Hydrogen bonding in two ammonium salts of 5-sulfosalicylic acid: ammonium 3-carboxy-4-hydroxybenzenesulfonate monohydrate and triammonium 3-carboxy-4-hydroxybenzenesulfonate 3-carboxylato-4-hydroxybenzenesulfonate
Smith, Graham; Wermuth, Urs D.; Acta Crystallographica Section C 69 (2013) 534–537; doi:10.1107/S0108270113008846

data_2018954
_publ_section_title
;
 Hydrogen bonding in two ammonium salts of 5-sulfosalicylic acid: ammonium
 3-carboxy-4-hydroxybenzenesulfonate monohydrate and triammonium
 3-carboxy-4-hydroxybenzenesulfonate
 3-carboxylato-4-hydroxybenzenesulfonate
;
_journal_coeditor_code           FG3289
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              534
_journal_page_last               537
_journal_paper_doi               10.1107/S0108270113008846
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '3N H4 + , C7 H4 O6 S 2- , C7 H5 O6 S -'
_chemical_formula_moiety         '3(H4 N +), C7 H4 O6 S 2-, C7 H5 O6 S -'
_chemical_formula_sum            'C14 H21 N3 O12 S2'
_chemical_formula_weight         487.48
_chemical_name_common            'triammonium 5-sulfosalicylate'
_chemical_name_systematic
;
Triammonium 3-carboxy-4-hydroxybenzenesulfonate
3-carboxylato-4-hydroxybenzenesulfonate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.990(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7682(8)
_cell_length_b                   5.0027(2)
_cell_length_c                   21.2122(10)
_cell_measurement_reflns_used    4309
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.63
_cell_measurement_theta_min      3.25
_cell_volume                     1948.20(15)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008) within WinGX (Farrugia, 2012)
;
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 16.077
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Gemini-S CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6235
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.346
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2010)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.216
_refine_ls_abs_structure_details 'Flack (1983), 1668 Friedel pairs'
_refine_ls_abs_structure_Flack   0.47(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3804
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0372P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                3399
_reflns_number_total             3804
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3289.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2018954
_cod_database_fobs_code          2018954