Carbamothioate-mediated Selectfluor™ oxidation for the synthesis of benzenesulfonyl fluorides in chalcone derivatives
Jiang, Boye; Zhang, Juan; Wang, Boning; Zhou, Airui; Zou, Yan; Meng, Qingguo; Zhao, Qingjie; Chai, Xiaoyun; Gai, Conghao; RSC Advances 15 (2025) 22018–22022; doi:10.1039/D5RA03427B

data_7250601
_publ_section_title
;
 Carbamothioate-mediated Selectfluor&#x2122; oxidation for the synthesis
 of benzenesulfonyl fluorides in chalcone derivatives
;
_journal_issue                   27
_journal_name_full               'RSC Advances'
_journal_page_first              22018
_journal_page_last               22022
_journal_paper_doi               10.1039/D5RA03427B
_journal_volume                  15
_journal_year                    2025
_chemical_formula_sum            'C17 H12 F2 O4 S'
_chemical_formula_weight         350.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2025-03-10 deposited with the CCDC.	2025-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.279(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8190(8)
_cell_length_b                   14.7869(15)
_cell_length_c                   14.7647(15)
_cell_measurement_reflns_used    9208
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      66.8173
_cell_measurement_theta_min      4.2320
_cell_volume                     1488.4(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1365)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_diffrn_ambient_temperature      150.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker D8 VENTURE DUO PHOTON III'
_diffrn_radiation_monochromator  'Helios MX Multilayer Optic'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16460
_diffrn_reflns_theta_full        66.96
_diffrn_reflns_theta_max         66.96
_diffrn_reflns_theta_min         4.23
_diffrn_source                   'Microfocus sealed tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.06
_diffrn_source_type              'Incoatec Ius 3.0'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.343
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.518
_refine_diff_density_min         -0.564
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.1209
_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^)+(0.1940P)^2^+11.1720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3603
_refine_ls_wR_factor_ref         0.3626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2316
_reflns_number_total             2595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra03427b2.cif
_cod_data_source_block           250116b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7250601
_shelx_res_checksum              28487