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_2312626
_publ_section_title
;
 A comprehensive characterization of thiophosgene in the solid state
;
_journal_coeditor_code           DQ5061SUP1
_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_formula_moiety         '2(C0.5 Cl S0.5)'
_chemical_formula_sum            'C Cl2 S'
_chemical_formula_weight         114.97
_chemical_name_systematic        Thiophosgene
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_audit_creation_date             2023-11-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   6.0132(6)
_cell_length_b                   6.0132(6)
_cell_length_c                   6.5130(9)
_cell_measurement_reflns_used    1635
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.74
_cell_measurement_theta_min      8.51
_cell_volume                     203.95(4)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.88, Darmstadt 2019
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'hybrid photon-counting area detector'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS3 R 300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
 1009 frames, detector distance = 40 mm
;
_diffrn_measurement_device       '4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1137
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         68.758
_diffrn_reflns_theta_min         8.513
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_target            Cu
_diffrn_source_type              'XENOCS GENIX 3D CU HIGH FLUX'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    17.200
_exptl_absorpt_correction_T_max  0.1713
_exptl_absorpt_correction_T_min  0.0115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             112
_exptl_crystal_preparation       'Grown by slow cooling in 0.3 mm kapillary'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.19(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     10
_refine_ls_number_reflns         143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0882P)^2^+0.0819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1414
_reflns_d_resolution_high        0.827
_reflns_d_resolution_low         6.513
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              6
_reflns_limit_h_min              -6
_reflns_limit_k_max              7
_reflns_limit_k_min              -2
_reflns_limit_l_max              7
_reflns_limit_l_min              -7
_reflns_number_gt                130
_reflns_number_total             143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dq5061.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 2312626--2312648.cif.'
_cod_original_cell_volume        203.95(5)
_cod_database_code               2312626
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.079
_shelx_estimated_absorpt_t_min   0.079
_olex2_refinement_description
;
1. Shared sites
{Cl1, S1}
2. Uiso/Uaniso restraints and constraints
Uanis(Cl1) = Uanis(S1)
3. Others
 Fixed Sof: Cl1(0.333333) S1(0.16666)
;
_shelx_res_checksum              51507
_shelx_hkl_checksum              89254
_olex2_submission_special_instructions 'No special instructions were received'