#------------------------------------------------------------------------------ #$Date: 2016-02-14 04:40:26 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176432 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/49/2104907.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_2104907 loop_ _publ_author_name 'Sohn, Yoo Jung' 'Sparta, Karine M.' 'Meven, Martin' 'Heger, Gernot' _publ_section_title ; Disorder of (NH~4~)~3~H(SO~4~)~2~ in the high-temperature phase I ; _journal_coeditor_code EB5009 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 116 _journal_page_last 121 _journal_paper_doi 10.1107/S0108768111007269 _journal_volume 67 _journal_year 2011 _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 166 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-R 3 2"' _symmetry_space_group_name_H-M 'R -3 m :H' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 _cell_length_a 5.907(3) _cell_length_b 5.907(3) _cell_length_c 22.570(10) _cell_measurement_reflns_used 20 _cell_measurement_temperature 413(2) _cell_measurement_theta_max 12.04 _cell_measurement_theta_min 8.37 _cell_volume 682.0(6) _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 413(2) _diffrn_measured_fraction_theta_full 0.94 _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'single-crystal diffractometer HEiDi' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator 'Cu (420)' _diffrn_radiation_probe neutron _diffrn_radiation_source 'nuclear reactor' _diffrn_radiation_type neutron _diffrn_radiation_wavelength 0.555 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.1426 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 1164 _diffrn_reflns_theta_full 17.16 _diffrn_reflns_theta_max 29.92 _diffrn_reflns_theta_min 4.2 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time '480 min' _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.017 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.805(2) _exptl_crystal_density_method 'not measured' _exptl_crystal_description cuboid _exptl_crystal_F_000 95 _exptl_crystal_size_max 3 _exptl_crystal_size_mid 3 _exptl_crystal_size_min 3 _exptl_crystal_size_rad 0 _refine_diff_density_max 4.89 _refine_diff_density_min -3.51 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.51 _refine_ls_hydrogen_treatment refall _refine_ls_number_constraints 0 _refine_ls_number_parameters 48 _refine_ls_number_reflns 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2689 _refine_ls_R_factor_gt 0.0556 _refine_ls_shift/su_max 0.0281 _refine_ls_shift/su_mean 0.0085 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details w=1/(\s^2^(I)+0.0004I^2^) _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.1091 _reflns_number_gt 133 _reflns_number_total 452 _reflns_threshold_expression I>3\s(I) _cod_data_source_file eb5009.cif _cod_data_source_block I _cod_original_sg_symbol_Hall '-R 3;-2"' _cod_original_sg_symbol_H-M 'R -3 m' _cod_database_code 2104907 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z 3 -x+y,-x,z 4 y,x,-z 5 x-y,-y,-z 6 -x,-x+y,-z 7 -x,-y,-z 8 y,-x+y,-z 9 x-y,x,-z 10 -y,-x,z 11 -x+y,y,z 12 x,x-y,z 13 x+2/3,y+1/3,z+1/3 14 -y+2/3,x-y+1/3,z+1/3 15 -x+y+2/3,-x+1/3,z+1/3 16 y+2/3,x+1/3,-z+1/3 17 x-y+2/3,-y+1/3,-z+1/3 18 -x+2/3,-x+y+1/3,-z+1/3 19 -x+2/3,-y+1/3,-z+1/3 20 y+2/3,-x+y+1/3,-z+1/3 21 x-y+2/3,x+1/3,-z+1/3 22 -y+2/3,-x+1/3,z+1/3 23 -x+y+2/3,y+1/3,z+1/3 24 x+2/3,x-y+1/3,z+1/3 25 x+1/3,y+2/3,z+2/3 26 -y+1/3,x-y+2/3,z+2/3 27 -x+y+1/3,-x+2/3,z+2/3 28 y+1/3,x+2/3,-z+2/3 29 x-y+1/3,-y+2/3,-z+2/3 30 -x+1/3,-x+y+2/3,-z+2/3 31 -x+1/3,-y+2/3,-z+2/3 32 y+1/3,-x+y+2/3,-z+2/3 33 x-y+1/3,x+2/3,-z+2/3 34 -y+1/3,-x+2/3,z+2/3 35 -x+y+1/3,y+2/3,z+2/3 36 x+1/3,x-y+2/3,z+2/3 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 0 0.4093(3) 0.052(2) Uani d . 1 . . N N1 0 0 0 0.0569(18) Uani d . 1 . . N N2 0 0 0.1993(2) 0.0642(11) Uani d . 1 . . O O1 0.0379(7) -0.0379(7) 0.3435(3) 0.067(3) Uani d . 0.3333 . . O O2 0.1348(2) -0.1348(2) 0.57103(13) 0.0741(13) Uani d . 1 . . H H1 0.464(2) -0.464(2) -0.0023(12) 0.063(6) Uiso d . 0.1667 . . H H4 0.0542(17) -0.0542(17) 0.1620(6) 0.093(7) Uani d . 0.3333 . . H H5 0.1381(19) -0.0321(17) 0.2122(4) 0.126(7) Uani d . 0.5 . . H H3 0.041(4) -0.041(4) -0.031(2) 0.087(15) Uiso d . 0.1667 . . H H2 -0.0884(12) 0.0884(12) -0.0230(8) 0.116(8) Uani d . 0.5 . . 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 _atom_site_aniso_type_symbol S 0.062(3) 0.062(3) 0.031(4) 0.0311(15) 0 0 S N1 0.058(2) 0.058(2) 0.055(3) 0.0290(11) 0 0 N N2 0.0581(12) 0.0581(12) 0.077(2) 0.0290(6) 0 0 N O1 0.074(5) 0.074(5) 0.050(3) 0.033(3) 0.0020(15) -0.0020(15) O O2 0.0814(15) 0.0814(15) 0.0809(17) 0.0568(16) -0.0015(7) 0.0015(7) O H4 0.088(8) 0.088(8) 0.091(9) 0.034(7) 0.027(5) -0.027(5) H H5 0.079(7) 0.096(8) 0.210(9) 0.050(7) 0.002(5) 0.038(5) H H2 0.119(8) 0.119(8) 0.139(14) 0.079(9) -0.015(5) 0.015(5) H loop_ _atom_type_symbol _atom_type_scat_source H International_Tables_Vol_C N International_Tables_Vol_C O International_Tables_Vol_C S International_Tables_Vol_C loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 0 6 0 3 0 2 2 0 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 S O2 . . 4_556 122.5(4) yes O1 S O2 . . 5_556 100.2(3) yes O1 S O2 . . 6_556 100.2(3) yes O1 S O2 2_555 . 4_556 100.2(3) yes O1 S O2 2_555 . 5_556 100.2(3) yes O1 S O2 2_555 . 6_556 122.5(4) yes O1 S O2 3_555 . 4_556 100.2(3) yes O1 S O2 3_555 . 5_556 122.5(4) yes O1 S O2 3_555 . 6_556 100.2(3) yes O2 S O2 4_556 . 5_556 111.0(3) yes O2 S O2 4_556 . 6_556 111.0(3) yes O2 S O2 5_556 . 6_556 111.0(3) yes H2 N1 H2 . . 2_555 97.4(10) yes H2 N1 H2 . . 3_555 97.4(10) yes H3 N1 H2 4_555 . . 89(2) yes H3 N1 H2 5_555 . . 131(2) yes H3 N1 H2 6_555 . . 131(2) yes H2 N1 H2 2_555 . 3_555 97.4(9) yes H4 N2 H5 . . . 76.0(9) yes H4 N2 H5 . . 2_555 130.6(8) yes H4 N2 H5 . . 3_555 110.1(8) yes H5 N2 H5 . . 2_555 111.4(8) yes H5 N2 H5 . . 3_555 111.4(10) yes H5 N2 H5 2_555 . 3_555 111.4(10) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S O1 . . 1.535(9) yes S O1 . 2_555 1.535(9) yes S O1 . 3_555 1.535(9) yes S O2 . 4_556 1.449(3) yes S O2 . 5_556 1.449(3) yes S O2 . 6_556 1.449(3) yes N1 H3 . . 0.82(4) yes N1 H3 . 2_555 0.82(4) yes N1 H3 . 3_555 0.82(4) yes N1 H3 . 4_555 0.82(4) yes N1 H3 . 5_555 0.82(4) yes N1 H3 . 6_555 0.82(4) yes N1 H2 . . 1.042(12) yes N1 H2 . 2_555 1.042(12) yes N1 H2 . 3_555 1.042(12) yes N1 H2 . 4_555 1.042(12) yes N1 H2 . 5_555 1.042(12) yes N1 H2 . 6_555 1.042(12) yes N2 H4 . . 1.009(14) yes N2 H4 . 2_555 1.009(14) yes N2 H4 . 3_555 1.009(14) yes N2 H5 . . 0.970(13) yes N2 H5 . 2_555 0.970(15) yes N2 H5 . 3_555 0.970(10) yes N2 H5 . 10_555 0.970(13) yes N2 H5 . 11_555 0.970(15) yes N2 H5 . 12_555 0.970(10) yes