Ketosulfonylmethylenation and Sulfonylethyleneation of Imidazoheterocycles with Dimethylformamide as Methylene Source
Guo, Tao; Hu, Penghua; Liu, Yu; Zhang, Panke; Zhao, Yun-Hui; Zhu, Congjun; Chemical Communications  (2023) –; doi:10.1039/D3CC03850E

data_7132154
_publ_section_title
;
 Ketosulfonylmethylenation and Sulfonylethyleneation of
 Imidazoheterocycles with Dimethylformamide as Methylene Source
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03850E
_journal_year                    2023
_chemical_formula_sum            'C29 H23 N3 O5 S'
_chemical_formula_weight         525.56
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-06-22 deposited with the CCDC.	2023-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                79.211(2)
_cell_angle_beta                 77.257(2)
_cell_angle_gamma                80.078(2)
_cell_formula_units_Z            2
_cell_length_a                   7.1153(4)
_cell_length_b                   12.1904(7)
_cell_length_c                   14.8931(8)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.84
_cell_volume                     1226.09(12)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31127
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.550
_diffrn_reflns_theta_min         2.391
_exptl_absorpt_coefficient_mu    0.180
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0647P)^2^+0.1359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4432
_reflns_number_total             5555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03850e2.cif
_cod_data_source_block           mo_20220910ge_0m_a
_cod_database_code               7132154
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.956
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              97332
_shelx_hkl_checksum              32001