Tf<sub>2</sub>O-activated modular assembly of tetrasubstituted alkenes.
Ye, Weijian; Chen, Yuqi; Liu, Xiangning; Huang, Yiran; Zhang, Yuanyuan; Wan, Xiaobing; Organic & biomolecular chemistry 23 (2025) 8181–8185; doi:10.1039/d5ob00951k

data_7160685
_publ_section_title
;
 Tf<sub>2</sub>O-activated modular assembly of tetrasubstituted alkenes.
;
_journal_issue                   36
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8181
_journal_page_last               8185
_journal_paper_doi               10.1039/d5ob00951k
_journal_volume                  23
_journal_year                    2025
_chemical_formula_moiety         'C18 H18 Br N O3 S2'
_chemical_formula_sum            'C18 H18 Br N O3 S2'
_chemical_formula_weight         440.35
_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'
_symmetry_Int_Tables_number      14
_audit_block_doi                 10.5517/ccdc.csd.cc2n57fj
_audit_creation_date             2025-04-30
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-04-30 deposited with the CCDC.	2025-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.006(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2624(16)
_cell_length_b                   10.7737(17)
_cell_length_c                   14.804(3)
_cell_measurement_reflns_used    2709
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      24.7340
_cell_measurement_theta_min      2.2540
_cell_volume                     1941.2(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      223.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4471
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.8691
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -88.00 -57.00   1.00   27.00    --  -13.65 178.00-180.00   31
  2  \w    -81.00 -14.00   1.00   27.00    --  -13.65   0.00   0.00   67
  3  \w      6.00  69.00   1.00   27.00    --  -13.65   0.00   0.00   63
  4  \w    -20.00  21.00   1.00   27.00    --  -13.65  37.00-120.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0447787000
_diffrn_orient_matrix_UB_12      0.0319930000
_diffrn_orient_matrix_UB_13      0.0244688000
_diffrn_orient_matrix_UB_21      -0.0018991000
_diffrn_orient_matrix_UB_22      0.0447017000
_diffrn_orient_matrix_UB_23      -0.0353458000
_diffrn_orient_matrix_UB_31      -0.0372907000
_diffrn_orient_matrix_UB_32      0.0362554000
_diffrn_orient_matrix_UB_33      0.0218932000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_Laue_measured_fraction_full 0.9997
_diffrn_reflns_Laue_measured_fraction_max 0.8691
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11052
_diffrn_reflns_point_group_measured_fraction_full 0.9997
_diffrn_reflns_point_group_measured_fraction_max 0.8691
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         30.48
_diffrn_reflns_theta_min         2.30
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       block
_exptl_crystal_F_000             896.0
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.7576
_refine_diff_density_min         -1.3492
_refine_diff_density_rms         0.1543
_refine_ls_d_res_high            0.7007
_refine_ls_d_res_low             8.8573
_refine_ls_goodness_of_fit_ref   0.9194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    30
_refine_ls_number_parameters     229
_refine_ls_number_reflns         5137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9194
_refine_ls_R_factor_all          0.1342
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.2056
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -17
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -11
_reflns_number_gt                2367
_reflns_number_total             5911
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ob00951k2.cif
_cod_data_source_block           g250429g_auto
_cod_depositor_comments
'Adding full bibliography for 7160684--7160685.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7160685
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C4(H4), C6(H6), C7(H7), C18(H18), C3(H3), C16(H16), C17(H17), C15(H15)
2.b Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C12(H12a,H12b,H12c), C1(H1a,H1b,H1c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.249
_oxdiff_exptl_absorpt_empirical_full_min 0.819