H-Bonding Dependent Structures of (NH4+)3H+(SO42-)2. Mechanisms of Phase Transitions
Paulina M. Dominiak; Joanna Herold; Waclaw Kolodziejski; Krzysztof Woźniak; Inorganic Chemistry 42 (2003) 1590–1598; doi:10.1021/ic025705b

data_4313262
_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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0521P)^2^+1.0120P] where P=(Fo^2^+2Fc^2^)/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