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_2242527
_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          '[Li2 (C6 H4 O8 S2) (H2 O)2]2, H2 O'
_chemical_formula_moiety         '2(C6 H8 Li2 O10 S2), H2 O'
_chemical_formula_sum            'C12 H18 Li4 O21 S4'
_chemical_formula_weight         654.26
_chemical_name_systematic
;
\m-4,5-Dihydroxybenzene-1,3-disulfonato-bis[aqualithium(I)] hemihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.997(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5847(18)
_cell_length_b                   7.4498(15)
_cell_length_c                   17.599(4)
_cell_measurement_reflns_used    3529
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.816
_cell_measurement_theta_min      2.236
_cell_volume                     1224.4(4)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_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 0.986
_diffrn_measured_fraction_theta_max 0.981
_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  0.0494
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15864
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.848
_diffrn_reflns_theta_min         2.236
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_description       plank
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.479
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2851
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0437P)^2^+1.2637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                2313
_reflns_number_total             2851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2730sup1.cif
_cod_data_source_block           LiTiron
_cod_original_cell_volume        1224.5(4)
_cod_database_code               2242527
_cod_database_fobs_code          2242527
_shelx_estimated_absorpt_t_min   0.892
_shelx_estimated_absorpt_t_max   0.980
_shelx_hkl_checksum              90373
_shelx_res_checksum              28601