Brucinium toluene-4-sulfonate trihydrate at 130 K
Graham Smith; Urs D. Wermuth; Peter C. Healy; David J. Young; Jonathan M. White; Acta Crystallographica Section E 61 (2005) o2646–o2648; doi:10.1107/S1600536805022695

data_2206359
_publ_section_title
;
 Brucinium toluene-4-sulfonate trihydrate at 130 K
;
_journal_coeditor_code           BT6697
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2646
_journal_page_last               o2648
_journal_paper_doi               10.1107/S1600536805022695
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C23 H27 N2 O4 + , C7 H7 O3 S - , 3H2 O'
_chemical_formula_moiety         'C23 H27 N2 O4 + , C7 H7 O3 S - , 3H2 O'
_chemical_formula_sum            'C30 H40 N2 O10 S'
_chemical_formula_weight         620.71
_chemical_melting_point          487.6(12)
_chemical_name_common            'brucinium toluene-4-sulfonate trihydrate '
_chemical_name_systematic
;
2,3-dimethoxy-10-oxostrychnidinium toluene-4-sulfonate trihydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 93.400(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1813(9)
_cell_length_b                   30.862(2)
_cell_length_c                   7.7875(6)
_cell_measurement_reflns_used    3782
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      22.41
_cell_measurement_theta_min      2.59
_cell_volume                     2922.5(4)
_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
_computing_structure_solution    'SHELXTL (Bruker, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.1101
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            18490
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         1.32
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.400
_refine_ls_abs_structure_details 'Flack (1983), with 5742 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.844
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         12628
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.844
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0263P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                8427
_reflns_number_total             12628
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            bt6697.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '486.5--488.8' was changed to
'487.6(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 '486.5--488.8' was changed to
'487.6(12)' - 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      'P 21'
_cod_database_code               2206359
_cod_database_fobs_code          2206359