Crystal structure of 3β-acetoxyandrosta-5,16-dien-17-yl trifluoromethanesulfonate
Zhou, Shengjun; Huang, Huaqi; Zhang, Ting; Wang, Dangfeng; Huang, Rongbin; Acta Crystallographica Section E 71 (2015) o404–o405; doi:10.1107/S2056989015009123

data_2240699
_publ_contact_author
;
      Rongbin Huang
      Department of Chemistry
      Xiamen University
      Xiamen 361005
      People's Republic of China
;
_publ_section_title
;
 Crystal structure of 3\b-acetoxyandrosta-5,16-dien-17-yl
 trifluoromethanesulfonate
;
_journal_coeditor_code           CV5486
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o404
_journal_page_last               o405
_journal_paper_doi               10.1107/S2056989015009123
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C22 H29 F3 O5 S'
_chemical_formula_moiety         'C22 H29 F3 O5 S'
_chemical_formula_sum            'C22 H29 F3 O5 S'
_chemical_formula_weight         462.51
_chemical_name_common
;
3\b-Acetoxyandrosta-5,16-dien-17-yl trifluoromethanesulfonate
;
_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-(trifluoromethylsulfonyloxy)-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                   8.0734(10)
_cell_length_b                   9.9640(12)
_cell_length_c                   27.6900(15)
_cell_measurement_temperature    173
_cell_volume                     2227.5(4)
_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      173
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            22017
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.248
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.659
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 934 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0997P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1888
_reflns_number_gt                3185
_reflns_number_total             5098
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv5486sup1.cif
_cod_data_source_block           I
_cod_database_code               2240699
_cod_database_fobs_code          2240699
_shelx_estimated_absorpt_t_min   0.980
_shelx_estimated_absorpt_t_max   0.984
_shelx_hkl_checksum              84124
_shelx_res_checksum              64735