‘Photo-Catalyzed Acetoxysulfoximination of Styrene with Sulfoximidoyl Thianthrenium Salt
Yang, Yu-Ming; Zhang, Cairong; Yang, Hanlun; Tang, Zhen-Yu; Chemical Communications  (2022) –; doi:10.1039/D2CC02542F

data_7130312
_publ_section_title
;
 &#x2018;Photo-Catalyzed Acetoxysulfoximination of Styrene with
 Sulfoximidoyl Thianthrenium Salt
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02542F
_journal_year                    2022
_chemical_absolute_configuration S
_chemical_formula_moiety         '2(C19 H16 N O S3), B F4'
_chemical_formula_sum            'C38 H32 B F4 N2 O2 S6'
_chemical_formula_weight         827.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-16 deposited with the CCDC.	2022-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.272(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3475(4)
_cell_length_b                   18.7873(8)
_cell_length_c                   13.0343(6)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.648
_cell_measurement_theta_min      2.938
_cell_volume                     2022.86(16)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32222
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         2.938
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0666 before and 0.0549 after correction.
The Ratio of minimum to maximum transmission is 0.9150.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.173
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 2671 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.62(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         9274
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.0539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                6991
_reflns_number_total             9274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02542f2.cif
_cod_data_source_block           111_sq
_cod_database_code               7130312
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.905
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C31(H31), C30(H30), C20(H20), C33(H33), C28(H28), C37(H37), C34(H34),
 C29(H29), C21(H21), C19(H19), C1(H1), C3(H3), C9(H9), C15(H15), C8(H8),
 C36(H36), C4(H4), C35(H35), C11(H11), C22(H22), C10(H10), C23(H23), C17(H17),
 C16(H16), C2(H2), C18(H18)
2.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              14370
_shelx_hkl_checksum              58896
_shelx_fab_checksum              44951
_olex2_submission_special_instructions 'No special instructions were received'