#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/54/2105486.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_2105486
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         247.2
_chemical_name_systematic        ' ?'
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 101.75(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.473(8)
_cell_length_b                   5.849(3)
_cell_length_c                   10.131(5)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    250
_cell_measurement_theta_max      18.57
_cell_measurement_theta_min      12.92
_cell_volume                     897.7(8)
_computing_cell_refinement       DIF4N
_computing_data_collection       'DIF4N (modified Linux version of DIF4)'
_computing_data_reduction        'PRON (Scherf, 1998)'
_computing_molecular_graphics    'Atoms 5.1'
_computing_publication_material
'Jana2006 (Petricek, Dusek & Palatinus, 2006)'
_computing_structure_refinement
'Jana2006 (Petricek, Dusek & Palatinus, 2006)'
_diffrn_ambient_temperature      250
_diffrn_measured_fraction_theta_full 0.94
_diffrn_measurement_device       'single-crystal diffractometer HEiDi'
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'Cu (220)'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'nuclear reactor'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.87
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1770
_diffrn_reflns_theta_full        15.43
_diffrn_reflns_theta_max         37.5
_diffrn_reflns_theta_min         3.27
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '360 min'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.002
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.829(2)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             126
_exptl_crystal_size_max          3
_exptl_crystal_size_mid          3
_exptl_crystal_size_min          3
_exptl_crystal_size_rad          0
_refine_diff_density_max         0.97
_refine_diff_density_min         -1.59
_refine_ls_extinction_coef       87E2(4)
_refine_ls_extinction_method
'B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_ref   3.26
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_constraints    2
_refine_ls_number_parameters     208
_refine_ls_number_reflns         1503
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.0359
_refine_ls_shift/su_mean         0.0094
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(σ²(I)+0.0004I²)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1402
_reflns_number_gt                1092
_reflns_number_total             1503
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            hw5024.cif
_cod_data_source_block           II
_cod_database_code               2105486
_cod_database_fobs_code          2105486
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x+1/2,y,-z+1/2
3 -x,-y,-z
4 x+1/2,-y,z+1/2
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 0.3614(5) 0.4667(11) 0.4624(6) 0.025(2) Uani d 1 4
S S2 0.1343(4) 0.0314(10) 0.5395(7) 0.0218(18) Uani d 1 4
N N1 0.75 0.0214(6) 0.75 0.0280(10) Uani d 1 2
N N2 0.75 0.4803(6) 0.25 0.0298(11) Uani d 1 2
N N3 0.44921(19) 0.5239(4) 0.1557(3) 0.0317(8) Uani d 1 4
N N4 0.05054(19) 0.9689(4) 0.8504(3) 0.0324(9) Uani d 1 4
O O1 0.2641(2) 0.4315(7) 0.4463(4) 0.0382(12) Uani d 1 4
O O2 0.2339(2) 0.0620(7) 0.5610(4) 0.0381(12) Uani d 1 4
O O3 0.4011(2) 0.4449(7) 0.6054(3) 0.0320(11) Uani d 1 4
O O4 0.1012(2) 0.0006(6) 0.3945(4) 0.0328(11) Uani d 1 4
O O5 0.3769(2) 0.6950(6) 0.4132(4) 0.0345(11) Uani d 1 4
O O6 0.1200(2) 0.8291(6) 0.6154(4) 0.0336(11) Uani d 1 4
O O7 0.3956(2) 0.2909(6) 0.3836(4) 0.0341(11) Uani d 1 4
O O8 0.0982(2) 0.2365(6) 0.5884(4) 0.0343(11) Uani d 1 4
H H1 0.2489 0.2061 0.5143 0.0396(17) Uiso d 0.651(14) 4
H H2 0.2511 0.2939 0.4857 0.0396(17) Uiso d 0.349(14) 4
H H3 0.7138(7) 0.382(3) 0.1871(13) 0.108(5) Uani d 1 4
H H4 0.7849(8) 0.114(2) 0.8230(10) 0.092(4) Uani d 1 4
H H5 0.7045(10) 0.556(3) 0.274(2) 0.150(8) Uani d 1 4
H H6 0.7954(10) 0.946(4) 0.722(2) 0.167(9) Uani d 1 4
H H7 0.5100(8) 0.538(2) 0.1804(15) 0.094(5) Uani d 1 4
H H8 0.9872(7) 0.930(2) 0.8401(12) 0.080(4) Uani d 1 4
H H9 0.4259(8) 0.685(2) 0.1304(11) 0.089(4) Uani d 1 4
H H10 0.0804(7) 0.8798(17) 0.9281(9) 0.071(3) Uani d 1 4
H H11 0.4377(7) 0.413(2) 0.0783(12) 0.086(4) Uani d 1 4
H H12 0.0590(6) 0.1404(13) 0.8702(8) 0.062(3) Uani d 1 4
H H13 0.4277(8) 0.464(2) 0.2334(10) 0.086(4) Uani d 1 4
H H14 0.0721(7) 0.9245(16) 0.7654(10) 0.072(4) Uani d 1 4
loop_
_atom_type_symbol
_atom_type_scat_length_neutron
_atom_type_scat_source
H -3.739 International_Tables_Vol_C
N 9.360 International_Tables_Vol_C
O 5.803 International_Tables_Vol_C
S 2.847 International_Tables_Vol_C
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
0 4 0
0 0 -6
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 S1 O3 . . 107.9(5) y
O1 S1 O5 . . 108.7(5) y
O1 S1 O7 . . 108.2(4) y
O3 S1 O5 . . 110.7(4) y
O3 S1 O7 . . 110.7(5) y
O5 S1 O7 . . 110.6(5) y
O2 S2 O4 . . 107.1(5) y
O2 S2 O6 . 1_545 106.1(4) y
O2 S2 O8 . . 107.6(4) y
O4 S2 O6 . 1_545 111.8(4) y
O4 S2 O8 . . 111.3(4) y
O6 S2 O8 1_545 . 112.5(5) y
H4 N1 H4 . 2_656 113.1(10) y
H4 N1 H6 . 1_545 99.0(14) y
H4 N1 H6 . 2_646 111.8(16) y
H4 N1 H6 2_656 1_545 111.8(16) y
H4 N1 H6 2_656 2_646 99.0(14) y
H6 N1 H6 1_545 2_646 122.9(19) y
H3 N2 H3 . 2_655 105.4(13) y
H3 N2 H5 . . 95.3(14) y
H3 N2 H5 . 2_655 120.1(17) y
H3 N2 H5 2_655 . 120.1(17) y
H3 N2 H5 2_655 2_655 95.3(14) y
H5 N2 H5 . 2_655 121.4(17) y
H7 N3 H9 . . 105.8(10) y
H7 N3 H11 . . 106.0(11) y
H7 N3 H13 . . 107.9(12) y
H9 N3 H11 . . 113.6(9) y
H9 N3 H13 . . 111.8(11) y
H11 N3 H13 . . 111.2(10) y
H8 N4 H10 1_455 . 104.9(10) y
H8 N4 H12 1_455 1_565 109.2(9) y
H8 N4 H14 1_455 . 109.9(9) y
H10 N4 H12 . 1_565 110.0(8) y
H10 N4 H14 . . 111.3(9) y
H12 N4 H14 1_565 . 111.3(8) y
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
S1 O1 . 1.495(8) y
S1 O3 . 1.460(7) y
S1 O5 . 1.462(8) y
S1 O7 . 1.465(8) y
S2 O2 . 1.523(7) y
S2 O4 . 1.465(7) y
S2 O6 1_545 1.452(7) y
S2 O8 . 1.452(7) y
N1 H4 . 0.985(10) y
N1 H4 2_656 0.985(10) y
N1 H6 1_545 0.92(2) y
N1 H6 2_646 0.92(2) y
N2 H3 . 0.953(14) y
N2 H3 2_655 0.953(14) y
N2 H5 . 0.906(19) y
N2 H5 2_655 0.906(19) y
N3 H7 . 0.927(12) y
N3 H9 . 1.023(12) y
N3 H11 . 1.005(12) y
N3 H13 . 0.980(12) y
N4 H8 1_455 0.991(11) y
N4 H10 . 0.978(10) y
N4 H12 1_565 1.027(8) y
N4 H14 . 1.018(11) y
