Tungsten disulfide thin films <i>via</i> electrodeposition from a single source precursor.
Thomas, Shibin; Greenacre, Victoria K.; Smith, Danielle E.; Noori, Yasir J.; Abdelazim, Nema M.; Hector, Andrew L.; de Groot, C. H. Kees; Levason, William; Bartlett, Philip N.; Reid, Gillian; Chemical communications (Cambridge, England) 57 (2021) 10194–10197; doi:10.1039/d1cc03297f

data_7128938
_publ_section_title
;
 Tungsten disulfide thin films <i>via</i> electrodeposition from a single
 source precursor.
;
_journal_issue                   79
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10194
_journal_page_last               10197
_journal_paper_doi               10.1039/d1cc03297f
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'S4 W, 2(C16 H36 N)'
_chemical_formula_sum            'C32 H72 N2 S4 W'
_chemical_formula_weight         797.00
_chemical_name_systematic        (C16H72N2)WS4
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-17 deposited with the CCDC.	2021-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   35.5582(6)
_cell_length_b                   28.7216(5)
_cell_length_c                   15.5658(4)
_cell_measurement_reflns_used    13763
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.5820
_cell_measurement_theta_min      3.1800
_cell_volume                     15897.2(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.906
_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    -49.00  74.00   1.00    1.00    --  -15.80  60.00 150.00  123
  2  \w   -105.00 -24.00   1.00    1.00    --  -15.80 -57.00-150.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0037576000
_diffrn_orient_matrix_UB_12      -0.0013090000
_diffrn_orient_matrix_UB_13      -0.0446808000
_diffrn_orient_matrix_UB_21      -0.0009743000
_diffrn_orient_matrix_UB_22      -0.0246439000
_diffrn_orient_matrix_UB_23      0.0020333000
_diffrn_orient_matrix_UB_31      -0.0195697000
_diffrn_orient_matrix_UB_32      0.0009762000
_diffrn_orient_matrix_UB_33      -0.0086482000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23617
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.001
_diffrn_reflns_theta_min         2.977
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       block
_exptl_crystal_F_000             6656
_exptl_crystal_preparation       'Slow evporation from water'
_exptl_crystal_recrystallization_method 'Slow evaporation from water'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         2.810
_refine_diff_density_min         -2.964
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details
;
 Flack x determined using 4164 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         10952
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0978P)^2^+3.1336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1446
_reflns_Friedel_coverage         0.848
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.821
_reflns_number_gt                10148
_reflns_number_total             10952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03297f2.cif
_cod_data_source_block           tba2ws4
_cod_depositor_comments          'Adding full bibliography for 7128938.cif.'
_cod_database_code               7128938
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C32H72N2WS4
_chemical_oxdiff_usercomment     'Yellow Block'
_shelx_estimated_absorpt_t_max   0.367
_shelx_estimated_absorpt_t_min   0.303
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C16) = Uanis(C20)
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C23(H23A,H23B), C2(H2A,H2B), C29(H29A,H29B), C26(H26A,H26B),
 C17(H17A,H17B), C3(H3A,H3B), C9(H9A,H9B), C1(H1A,H1B), C18(H18A,H18B),
 C13(H13A,H13B), C21(H21A,H21B), C10(H10A,H10B), C19(H19A,H19B), C22(H22A,H22B),
  C6(H6A,H6B), C31(H31A,H31B), C11(H11A,H11B), C5(H5A,H5B), C7(H7A,H7B),
 C14(H14A,H14B), C30(H30A,H30B), C15(H15A,H15B), C27(H27A,H27B)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C32(H32A,H32B,H32C), C24(H24A,H24B,
 H24C), C28(H28A,H28B,H28C), C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C16(H16A,H16B,
 H16C)
;
_shelx_res_checksum              41395
_shelx_hkl_checksum              60437
_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 2.851
_oxdiff_exptl_absorpt_empirical_full_min 0.327