A facile access to <i>N</i>-sulfonylthioimidates and their use for the transformation to 3,4-dihydroquinazolines.
Wu, Jia-Yu; Liao, Wei-Jr; Lin, Xiu-Yi; Liang, Chien-Fu; Organic & biomolecular chemistry 18 (2020) 8881–8885; doi:10.1039/d0ob01963a

data_7157799
_publ_section_title
;
 A facile access to <i>N</i>-sulfonylthioimidates and their use for the
 transformation to 3,4-dihydroquinazolines.
;
_journal_issue                   43
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8881
_journal_page_last               8885
_journal_paper_doi               10.1039/d0ob01963a
_journal_volume                  18
_journal_year                    2020
_chemical_formula_moiety         'C22 H21 N O2 S2'
_chemical_formula_sum            'C22 H21 N O2 S2'
_chemical_formula_weight         395.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-06-28
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2020-10-13 deposited with the CCDC.	2020-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.189(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0525(5)
_cell_length_b                   15.8806(10)
_cell_length_c                   15.2504(10)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.383
_cell_measurement_theta_min      3.062
_cell_volume                     1945.0(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29071
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         26.402
_diffrn_reflns_theta_min         2.894
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0793 before and 0.0392 after correction.
The Ratio of minimum to maximum transmission is 0.9153.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+1.1647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3597
_reflns_number_total             3899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ob01963a2.cif
_cod_data_source_block           132741_0m_pl
_cod_database_code               7157799
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00S(H00A,H00B), C00V(H00C,H00D)
2.b Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00M(H00M), C00N(H00N), C00O(H00O), C00U(H00U), C010(H010),
 C011(H011), C014(H014), C017(H017), C019(H019), C01A(H01A), C01C(H01C),
 C01D(H01D), C01F(H01F)
2.c Idealised Me refined as rotating group:
 C01I(H01B,H01E,H01G)
;
_shelx_res_checksum              76300
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'