#------------------------------------------------------------------------------
#$Date: 2016-02-14 15:26:36 +0100 (dom 14 de feb de 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/56/2005680.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2005680
loop_
_publ_author_name
'Kemnitz, E.'
'Werner, C.'
'Trojanov, S.'
_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          'H2 S O4'
_chemical_formula_structural     'H2 S O4'
_chemical_formula_sum            'H2 O4 S'
_chemical_formula_weight         98.08
_chemical_melting_point          10.5
_chemical_name_common            'sulfuric acid'
_chemical_name_systematic        'dihydrogen sulfate'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.
_cell_angle_beta                 111.39(3)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   8.181(2)
_cell_length_b                   4.6960(10)
_cell_length_c                   8.563(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      11
_cell_volume                     306.31(14)
_computing_structure_refinement  SHELXL93
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      113(2)
_diffrn_measurement_device       'Stoe-STADI four-circle'
_diffrn_measurement_method       θ-2θ
_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    0.0086
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            453
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         5.10
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_time  1260
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             200
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.325
_refine_ls_extinction_coef       0.029(4)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.139
_refine_ls_goodness_of_fit_obs   1.155
_refine_ls_hydrogen_treatment    'refall isotropically'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_restrained_S_obs      1.155
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_obs          0.0212
_refine_ls_shift/esd_max         -0.446
_refine_ls_shift/esd_mean        0.141
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0269P)^2^ + 0.5004P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0623
_refine_ls_wR_factor_obs         0.0576
_reflns_number_observed          425
_reflns_number_total             453
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            sk1004.cif
_cod_data_source_block           I
_cod_original_cell_volume        306.31(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'H2 O4 S1'
_cod_database_code               2005680
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
S 0.0069(2) 0.0093(2) 0.0142(2) 0.000 0.0056(2) 0.000
O1 0.0113(4) 0.0172(5) 0.0254(5) -0.0061(4) 0.0092(4) -0.0054(4)
O2 0.0112(5) 0.0189(5) 0.0176(5) -0.0019(4) 0.0060(4) 0.0051(4)
loop_
_atom_site_label
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
S 1 0 0.07450(9) 0.25 0.0097(2) Uani d S S
O1 1 -0.15928(13) -0.0822(2) 0.17792(13) 0.0173(2) Uani d . O
O2 1 0.00920(13) 0.2733(2) 0.11080(12) 0.0157(2) Uani d . O
H 1 0.0883(35) 0.3275(53) 0.1281(30) 0.035(7) Uiso d . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 S O1 . 2 117.87(9) no
O1 S O2 . 2 110.70(6) no
O1 S O2 2 2 105.85(6) no
O1 S O2 . . 105.85(6) no
O1 S O2 2 . 110.70(6) no
O2 S O2 2 . 105.22(8) no
S O2 H . . 112.(2) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S O1 . 1.4261(10) no
S O1 2 1.4261(10) no
S O2 2 1.5374(10) no
S O2 . 1.5374(10) no
O2 H . 0.66(3) no
