(7) 0.82284(7) 0.01536(18) Uani 1 1 d . . . . .
Cl4 Cl 0.17410(11) 0.55425(7) 0.45966(7) 0.01712(19) Uani 1 1 d . . . . .
Cl1 Cl 0.07405(11) 0.70047(7) 0.63800(8) 0.01739(19) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Se2 W2 Cl5 98.24(2) . . ?
Se2 W2 Cl7 101.18(2) . . ?
Se2 W2 Cl6 97.65(2) . . ?
Se2 W2 Cl8 101.49(2) . . ?
Cl5 W2 Cl6 85.15(3) . . ?
Cl7 W2 Cl5 160.17(3) . . ?
Cl7 W2 Cl6 88.32(3) . . ?
Cl8 W2 Cl5 88.58(3) . . ?
Cl8 W2 Cl7 91.45(3) . . ?
Cl8 W2 Cl6 160.52(3) . . ?
Se1 W1 Cl3 101.46(2) . . ?
Se1 W1 Cl2 101.15(2) . . ?
Se1 W1 Cl4 101.98(2) . . ?
Se1 W1 Cl1 101.66(3) . . ?
Cl3 W1 Cl2 87.74(3) . . ?
Cl3 W1 Cl4 87.68(3) . . ?
Cl3 W1 Cl1 156.88(3) . . ?
Cl4 W1 Cl2 156.87(3) . . ?
Cl1 W1 Cl2 88.06(3) . . ?
Cl1 W1 Cl4 87.30(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W2 Se2 2.2128(4) . ?
W2 Cl5 2.3419(8) . ?
W2 Cl7 2.2762(9) . ?
W2 Cl6 2.3949(8) . ?
W2 Cl8 2.2689(8) . ?
W1 Se1 2.2099(4) . ?
W1 Cl3 2.2944(9) . ?
W1 Cl2 2.3048(8) . ?
W1 Cl4 2.3045(8) . ?
W1 Cl1 2.3038(9) . ?
