Layered structures in proton-transfer compounds of 5-sulfosalicylic acid with the aromatic polyamines 2,6-diaminopyridine and 1,4-phenylenediamine
Graham Smith; Urs D. Wermuth; Peter C. Healy; Acta Crystallographica Section C 61 (2005) o555–o558; doi:10.1107/S010827010502439X

data_2015093
_publ_section_title
;
 Layered structures in proton-transfer compounds of 5-sulfosalicylic
 acid with the aromatic polyamines 2,6-diaminopyridine and
 1,4-phenylenediamine
;
_journal_coeditor_code           TA1503
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o555
_journal_page_last               o558
_journal_paper_doi               10.1107/S010827010502439X
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C5 H8 N3 +, C7 H5 O6 S -, H2 O'
_chemical_formula_moiety         'C5 H8 N3 +, C7 H5 O6 S -, H2 O'
_chemical_formula_sum            'C12 H15 N3 O7 S'
_chemical_formula_weight         345.34
_chemical_melting_point          525.0(10)
_chemical_name_common
'2,6-diaminopyridinium 5-sulfosalicylate monohydrate'
_chemical_name_systematic
;
2,6-diaminopyridinium 3-carboxy-4-hydroxybenzenesulfonate monohydrate'
;
_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                 105.001(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4778(15)
_cell_length_b                   13.085(2)
_cell_length_c                   6.7562(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      15.8
_cell_measurement_theta_min      12.6
_cell_volume                     723.9(2)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Software
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
1999)
;
_computing_data_reduction
;
TeXsan for Windows (Molecular Structure Corporation, 1999)
;
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC 7R'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0136
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1965
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        0.50
_diffrn_standards_interval_time  150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.237
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.06(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         1726
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.886
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0335
_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^)+(0.10P)^2^+0.0953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.096
_refine_ls_wR_factor_ref         0.112
_reflns_number_gt                1406
_reflns_number_total             1726
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ta1503.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '524--526' was changed to '525.0(10)'
- 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 '524--526' was changed to '525.0(10)'
- 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               2015093
_cod_database_fobs_code          2015093