(CF3CO)2O/CF3SO3H-mediated synthesis of 1,3-diketones from carboxylic acids and aromatic ketones.
Kim, JungKeun; Shokova, Elvira; Tafeenko, Victor; Kovalev, Vladimir; Beilstein journal of organic chemistry 10 (2014) 2270–2278; doi:10.3762/bjoc.10.236

data_4029969
_publ_section_title
;
 (CF3CO)2O/CF3SO3H-mediated synthesis of 1,3-diketones from carboxylic
 acids and aromatic ketones.
;
_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              2270
_journal_page_last               2278
_journal_paper_doi               10.3762/bjoc.10.236
_journal_volume                  10
_journal_year                    2014
_chemical_formula_moiety         'C18 H14 Br2 N2'
_chemical_formula_sum            'C18 H14 Br2 N2'
_chemical_formula_weight         418.13
_chemical_melting_point          420
_chemical_name_common
7-bromo-3-(bromphenyl)-2,4-dihydro-indeno[1,2-c]pyrazole
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.5770(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.77210(10)
_cell_length_b                   11.6674(4)
_cell_length_c                   28.3435(7)
_cell_measurement_reflns_used    22576
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      72.41
_cell_measurement_theta_min      3.79
_cell_volume                     1577.51(7)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 Pilatus100K
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  none
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            7328
_diffrn_reflns_theta_full        70.98
_diffrn_reflns_theta_max         70.98
_diffrn_reflns_theta_min         4.10
_diffrn_source                   'Cu GeniX 3D'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.484
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.27
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             824
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .06
_exptl_crystal_size_min          .03
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                2197
_reflns_number_total             3049
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1860-5397-10-236-S5.cif
_cod_data_source_block           jk113a
_cod_depositor_comments
'Adding full bibliography for 4029967--4029970.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4029969