Water-induced pseudo-quadruple hydrogen-bonding motifs in xanthine–inorganic acid complexes
Sridhar, Balasubramanian; Acta Crystallographica Section C 67 (2011) o382–o386; doi:10.1107/S0108270111036493

data_2018242
_publ_section_title
;
 Water-induced pseudo-quadruple hydrogen-bonding motifs in
 xanthine--inorganic acid complexes
;
_journal_coeditor_code           DN3164
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o382
_journal_page_last               o386
_journal_paper_doi               10.1107/S0108270111036493
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C5 H5 N4 O2 +, H O4 S -, H2 O'
_chemical_formula_moiety         'C5 H5 N4 O2 +, H O4 S -, H2 O'
_chemical_formula_sum            'C5 H8 N4 O7 S'
_chemical_formula_weight         268.21
_chemical_name_common            'Xanthinium hydrogen sulfate hydrate'
_chemical_name_systematic
;
2,6-dioxo-1,2,3,6-tetrahydro-9<i>H</i>-purin-7-ium hydrogen sulfate monohydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.510(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.183(5)
_cell_length_b                   24.805(5)
_cell_length_c                   7.701(5)
_cell_measurement_reflns_used    9350
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.72
_cell_volume                     962.7(11)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10396
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.335
_refine_ls_abs_structure_details
'Flack & Bernardinelli (2000), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   0.13(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         3998
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.1425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                3939
_reflns_number_total             3998
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn3164.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2018242
_cod_database_fobs_code          2018242