Access to benzo-fused nine-membered heterocyclic alkenes with a trifluoromethyl carbinol moiety <i>via</i> a double decarboxylative formal ring-expansion process under palladium catalysis.
Das, Pulakesh; Gondo, Satoshi; Nagender, Punna; Uno, Hiroto; Tokunaga, Etsuko; Shibata, Norio; Chemical science 9 (2018) 3276–3281; doi:10.1039/c7sc05447e

data_1548997
_publ_section_title
;
 Access to benzo-fused nine-membered heterocyclic alkenes with a
 trifluoromethyl carbinol moiety <i>via</i> a double decarboxylative
 formal ring-expansion process under palladium catalysis.
;
_journal_issue                   13
_journal_name_full               'Chemical science'
_journal_page_first              3276
_journal_page_last               3281
_journal_paper_doi               10.1039/c7sc05447e
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C25 H22 F3 N O3 S'
_chemical_formula_sum            'C25 H22 F3 N O3 S'
_chemical_formula_weight         473.51
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2017-09-16 deposited with the CCDC.
2018-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   16.8152(3)
_cell_length_b                   15.0512(3)
_cell_length_c                   17.5637(4)
_cell_measurement_reflns_used    34842
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.01
_cell_volume                     4445.18(16)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0274
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40949
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1968.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.440
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5057
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0607P)^2^+1.7845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1214
_reflns_number_gt                4162
_reflns_number_total             5057
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c7sc05447e2.cif
_cod_data_source_block           170512plakesh1
_cod_depositor_comments
'Adding full bibliography for 1548996--1548999.cif.'
_cod_database_code               1548997