In(OTf)3-catalyzed intramolecular hydroarylation of α-phenylallyl β-ketosulfones – synthesis of sulfonyl 1-benzosuberones and 1-tetralones
Chang, Meng-Yang; Lai, Kai-Xiang; Chang, Yu-Lun; RSC Advances 10 (2020) 18231–18244; doi:10.1039/D0RA01962C

data_7240514
_publ_section_title
;
 In(OTf)3-catalyzed intramolecular hydroarylation of \a-phenylallyl
 \b-ketosulfones -- synthesis of sulfonyl 1-benzosuberones and
 1-tetralones
;
_journal_issue                   31
_journal_name_full               'RSC Advances'
_journal_page_first              18231
_journal_page_last               18244
_journal_paper_doi               10.1039/D0RA01962C
_journal_volume                  10
_journal_year                    2020
_chemical_formula_sum            'C26 H26 O5 S'
_chemical_formula_weight         450.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2019-05-13 deposited with the CCDC.	2020-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.713(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4857(9)
_cell_length_b                   9.6877(5)
_cell_length_c                   17.1467(9)
_cell_measurement_reflns_used    5979
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3693
_cell_measurement_theta_min      2.3757
_cell_volume                     2547.4(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0316
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22006
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.419
_diffrn_reflns_theta_min         2.376
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabullar
_exptl_crystal_F_000             952
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_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.372
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+1.3705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4180
_reflns_number_total             5222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra01962c2.cif
_cod_data_source_block           190317lt_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7240513--7240516.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7240514
_shelxl_version_number           2014/6
_shelx_res_checksum              21210
_shelx_fab_checksum              13087