Synthesis of Dihydropyrroles from In Situ-Generated Zwitterions via Rh2(adc)4/TBAI Dual Catalysis
Xu, Huaping; Kong, Xiaoyu; Cen, Mengjie; Xu, Ze-Feng; Duan, Shengguo; Li, Chuan-Ying; Chemical Communications  (2022) –; doi:10.1039/D2CC04674A

data_7130841
_publ_section_title
;
 Synthesis of Dihydropyrroles from In Situ-Generated Zwitterions via
 Rh2(adc)4/TBAI Dual Catalysis
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04674A
_journal_year                    2022
_chemical_formula_sum            'C24 H23 N O4 S2'
_chemical_formula_weight         453.55
_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
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-07-17 deposited with the CCDC.	2022-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.281(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.278(6)
_cell_length_b                   12.642(7)
_cell_length_c                   16.165(9)
_cell_measurement_reflns_used    2849
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.87
_cell_measurement_theta_min      2.46
_cell_volume                     2234(2)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13745
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.579
_diffrn_reflns_theta_min         1.992
_exptl_absorpt_coefficient_mu    0.269
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0750P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3321
_reflns_number_total             5109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04674a2.cif
_cod_data_source_block           HZ_15_0m_a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7130841
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.971
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              21131
_shelx_hkl_checksum              17184