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_1548998
_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 O4 S'
_chemical_formula_sum            'C25 H22 F3 N O4 S'
_chemical_formula_weight         489.51
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2017-12-03 deposited with the CCDC.
2018-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.3044(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   16.8716(4)
_cell_length_b                   7.8975(2)
_cell_length_c                   16.7075(5)
_cell_measurement_reflns_used    6414
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.10
_cell_volume                     2226.13(10)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16650
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.360
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5072
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0505P)^2^+0.7087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                4728
_reflns_number_total             5072
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c7sc05447e2.cif
_cod_data_source_block           20170926-sample2
_cod_depositor_comments
'Adding full bibliography for 1548996--1548999.cif.'
_cod_original_cell_volume        2226.13(11)
_cod_database_code               1548998