16β-Bromo-17α-hydroxypregn-4-ene-3,11,20-trione methanol solvate
Zhang Haitao; Nie, Qiang; Chen, Ying; Wang, Jingkang; Zhou,Lina; Acta Crystallographica Section E 62 (2006) o4075–o4077; doi:10.1107/S1600536806033423

data_2210256
_publ_section_title
;
 16\b-Bromo-17\a-hydroxypregn-4-ene-3,11,20-trione methanol solvate
;
_journal_coeditor_code           HB2124
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4075
_journal_page_last               o4077
_journal_paper_doi               10.1107/S1600536806033423
_journal_volume                  62
_journal_year                    2006
_chemical_formula_moiety         'C21 H27 Br O4, C H4 O'
_chemical_formula_sum            'C22 H31 Br O5'
_chemical_formula_weight         455.38
_chemical_melting_point          472.2
_chemical_name_systematic
;
 17-acetyl-16-bromo-17-hydroxy-10,13-dimethyl-1,6,7,8,9,10,12,13,14,
15,16,17-dodecahydro-2H-cyclopenta[a]phenanthrene-3,11-dione
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6030(17)
_cell_length_b                   12.235(2)
_cell_length_c                   20.001(4)
_cell_measurement_reflns_used    16668
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.05
_cell_volume                     2105.3(7)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, date)'
_computing_data_reduction        RAPID-AUTO
_computing_molecular_graphics    'SHELXTL97 (Bruker, 1998)'
_computing_publication_material  SHELXTL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-axis rapid IP area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20576
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    1.983
_exptl_absorpt_correction_T_max  0.670
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.401
_refine_ls_abs_structure_details 'Flack (1983), 2065 Friedel pairs'
_refine_ls_abs_structure_Flack   0.016(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.8713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                4133
_reflns_number_total             4815
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2124.cif
_cod_data_source_block           I
_cod_database_code               2210256
_cod_database_fobs_code          2210256