Pregnenolone hemisuccinate: a <i>P</i>1 structure with <i>Z</i>' = 4
Bernès, Sylvain; Torrens, Hugo; López-Giral, Angela; Buttenklepper, Alfredo; Acta Crystallographica Section E 59 (2003) o1372–o1375; doi:10.1107/S160053680301835X

data_2202634
_publ_section_title
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 Pregnenolone hemisuccinate: a <i>P</i>1 structure with <i>Z</i>' = 4
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_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1372
_journal_page_last               o1375
_journal_paper_doi               10.1107/S160053680301835X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C25 H36 O5'
_chemical_formula_moiety         'C25 H36 O5'
_chemical_formula_sum            'C25 H36 O5'
_chemical_formula_weight         416.54
_chemical_melting_point          453.0(10)
_chemical_name_common            'Pregnenolone hemisuccinate'
_chemical_name_systematic
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Succinic acid mono(17-acetyl-10,13-dimethyl-2,3,4,7,8,9,10,11,12,13,14,
15,16,17-tetradecahydro-1H-cyclopenta[a]phenanthren-3-yl) ester
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL-Plus
_cell_angle_alpha                96.925(9)
_cell_angle_beta                 104.907(6)
_cell_angle_gamma                95.201(8)
_cell_formula_units_Z            4
_cell_length_a                   11.4692(10)
_cell_length_b                   11.8174(12)
_cell_length_c                   17.6837(14)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    298.0(10)
_cell_measurement_theta_max      11.98
_cell_measurement_theta_min      2.40
_cell_volume                     2280.7(4)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'SHELXTL-Plus and MERCURY 1.1.2 (CCDC, 2002)'
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  SHELXTL-Plus
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1998)'
_diffrn_ambient_temperature      298.0(10)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9296
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.215
_refine_ls_extinction_coef       0.0083(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL-Plus
_refine_ls_goodness_of_fit_ref   1.260
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         7990
_refine_ls_number_restraints     795
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0664
_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^)+(0.1P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.1910
_reflns_number_gt                5778
_reflns_number_total             7990
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fl6046.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '452-454 K' was changed to
'453.0(10)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '452-454 K' was changed to
'453.0(10)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2202634
_cod_database_fobs_code          2202634