Solasodine monohydrate: an authentic structural characterization and a reinterpretation of a previous report
Vega Baez, José Luis; Meza-Reyes, Socorro; Montiel Smith, Sara; Sandoval Ramírez, Jesús; Bernès, Sylvain; Acta Crystallographica Section E 62 (2006) o4741–o4743; doi:10.1107/S1600536806038554

data_2210603
_publ_section_title
;
 Solasodine monohydrate: an authentic structural characterization and a
 reinterpretation of a previous report
;
_journal_coeditor_code           FL2056
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4741
_journal_page_last               o4743
_journal_paper_doi               10.1107/S1600536806038554
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C27 H43 N O2 , H2 O'
_chemical_formula_moiety         'C27 H43 N O2 , H2 O'
_chemical_formula_sum            'C27 H45 N O3'
_chemical_formula_weight         431.64
_chemical_name_common            'Solasodine monohydrate'
_chemical_name_systematic
;
[(22R,25R)-spirosol-5-en-3\b-ol] monohydrate
;
_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   'see text'
_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                   7.6497(8)
_cell_length_b                   9.6076(17)
_cell_length_c                   33.445(5)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      12.33
_cell_measurement_theta_min      4.75
_cell_volume                     2458.0(6)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  SHELXTL-Plus
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1998)'
_diffrn_ambient_temperature      296.0(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            3574
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.146
_refine_diff_density_min         -0.153
_refine_ls_extinction_coef       0.0025(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL-Plus (Sheldrick, 1998)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         2517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0474P)^2^+0.2778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                2112
_reflns_number_total             2517
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fl2056.cif
_cod_data_source_block           I
_cod_database_code               2210603
_cod_database_fobs_code          2210603