Two crystallographic forms and the absolute structure of 5α,14α-androstane
Crittenden, Christopher M.; DiPasquale, Antonio G.; Acta Crystallographica Section C 77 (2021) –; doi:10.1107/S2053229621008408

data_2022420
_publ_section_title
;
 Two crystallographic forms and the absolute structure of
 5\a,14\a-androstane
;
_journal_coeditor_code           YP3218
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229621008408
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_iupac          '2C19 H31 O0.50, C19 H32'
_chemical_formula_moiety         '2(C19 H31 O0.50), C19 H32'
_chemical_formula_sum            'C57 H94 O'
_chemical_formula_weight         795.32
_chemical_name_common            '5\a,14\a-Androstane, Form II w/ impurity'
_chemical_name_systematic        '5\a,14\a-Androstane, Form II w/ impurity'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.16990(10)
_cell_length_b                   22.1480(3)
_cell_length_c                   29.8734(5)
_cell_measurement_reflns_used    31747
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.8190
_cell_measurement_theta_min      2.0270
_cell_volume                     4743.86(12)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
ORTEP-32 (Farrugia, 2012) and <i>Mercury</i> (Macrae <i>et al.</i>,
2020)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
WinGX (Farrugia, 2012) and SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
WinGX (Farrugia, 2012) and SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            59898
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         75.097
_diffrn_reflns_theta_min         2.483
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2021)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.342
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3326 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_coef       0.00062(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         9113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+1.8106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                8487
_reflns_number_total             9113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3218sup1.cif
_cod_data_source_block           Form_II_impure
_cod_database_code               2022420
_shelx_estimated_absorpt_t_min   0.917
_shelx_estimated_absorpt_t_max   0.986
_shelx_hkl_checksum              5548
_shelx_res_checksum              99001
_cod_database_fobs_code 2022420