Trimerization Products of Trifluoroacetone: Critical Solvent Effect on Position and Kinetics of Anomeric Equilibria
Pierre-Loïc Saaidi; Mathieu Guyonnet; Erwann Jeanneau; Paul Fleurat-Lessard; Jens Hasserodt; Journal of Organic Chemistry 73 (2008) 1209–1216; doi:10.1021/jo701669p

data_4023250
_publ_contact_author_address
;Centre de Diffractom\'etrie Henri Longchambon
Universit\'e Claude Bernard Lyon1
43 boulevard du 11 novembre 1918
F-69622 Villeurbanne cedex
France
;
_publ_contact_author_email       erwann.jeanneau@univ-lyon1.fr
_publ_contact_author_fax         '+33 472 431 160'
_publ_contact_author_name        'Erwann Jeanneau'
_publ_contact_author_phone       '+33 472 431 859'
_publ_section_title
;
 Trimerization Products of Trifluoroacetone: Critical Solvent Effect
 on Position and Kinetics of Anomeric Equilibria
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1209
_journal_page_last               1216
_journal_paper_doi               10.1021/jo701669p
_journal_volume                  73
_journal_year                    2008
_chemical_formula_moiety         'C9 H9 F9 O3'
_chemical_formula_sum            'C9 H9 F9 O3'
_chemical_formula_weight         336.15
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-04-24
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 102.074(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6113(3)
_cell_length_b                   9.9494(3)
_cell_length_c                   16.4236(5)
_cell_measurement_reflns_used    2857
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.679
_cell_volume                     1216.21(7)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5527
_diffrn_reflns_theta_full        27.321
_diffrn_reflns_theta_max         27.879
_diffrn_reflns_theta_min         2.408
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0791
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2360
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.000405
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.27 0.910 0.801 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0757
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0719
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                2360
_reflns_number_total             2784
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0661
_oxford_refine_ls_scale          1.162(4)
_oxford_reflns_number_all        2777
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            jo701669p-File003.cif
_cod_data_source_block           A
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4023250