Reinvestigation of Crystalline Sulfuric Acid and Oxonium Hydrogensulfate
Kemnitz, E.; Werner, C.; Trojanov, S.; Acta Crystallographica Section C 52 (1996) 2665–2668; doi:10.1107/S0108270196006749

data_2005681
_publ_section_title
;
 Reinvestigation of Crystalline Sulfuric Acid and Oxonium
 Hydrogensulfate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2665
_journal_page_last               2668
_journal_paper_doi               10.1107/S0108270196006749
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '(H3 O)(H S O4)'
_chemical_formula_structural     '(H3 O)(H S O4)'
_chemical_formula_sum            'H4 O5 S'
_chemical_formula_weight         116.09
_chemical_melting_point          8.5
_chemical_name_common            'sulfuric acid monohydrate'
_chemical_name_systematic        'oxonium hydrogen sulfate'
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.
_cell_angle_beta                 106.18(3)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   7.0770(10)
_cell_length_b                   6.9550(10)
_cell_length_c                   8.150(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      9
_cell_volume                     385.26(14)
_computing_structure_refinement  SHELXL-93
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'Stoe-STADI four-circle'
_diffrn_measurement_method       \q-2\q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0091
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2384
_diffrn_reflns_theta_max         40
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        6.2
_diffrn_standards_interval_time  150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             240
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.097
_refine_diff_density_min         -1.248
_refine_ls_extinction_coef       3.25(9)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.126
_refine_ls_goodness_of_fit_obs   1.145
_refine_ls_hydrogen_treatment    'refall isotropically'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         2364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.394
_refine_ls_restrained_S_obs      1.145
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_obs          0.0332
_refine_ls_shift/esd_max         0.073
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0604P)^2^ + 0.0491P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1075
_refine_ls_wR_factor_obs         0.0858
_reflns_number_observed          2224
_reflns_number_total             2384
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            sk1004.cif
_cod_data_source_block           II
_cod_original_cell_volume        385.26(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2005681