<i>Ab initio</i> structure determination of a pharmaceutical compound, prednisolone succinate, from synchrotron powder data by combination of a genetic algorithm and the maximum entropy method
Nishibori, Eiji; Ogura, Tadakatsu; Aoyagi, Shinobu; Sakata, Makoto; Journal of Applied Crystallography 41 (2008) 292–301; doi:10.1107/S0021889808001520

data_2300193
_publ_section_title
;
 <i>Ab initio</i> structure determination of a pharmaceutical compound,
 prednisolone succinate, from synchrotron powder data by combination of
 a genetic algorithm and the maximum entropy method
;
_journal_coeditor_code           DB5036
_journal_issue                   2
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              292
_journal_page_last               301
_journal_paper_doi               10.1107/S0021889808001520
_journal_volume                  41
_journal_year                    2008
_chemical_formula_moiety         'C25 H32 O8, C25 H32 O8'
_chemical_formula_sum            'C50 H64 O16'
_chemical_formula_weight         920.20
_chemical_name_common            'prednisolone succinate'
_chemical_name_systematic
' 11\b,17-dihydroxypregna-1,4-diene-3,20-dione-21-succinate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_cell_angle_alpha                90.00000
_cell_angle_beta                 98.1462(8)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   21.1388(3)
_cell_length_b                   9.1628(1)
_cell_length_c                   24.5916(4)
_cell_measurement_temperature    400
_cell_volume                     4715.10(11)
_computing_cell_refinement       'SP (Nishibori et al., 2007)'
_computing_molecular_graphics    'PyMOL (DeLano, 2002)'
_computing_structure_refinement  'SP (Nishibori et al., 2007)'
_computing_structure_solution    'GAIA (Nishibori et al., 2007)'
_diffrn_ambient_temperature      300
_diffrn_detector                 'imaging plate'
_diffrn_detector_type            'FUJIFILM BAS-MS2040'
_diffrn_measurement_device_type  'large Debye-Scherrer camera'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.00140
_diffrn_source                   synchrotron
_diffrn_source_type              'SPring-8 BL02B2'
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.297
_pd_char_colour                  white
_pd_instr_location
' large Debye-Scherrer camera, BL02B2, SPring-8 (Japan)'
_pd_meas_2theta_range_inc        0.01
_pd_meas_2theta_range_max        74.5
_pd_meas_2theta_range_min        3.
_pd_meas_number_of_points        7151
_pd_meas_scan_method             fixed
_pd_proc_2theta_range_inc        0.010
_pd_proc_2theta_range_max        58.000
_pd_proc_2theta_range_min        3.000
_pd_proc_info_data_reduction     none
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function  'split Pearson VII'
_pd_proc_ls_pref_orient_corr     ' ?'
_pd_proc_ls_profile_function     'split Pearson VII'
_pd_proc_ls_prof_R_factor        0.0077
_pd_proc_ls_prof_wR_expected     0.0030
_pd_proc_ls_prof_wR_factor       0.0129
_pd_proc_wavelength              1.00140
_pd_spec_mounting                ' Lindemann glass capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_spec_size_axial              3
_pd_spec_size_equat              0.4
_refine_ls_extinction_method     none
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    64
_refine_ls_number_parameters     205
_refine_ls_number_restraints     250
_refine_ls_R_I_factor            0.0480
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_scheme      sigma
_cod_data_source_file            db5036.cif
_cod_data_source_block           400K
_cod_original_cell_volume        4715.1(2)
_cod_original_sg_symbol_H-M      'I 2'
_cod_database_code               2300193