Construction of sterically congested oxindole derivatives via visible-light-induced radical-coupling
Shen, Yanling; Lei, Ning; Lu, Cong; Xi, Dailin; Geng, Xinxin; Tao, Pan; Su, Zhishan; Zheng, Ke; Chemical Science  (2021) –; doi:10.1039/D1SC05273J

data_1565316
_publ_section_title
;
 Construction of sterically congested oxindole derivatives via
 visible-light-induced radical-coupling
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC05273J
_journal_year                    2021
_chemical_formula_moiety         'C30 H23 Cl F9 N O2'
_chemical_formula_sum            'C30 H23 Cl F9 N O2'
_chemical_formula_weight         635.94
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-07-14 deposited with the CCDC.	2021-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                114.164(2)
_cell_angle_beta                 91.725(2)
_cell_angle_gamma                103.585(2)
_cell_formula_units_Z            4
_cell_length_a                   12.6563(9)
_cell_length_b                   14.4425(11)
_cell_length_c                   16.7878(12)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.47
_cell_volume                     2693.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43802
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.423
_diffrn_reflns_theta_min         2.470
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  0.9836
_exptl_absorpt_correction_T_min  0.9220
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM, PE'
_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.302
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         9906
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0395P)^2^+2.7195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7986
_reflns_number_total             9906
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05273j2.cif
_cod_data_source_block           zhk009
_cod_depositor_comments
;

2022-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C60 H46 Cl2 F18 N2 O4'
_cod_original_formula_weight         1271.89
_cod_original_formula_moiety         '2(C30 H23 Cl F9 N O2)'
_cod_original_formula_units_Z            2
_cod_database_code               1565316
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.926
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              28305
_shelx_hkl_checksum              34701