Photo-Lewis Acid Generator Based on Radical-Free 6π Photo-Cyclization Reaction.
Mizutsu, Ryo; Asato, Ryosuke; Martin, Colin J.; Yamada, Mihoko; Nishikawa, Yoshiko; Katao, Shohei; Yamada, Miku; Nakashima, Takuya; Kawai, Tsuyoshi; Journal of the American Chemical Society 141 (2019) 20043–20047; doi:10.1021/jacs.9b11821

data_4133780
_publ_section_title
;
 Photo-Lewis Acid Generator Based on Radical-Free 6\p Photo-Cyclization
 Reaction.
;
_journal_issue                   51
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20043
_journal_page_last               20047
_journal_paper_doi               10.1021/jacs.9b11821
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C31 H21 F3 O3 S3'
_chemical_formula_sum            'C31 H21 F3 O3 S3'
_chemical_formula_weight         594.68
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 102.722(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   16.3908(3)
_cell_length_b                   8.62288(17)
_cell_length_c                   19.0929(4)
_cell_measurement_reflns_used    26464
_cell_measurement_temperature    103
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.19
_cell_volume                     2632.26(12)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      103
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35733
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         2.548
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224.00
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     363
_refine_ls_number_reflns         4822
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0348P)^2^+2.0393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4038
_reflns_number_total             4822
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja9b11821_si_002.cif
_cod_data_source_block           1O
_cod_depositor_comments
'Adding full bibliography for 4133779--4133780.cif.'
_cod_original_cell_volume        2632.27(12)
_cod_database_code               4133780
_shelx_res_checksum              88679
_shelx_hkl_checksum              658