Aromatization-Driven Cascade [1,5]-Hydride Transfer/Spirocyclization Promoted by Fluorinated Alcohols.
Lv, Xintong; Hu, Fangzhi; Duan, Kang; Li, Shuai-Shuai; Liu, Qing; Xiao, Jian; The Journal of organic chemistry 84 (2019) 1833–1844; doi:10.1021/acs.joc.8b02754

data_4033758
_publ_section_title
;
 Aromatization-Driven Cascade [1,5]-Hydride Transfer/Spirocyclization
 Promoted by Fluorinated Alcohols.
;
_journal_issue                   4
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1833
_journal_page_last               1844
_journal_paper_doi               10.1021/acs.joc.8b02754
_journal_volume                  84
_journal_year                    2019
_chemical_formula_sum            'C26 H35 N O'
_chemical_formula_weight         377.55
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.211(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.6979(7)
_cell_length_b                   14.6830(5)
_cell_length_c                   18.0759(9)
_cell_measurement_reflns_used    4993
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.0780
_cell_measurement_theta_min      3.9280
_cell_volume                     4590.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14770
_diffrn_reflns_theta_full        67.25
_diffrn_reflns_theta_max         67.25
_diffrn_reflns_theta_min         3.95
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  0.9476
_exptl_absorpt_correction_T_min  0.9431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4123
_refine_ls_number_restraints     798
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0930P)^2^+3.1703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.1988
_reflns_number_gt                2997
_reflns_number_total             4123
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo8b02754_si_002.cif
_cod_data_source_block           exp_8277
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4033758