#------------------------------------------------------------------------------
#$Date: 2022-01-20 01:52:26 +0200 (Thu, 20 Jan 2022) $
#$Revision: 272142 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/93/7709324.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_7709324
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         'C2 H3 Cl4 N Se W'
_chemical_formula_sum            'C2 H3 Cl4 N Se W'
_chemical_formula_weight         445.66
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-11-15 deposited with the CCDC.	2022-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 88.834(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.8784(2)
_cell_length_b                   7.8378(4)
_cell_length_c                   14.8140(6)
_cell_measurement_reflns_used    6299
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.8000
_cell_measurement_theta_min      2.7360
_cell_volume                     682.39(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (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 2014/5 (Sheldrick, 2014)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -99.00  23.00   0.50    0.55    --   -9.30 -60.00-150.00  244
  2  ω    -41.00  80.00   0.50    0.55    --   -9.30  57.00 -60.00  242
  3  ω    -99.00  26.00   0.50    0.55    --   -9.30 -38.00 -30.00  250
  4  ω    -41.00   6.00   0.50    0.55    --   -9.30  57.00  90.00   94
  5  ω    -61.00 -35.00   0.50    0.55    --    5.00 -60.00  90.00   52
  6  ω    -32.00  -1.00   0.50    0.55    --   -9.10 -57.00  90.00   62
  7  ω    -79.00 -38.00   0.50    0.55    --   -9.10 -57.00  90.00   82
  8  ω    -44.00  80.00   0.50    0.55    --   -9.10  38.00  60.00  248
  9  ω    -44.00  80.00   0.50    0.55    --   -9.10  38.00-180.00  248
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 κ goniometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0149397000
_diffrn_orient_matrix_UB_12      0.0135376000
_diffrn_orient_matrix_UB_13      -0.0471110000
_diffrn_orient_matrix_UB_21      -0.0061072000
_diffrn_orient_matrix_UB_22      -0.0892608000
_diffrn_orient_matrix_UB_23      -0.0074408000
_diffrn_orient_matrix_UB_31      -0.1195506000
_diffrn_orient_matrix_UB_32      0.0062410000
_diffrn_orient_matrix_UB_33      -0.0045422000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  mirror
_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  0.0615
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17488
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.695
_diffrn_reflns_theta_min         2.750
_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    11.860
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.169
_exptl_crystal_description       needle
_exptl_crystal_F_000             396
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.539
_refine_diff_density_min         -3.229
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         1882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0390
_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/[σ²(Fo²)+(0.0665P)²+2.5737P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1646
_reflns_number_total             1882
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt03980f3.cif
_cod_data_source_block           vg9177-95_2a
_cod_database_code               7709324
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'W Se Cl4 C2 N H3'
_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   0.648
_shelx_estimated_absorpt_t_min   0.200
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H2C(0.5)
3.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 106 electrons were 
found in a volume of 252Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1.25[C6H6] per Unit Cell 
which account for 105 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 2.579
_oxdiff_exptl_absorpt_empirical_full_min 0.467
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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
W1 W 0.41484(5) 0.750000 0.70115(2) 0.03260(15) Uani 1 2 d S T P . .
Se1 Se 0.64901(15) 0.750000 0.81781(6) 0.0457(3) Uani 1 2 d S T P . .
Cl1 Cl 0.5970(2) 0.5397(3) 0.61587(10) 0.0410(4) Uani 1 1 d . . . . .
Cl2 Cl 0.1555(3) 0.5463(2) 0.75162(10) 0.0392(4) Uani 1 1 d . . . . .
N1 N 0.1791(12) 0.750000 0.5766(5) 0.040(2) Uani 1 2 d S T P . .
C1 C 0.0632(13) 0.750000 0.5149(6) 0.0341(19) Uani 1 2 d S T P . .
C2 C -0.0793(15) 0.750000 0.4370(6) 0.039(2) Uani 1 2 d S T P . .
H2A H -0.109141 0.867862 0.418593 0.058 Uiso 0.5 1 calc R U P A -1
H2B H -0.223578 0.693049 0.451990 0.058 Uiso 0.5 1 calc R U P A -1
H2C H -0.002145 0.689089 0.387367 0.058 Uiso 0.5 1 calc R U P A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
Se1 W1 Cl1 97.83(4) . . ?
Se1 W1 Cl1 97.83(4) . 4_575 ?
Se1 W1 Cl2 99.32(4) . . ?
Se1 W1 Cl2 99.32(4) . 4_575 ?
Se1 W1 N1 178.40(18) . . ?
Cl1 W1 Cl1 90.30(9) . 4_575 ?
Cl1 W1 N1 81.05(13) 4_575 . ?
Cl1 W1 N1 81.05(13) . . ?
Cl2 W1 Cl1 162.78(6) . 4_575 ?
Cl2 W1 Cl1 162.78(6) 4_575 . ?
Cl2 W1 Cl1 88.83(6) . . ?
Cl2 W1 Cl1 88.83(6) 4_575 4_575 ?
Cl2 W1 Cl2 86.95(9) 4_575 . ?
Cl2 W1 N1 81.83(14) . . ?
Cl2 W1 N1 81.83(14) 4_575 . ?
C1 N1 W1 179.8(7) . . ?
N1 C1 C2 179.3(9) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
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
W1 Se1 2.2312(9) . ?
W1 Cl1 2.3248(17) 4_575 ?
W1 Cl1 2.3248(17) . ?
W1 Cl2 2.3208(17) 4_575 ?
W1 Cl2 2.3208(17) . ?
W1 N1 2.330(7) . ?
N1 C1 1.151(12) . ?
C1 C2 1.440(13) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.289 -0.456 0.000 252.1 106.0 '2.5 C6H6'
