#------------------------------------------------------------------------------
#$Date: 2017-10-13 03:08:28 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201955 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/56/2005681.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_2005681
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          '(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       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    0.0091
_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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
S1 0.01426(10) 0.00903(9) 0.00854(9) -0.00009(4) 0.00126(5) 0.00023(3)
O1 0.0219(2) 0.0125(2) 0.0088(2) -0.00061(15) 0.00135(14) 0.00179(13)
O2 0.0188(2) 0.0113(2) 0.0185(2) 0.0032(2) 0.0009(2) -0.0023(2)
O3 0.0216(2) 0.0147(2) 0.0114(2) -0.0005(2) 0.00259(14) -0.00453(14)
O4 0.0162(2) 0.0221(3) 0.0164(2) -0.0030(2) 0.0022(2) 0.0068(2)
O5 0.0181(2) 0.0122(2) 0.0153(2) -0.00073(15) 0.0017(2) 0.00349(15)
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_type_symbol
S1 1 0.75032(2) 0.15816(2) 0.04183(2) 0.01100(8) Uani d S
O1 1 0.82689(8) 0.06899(8) 0.21041(6) 0.01500(10) Uani d O
O2 1 0.61382(8) 0.31432(8) 0.04153(8) 0.01707(11) Uani d O
O3 1 0.66823(8) 0.01651(8) -0.08874(6) 0.01629(11) Uani d O
O4 1 0.93770(8) 0.24719(9) 0.00759(7) 0.01874(12) Uani d O
O5 1 0.72575(8) 0.69970(8) 0.17478(7) 0.01579(11) Uani d O
H2 1 0.6083(27) 0.7074(31) 0.1053(28) 0.036(5) Uiso d H
H1 1 0.8975(25) 0.3144(25) -0.0780(24) 0.024(4) Uiso d H
H3 1 0.7124(26) 0.6254(32) 0.2663(24) 0.034(5) Uiso d H
H4 1 0.7562(25) 0.8179(28) 0.1927(24) 0.028(4) 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
_geom_angle_publ_flag
O3 S1 O2 112.14(4) no
O3 S1 O1 111.63(4) no
O2 S1 O1 112.93(4) no
O3 S1 O4 109.03(4) no
O2 S1 O4 107.54(4) no
O1 S1 O4 103.02(4) no
S1 O4 H1 105.5(13) no
H2 O5 H3 105.3(18) no
H2 O5 H4 101.7(17) no
H3 O5 H4 118.3(18) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
S1 O3 1.4478(6) no
S1 O2 1.4531(6) no
S1 O1 1.4666(6) no
S1 O4 1.5576(6) no
O4 H1 0.82(2) no
O5 H2 0.87(2) no
O5 H3 0.93(2) no
O5 H4 0.85(2) no
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 10662067
