An advanced approach combining solid-state NMR with powder diffraction applied to newly synthesized iso-thio-uronium salts.
Rohlíček, Jan; Eigner, Václav; Czernek, Jiří; Brus, Jiří; Journal of applied crystallography 58 (2025) 321–332; doi:10.1107/S1600576724012378

data_2300746
_publ_section_title
;
 An advanced approach combining solid-state NMR with powder diffraction
 applied to newly synthesized iso-thio-uronium salts.
;
_journal_coeditor_code           UI5023
_journal_issue                   'Pt 2'
_journal_name_full               'Journal of applied crystallography'
_journal_page_first              321
_journal_page_last               332
_journal_paper_doi               10.1107/S1600576724012378
_journal_volume                  58
_journal_year                    2025
_chemical_formula_moiety         'C10 H13 N2 S, B F4'
_chemical_formula_sum            'C10 H13 B F4 N2 S'
_chemical_formula_weight         280.10
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 91.387(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.6817(4)
_cell_length_b                   7.4235(5)
_cell_length_c                   29.057(2)
_cell_measurement_reflns_used    1752
_cell_measurement_temperature    95
_cell_measurement_theta_max      74.10
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_cell_volume                     1225.21(15)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      95
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
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_diffrn_reflns_av_unetI/netI     0.053
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_diffrn_reflns_limit_k_min       -6
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_diffrn_reflns_limit_l_min       -34
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_diffrn_reflns_theta_min         3.043
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_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colourless
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_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.0002406
_refine_ls_shift/su_mean         0.0000140
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +14.05P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
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_reflns_limit_h_max              6
_reflns_limit_h_min              -6
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                2099
_reflns_number_total             2368
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.66
_oxford_diffrn_Wilson_scale      0.02
_oxford_refine_ls_r_factor_ref   0.0834
_oxford_refine_ls_scale          7.3(5)
_oxford_reflns_number_all        2368
_cod_data_source_file            ui5023.cif
_cod_data_source_block           1BF4_VE_2A
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 2300745--2300749.cif.
;
_cod_original_cell_volume        1225.20(14)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               2300746
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0834
_oxford_refine_ls_wr_factor_all  0.2236