#------------------------------------------------------------------------------ #$Date: 2012-02-24 19:13:23 +0200 (Fri, 24 Feb 2012) $ #$Revision: 34330 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/31/32/4313263.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_4313263 loop_ _publ_author_name 'Paulina M. Dominiak' 'Joanna Herold' 'Waclaw Kolodziejski' 'Krzysztof Wo\'zniak' _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_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 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 101.81(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 15.390(3) _cell_length_b 5.8480(12) _cell_length_c 10.140(2) _cell_measurement_reflns_used 5000 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 45 _cell_measurement_theta_min 4 _cell_volume 893.3(3) _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 1024 _diffrn_measured_fraction_theta_full 0.960 _diffrn_measured_fraction_theta_max 0.960 _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 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 7795 _diffrn_reflns_theta_full 28.80 _diffrn_reflns_theta_max 28.80 _diffrn_reflns_theta_min 3.74 _diffrn_standards_decay_% 2 _diffrn_standards_interval_count '50 frames' _diffrn_standards_number '1 frame' _exptl_absorpt_coefficient_mu 0.623 _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.838 _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 0.484 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.069 _refine_ls_extinction_coef 0.068(4) _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 1.120 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 86 _refine_ls_number_reflns 1115 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.120 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0369 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+1.2942P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0900 _refine_ls_wR_factor_ref 0.0957 _reflns_number_gt 962 _reflns_number_total 1115 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic025705b_s1_2.cif _[local]_cod_data_source_block PhaseII _cod_database_code 4313263 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 0.11413(3) 0.21838(8) 0.96135(5) 0.0283(2) Uani 1 1 d . . . O1 O 0.01446(10) 0.1852(3) 0.94264(17) 0.0437(4) Uani 1 1 d . . . O2 O 0.15028(11) 0.2232(3) 1.10530(15) 0.0444(4) Uani 1 1 d . . . O3 O 0.12907(11) 0.4330(3) 0.89840(17) 0.0477(5) Uani 1 1 d . . . O4 O 0.14878(11) 0.0270(3) 0.89800(17) 0.0471(5) Uani 1 1 d . . . N1 N 0.30105(16) 0.7759(4) 0.8473(2) 0.0382(5) Uani 1 1 d . . . N2 N 0.5000 0.2303(5) 0.7500 0.0333(6) Uani 1 2 d S . . H1 H 0.322(4) 0.861(10) 0.897(6) 0.13(2) Uiso 1 1 d . . . H2 H 0.246(3) 0.807(7) 0.849(4) 0.092(13) Uiso 1 1 d . . . H3 H 0.317(3) 0.784(7) 0.788(6) 0.095(16) Uiso 1 1 d . . . H4 H 0.305(3) 0.645(8) 0.879(4) 0.097(14) Uiso 1 1 d . . . H5 H 0.466(3) 0.294(7) 0.772(5) 0.110(18) Uiso 1 1 d . . . H6 H 0.474(3) 0.157(8) 0.693(4) 0.101(15) Uiso 1 1 d . . . H1O H 0.0000 0.0000 1.0000 0.16(3) Uiso 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0290(3) 0.0286(3) 0.0276(3) 0.00018(17) 0.00605(18) 0.00311(17) O1 0.0249(8) 0.0563(11) 0.0491(9) -0.0013(8) 0.0054(6) 0.0021(6) O2 0.0406(9) 0.0634(11) 0.0270(8) 0.0020(7) 0.0021(6) -0.0070(7) O3 0.0495(9) 0.0364(9) 0.0554(10) 0.0173(7) 0.0062(7) 0.0017(7) O4 0.0435(9) 0.0390(9) 0.0629(10) -0.0178(8) 0.0204(7) 0.0003(7) N1 0.0458(12) 0.0345(11) 0.0354(11) 0.0005(8) 0.0110(9) 0.0073(8) N2 0.0345(14) 0.0366(14) 0.0283(12) 0.000 0.0056(11) 0.000 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 111.65(11) . . ? O4 S1 O2 111.19(11) . . ? O3 S1 O2 111.32(10) . . ? O4 S1 O1 107.49(10) . . ? O3 S1 O1 107.65(10) . . ? O2 S1 O1 107.30(10) . . ? S1 O1 H1O 108.60(11) . . ? H1 N1 H2 98(5) . . ? H1 N1 H3 111(5) . . ? H2 N1 H3 121(5) . . ? H1 N1 H4 112(5) . . ? H2 N1 H4 101(4) . . ? H3 N1 H4 113(4) . . ? H5 N2 H6 103(6) . . ? 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 1.4456(15) . ? S1 O3 1.4478(16) . ? S1 O2 1.4521(16) . ? S1 O1 1.5191(16) . ? O1 H1O 1.2702(18) . ? N1 H1 0.73(6) . ? N1 H2 0.87(5) . ? N1 H3 0.70(6) . ? N1 H4 0.83(5) . ? N2 H5 0.71(5) . ? N2 H6 0.76(4) . ?