Generation of Chirality in Guest Aromatic Ketones Included in the Crystals of Steroidal Bile Acids
Maria Gdaniec; Tadeusz Połoński; Journal of the American Chemical Society 120 (1998) 7353–7354; doi:10.1021/ja9807441

data_4116789
_publ_contact_author
;
    Maria Gdaniec
    Faculty of Chemistry
    A.Mickiewicz University
    60-780 Pozna\'n
    Poland
;
_publ_contact_author_email       mg31@krystal.amu.edu.pl
_publ_contact_author_fax         '48 61 8658 008'
_publ_contact_author_phone       '48 61 8699181 ext. 489'
_publ_section_title
;
 Generation of Chirality in Guest Aromatic Ketones Included in the
 Crystals of Steroidal Bile Acids
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7353
_journal_page_last               7354
_journal_paper_doi               10.1021/ja9807441
_journal_volume                  120
_journal_year                    1998
_chemical_compound_source        'T. Polonski'
_chemical_formula_moiety         'C24 H40 O5 . C9 H9 O1 F1'
_chemical_formula_sum            'C33 H49 F O6'
_chemical_formula_weight         560.72
_chemical_name_common            'cholic acid 4-fluoropropiophenone clathrate'
_chemical_name_systematic
; 
3\alpha,7\alpha,12\alpha-trihydroxy-5\beta-cholan-24-oic acid 
4-fluoropropiophenone clathrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 113.24(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.668(3)
_cell_length_b                   8.150(4)
_cell_length_c                   12.064(2)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      4.5
_cell_volume                     1505.9(9)
_computing_cell_refinement       'Kuma KM-4 software (Kuma Diffraction, 1991)'
_computing_data_collection       'Kuma KM-4 sofware (Kuma Diffraction, 1991)'
_computing_data_reduction        'Kuma KM-4 software (Kuma Diffraction, 1991)'
_computing_molecular_graphics
'Stereochemical Workstation (Siemens Analytical X-Ray Instruments, Inc., 1989)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'KM-4 four-circle diffractometer'
_diffrn_measurement_method       '\w/2\q scan'
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2661
_diffrn_reflns_theta_max         24.05
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        4
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       needle
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(208)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.114
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         2065
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.150
_refine_ls_restrained_S_obs      1.114
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_obs          0.0461
_refine_ls_shift/esd_max         -0.010
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.2407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1356
_refine_ls_wR_factor_obs         0.1016
_reflns_number_observed          1685
_reflns_number_total             2577
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9807441_2.cif
_cod_data_source_block           5_CA
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.2407P] 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^)+(0.0573P)^2^+0.2407P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1505.8(8)
_cod_original_formula_sum        'C33 H49 F1 O6'
_cod_database_code               4116789