Conformation of 17-chloro-16-formylandrosta-5,16-dien-3β-yl acetate and 17-chloroandrosta-5,16-dien-3β-yl acetate
Ramos Silva, Manuela; Moreira, Vânia M.; Cardoso, Cláudia; Matos Beja, Ana; Salvador, Jorge A. R.; Acta Crystallographica Section C 64 (2008) o529–o531; doi:10.1107/S0108270108025997

data_2016759
_publ_section_title
;
 Conformation of 17-chloro-16-formylandrosta-5,16-dien-3\b-yl acetate
 and 17-chloroandrosta-5,16-dien-3\b-yl acetate
;
_journal_coeditor_code           GD3236
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o529
_journal_page_last               o531
_journal_paper_doi               10.1107/S0108270108025997
_journal_volume                  64
_journal_year                    2008
_chemical_formula_moiety         'C21 H29 Cl O2'
_chemical_formula_sum            'C21 H29 Cl O2'
_chemical_formula_weight         348.89
_chemical_name_systematic
;
17-chloro-androsta-5,16-dien-3\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
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.0271(2)
_cell_length_b                   15.4064(6)
_cell_length_c                   20.6081(9)
_cell_measurement_reflns_used    4499
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.1532
_cell_measurement_theta_min      2.3779
_cell_volume                     1913.58(13)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35093
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.250
_refine_ls_abs_structure_details 'Flack (1983), with 1496 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.14(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0733P)^2^+0.1121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1648
_reflns_number_gt                2487
_reflns_number_total             3615
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd3236.cif
_cod_data_source_block           II
_cod_database_code               2016759
_cod_database_fobs_code          2016759