CO2-facilitated radical sequential (3 + 2) annulation of 1,6-enynes via cooperation of sulfinate catalysis and photocatalysis
Gao, Yuzhen; Liu, Siqing; Su, Weiping; Green Chemistry 25 (2023) 7335–7343; doi:10.1039/D3GC02326E

data_7247198
_publ_section_title
;
 CO2-facilitated radical sequential (3 + 2) annulation of 1,6-enynes via
 cooperation of sulfinate catalysis and photocatalysis
;
_journal_issue                   18
_journal_name_full               'Green Chemistry'
_journal_page_first              7335
_journal_page_last               7343
_journal_paper_doi               10.1039/D3GC02326E
_journal_volume                  25
_journal_year                    2023
_chemical_formula_sum            'C30 H23 N O3 S'
_chemical_formula_weight         477.55
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2023-03-16 deposited with the CCDC.	2023-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                69.743(4)
_cell_angle_beta                 74.537(4)
_cell_angle_gamma                81.231(4)
_cell_formula_units_Z            2
_cell_length_a                   8.3269(8)
_cell_length_b                   11.8421(12)
_cell_length_c                   13.6257(14)
_cell_measurement_reflns_used    7423
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.83
_cell_volume                     1212.2(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1690
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49873
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.1450
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.2314
_reflns_number_gt                3277
_reflns_number_total             6013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3gc02326e2.cif
_cod_data_source_block           gao
_cod_depositor_comments
'Adding full bibliography for 7247197--7247199.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7247198