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_2015249
_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, 4H2 O'
_chemical_formula_moiety         'C23 H26 N2 O4, 4H2 O'
_chemical_formula_sum            'C23 H34 N2 O8'
_chemical_formula_weight         466.52
_chemical_melting_point          378
_chemical_name_common            'brucine tetrahydrate '
_chemical_name_systematic
;
2,3-dimethoxystrychnidin-10-one--water (1/4)
;
_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
_audit_creation_method           'SHELXL97 (Sheldrick, 1997)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.555(2)
_cell_length_b                   11.531(3)
_cell_length_c                   26.492(8)
_cell_measurement_reflns_used    2584
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.53
_cell_measurement_theta_min      2.70
_cell_volume                     2307.9(11)
_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  'SHELXTL?? and WinGX'
_computing_structure_solution
'SHELXTL?? (Bruker, 1997) and WinGX (Farrugia, 1999)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            11874
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.208
_refine_ls_extinction_coef       0.0025(4)
_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   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         2346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                1727
_reflns_number_total             2346
_reflns_threshold_expression     'F^2^ >2\s(F^2^) '
_cod_data_source_file            gz1028.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'P 2ac 2ab '
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               2015249