#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/32/4313262.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4313262
loop_
_publ_author_name
'Paulina M. Dominiak'
'Joanna Herold'
'Waclaw Kolodziejski'
'Krzysztof Woźniak'
_publ_contact_author_address
;    Chemistry Department
    The University of Warsaw
    ul. Pasteura 1
    02 093 Warszawa
    Poland
;
_publ_contact_author_email       kwozniak@chem.uw.edu.pl
_publ_contact_author_fax         48(22)8222892
_publ_contact_author_name        'Krzysztof Wozniak'
_publ_contact_author_phone       48(22)8222892
_publ_section_title
;
 H-Bonding Dependent Structures of (NH4+)3H+(SO42-)2. Mechanisms of Phase
 Transitions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1590
_journal_page_last               1598
_journal_paper_doi               10.1021/ic025705b
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         (NH4)3H(SO4)2
_chemical_formula_sum            'H13 N3 O8 S2'
_chemical_formula_weight         247.25
_chemical_name_systematic
;
triammonium hydrogen disulphate
;
_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                90.46(3)
_cell_angle_beta                 110.04(3)
_cell_angle_gamma                100.62(3)
_cell_formula_units_Z            4
_cell_length_a                   8.2670(17)
_cell_length_b                   10.081(2)
_cell_length_c                   11.585(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      45
_cell_measurement_theta_min      4
_cell_volume                     888.8(4)
_computing_cell_refinement       CrysAlisRED
_computing_data_collection       CrysAlisCCD
_computing_data_reduction        CrysAlisRED
_computing_molecular_graphics    Diamond
_computing_publication_material  ShelxTL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '1 frame'
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       'omega scan'
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16194
_diffrn_reflns_theta_full        28.77
_diffrn_reflns_theta_max         28.77
_diffrn_reflns_theta_min         3.13
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  65
_diffrn_standards_number         13
_exptl_absorpt_coefficient_mu    0.626
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.6
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.0236(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0405
_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)+(0.0521P)²+1.0120P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1269
_reflns_number_gt                3279
_reflns_number_total             4332
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025705b_s1_1.cif
_cod_data_source_block           PhaseV
_cod_original_cell_volume        888.8(3)
_cod_database_code               4313262
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.71984(7) 0.45502(5) 0.41258(5) 0.01289(16) Uani 1 1 d . . .
O1 O 0.5259(2) 0.43334(16) 0.34211(16) 0.0206(4) Uani 1 1 d . . .
O2 O 0.7923(2) 0.60106(15) 0.42045(15) 0.0175(3) Uani 1 1 d . . .
O3 O 0.7469(2) 0.40813(16) 0.53584(15) 0.0199(4) Uani 1 1 d . . .
O4 O 0.7981(2) 0.37876(16) 0.34543(15) 0.0196(4) Uani 1 1 d . . .
S2 S 0.26978(7) 0.53473(5) 0.08043(5) 0.01290(16) Uani 1 1 d . . .
O5 O 0.4689(2) 0.54733(17) 0.14394(16) 0.0208(4) Uani 1 1 d . . .
O6 O 0.1898(2) 0.39216(15) 0.07609(15) 0.0188(3) Uani 1 1 d . . .
O7 O 0.2437(2) 0.58060(17) -0.04213(15) 0.0215(4) Uani 1 1 d . . .
O8 O 0.2130(2) 0.62012(17) 0.15446(14) 0.0195(4) Uani 1 1 d . . .
S21 S 0.27014(7) 0.03545(5) 0.30387(5) 0.01285(16) Uani 1 1 d . . .
O21 O 0.4719(2) 0.05789(17) 0.33771(16) 0.0208(4) Uani 1 1 d . . .
O22 O 0.2072(2) -0.10950(15) 0.30397(15) 0.0186(3) Uani 1 1 d . . .
O23 O 0.2426(2) 0.11301(16) 0.39894(14) 0.0195(4) Uani 1 1 d . . .
O24 O 0.2001(2) 0.08501(17) 0.18246(14) 0.0199(4) Uani 1 1 d . . .
S22 S 0.72566(7) 0.95681(5) 0.19845(5) 0.01291(16) Uani 1 1 d . . .
O25 O 0.5315(2) 0.93412(16) 0.16990(15) 0.0195(4) Uani 1 1 d . . .
O26 O 0.7899(2) 1.10207(15) 0.19274(15) 0.0188(3) Uani 1 1 d . . .
O27 O 0.7614(2) 0.87637(17) 0.10740(15) 0.0204(4) Uani 1 1 d . . .
O28 O 0.8074(2) 0.91563(17) 0.32312(15) 0.0202(4) Uani 1 1 d . . .
N1 N 0.1004(3) 0.8473(2) 0.01239(19) 0.0165(4) Uani 1 1 d . . .
N2 N 0.5069(3) 0.7451(2) 0.3831(2) 0.0159(4) Uani 1 1 d . . .
N3 N 0.1073(3) 0.3505(2) 0.2942(2) 0.0176(4) Uani 1 1 d . . .
N4 N 0.5030(3) 0.2433(2) 0.11237(19) 0.0159(4) Uani 1 1 d . . .
N21 N 0.9078(3) 0.6527(2) 0.21753(19) 0.0157(4) Uani 1 1 d . . .
N23 N 0.9033(3) 0.1544(2) 0.48603(19) 0.0159(4) Uani 1 1 d . . .
H1 H 0.134(4) 0.873(3) -0.050(3) 0.032(8) Uiso 1 1 d . . .
H2 H -0.010(5) 0.826(4) -0.022(3) 0.045(10) Uiso 1 1 d . . .
H3 H 0.148(5) 0.799(4) 0.053(4) 0.043(11) Uiso 1 1 d . . .
H4 H 0.133(4) 0.922(4) 0.063(3) 0.035(9) Uiso 1 1 d . . .
H5A H 0.581(5) 0.705(4) 0.387(3) 0.043(10) Uiso 1 1 d . . .
H5B H 0.465(5) 0.765(4) 0.315(4) 0.057(12) Uiso 1 1 d . . .
H6A H 0.556(4) 0.826(3) 0.426(3) 0.020(7) Uiso 1 1 d . . .
H6B H 0.441(4) 0.697(3) 0.412(3) 0.018(7) Uiso 1 1 d . . .
H7 H 0.163(4) 0.419(3) 0.344(3) 0.032(8) Uiso 1 1 d . . .
H8 H 0.001(5) 0.339(4) 0.284(3) 0.042(10) Uiso 1 1 d . . .
H9 H 0.144(4) 0.287(3) 0.326(3) 0.027(8) Uiso 1 1 d . . .
H10 H 0.116(5) 0.375(4) 0.221(4) 0.043(10) Uiso 1 1 d . . .
H11A H 0.462(5) 0.253(3) 0.166(3) 0.042(10) Uiso 1 1 d . . .
H11B H 0.579(5) 0.198(4) 0.141(3) 0.046(10) Uiso 1 1 d . . .
H12A H 0.427(4) 0.188(3) 0.056(3) 0.028(8) Uiso 1 1 d . . .
H12B H 0.547(4) 0.313(3) 0.092(3) 0.024(8) Uiso 1 1 d . . .
H21 H 0.855(4) 0.585(3) 0.167(3) 0.017(7) Uiso 1 1 d . . .
H22 H 1.013(5) 0.665(3) 0.233(3) 0.033(9) Uiso 1 1 d . . .
H23 H 0.868(4) 0.718(4) 0.184(3) 0.033(9) Uiso 1 1 d . . .
H24 H 0.889(4) 0.625(3) 0.288(3) 0.027(8) Uiso 1 1 d . . .
H27 H 0.860(5) 0.130(4) 0.539(4) 0.042(10) Uiso 1 1 d . . .
H28 H 1.013(5) 0.167(3) 0.527(3) 0.036(9) Uiso 1 1 d . . .
H29 H 0.868(5) 0.213(4) 0.441(4) 0.051(11) Uiso 1 1 d . . .
H30 H 0.868(4) 0.081(3) 0.432(3) 0.033(8) Uiso 1 1 d . . .
H5O H 0.493(4) 0.497(3) 0.227(3) 0.062(12) Uiso 1 1 d . . .
H21O H 0.502(6) 0.007(5) 0.269(5) 0.13(2) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 S1 O3 110.97(10) . . ?
O4 S1 O2 110.60(10) . . ?
O3 S1 O2 110.54(10) . . ?
O4 S1 O1 108.28(10) . . ?
O3 S1 O1 108.72(10) . . ?
O2 S1 O1 107.62(10) . . ?
S1 O1 H5O 110.5(13) . . ?
O8 S2 O7 112.34(10) . . ?
O8 S2 O6 111.95(10) . . ?
O7 S2 O6 111.94(10) . . ?
O8 S2 O5 107.04(10) . . ?
O7 S2 O5 106.18(10) . . ?
O6 S2 O5 106.94(10) . . ?
S2 O5 H5O 108.7(18) . . ?
O23 S21 O24 112.52(10) . . ?
O23 S21 O22 112.24(10) . . ?
O24 S21 O22 112.28(10) . . ?
O23 S21 O21 105.66(10) . . ?
O24 S21 O21 106.77(10) . . ?
O22 S21 O21 106.81(10) . . ?
S21 O21 H21O 110(3) . . ?
O27 S22 O28 110.67(10) . . ?
O27 S22 O26 110.36(10) . . ?
O28 S22 O26 110.31(10) . . ?
O27 S22 O25 109.14(10) . . ?
O28 S22 O25 108.26(10) . . ?
O26 S22 O25 108.03(10) . . ?
H1 N1 H2 102(3) . . ?
H1 N1 H3 117(4) . . ?
H2 N1 H3 119(4) . . ?
H1 N1 H4 104(3) . . ?
H2 N1 H4 112(3) . . ?
H3 N1 H4 102(3) . . ?
H5A N2 H5B 110(4) . . ?
H5A N2 H6A 109(3) . . ?
H5B N2 H6A 103(3) . . ?
H5A N2 H6B 105(3) . . ?
H5B N2 H6B 117(3) . . ?
H6A N2 H6B 113(3) . . ?
H7 N3 H8 109(3) . . ?
H7 N3 H9 107(3) . . ?
H8 N3 H9 108(3) . . ?
H7 N3 H10 104(3) . . ?
H8 N3 H10 106(3) . . ?
H9 N3 H10 122(3) . . ?
H11A N4 H11B 106(3) . . ?
H11A N4 H12A 107(3) . . ?
H11B N4 H12A 101(3) . . ?
H11A N4 H12B 115(3) . . ?
H11B N4 H12B 109(3) . . ?
H12A N4 H12B 118(3) . . ?
H21 N21 H22 111(3) . . ?
H21 N21 H23 106(3) . . ?
H22 N21 H23 111(3) . . ?
H21 N21 H24 102(3) . . ?
H22 N21 H24 106(3) . . ?
H23 N21 H24 120(3) . . ?
H27 N23 H28 102(3) . . ?
H27 N23 H29 121(4) . . ?
H28 N23 H29 117(3) . . ?
H27 N23 H30 103(3) . . ?
H28 N23 H30 112(3) . . ?
H29 N23 H30 101(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O4 1.4605(17) . ?
S1 O3 1.4640(16) . ?
S1 O2 1.4731(16) . ?
S1 O1 1.5019(17) . ?
O1 H5O 1.44(4) . ?
S2 O8 1.4524(16) . ?
S2 O7 1.4538(17) . ?
S2 O6 1.4600(16) . ?
S2 O5 1.5360(17) . ?
O5 H5O 1.07(4) . ?
S21 O23 1.4492(16) . ?
S21 O24 1.4570(16) . ?
S21 O22 1.4581(16) . ?
S21 O21 1.5485(17) . ?
O21 H21O 1.06(5) . ?
S22 O27 1.4650(17) . ?
S22 O28 1.4693(17) . ?
S22 O26 1.4730(16) . ?
S22 O25 1.4959(17) . ?
N1 H1 0.88(4) . ?
N1 H2 0.84(4) . ?
N1 H3 0.75(4) . ?
N1 H4 0.89(4) . ?
N2 H5A 0.78(4) . ?
N2 H5B 0.79(4) . ?
N2 H6A 0.90(3) . ?
N2 H6B 0.82(3) . ?
N3 H7 0.85(4) . ?
N3 H8 0.83(4) . ?
N3 H9 0.79(3) . ?
N3 H10 0.91(4) . ?
N4 H11A 0.82(4) . ?
N4 H11B 0.82(4) . ?
N4 H12A 0.85(3) . ?
N4 H12B 0.81(3) . ?
N21 H21 0.84(3) . ?
N21 H22 0.81(4) . ?
N21 H23 0.83(4) . ?
N21 H24 0.92(3) . ?
N23 H27 0.83(4) . ?
N23 H28 0.85(4) . ?
N23 H29 0.82(4) . ?
N23 H30 0.90(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O27 0.88(4) 2.68(3) 3.311(3) 129(3) 2_675
N1 H3 O8 0.75(4) 2.21(4) 2.936(3) 164(4) .
N1 H3 O7 0.75(4) 2.81(4) 3.270(3) 123(3) .
N1 H4 O22 0.89(4) 2.68(3) 3.189(3) 117(3) 1_565
N2 H5A O2 0.78(4) 2.13(4) 2.904(3) 173(3) .
N2 H5B O8 0.79(4) 2.47(4) 2.985(3) 124(3) .
N2 H5B O25 0.79(4) 2.53(4) 3.170(3) 140(3) .
N3 H9 O23 0.79(3) 2.13(4) 2.925(3) 176(3) .
N3 H9 O24 0.79(3) 2.82(3) 3.287(3) 120(3) .
N3 H10 O6 0.91(4) 1.97(4) 2.849(3) 162(3) .
N3 H10 O8 0.91(4) 2.66(4) 3.307(3) 129(3) .
N4 H11A O24 0.82(4) 2.55(3) 3.069(3) 122(3) .
N4 H11A O1 0.82(4) 2.57(4) 3.198(3) 135(3) .
N21 H21 O6 0.84(3) 2.73(3) 3.223(3) 119(2) 2_665
N21 H23 O27 0.83(4) 2.03(4) 2.858(3) 177(3) .
N21 H23 O28 0.83(4) 2.77(3) 3.266(3) 120(3) .
N23 H29 O3 0.82(4) 2.74(4) 3.202(3) 117(3) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 10745320
