Crystal structures of sodium-, lithium-, and ammonium 4,5-dihydroxybenzene-1,3-disulfonate (tiron) hydrates
Herbst-Gervasoni, Corey J.; Gau, Michael R.; Zdilla, Michael J.; Valentine, Ann M.; Acta Crystallographica Section E 74 (2018) 918–925; doi:10.1107/S2056989018008009

data_2242526
_publ_section_title
;
 Crystal structures of sodium-, lithium-, and ammonium
 4,5-dihydroxybenzene-1,3-disulfonate (tiron) hydrates
;
_journal_coeditor_code           ZL2730
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              918
_journal_page_last               925
_journal_paper_doi               10.1107/S2056989018008009
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '2N H4 +, C6 H4 O8 S2 2-, H2 O'
_chemical_formula_moiety         '2(N H4 +), C6 H4 O8 S2 2-, H2 O'
_chemical_formula_sum            'C6 H14 N2 O9 S2'
_chemical_formula_weight         322.31
_chemical_name_common            'NH4 Tiron'
_chemical_name_systematic
;
Diammonium 4,5-dihydroxybenzene-1,3-disulfonate monohydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.5023(15)
_cell_length_b                   18.779(4)
_cell_length_c                   20.236(4)
_cell_measurement_reflns_used    511
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.015
_cell_measurement_theta_min      2.959
_cell_volume                     2471.0(9)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1471
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12544
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.339
_diffrn_reflns_theta_min         2.013
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       plank
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.531
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2255
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+0.6346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                1354
_reflns_number_total             2255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2730sup1.cif
_cod_data_source_block           NH4Tiron
_cod_original_cell_volume        2470.9(9)
_cod_database_code               2242526
_cod_database_fobs_code          2242526
_shelx_estimated_absorpt_t_min   0.956
_shelx_estimated_absorpt_t_max   0.983
_shelx_hkl_checksum              99892
_shelx_res_checksum              73191