16β-Bromo-17-hydroxypregn-4-ene-3,11,20-trione chloroform solvate
Nie, Qiang; Wang, Jing-Kang; Zhou, Lina; Acta Crystallographica Section E 62 (2006) o1777–o1779; doi:10.1107/S1600536806012220

data_2208909
_publ_section_title
;
 16\b-Bromo-17-hydroxypregn-4-ene-3,11,20-trione chloroform solvate
;
_journal_coeditor_code           HK2025
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1777
_journal_page_last               o1779
_journal_paper_doi               10.1107/S1600536806012220
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C21 H27 Br O4, C H Cl3'
_chemical_formula_moiety         'C21 H27 Br O4, C H Cl3'
_chemical_formula_sum            'C22 H28 Br Cl3 O4'
_chemical_formula_weight         542.70
_chemical_melting_point          472.2
_chemical_name_common
;
16\b-Bromo-17-hydroxypregn-4-ene-3,11,20-trione chloroform solvate
;
_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
 chloroform solvate
;
_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                   10.443(2)
_cell_length_b                   12.324(3)
_cell_length_c                   18.927(4)
_cell_measurement_reflns_used    16366
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.31
_cell_volume                     2435.9(9)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 2004)'
_computing_data_reduction        RAPID-AUTO
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP area-detector'
_diffrn_measurement_method       '\f? \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  0.0817
_diffrn_reflns_av_sigmaI/netI    0.1416
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20190
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    2.042
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.301
_refine_ls_abs_structure_details 'Flack (1983), with 1972 Friedel pairs'
_refine_ls_abs_structure_Flack   0.010(10)
_refine_ls_extinction_coef       0.0070(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4527
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0364P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0912
_reflns_number_gt                3310
_reflns_number_total             4527
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2025.cif
_cod_data_source_block           I
_cod_database_code               2208909
_cod_database_fobs_code          2208909