Clostebol acetate
Maccaroni, Elisabetta; Mele, Andrea; Del Rosso, Renato; Malpezzi, Luciana; Acta Crystallographica Section E 67 (2011) o1952–o1953; doi:10.1107/S1600536811026560

data_2231377
_publ_section_title
;
 Clostebol acetate
;
_journal_coeditor_code           ZL2382
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1952
_journal_page_last               o1953
_journal_paper_doi               10.1107/S1600536811026560
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C21 H29 Cl O3'
_chemical_formula_moiety         'C21 H29 Cl O3'
_chemical_formula_sum            'C21 H29 Cl O3'
_chemical_formula_weight         364.89
_chemical_name_common            'clostebol acetate'
_chemical_name_systematic
;
(8<i>R</i>,9<i>S</i>,10<i>R</i>,13<i>S</i>,14<i>S</i>,17<i>S</i>)-4-chloro-
3-oxoandrost-4-en-17\b-yl acetate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7400(10)
_cell_length_b                   12.631(2)
_cell_length_c                   19.275(2)
_cell_measurement_reflns_used    3284
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2.66
_cell_volume                     1884.4(4)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL/NT (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8471
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  0.9784
_exptl_absorpt_correction_T_min  0.9451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.165
_refine_diff_density_min         -0.153
_refine_ls_abs_structure_details 'Flack (1983), 1392 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(6)
_refine_ls_extinction_coef       0.0024(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                2586
_reflns_number_total             3325
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            zl2382.cif
_cod_data_source_block           I
_cod_database_code               2231377
_cod_database_fobs_code          2231377