Bis(1,2,3,5-tetramethyl-4-nitropyrazolium) dihydronium tris(4-methyl-3,5-dinitrobenzenesulfonate) forms <i>C</i>(8) chains through O—H···O bonding <i>via</i> the dihydronium cation
Janet M. S. Skakle; James L. Wardell; Acta Crystallographica Section E 62 (2006) o1402–o1404; doi:10.1107/S1600536806008749

data_2208654
_publ_section_title
;
 Bis(1,2,3,5-tetramethyl-4-nitropyrazolium) dihydronium
 tris(4-methyl-3,5-dinitrobenzenesulfonate) forms <i>C</i>(8) chains
 through O---H&#x00B7;&#x00B7;&#x00B7;O bonding <i>via</i> the
 dihydronium cation
;
_journal_coeditor_code           LH2008
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1402
_journal_page_last               o1404
_journal_paper_doi               10.1107/S1600536806008749
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '2C7 H12 N3 O2 +, H5 O2 +, 3C7 H5 N2 O7 S -'
_chemical_formula_moiety         '2C7 H12 N3 O2 +, H5 O2 +, 3C7 H5 N2 O7 S -'
_chemical_formula_sum            'C35 H44 N12 O27 S3'
_chemical_formula_weight         1161.00
_chemical_name_systematic
;
Bis[1,2,3,5-tetramethyl-4-nitropyrazolium] dihydronium
tris(4-methyl-3,5-dinitrobenzenesulfonate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.7241(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.0927(5)
_cell_length_b                   8.17230(10)
_cell_length_c                   24.0602(6)
_cell_measurement_reflns_used    10634
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     4913.52(17)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) and COLLECT'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'DENZO and COLLECT'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement
'OSCAIL (McArdle, 2003) and SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker--Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            53726
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.99000
_exptl_absorpt_correction_T_min  0.83441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.591
_refine_ls_extinction_coef       0.0067(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         11088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0891P)^2^+0.908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1454
_reflns_number_gt                8214
_reflns_number_total             11088
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2008.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2208654
_cod_database_fobs_code          2208654