Methyl 4β-bromo-7α-cathyloxy-3-oxo-5β-cholanoate
Héctor Novoa de Armas; Norbert M. Blaton; Oswald M. Peeters; Camiel J. De Ranter; Ramón Pomés Hernández; Francisco Coll Manchado; Roxana Pérez Gil; Acta Crystallographica Section C 55 (1999) 599–601; doi:10.1107/S0108270198016400

data_2008387
_publ_section_title
;
 Methyl 4\b-bromo-7\a-cathyloxy-3-oxo-5\b-cholanoate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              599
_journal_page_last               601
_journal_paper_doi               10.1107/S0108270198016400
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         'C28 H43 Br O6'
_chemical_formula_sum            'C28 H43 Br O6'
_chemical_formula_weight         555.55
_chemical_name_systematic
' Methyl-4\b-bromine-7\a-cathyloxy-3-oxo-5\b-cholanoate'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7585(5)
_cell_length_b                   15.6060(10)
_cell_length_c                   22.8759(9)
_cell_measurement_reflns_used    78
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      56.3
_cell_measurement_theta_min      7.7
_cell_volume                     2769.8(3)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'DIAMOND (Bergerhoff, 1996)'
_computing_publication_material
; PLATON (Spek, 1990), PARST (Nardelli, 1983, 1995) and PARSTCIF
(Nardelli, 1991)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Siemens P4 four-circle'
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            3609
_diffrn_reflns_reduction_process ?
_diffrn_reflns_theta_full        68.99
_diffrn_reflns_theta_max         68.99
_diffrn_reflns_theta_min         3.43
_diffrn_standards_decay_%        <1.0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.335
_exptl_absorpt_correction_T_max  0.721
_exptl_absorpt_correction_T_min  0.373
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.3322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.344
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_coef       0.0052(3)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997a)'
_refine_ls_goodness_of_fit_all   1.071
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         3398
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.054
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+1.1796P]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.138
_reflns_number_gt                2803
_reflns_number_total             3398
_reflns_threshold_expression     F>2\s(F)
_cod_data_source_file            na1393.cif
_cod_data_source_block           na1393
_cod_depositor_comments
;
 Changing the _atom_site_occupancy data item value from '.' to '1'
 for all fully occupied atom sites.

 Antanas Vaitkus,
 2017-02-10

The following automatic conversions were performed:

'_refine_ls_matrix_type' value 'Full' changed to 'full' 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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value ' calc
w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+1.1796P]' 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^)+(0.0727P)^2^+1.1796P]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      ' P 21 21 21 '
_cod_database_code               2008387