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_7160684
_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         'C21 H24 Br N O3 S2'
_chemical_formula_sum            'C21 H24 Br N O3 S2'
_chemical_formula_weight         482.43
_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
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2mdqnf
_audit_creation_date             2025-02-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-19 deposited with the CCDC.	2025-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.645(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1305(18)
_cell_length_b                   17.689(2)
_cell_length_c                   12.4682(19)
_cell_measurement_reflns_used    3260
_cell_measurement_temperature    223.15
_cell_measurement_theta_max      23.7340
_cell_measurement_theta_min      2.0700
_cell_volume                     2265.6(6)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      223.15
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.8644
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0964
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.8644
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13874
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.8644
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         30.67
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    2.019
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72062
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             992.0
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.2994
_refine_diff_density_min         -1.2995
_refine_diff_density_rms         0.2237
_refine_ls_d_res_high            0.6968
_refine_ls_d_res_low             9.7523
_refine_ls_goodness_of_fit_ref   1.0382
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    38
_refine_ls_number_parameters     258
_refine_ls_number_reflns         6997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0382
_refine_ls_R_factor_all          0.1436
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          -0.0006
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.3348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1503
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -15
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              -8
_reflns_number_gt                2843
_reflns_number_total             6045
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ob00951k2.cif
_cod_data_source_block           g250219b_auto
_cod_depositor_comments
'Adding full bibliography for 7160684--7160685.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7160684
_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:
 C8(H8), C7(H7), C11(H11), C10(H10), C17(H17), C16(H16), C14(H14), C13(H13),
 N1(H1)
2.b Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C5(H5a,H5b,H5c), C19(H19a,H19b,H19c), C20(H20a,H20b,
 H20c), C1(H1a,H1b,H1c)
;
_olex2_submission_special_instructions 'No special instructions were received'