A steroid derivative that crystallizes with three molecules in the asymmetric unit
Brock, Carolyn Pratt; Stoilov, Ivan; Watt, David S.; Acta Crystallographica Section C 50 (1994) 434–438; doi:10.1107/S0108270193009230

data_2009526
_publ_contact_author
;
                                 Prof. Carolyn P. Brock
                                 Department of Chemistry
                                 University of Kentucky
                                 Lexington, KY  40506-0055
                                 USA
;
_publ_section_title
;
 A steroid derivative that crystallizes with three molecules in the
 asymmetric unit
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              434
_journal_page_last               438
_journal_paper_doi               10.1107/S0108270193009230
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         'C30 H54 O'
_chemical_formula_sum            'C30 H54 O'
_chemical_formula_weight         430.76
_chemical_melting_point          424
_chemical_name_systematic
;
(20R,23S,24R)-5\a-dinosteran-29-ol
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_type_scat_source
'International Tables for X-ray Crystallography (1974, Vol. IV, Table 2.4.6A)'
_audit_creation_method           'created by C P Brock'
_cell_angle_alpha                90
_cell_angle_beta                 90.068(6)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   6.6289(5)
_cell_length_b                   12.5448(14)
_cell_length_c                   49.810(4)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    294.0(10)
_cell_measurement_theta_max      10.3
_cell_measurement_theta_min      8.2
_cell_volume                     4142.1(6)
_computing_cell_refinement       CAD-4-VAX
_computing_data_collection       'CAD-4-VAX (Enraf-Nonius, 1988)'
_computing_data_reduction        'local program (Brock)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1965)'
_computing_publication_material
'ORFFE (Busing, Martin & Levy, 1964);  local program (Brock)'
_computing_structure_refinement
;local program [based on Ibers' least-squares program, which is in turn based
on ORFLS (Busing, Martin & Levy, 1962)]
;
_computing_structure_solution    'DIRDIF (Beurskens et al., 1983)'
_diffrn_measurement_device       'Enraf-Nonius CAD-4VAX diffractometer'
_diffrn_measurement_method
'\w scans;  stationary background measurements'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            7618
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        1.9
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.056
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.036
_exptl_crystal_description
;
Very thin blades;  the plate normal is c* and the
long direction is a.
;
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.31
_refine_ls_abs_structure_details
;
Absolute configuration was chosen to correspond with that expected from
the synthetic pathway
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.62
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     372
_refine_ls_number_reflns         2377
_refine_ls_R_factor_obs          0.075
_refine_ls_shift/esd_max         0.01
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.068
_reflns_number_observed          2377
_reflns_number_total             7618
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            cr1061.cif
_cod_data_source_block           STOILOV
_cod_original_cell_volume        4142.1(7)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2009526