#------------------------------------------------------------------------------ #$Date: 2008-03-30 12:21:05 +0200 (Sun, 30 Mar 2008) $ #$Revision: 321 $ #$URL: svn://www.crystallography.net/cod/cif/2/2100626.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_2100626 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 _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 21/a' _atom_type_scat_source International_Tables_Vol_C _audit_creation_method enCIFer _cell_angle_alpha 90 _cell_angle_beta 92.19(13) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.26(2) _cell_length_b 4.517(9) _cell_length_c 6.497(10) _cell_measurement_reflns_used 12 _cell_measurement_temperature 240 _cell_measurement_theta_max 22.5 _cell_measurement_theta_min 17.5 _cell_volume 418.2(11) _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 '240K ' _diffrn_measured_fraction_theta_max 0.6974 _diffrn_measurement_device_type 'four circle diffractometer' _diffrn_measurement_method \w _diffrn_radiation_monochromator 'Cu (220)' _diffrn_radiation_type neutron _diffrn_radiation_wavelength 0.8724 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 1695 _diffrn_reflns_theta_max 37.47 _diffrn_reflns_theta_min 3.51 _diffrn_standards_decay_% 0.7 _diffrn_standards_interval_time 540 _diffrn_standards_number 2 _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_000 118.6 _exptl_crystal_size_max 5 _exptl_crystal_size_mid 3 _exptl_crystal_size_min 3 _refine_diff_density_max 0.51 _refine_diff_density_min -0.48 _refine_ls_extinction_coef 0.05425 _refine_ls_extinction_method 'secondary Type I, isotropic, Gaussian (Zachariasen, 1967)' _refine_ls_goodness_of_fit_ref 2.21 _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 0.0458 _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 0.0544 _reflns_number_gt 630 _reflns_number_total 845 _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 8 2 0 8 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(7) -0.0075(4) 0.2603(2) 0.0309(3) Uani 1.00 P P 0.12432(10) 0.5238(5) 0.7633(2) 0.0178(5) Uani 1.00 O O1 0.07640(10) 0.4034(6) 0.9526(3) 0.0392(7) Uani 1.00 O O2 0.05160(10) 0.6604(5) 0.6104(3) 0.0304(7) Uani 1.00 O O3 0.19250(10) 0.7757(6) 0.8310(3) 0.0284(7) Uani 1.00 O O4 0.18020(10) 0.2764(5) 0.6662(3) 0.0262(7) Uani 1.00 H H1 -0.0097(5) 0.526(2) 0.0162(11) 0.0310(10) Uiso 0.50 H H2 0.0067(5) 0.534(2) 0.5249(9) 0.0320(10) Uiso 0.50 H H3 0.1847(2) 0.0057(13) 0.7562(5) 0.042(3) 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 0.0314(4) 0.0283(12) 0.0334(5) . . 0.0066(6) P 0.0179(5) 0.0141(15) 0.0216(6) . 0.0011(4) 0.0031(7) O1 0.0292(7) 0.050(2) 0.0403(8) 0.0175(7) 0.0179(6) 0.0268(8) O2 0.0289(7) 0.0270(19) 0.0339(8) -0.0046(7) -0.0120(5) 0.0093(8) O3 0.0307(8) 0.018(2) 0.0355(8) . -0.0122(5) -0.0034(7) O4 0.0313(7) 0.0169(18) 0.0307(7) . 0.0083(5) -0.0036(7) H3 0.0340(10) 0.048(4) 0.0420(10) . . -0.0130(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance P O1 . 1.529(3) P O2 . 1.538(3) P O3 . 1.549(3) P O4 . 1.523(3) Tl O1 9 2.806(7) Tl O4 13 2.920(4) Tl O3 13 2.936(2) Tl O2 10 2.970(7) Tl O4 . 2.999(5) Tl O3 12 3.127(8) Tl O2 7 3.146(2) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 P O2 110.55(5) O1 P O3 109.13(3) O1 P O4 109.21(3) O2 P O3 106.79(3) O2 P O4 112.18(5) O3 P O4 108.88(4) 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 1.032(7) 1.422(7) 2.448(7) 172.3(4) O2 H2 O2 . 7 1.010(8) 1.475(9) 2.483(8) 174.9(6) O3 H3 O4 10 . 1.150(6) 1.356(6) 2.506(6) 177.2(4)