A comprehensive characterization of thiophosgene in the solid state
Tambornino, Frank; Ringelband, Sven; Parker, Stewart F.; Howard, Christopher M.; Fortes, Dominic; Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials 80 (2024) 495–503; doi:10.1107/S2052520624007583

data_2312629
_publ_section_title
;
 A comprehensive characterization of thiophosgene in the solid state
;
_journal_issue                   5
_journal_name_full
'Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials'
_journal_page_first              495
_journal_page_last               503
_journal_paper_doi               10.1107/S2052520624007583
_journal_volume                  80
_journal_year                    2024
_chemical_compound_source        'Sigma Aldrich 115150'
_chemical_formula_moiety         'C Cl2 S'
_chemical_formula_sum            'C Cl2 S'
_chemical_formula_weight         114.97
_chemical_melting_point          234
_chemical_name_common            thiophosgene
_chemical_name_systematic        'carbonothioyl dichloride'
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_audit_creation_date             2024-04-10T20:00
_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_update_record
' 2024-04-10T20:00  Initial CIF as created by GSAS2CIF'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                120.0
_cell_formula_units_Z            2
_cell_length_a                   5.949930(20)
_cell_length_b                   5.94993
_cell_length_c                   6.248669(27)
_cell_measurement_temperature    40
_cell_volume                     191.5763(10)
_computing_data_collection       'HRPD DAE3, IBEX'
_computing_data_reduction
'Mantid (Arnold <i>et al</i>., 2014: Mantid, 2013)'
_computing_structure_refinement  GSAS
_diffrn_ambient_temperature      40
_diffrn_measurement_device_type
'HRPD, High Resolution Neutron Powder Diffractometer'
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           white-beam
_diffrn_radiation_wavelength     0.5-8.2
_diffrn_source                   'spallation source'
_diffrn_source_type              'ISIS TS1 beamline HRPD'
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_process_details
;   GSAS Absorption/surface roughness correction: function number 0
 No correction is applied.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.9931
_exptl_crystal_density_method    'not measured'
_exptl_crystal_recrystallization_method 'Immersion in liquid nitrogen'
_pd_block_id                     2024-04-10T20:00|40K|Chris|HRPD
_pd_calc_method                  'Rietveld Refinement'
_pd_char_particle_morphology     'coarse powder'
_pd_instr_dist_spec/detc         965
_pd_instr_dist_src/spec          95000
_pd_instr_location
;
High Resolution Powder Diffractometer, ISIS neutron spallation source,
 Rutherford Appleton Laboratory, Oxfordshire, U.K.
;
_pd_meas_2theta_fixed            168.33
_pd_meas_number_of_points        4610
_pd_meas_scan_method             tof
_pd_phase_name                   thiophosgene
_pd_proc_info_data_reduction
'Incident-beam normalisation and instrumental efficiency correction'
_pd_proc_info_datetime           2024-04-10T20:00:45
_pd_proc_info_excluded_regions
;
;
_pd_proc_ls_background_function
;   GSAS Background function number 1 with  6 terms.
 Shifted Chebyshev function of 1st kind
      1:   0.961880     2:  -0.471000     3:   0.151395     4:   1.346550E-02
      5:   2.534970E-02 6:   3.436710E-02
;
_pd_proc_ls_peak_cutoff          0.00050
_pd_proc_ls_profile_function
;
 TOF Profile function number 3 with  21 terms
 Profile coefficients for exponential pseudovoigt
  convolution Von Dreele, 1990 (unpublished)
 #1 (alp  ) =   3.3265 #2 (bet-0) = 0.028841 #3 (bet-1) = 0.010867
 #4 (sig-0) =      0.0 #5 (sig-1) =    458.6 #6 (sig-2) =    -23.1
 #7 (gam-0) =     0.00 #8 (gam-1) =    30.18 #9 (gam-2) =     0.00
 #10(gsf  ) =     0.00 #11(g1ec ) =     0.00 #12(g2ec ) =     0.00
 #13(rstr ) =    0.000 #14(rsta ) =    0.000 #15(rsca ) =    0.000
 #16(L11)   =    0.000 #17(L22)   =    0.000 #18(L33)   =    0.000
 #19(L12)   =    0.000 #20(L13)   =    0.000 #21(L23)   =    0.000
 Peak tails are ignored  where the intensity is below 0.0005 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_prof_R_factor        0.1190
_pd_proc_ls_prof_wR_expected     0.0819
_pd_proc_ls_prof_wR_factor       0.0807
_pd_proc_number_of_points        4610
_pd_spec_mounting
;
Aluminium-framed slab can with vanadium windows, shielded with Gd foil
;
_pd_spec_mount_mode              reflection
_pd_spec_size_axial              18
_pd_spec_size_equat              23
_pd_spec_size_thick              10
_refine_ls_goodness_of_fit_all   0.99
_refine_ls_matrix_type           full
_refine_ls_number_parameters     20
_refine_ls_number_restraints     0
_refine_ls_R_Fsqd_factor         0.06339
_refine_ls_shift/su_max          0.02
_refine_ls_shift/su_mean         0.00
_reflns_d_resolution_high        0.650
_reflns_d_resolution_low         2.576
_reflns_limit_h_max              20
_reflns_limit_h_min              0
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_total             258
_cod_data_source_file            dq5061.cif
_cod_data_source_block           40K_publ
_cod_depositor_comments
'Adding full bibliography for 2312626--2312648.cif.'
_cod_original_cell_volume        191.5760(10)
_cod_original_sg_symbol_Hall     -P_6c
_cod_database_code               2312629
_gsas_exptl_extinct_corr_t_min   1.00000
_gsas_exptl_extinct_corr_t_max   1.00000