2,3-Dimethoxy-10-oxostrychnidinium 3-carboxybenzoate trihydrate: the 1:1 proton-transfer compound of brucine with isophthalic acid
Graham Smith; Urs D. Wermuth; David J. Young; Jonathan M. White; Acta Crystallographica Section E 62 (2006) o1553–o1555; doi:10.1107/S1600536806010026

data_2208595
_publ_section_title
;
 2,3-Dimethoxy-10-oxostrychnidinium 3-carboxybenzoate trihydrate: the
 1:1 proton-transfer compound of brucine with isophthalic acid
;
_journal_coeditor_code           FL2011
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1553
_journal_page_last               o1555
_journal_paper_doi               10.1107/S1600536806010026
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C23 H27 N2 O4 + , C8 H5 O4 - , 3H2 O'
_chemical_formula_moiety         'C23 H27 N2 O4 + , C8 H5 O4 - , 3H2 O'
_chemical_formula_sum            'C31 H38 N2 O11'
_chemical_formula_weight         614.63
_chemical_melting_point          456.1(15)
_chemical_name_common            'brucinium hydrogen isophthalate trihydrate'
_chemical_name_systematic
;
2,3-dimethoxy-10-oxostrychnidinium 3-carboxybenzoate trihydrate
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                   12.4560(9)
_cell_length_b                   29.3559(19)
_cell_length_c                   8.0020(5)
_cell_measurement_reflns_used    2302
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      21.36
_cell_measurement_theta_min      2.55
_cell_volume                     2926.0(3)
_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) in WinGX'
_computing_structure_solution
'SHELXS97 (Sheldrick, 1997) in 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 Model CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_av_sigmaI/netI    0.1296
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            18440
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         3815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0105P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                2474
_reflns_number_total             3815
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fl2011.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '454.6--457.6' was changed to
'456.1(15)' - 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 '454.6--457.6' was changed to
'456.1(15)' - 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               2208595
_cod_database_fobs_code          2208595