The generation of difluoroenolates from trifluoroethanol and reproducible syntheses of α,α-difluoro-β-hydroxy ketones
Balnaves, Andrew S.; Gelbrich, Thomas; Hursthouse, Michael B.; Light, Mark E.; Palmer, Michael J.; Percy, Jonathan M.; Journal of the Chemical Society, Perkin Transactions 1  (1999) 2525–; doi:10.1039/a902966d

data_7213079
_publ_section_title
;
 The generation of difluoroenolates from trifluoroethanol and reproducible
 syntheses of \a,\a-difluoro-\b-hydroxy ketones
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2525
_journal_paper_doi               10.1039/a902966d
_journal_year                    1999
_chemical_formula_sum            'C20 H21 F2 N O3'
_chemical_formula_weight         361.38
_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
_cell_angle_alpha                80.96(3)
_cell_angle_beta                 76.495(11)
_cell_angle_gamma                70.767(13)
_cell_formula_units_Z            2
_cell_length_a                   7.7023(13)
_cell_length_b                   9.925(2)
_cell_length_c                   13.356(2)
_cell_measurement_temperature    150(2)
_cell_volume                     933.8(3)
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Enraf Nonius FAST TV area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enraf Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0791
_diffrn_reflns_av_sigmaI/netI    0.1469
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3767
_diffrn_reflns_theta_max         24.85
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  1.369
_exptl_absorpt_correction_T_min  1.098
_exptl_absorpt_correction_type   'Empirical, DIFABS'
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_F_000             380
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.648
_refine_ls_goodness_of_fit_obs   0.852
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         2431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.648
_refine_ls_restrained_S_obs      0.852
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_obs          0.0429
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1054
_refine_ls_wR_factor_obs         0.0975
_reflns_number_observed          1311
_reflns_number_total             2431
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902966Dsup1.cif
_cod_data_source_block           3h
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7213079