Methyl 3β-Bromine-7α-hydroxy-5β-cholan-24-oate
Dago Morales, Angel; Pomés Hernández, Ramón; Coll Manchado, Francisco; Pérez Gil, Roxana; Punte, Graciela; Echeverría, Gustavo; Acta Crystallographica Section C 53 (1997) 1881–1883; doi:10.1107/S0108270197007464

data_2006804
_publ_section_title
;
 Methyl 3\b-Bromine-7\a-hydroxy-5\b-cholan-24-oate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1881
_journal_page_last               1883
_journal_paper_doi               10.1107/S0108270197007464
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C25 H41 Br O3'
_chemical_formula_structural     'C25 H41 Br O3'
_chemical_formula_sum            'C25 H41 Br O3'
_chemical_formula_weight         469.49
_chemical_melting_point          146.5(4)
_chemical_name_systematic
;
 Methyl 3\b-bromine-7\a-hydroxy-5\b-cholan-24-oate
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.641(3)
_cell_length_b                   16.5340(10)
_cell_length_c                   18.569(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      36
_cell_measurement_theta_min      8
_cell_volume                     2345.9(10)
_computing_cell_refinement       'CAD-4 EXPRESS Software'
_computing_data_collection       'CAD-4 EXPRESS Software (Enraf-Nonius, 1994)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  'SHELXL93 and PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1991)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       '\w-2\q scan technique'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.1340
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4100
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        2.1
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.775
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.764
_refine_ls_abs_structure_details
;
 the absolute stereochemistry was known prior to the X-ray analysis and the
 results of the Friedel refinement are in complete agreement with it.  35
 Friedel pairs were used in the refinement (Flack, 1983)
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.169
_refine_ls_goodness_of_fit_obs   1.169
_refine_ls_hydrogen_treatment
;
 All H-atom parameters were refined as riding atoms with a common isotropic
 displacement parameter
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_restrained_S_obs      1.169
_refine_ls_R_factor_all          0.2017
_refine_ls_R_factor_obs          .0501
_refine_ls_shift/esd_max         -0.005
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0229P)^2^+2.0363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1271
_refine_ls_wR_factor_obs         .0771
_reflns_number_observed          1583
_reflns_number_total             3873
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1305.cif
_cod_data_source_block           C25H41BrO3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '146.1-146.9' was changed to
'146.5(4)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '146.1-146.9' was changed to
'146.5(4)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0229P)^2^+2.0363P] 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^)+(0.0229P)^2^+2.0363P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2006804