Two pseudopolymorphic hydrates of brucine: brucine‒water (1/4) and brucine‒water (1/5.25) at 130 K
Graham Smith; Urs D. Wermuth; Peter C. Healy; Jonathan M. White; Acta Crystallographica Section C 62 (2006) o203–o207; doi:10.1107/S0108270106005944

data_2015250
_publ_section_title
;
 Two pseudopolymorphic hydrates of brucine: brucine--water (1/4) and
 brucine--water (1/5.25) at 130 K
;
_journal_coeditor_code           GZ1028
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o203
_journal_page_last               o207
_journal_paper_doi               10.1107/S0108270106005944
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C23 H26 N2 O4, 5.25H2 O'
_chemical_formula_moiety         'C23 H26 N2 O4, 5.25H2 O'
_chemical_formula_sum            'C23 H36.5 N2 O9.25'
_chemical_formula_weight         489.0
_chemical_melting_point          387.5(7)
_chemical_name_common            'brucine 5.25-hydrate'
_chemical_name_systematic
;
2,3-dimethoxystrychnidin-10-one--water (1/5.25)
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL97 (Sheldrick, 1997)'
_cell_angle_alpha                90.00
_cell_angle_beta                 96.202(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.351(5)
_cell_length_b                   12.200(3)
_cell_length_c                   16.972(4)
_cell_measurement_reflns_used    4189
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      24.89
_cell_measurement_theta_min      2.19
_cell_volume                     4806.7(19)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997) and WinGX'
_computing_structure_solution
'SHELXS97 (Sheldrick, 1997) and WinGX (Farrugia, 1999)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker CCD area-detector diffractometer'
_diffrn_measurement_method       '\f  and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0978
_diffrn_reflns_av_sigmaI/netI    0.0979
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12710
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.283
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         4461
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0655
_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^)+(0.0961P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1729
_reflns_number_gt                3673
_reflns_number_total             4461
_reflns_threshold_expression     'I >2\s(I)'
_cod_data_source_file            gz1028.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '386.9-388.2' was changed to
'387.5(7)' - 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 '386.9-388.2' was changed to
'387.5(7)' - 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_original_sg_symbol_H-M      'C 2'
_cod_database_code               2015250