Construction of 1,3,4-oxadiazolines bearing CF3-quaternary centers via amino-assisted [3 + 2] cycloadditions
Zhu, Yannan; Bo, Fang; Wang, Xuying; Jiang, Qianxi; Li, Qiuyun; Han, Zhongfei; Wang, Yi-Ning; Qi, Gang; Organic & Biomolecular Chemistry 22 (2024) 1391–1394; doi:10.1039/D3OB02096G

data_7159837
_publ_section_title
;
 Construction of 1,3,4-oxadiazolines bearing CF3-quaternary centers via
 amino-assisted [3 + 2] cycloadditions
;
_journal_issue                   7
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              1391
_journal_page_last               1394
_journal_paper_doi               10.1039/D3OB02096G
_journal_volume                  22
_journal_year                    2024
_chemical_formula_sum            'C29 H24 F3 N3 O3 S'
_chemical_formula_weight         551.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc27yqmk
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-05-16 deposited with the CCDC.	2024-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                100.472(3)
_cell_angle_beta                 92.038(3)
_cell_angle_gamma                92.699(3)
_cell_formula_units_Z            4
_cell_length_a                   9.2123(3)
_cell_length_b                   13.9474(6)
_cell_length_c                   20.6800(7)
_cell_measurement_temperature    113(2)
_cell_volume                     2607.33(17)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.892
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29273
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.165
_diffrn_reflns_theta_min         1.940
_exptl_absorpt_coefficient_mu    0.183
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.0083(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         15051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0624
_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^)+(0.0876P)^2^+0.4999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10893
_reflns_number_total             15051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob02096g2.cif
_cod_data_source_block           r20210513b
_cod_database_code               7159837
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              7352