#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/54/2105485.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_2105485
loop_
_publ_author_name
'Sohn, Yoo Jung'
'Sparta, Karine M.'
'Prinz, Sebastian'
'Meven, Martin'
'Roth, Georg'
'Heger, Gernot'
_publ_section_title
;
 Proton ordering in (NH₄)₃H(SO₄)₂ at low-temperature phase
 transitions
;
_journal_coeditor_code           HW5024
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              336
_journal_page_last               343
_journal_paper_doi               10.1107/S2052519213013092
_journal_volume                  69
_journal_year                    2013
_chemical_formula_moiety         'H O8 S2, 3(H4 N)'
_chemical_formula_sum            'H13 N3 O8 S2'
_chemical_formula_weight         247.25
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.44(5)
_cell_angle_beta                 110.07(6)
_cell_angle_gamma                100.64(5)
_cell_formula_units_Z            4
_cell_length_a                   8.282(4)
_cell_length_b                   10.095(5)
_cell_length_c                   11.613(6)
_cell_measurement_reflns_used    17019
_cell_measurement_temperature    126
_cell_measurement_theta_max      64.45
_cell_measurement_theta_min      5.35
_cell_volume                     893.6(9)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1996)'
_computing_molecular_graphics    'Atoms 5.1'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      126
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'rotation method'
_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  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21478
_diffrn_reflns_theta_full        32.05
_diffrn_reflns_theta_max         32.05
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.9422
_exptl_absorpt_correction_T_min  0.7965
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.654
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         6139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0555P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                3270
_reflns_number_total             6139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            hw5024.cif
_cod_data_source_block           I
_cod_original_cell_volume        893.6(8)
_cod_database_code               2105485
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_symmetry_multiplicity
S S1 0.27434(8) -0.45664(6) 0.30120(6) 0.01303(14) Uani d 1 1
S S2 0.73018(8) -0.53509(6) 0.19599(6) 0.01292(14) Uani d 1 1
S S3 0.28036(8) 0.04511(6) 0.08780(6) 0.01307(14) Uani d 1 1
S S4 0.73056(8) -0.03433(6) 0.41981(6) 0.01277(14) Uani d 1 1
O O1 0.4686(3) -0.4342(2) 0.32952(19) 0.0207(4) Uani d 1 1
O O2 0.5280(3) -0.5579(2) 0.1617(2) 0.0214(4) Uani d 1 1
O O3 0.2100(3) -0.60192(18) 0.30772(18) 0.0181(4) Uani d 1 1
O O4 0.7926(3) -0.39041(18) 0.19578(18) 0.0187(4) Uani d 1 1
O O5 0.2384(3) -0.3761(2) 0.39211(18) 0.0199(4) Uani d 1 1
O O6 0.7568(3) -0.6131(2) 0.10102(18) 0.0199(4) Uani d 1 1
O O7 0.1918(3) -0.4163(2) 0.17651(18) 0.0193(4) Uani d 1 1
O O8 0.8000(3) -0.5844(2) 0.31794(18) 0.0196(4) Uani d 1 1
O O9 0.4743(3) 0.0669(2) 0.15845(19) 0.0211(4) Uani d 1 1
O O10 0.5304(3) -0.0470(2) 0.3564(2) 0.0215(4) Uani d 1 1
O O11 0.2076(3) -0.10103(17) 0.07996(17) 0.0173(4) Uani d 1 1
O O12 0.8113(3) 0.10747(18) 0.42362(17) 0.0187(4) Uani d 1 1
O O13 0.2532(3) 0.0915(2) -0.03586(18) 0.0200(4) Uani d 1 1
O O14 0.7866(3) -0.1204(2) 0.34556(18) 0.0197(4) Uani d 1 1
O O15 0.2013(3) 0.12149(19) 0.15426(17) 0.0188(4) Uani d 1 1
O O16 0.7558(3) -0.0803(2) 0.54178(18) 0.0200(4) Uani d 1 1
N N1 0.5028(3) -0.2577(3) 0.6124(2) 0.0163(5) Uani d 1 1
N N2 0.5078(3) -0.7555(3) -0.1168(2) 0.0163(5) Uani d 1 1
N N3 0.1012(3) -0.6529(3) 0.5127(2) 0.0176(5) Uani d 1 1
N N4 0.0963(3) 0.3453(3) 0.0141(2) 0.0172(5) Uani d 1 1
N N5 0.0918(4) -0.1523(3) 0.2823(3) 0.0172(5) Uani d 1 1
N N6 0.1081(4) -0.1497(3) -0.2045(2) 0.0181(5) Uani d 1 1
H H1 0.499(7) -0.538(5) 0.220(5) 0.061(15) Uiso d 1 1
H H2 0.517(6) -0.011(4) 0.280(4) 0.051(13) Uiso d 1 1
H H3 0.549(4) -0.193(3) 0.596(3) 0.013(8) Uiso d 1 1
H H4 0.421(6) -0.317(4) 0.545(4) 0.043(12) Uiso d 1 1
H H5 0.587(5) -0.308(4) 0.642(4) 0.034(10) Uiso d 1 1
H H6 0.443(6) -0.246(4) 0.672(4) 0.039(11) Uiso d 1 1
H H7 0.428(5) -0.800(3) -0.087(3) 0.018(8) Uiso d 1 1
H H8 0.561(4) -0.672(3) -0.069(3) 0.018(8) Uiso d 1 1
H H9 0.467(7) -0.737(5) -0.188(5) 0.058(14) Uiso d 1 1
H H10 0.579(7) -0.794(5) -0.121(4) 0.046(13) Uiso d 1 1
H H11 0.134(6) -0.631(5) 0.453(5) 0.049(13) Uiso d 1 1
H H12 0.141(6) -0.712(5) 0.562(4) 0.045(12) Uiso d 1 1
H H13 0.126(5) -0.581(4) 0.558(4) 0.028(10) Uiso d 1 1
H H14 0.0000 -0.680(4) 0.487(3) 0.027(10) Uiso d 1 1
H H15 0.137(5) 0.363(4) -0.040(4) 0.026(10) Uiso d 1 1
H H16 0.127(5) 0.284(4) 0.059(4) 0.036(11) Uiso d 1 1
H H17 -0.016(6) 0.334(4) -0.026(4) 0.033(10) Uiso d 1 1
H H18 0.126(5) 0.417(4) 0.063(4) 0.027(10) Uiso d 1 1
H H19 0.112(6) -0.130(5) 0.222(5) 0.045(13) Uiso d 1 1
H H20 0.143(4) -0.087(3) 0.332(3) 0.014(8) Uiso d 1 1
H H21 -0.012(7) -0.170(4) 0.264(4) 0.042(13) Uiso d 1 1
H H22 0.127(5) -0.216(4) 0.313(3) 0.021(9) Uiso d 1 1
H H23 0.141(6) -0.224(4) -0.173(4) 0.032(10) Uiso d 1 1
H H24 0.116(5) -0.128(4) -0.273(4) 0.022(9) Uiso d 1 1
H H25 0.009(7) -0.167(5) -0.218(4) 0.048(14) Uiso d 1 1
H H26 0.170(5) -0.073(4) -0.163(4) 0.035(11) Uiso d 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
O5 S1 O7 110.70(13) y
O5 S1 O3 110.01(13) y
O7 S1 O3 110.25(13) y
O5 S1 O1 109.37(13) y
O7 S1 O1 108.47(14) y
O3 S1 O1 107.99(13) y
O6 S2 O4 112.52(13) y
O6 S2 O8 112.79(14) y
O4 S2 O8 112.22(13) y
O6 S2 O2 105.23(14) y
O4 S2 O2 106.78(14) y
O8 S2 O2 106.68(14) y
O15 S3 O13 110.94(13) y
O15 S3 O11 110.50(13) y
O13 S3 O11 110.32(13) y
O15 S3 O9 108.50(13) y
O13 S3 O9 108.79(14) y
O11 S3 O9 107.70(13) y
O16 S4 O12 112.32(13) y
O16 S4 O14 112.35(14) y
O12 S4 O14 111.73(13) y
O16 S4 O10 105.78(14) y
O12 S4 O10 107.24(14) y
O14 S4 O10 106.96(13) y
S2 O2 H1 113(4) y
S4 O10 H2 105(3) y
H3 N1 H4 116(4) y
H3 N1 H5 105(4) y
H4 N1 H5 101(4) y
H3 N1 H6 115(4) y
H4 N1 H6 107(4) y
H5 N1 H6 111(4) y
H7 N2 H8 108(3) y
H7 N2 H9 114(4) y
H8 N2 H9 106(4) y
H7 N2 H10 117(4) y
H8 N2 H10 110(4) y
H9 N2 H10 101(5) y
H11 N3 H12 124(5) y
H11 N3 H13 105(4) y
H12 N3 H13 105(4) y
H11 N3 H14 109(4) y
H12 N3 H14 104(4) y
H13 N3 H14 110(4) y
H15 N4 H16 119(4) y
H15 N4 H17 102(4) y
H16 N4 H17 115(4) y
H15 N4 H18 108(4) y
H16 N4 H18 105(4) y
H17 N4 H18 107(4) y
H19 N5 H20 104(4) y
H19 N5 H21 107(5) y
H20 N5 H21 116(4) y
H19 N5 H22 118(5) y
H20 N5 H22 106(3) y
H21 N5 H22 107(4) y
H23 N6 H24 120(4) y
H23 N6 H25 101(4) y
H24 N6 H25 104(4) y
H23 N6 H26 116(4) y
H24 N6 H26 96(3) y
H25 N6 H26 119(5) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
S1 O5 1.468(2) y
S1 O7 1.471(2) y
S1 O3 1.477(2) y
S1 O1 1.500(2) y
S2 O6 1.450(2) y
S2 O4 1.457(2) y
S2 O8 1.464(2) y
S2 O2 1.554(2) y
S3 O15 1.464(2) y
S3 O13 1.469(2) y
S3 O11 1.477(2) y
S3 O9 1.505(2) y
S4 O16 1.452(2) y
S4 O12 1.457(2) y
S4 O14 1.458(2) y
S4 O10 1.546(2) y
O2 H1 0.83(5) y
O10 H2 0.94(5) y
N1 H3 0.76(3) y
N1 H4 0.95(4) y
N1 H5 0.91(4) y
N1 H6 1.00(5) y
N2 H7 0.90(4) y
N2 H8 0.95(3) y
N2 H9 0.81(5) y
N2 H10 0.78(5) y
N3 H11 0.84(5) y
N3 H12 0.86(5) y
N3 H13 0.84(4) y
N3 H14 0.780(6) y
N4 H15 0.82(4) y
N4 H16 0.83(4) y
N4 H17 0.87(4) y
N4 H18 0.86(4) y
N5 H19 0.80(5) y
N5 H20 0.82(3) y
N5 H21 0.80(5) y
N5 H22 0.79(4) y
N6 H23 0.89(4) y
N6 H24 0.84(4) y
N6 H25 0.76(5) y
N6 H26 0.88(4) y
