Charge-assisted hydrogen bonding in three diaminobenzene salts
Zick, Patricia L.; Geiger, David K.; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618015553

data_2021373
_publ_section_title
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 Charge-assisted hydrogen bonding in three diaminobenzene salts
;
_journal_coeditor_code           OV3114
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618015553
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C6 H10 N2 2+, S O4 2-, 1.5H2 O'
_chemical_formula_moiety         'C6 H10 N2 2+, O4 S 2-, 1.5(H2 O)'
_chemical_formula_sum            'C6 H13 N2 O5.5 S'
_chemical_formula_weight         233.24
_chemical_name_systematic
;
Benzene-1,2-diaminium sulfate sesquihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.308(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.348(3)
_cell_length_b                   9.6720(9)
_cell_length_c                   7.5667(8)
_cell_measurement_reflns_used    6495
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      3.42
_cell_volume                     2018.9(4)
_computing_cell_refinement
;
APEX2 (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009) and Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean 8.3330
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART X2S benchtop'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'doubly curved silicon crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15241
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.087
_diffrn_reflns_theta_min         2.231
_diffrn_source                   'XOS X-beam microfocus source'
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2015)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.382
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2218
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+4.0638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                1881
_reflns_number_total             2218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ov3114sup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;

2019-09-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C6 H10 N2 2+), 2(O4 S 2-), 3(H2 O)'
_cod_original_formula_iupac      '2C6 H10 N2 2+, 2S O4 2-, 3H2 O'
_cod_original_formula_sum        'C12 H26 N4 O11 S2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     466.49
_cod_database_code               2021373
_cod_database_fobs_code          2021373
_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.984
_shelx_hkl_checksum              92775
_shelx_res_checksum              41491