#------------------------------------------------------------------------------ #$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/42/2104289.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_2104289 loop_ _publ_author_name 'Sohn, Yoo Jung' 'Loose, Anja' 'Merz, Michael' 'Sparta, Karine' 'Klapper, Helmut' 'Heger, Gernot' _publ_section_title ; Dynamic proton disorder and the II--I structural phase transition in (NH~4~)~3~H(SO~4~)~2~ ; _journal_coeditor_code GW5001 _journal_issue 1 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 36 _journal_page_last 44 _journal_paper_doi 10.1107/S0108768108041876 _journal_volume 65 _journal_year 2009 _chemical_formula_moiety 'H O8 S2, 3(H4 N)' _chemical_formula_sum 'H13 N3 O8 S2' _chemical_formula_weight 247.25 _chemical_melting_point 0 _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' _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 101.83(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.429(8) _cell_length_b 5.861(3) _cell_length_c 10.167(5) _cell_measurement_reflns_used 13 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 21.59 _cell_measurement_theta_min 17.33 _cell_volume 899.9(8) _computing_cell_refinement DIF4N _computing_data_collection 'DIF4N (modified Linux version of DIF4; Stoe & Cie, 1991)' _computing_data_reduction 'PRON (Scherf, 1998)' _computing_molecular_graphics 'Atoms 5.1' _computing_publication_material ??? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_measured_fraction_theta_full 0.89 _diffrn_measured_fraction_theta_max 0.89 _diffrn_measurement_device_type 'four circle diffractometer' _diffrn_measurement_method \w _diffrn_radiation_probe neutron _diffrn_radiation_type neutron _diffrn_radiation_wavelength 0.87238 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 1169 _diffrn_reflns_theta_full 37.47 _diffrn_reflns_theta_max 37.47 _diffrn_reflns_theta_min 3.31 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 600 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 0.218 _exptl_absorpt_correction_type none _exptl_crystal_colour white _exptl_crystal_density_diffrn 1.825 _exptl_crystal_density_meas 1.825 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cuboid _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 1.072 _refine_diff_density_min -1.241 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.973 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 120 _refine_ls_number_reflns 1143 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.973 _refine_ls_R_factor_gt 0.094 _refine_ls_shift/su_max 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1441 _reflns_number_gt 770 _reflns_number_total 1143 _reflns_threshold_expression >2sigma(I) _cod_data_source_file gw5001.cif _cod_data_source_block nonsplit _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2104289 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_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_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S S 0.1150(3) 0.2175(10) 0.4630(6) 0.0237(10) Uani d . 1 . . N N1 0.5 0.2298(5) 0.25 0.0296(6) Uani d S 1 . . N N2 0.19904(14) 0.2766(4) 0.1531(2) 0.0343(5) Uani d . 1 . . O O1 0.01474(18) 0.1836(6) 0.4428(4) 0.0386(8) Uani d . 1 . . O O2 0.1504(2) 0.2223(7) 0.6049(3) 0.0393(8) Uani d . 1 . . O O3 0.1286(2) 0.4326(6) 0.3982(4) 0.0416(8) Uani d . 1 . . O O4 0.1489(2) 0.0278(6) 0.3979(4) 0.0427(9) Uani d . 1 . . H H1 0 0 0 0.079(5) Uani d S 1 . . H H2 0.4648(7) 0.131(2) 0.1834(11) 0.105(4) Uani d . 1 . . H H3 0.4569(8) 0.310(3) 0.2747(19) 0.171(8) Uani d . 1 . . H H4 0.2601(6) 0.310(2) 0.1698(14) 0.117(5) Uani d . 1 . . H H5 0.1695(10) 0.387(3) 0.0978(16) 0.142(6) Uani d . 1 . . H H6 0.1900(7) 0.1303(17) 0.1146(12) 0.100(4) Uani d . 1 . . H H7 0.1772(8) 0.283(3) 0.2313(10) 0.127(5) Uani d . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S 0.022(2) 0.025(2) 0.024(3) 0.0034(19) 0.004(2) -0.002(2) N1 0.0288(11) 0.0327(14) 0.0260(15) 0 0.0025(12) 0 N2 0.0388(11) 0.0303(10) 0.0332(12) -0.0074(9) 0.0057(9) -0.0008(10) O1 0.0182(11) 0.0463(19) 0.050(2) 0.0017(12) 0.0032(12) -0.0020(16) O2 0.0345(13) 0.057(2) 0.0240(14) -0.0075(14) 0.0008(13) 0.0002(15) O3 0.0415(16) 0.0324(15) 0.049(2) 0.0023(13) 0.0048(14) 0.0176(15) O4 0.0364(14) 0.0354(16) 0.060(2) -0.0002(13) 0.0184(16) -0.0181(15) H1 0.026(3) 0.143(13) 0.064(7) -0.002(5) 0.001(4) 0.059(8) H2 0.087(6) 0.128(9) 0.085(7) 0.002(6) -0.015(5) -0.043(7) H3 0.089(7) 0.188(15) 0.222(17) 0.064(9) 0.002(9) -0.105(14) H4 0.058(5) 0.117(9) 0.172(11) -0.022(5) 0.014(6) -0.079(9) H5 0.135(10) 0.136(11) 0.157(13) 0.055(9) 0.035(9) 0.089(11) H6 0.094(6) 0.067(5) 0.130(10) -0.021(5) 0.001(6) -0.054(6) H7 0.130(9) 0.195(15) 0.069(6) -0.037(10) 0.050(6) -0.008(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0 0 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 S O4 . . 112.1(4) ? O2 S O3 . . 112.1(4) ? O4 S O3 . . 111.0(4) ? O2 S O1 . . 107.7(4) ? O4 S O1 . . 106.9(4) ? O3 S O1 . . 106.7(4) ? H2 N1 H3 . . 99.7(10) ? H4 N2 H5 . . 108.3(14) ? H4 N2 H6 . . 108.9(9) ? H5 N2 H6 . . 112.1(13) ? H4 N2 H7 . . 111.3(11) ? H5 N2 H7 . . 106.0(15) ? H6 N2 H7 . . 110.2(14) ? 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 S O2 . 1.434(7) ? S O4 . 1.446(6) ? S O3 . 1.458(6) ? S O1 . 1.531(5) ? N1 H2 . 0.969(11) ? N1 H3 . 0.891(12) ? N2 H4 . 0.943(9) ? N2 H5 . 0.918(13) ? N2 H6 . 0.941(9) ? N2 H7 . 0.925(10) ?