Brucine salts of <small>L</small>-α-hydroxy acids: brucinium hydrogen (<i>S</i>)-malate pentahydrate and anhydrous brucinium hydrogen (2<i>R</i>,3<i>R</i>)-tartrate at 130K
Graham Smith; Urs D. Wermuth; Jonathan M. White; Acta Crystallographica Section C 62 (2006) o353–o357; doi:10.1107/S0108270106017288

data_2015372
_publ_section_title
;
 Brucine salts of <small>L</small>-\a-hydroxy acids: brucinium hydrogen
 (<i>S</i>)-malate pentahydrate and anhydrous brucinium hydrogen
 (2<i>R</i>,3<i>R</i>)-tartrate at 130K
;
_journal_coeditor_code           GZ3010
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o353
_journal_page_last               o357
_journal_paper_doi               10.1107/S0108270106017288
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C23 H27 N2 O4 +, C4 H5 O5 -, 5H2 O'
_chemical_formula_moiety         'C23 H27 N2 O4 +, C4 H5 O5 -, 5H2 O'
_chemical_formula_sum            'C27 H42 N2 O14'
_chemical_formula_weight         618.63
_chemical_melting_point          494.6(12)
_chemical_name_common            'brucinium hydrogen L-malate pentahydrate'
_chemical_name_systematic
;
2,3-dimethoxy-10-oxostrychnidinium hydrogen (S)-malate pentahydrate
;
_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           'SHELXL97 (Sheldrick, 1997)'
_cell_angle_alpha                76.401(2)
_cell_angle_beta                 88.716(2)
_cell_angle_gamma                82.104(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2915(10)
_cell_length_b                   9.4337(9)
_cell_length_c                   16.9287(17)
_cell_measurement_reflns_used    2640
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      2.21
_cell_volume                     1428.5(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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7141
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.165
_refine_diff_density_min         -0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         5034
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.2077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                4397
_reflns_number_total             5034
_reflns_threshold_expression     'I >2\s(I)'
_cod_data_source_file            gz3010.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'none ' changed to 'none' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '493.5--495.8 ' was changed to
'494.6(12)' - 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 '493.5--495.8 ' was changed to
'494.6(12)' - the average value was taken and precision was
estimated.

'_exptl_absorpt_correction_type' value 'none ' changed to
'none' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     'P 1 '
_cod_original_sg_symbol_H-M      'P 1 '
_cod_database_code               2015372
_cod_database_fobs_code          2015372