#------------------------------------------------------------------------------ #$Date: 2009-11-16 02:43:51 +0100 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2100625.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_2100625 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _[local]_cod_cif_authors_sg_H-M 'P 21/a' loop_ _publ_author_name 'Oh, I.H.' 'Merz, M.' 'Mattauch, S.' 'Heger, G.' _publ_section_title ; Structural phase transition and hydrogen ordering of TlH~2~PO~4~ at low temperature ; _journal_coeditor_code LC5039 _journal_issue 4 _journal_name_full 'Acta Crystallographica, Section B' _journal_page_first 719 _journal_page_last 728 _journal_volume 62 _journal_year 2006 _chemical_formula_sum ' H2 O4 P Tl' _chemical_formula_weight 301.6 _symmetry_cell_setting monoclinic _atom_type_scat_source International_Tables_Vol_C _audit_creation_method enCIFer _cell_angle_alpha 90 _cell_angle_beta 91.67(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.331(7) _cell_length_b 4.535(2) _cell_length_c 6.514(3) _cell_measurement_reflns_used 20 _cell_measurement_temperature 298 _cell_measurement_theta_max 22.5 _cell_measurement_theta_min 17.5 _cell_volume 423.2(3) _computing_cell_refinement pron _computing_data_collection pron _computing_data_reduction pron _computing_molecular_graphics 'drawxtal(Finger and Kroeker, 2004)' _computing_structure_refinement 'prometheus(Zucker et al.,1983)' _diffrn_ambient_temperature '298K ' _diffrn_measured_fraction_theta_max 0.6207 _diffrn_measurement_device_type 'four circle diffractometer' _diffrn_measurement_method \w _diffrn_radiation_monochromator 'Cu (200)' _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.2413 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 2766 _diffrn_reflns_theta_max 50.992 _diffrn_reflns_theta_min 1.5 _diffrn_standards_decay_% 0.7 _diffrn_standards_interval_time 360 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.04 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 4.753 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description platelet _exptl_crystal_F_000 119 _exptl_crystal_size_max 5 _exptl_crystal_size_mid 3 _exptl_crystal_size_min 3 _refine_diff_density_max 0.65 _refine_diff_density_min -0.42 _refine_ls_extinction_coef 0.05425 _refine_ls_extinction_method 'secondary Type I, isotropic, Gaussian (Zachariasen, 1967)' _refine_ls_goodness_of_fit_ref 3.90 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 73 _refine_ls_number_reflns 699 _refine_ls_R_factor_gt 0.051 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details w=1/\s^2^(Fo^2^) _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0603 _reflns_number_gt 699 _reflns_number_total 814 _reflns_threshold_expression >3sigma(I) _[local]_cod_data_source_file lc5039.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x+1/2, -y-1/2, z' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 2 2 4 2 0 6 0 2 loop_ _atom_type_symbol H TL P O 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_occupancy Tl Tl 0.12833(5) -0.0049(2) 0.25850(10) 0.0389(3) Uani 1.00 P P 0.12455(8) 0.5207(3) 0.7608(2) 0.0237(4) Uani 1.00 O O1 0.07470(10) 0.3996(4) 0.9468(2) 0.0526(7) Uani 1.00 O O2 0.05391(10) 0.6547(3) 0.6063(2) 0.0417(6) Uani 1.00 O O3 0.19149(10) 0.7704(3) 0.8299(2) 0.0353(6) Uani 1.00 O O4 0.18173(10) 0.2726(3) 0.6680(2) 0.0340(5) Uani 1.00 H H1 -0.0088(5) 0.5245(18) 0.0161(11) 0.0419(7) Uiso 0.50 H H2 0.0078(4) 0.5308(15) 0.5232(9) 0.0382(6) Uiso 0.50 H H3 0.1845(2) 0.0052(7) 0.7544(4) 0.0516(7) Uani 1.00 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 Tl 0.0392(2) 0.0397(3) 0.0379(3) . . 0.0083(2) P 0.0230(3) 0.0219(5) 0.0265(4) . . 0.0051(3) O1 0.0402(6) 0.0623(7) 0.0553(6) 0.0244(5) 0.0259(4) 0.0359(5) O2 0.0410(5) 0.0359(5) 0.0469(5) -0.0097(4) -0.0200(4) 0.0139(4) O3 0.0391(5) 0.0239(5) 0.0423(5) -0.0148(3) 0.0024(3) -0.0037(4) O4 0.0421(5) 0.0240(5) 0.0366(5) -0.0028(3) 0.0113(3) -0.0044(4) H3 0.0408(7) 0.0680(10) 0.0460(9) -0.0062(8) . -0.0150(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance P O1 . 1.527(2) P O2 . 1.532(2) P O3 . 1.543(2) P O4 . 1.527(2) Tl O1 9 2.828(5) Tl O4 13 2.931(2) Tl O3 13 2.939(7) Tl O2 10 2.965(3) Tl O4 . 3.028(5) Tl O3 12 3.133(5) Tl O2 7 3.201(5) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 P O2 110.39(3) O1 P O3 109.50(2) O1 P O4 108.55(2) O2 P O3 107.08(2) O2 P O4 112.60(4) O3 P O4 108.67(3) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O1 H1 O1 9 7 1.040(7) 1.409(7) 2.445(7) 172.8(4) O2 H2 O2 . 7 1.012(6) 1.469(6) 2.480(6) 176.2(5) O3 H3 O4 10 . 1.176(3) 1.337(3) 2.512(3) 176.9(5)