Mixed dicationic and monocationic benzidine species in the proton-transfer compound of benzidine with 3,5-dinitrosalicylic acid
Graham Smith; Urs D. Wermuth; Jonathan M. White; Acta Crystallographica Section C 62 (2006) o402–o404; doi:10.1107/S010827010601821X

data_2015401
_publ_section_title
;
 Mixed dicationic and monocationic benzidine species in the
 proton-transfer compound of benzidine with 3,5-dinitrosalicylic acid
;
_journal_coeditor_code           AV3018
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o402
_journal_page_last               o404
_journal_paper_doi               10.1107/S010827010601821X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
'C12 H14 N2 2+, 2C12 H13 N2 +, 4C7 H3 N2 O7 -, 2C2 H6 O'
_chemical_formula_moiety
'C12 H14 N2 2+, 2C12 H13 N2 +, 4C7 H3 N2 O7 -, 2C2 H6 O'
_chemical_formula_sum            'C68 H64 N14 O30'
_chemical_formula_weight         1557.34
_chemical_name_systematic
;
1,1'-biphenyl-4,4'-diaminium bis(4'-amino-1,1'-biphenyl-4-aminium)
tetrakis(2-carboxy-4,6-dinitrophenolate) ethanol disolvate
;
_chemical_temperature_decomposition 481.3(16)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 109.154(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.862(2)
_cell_length_b                   10.5138(11)
_cell_length_c                   19.081(2)
_cell_measurement_reflns_used    1773
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      19.12
_cell_measurement_theta_min      2.26
_cell_volume                     3574.5(7)
_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 (Bruker, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Bruker SMART CCD'
_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  0.0634
_diffrn_reflns_av_sigmaI/netI    0.1197
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22178
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow--brown
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism '
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         8165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.1574
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0239P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                3072
_reflns_number_total             8165
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            av3018.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been given
as '479.7--482.9 (dec)'. The value was changed to '481.3(16)' - 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' tag was changed to
'_chemical_temperature_decomposition' since the value had been given
as '479.7--482.9 (dec)'. The value was changed to '481.3(16)' - 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_cell_volume        3574.6(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2015401
_cod_database_fobs_code          2015401