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_2015373
_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 O6 -'
_chemical_formula_moiety         'C23 H27 N2 O4 +, C4 H5 O6 -'
_chemical_formula_sum            'C27 H32 N2 O10'
_chemical_formula_weight         544.55
_chemical_melting_point          523.0(6)
_chemical_name_common            'brucinium hydrogen L-tartrate'
_chemical_name_systematic
;
2,3-dimethoxy-10-oxostrychnidinium hydrogen 2(R),3(R)-tartrate
;
_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                   12.2719(7)
_cell_length_b                   13.5151(8)
_cell_length_c                   14.3814(9)
_cell_measurement_reflns_used    4092
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      23.97
_cell_measurement_theta_min      2.65
_cell_volume                     2385.2(2)
_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 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  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0664
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15054
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         3088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0258P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                2514
_reflns_number_total             3088
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gz3010.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '522.4--523.6' was changed to
'523.0(6)' - 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 '522.4--523.6' was changed to
'523.0(6)' - 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_Hall     'P2ac 2ab'
_cod_database_code               2015373
_cod_database_fobs_code          2015373