Crystal structure of (3S)-3-acetoxy-17-(pyridin-3-yl)androsta-5,16-diene
Zhou, Shengjun; Huang, Huaqi; Huang, Rongbin; Acta Crystallographica Section E Crystallographic Communications 71 (2015) o146–; doi:10.1107/S2056989015001966

data_2019836
_publ_contact_author
;
Rongbin Huang
Department of Chemistry
Xiamen University
Xiamen 361005
People's Republic of China
;
_publ_section_title
;
 Crystal structure of (3S)-3-acetoxy-17-(pyridin-3-yl)androsta-5,16-diene
;
_journal_coeditor_code           HB7357
_journal_issue                   3
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              o146
_journal_paper_doi               10.1107/S2056989015001966
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C26 H33 N O2'
_chemical_formula_moiety         'C26 H33 N O2'
_chemical_formula_sum            'C26 H33 N O2'
_chemical_formula_weight         391.53
_chemical_name_common
(3<i>S</i>)-3-Acetoxy-17-(pyridin-3-yl)androsta-5,16-diene
_chemical_name_systematic
'(3<i>S</i>,8<i>R</i>,9<i>S</i>,10<i>R</i>,13<i>S</i>,14<i>S</i>)-10,13-Dimethyl-17-(pyridin-3-yl)-2,3,4,7,8,9,10,11,12,13,14,15-dodecahydro-1<i>H</i>-cyclopenta[<i>a</i>]phenanthren-3-yl acetate'
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5180(5)
_cell_length_b                   9.7274(5)
_cell_length_c                   30.2035(15)
_cell_measurement_reflns_used    1526
_cell_measurement_temperature    283(2)
_cell_measurement_theta_max      26.259
_cell_measurement_theta_min      3.268
_cell_volume                     2208.8(2)
_computing_cell_refinement
;
SAINT (Bruker, 2004)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT (Bruker, 2004)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009) and Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      283(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
Bruker SMART APEX 2000
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            12750
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         3.382
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.9748
_exptl_absorpt_correction_T_min  0.9713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0560P)^2^+0.2757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                3261
_reflns_number_total             4320
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7357sup1.cif
_cod_data_source_block           I
_cod_database_code               2019836
_cod_database_fobs_code          2019836
_shelx_estimated_absorpt_t_min   0.971
_shelx_estimated_absorpt_t_max   0.975
_shelx_hkl_checksum              56524
_shelx_res_checksum              91643