TfOH-catalyzed domino cycloisomerization/hydrolytic defluorination of 2,3-allenyl perfluoroalkyl ketones
Can Xue; Xin Huang; Shangze Wu; Jing Zhou; Jianxin Dai; Chunling Fu; Shengming Ma; Chem.Commun. 51 (2015) 17112–; doi:10.1039/C5cc06111C

data_7118112
_publ_section_title
;
 TfOH-catalyzed domino cycloisomerization/hydrolytic defluorination of
 2,3-allenyl perfluoroalkyl ketones
;
_journal_name_full               Chem.Commun.
_journal_page_first              17112
_journal_paper_doi               10.1039/C5cc06111C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C23 H17 F7 O2'
_chemical_formula_weight         458.37
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-04-13 deposited with the CCDC.
2015-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                108.215(10)
_cell_angle_beta                 105.015(10)
_cell_angle_gamma                110.595(7)
_cell_formula_units_Z            4
_cell_length_a                   13.635(4)
_cell_length_b                   13.766(4)
_cell_length_c                   14.405(7)
_cell_measurement_temperature    296(2)
_cell_volume                     2187.4(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22702
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.9422
_exptl_absorpt_correction_T_min  0.9340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.47
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         7576
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1732
_refine_ls_R_factor_gt           0.1199
_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^)+(0.1080P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2977
_refine_ls_wR_factor_ref         0.3230
_reflns_number_gt                3825
_reflns_number_total             7576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc06111c2.cif
_cod_data_source_block           z
_cod_original_cell_volume        2187.5(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7118112