(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_4029967
_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_sum            'C14 H12 F3 N O3'
_chemical_formula_weight         299.25
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                74.046(2)
_cell_angle_beta                 77.445(2)
_cell_angle_gamma                67.218(2)
_cell_formula_units_Z            4
_cell_length_a                   9.8661(2)
_cell_length_b                   12.1391(3)
_cell_length_c                   12.6797(3)
_cell_measurement_reflns_used    6201
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      72.69
_cell_measurement_theta_min      4.04
_cell_volume                     1335.61(6)
_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      293
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_details      ' 2687 frames, detector distance = 60 mm'
_diffrn_measurement_method       'rotation method'
_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  0.0889
_diffrn_reflns_av_sigmaI/netI    0.0865
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6122
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.00
_diffrn_reflns_theta_min         3.65
_diffrn_source                   'Cu GeniX 3D'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.152
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             616
_exptl_crystal_size_max          .18
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .16
_refine_diff_density_max         0.133
_refine_diff_density_min         -0.129
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.0017(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.701
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         4734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.701
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.354
_refine_ls_shift/su_mean         0.043
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                1611
_reflns_number_total             4734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1860-5397-10-236-S3.cif
_cod_data_source_block           jk89a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/Beilstein/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4029967--4029970.cif.
;
_cod_original_cell_volume        1335.61(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4029967