#------------------------------------------------------------------------------ #$Date: 2011-09-28 16:24:46 +0200 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/06/2100627.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_2100627 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 'H8 O16 P4 Tl4' _chemical_formula_weight 1206.4 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-C 1' _symmetry_space_group_name_H-M C-1 _atom_type_scat_source International_Tables_Vol_C _audit_creation_method enCIFer _cell_angle_alpha 90.09(5) _cell_angle_beta 92.21(3) _cell_angle_gamma 90.49(3) _cell_formula_units_Z 16 _cell_length_a 28.483(12) _cell_length_b 9.016(5) _cell_length_c 6.502(3) _cell_measurement_reflns_used 12 _cell_measurement_temperature 210 _cell_measurement_theta_max 22.5 _cell_measurement_theta_min 17.5 _cell_volume 1668.4(14) _computing_cell_refinement pron _computing_data_collection pron _computing_data_reduction pron _computing_molecular_graphics 'drawxtal(Finger and Kroeker, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 210 _diffrn_measured_fraction_theta_max 0.7025 _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 0.0621 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 3170 _diffrn_reflns_theta_max 37.80 _diffrn_reflns_theta_min 3.51 _diffrn_standards_decay_% 2.5 _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 4.820 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description platelet _exptl_crystal_F_000 474.3 _exptl_crystal_size_max 5 _exptl_crystal_size_mid 3 _exptl_crystal_size_min 3 _refine_diff_density_max 3.03 _refine_diff_density_min -2.28 _refine_ls_extinction_coef 0.00300(15) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.933 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 131 _refine_ls_number_reflns 2982 _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 1428 _reflns_number_total 2982 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file lc5039.cif _[local]_cod_chemical_formula_sum_orig ' H8 O16 P4 Tl4' _cod_depositor_comments ; The following automatic conversions were performed: '_diffrn_ambient_temperature' value '210K ' was changed to '210' - the value should be numeric and without a unit designator. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_database_code 2100627 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, -z' 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 Tl1 0.0644(3) 0.4990(10) 0.2650(10) 0.027(2) Uiso 1 Tl Tl2 0.1883(2) 0.2490(10) 0.7270(10) 0.029(2) Uiso 1 Tl Tl3 0.0639(3) 0.9950(10) 0.2530(10) 0.027(2) Uiso 1 Tl Tl4 0.1838(2) 0.7440(10) 0.749(2) 0.029(2) Uiso 1 P P1 0.0620(4) 0.261(2) 0.762(2) 0.016(2) Uiso 1 P P2 0.1881(4) 0.013(2) 0.231(2) 0.020(3) Uiso 1 P P3 0.0625(3) 0.761(2) 0.756(2) 0.013(2) Uiso 1 P P4 0.1876(4) 0.512(2) 0.231(2) 0.015(2) Uiso 1 O O1 0.0410(3) 0.2160(10) 0.9730(10) 0.019(2) Uiso 1 O O2 0.2148(4) 0.438(2) 0.064(2) 0.025(2) Uiso 1 O O3 0.0348(3) 0.686(2) 0.934(2) 0.020(2) Uiso 1 O O4 0.2092(3) 0.961(2) 0.032(2) 0.018(2) Uiso 1 O O5 0.0290(4) 0.323(2) 0.594(2) 0.022(2) Uiso 1 O O6 0.2263(4) 0.085(2) 374(2) 0.021(2) Uiso 1 O O7 0.0266(4) 0.828(2) 0.603(2) 0.023(3) Uiso 1 O O8 0.2266(4) 0.589(2) 0.375(2) 0.017(2) Uiso 1 O O9 0.0999(3) 0.388(2) 0.812(2) 0.021(2) Uiso 1 O O10 0.1509(4) 0.138(2) 0.181(2) 0.014(2) Uiso 1 O O11 0.0936(4) 0.886(2) 0.845(2) 0.024(2) Uiso 1 O O12 0.1571(3) 0.6360(10) 0.1540(10) 0.014(2) Uiso 1 O O13 0.0890(4) 0.138(2) 0.658(2) 0.014(2) Uiso 1 O O14 0.1591(4) 0.389(2) 0.332(2) 0.022(3) Uiso 1 O O15 0.0878(4) 0.640(2) 0.657(2) 0.019(2) Uiso 1 O O16 0.1559(3) 0.888(2) 0.317(2) 0.025(2) Uiso 1 H H1 0.9920(6) 0.267(3) 0.018(3) 0.048(4) Uiso 1 H H2 0.2509(9) 1.001(4) -0.010(3) 0.010(3) Uiso 1 H H3 0.9992(6) 0.254(3) 0.516(3) 0.023(2) Uiso 1 H H4 0.2567(5) -0.018(2) 0.538(2) 0.037(4) Uiso 1 H H5 0.1585(6) 0.775(2) 0.258(2) 0.030(4) Uiso 1 H H6 0.4065(7) 0.507(3) 0.223(3) 0.038(5) Uiso 1 H H7 0.3413(8) 0.243(4) 0.755(3) 0.038(4) Uiso 1 H H8 0.4066(6) 0.012(3) 0.243(3) 0.029(4) Uiso 1 loop_ _atom_type_symbol H TL P O loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 0 2 12 0 -1 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 O1 P1 O9 . . 105.7(9) O1 P1 O5 . . 118.3(9) O1 P1 O13 . . 114.7(9) O5 P1 O9 . . 106.5(9) O5 P1 O13 . . 105.1(9) O4 P2 O6 11 . 104.4(9) O4 P2 O10 11 . 111.70(10) O4 P2 O16 11 11 106.60(10) O3 P3 O7 . . 107.8(9) O3 P3 O11 . . 109.4(9) O3 P3 O15 . . 106.0(9) O7 P3 O11 . . 107.9(9) O7 P3 O15 . . 109.9(9) O11 P3 O15 . . 115.2(9) O2 P4 O8 . . 104.5(9) O2 P4 O12 . . 113.8(9) O2 P4 O14 . . 106.3(9) O8 P4 O12 . . 105.9(9) O8 P4 O14 . . 115.2(9) O12 P4 O14 . . 111.8(9) 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 P1 O1 . . 1.57(2) P1 O5 . . 1.53(2) P1 O9 . . 1.59(2) P1 O13 . . 1.52(2) P2 O4 . 11 1.53(2) P2 O6 . . 1.54(2) P2 O10 . . 1.58(2) P2 O16 . 11 1.57(2) P3 O3 . . 1.58(2) P3 O7 . . 1.53(2) P3 O11 . . 1.53(2) P3 O15 . . 1.47(2) P4 O2 . . 1.52(2) P4 O8 . . 1.58(2) P4 O12 . . 1.50(2) P4 O14 . . 1.53(2) Tl1 O3 . 9 2.850(10) Tl1 O5 . . 2.870(10) Tl1 O14 . . 2.90(2) Tl1 O15 . . 2.90(2) Tl1 O12 . . 3.020(10) Tl1 O1 . 9 3.23(2) Tl2 O2 9 . 2.85(2) Tl2 O9 . . 2.900(10) Tl2 O6 . 7 2.94(2) Tl2 O14 . . 2.96(2) Tl2 O6 . . 2.97(2) Tl2 O13 . . 3.010(10) Tl3 O1 . 10 2.76(3) Tl3 O16 . . 2.820(10) Tl3 O10 . 17 2.840(10) Tl3 O7 . . 2.96(2) Tl3 O11 . 9 2.99(2) Tl3 O13 . 17 2.99(2) Tl3 O7 . 14 3.21(2) Tl4 O4 9 . 2.75(2) Tl4 O15 . . 2.930(10) Tl4 O12 9 . 2.940(10) Tl4 O11 . . 2.97(2) Tl4 O8 . 8 3.090(10) Tl4 O8 . . 3.100(10) Tl4 O16 . . 3.170(10) 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 O3 H1 O1 5 15 0.94(2) 1.51(2) 2.44(3) 167.5(2) O2 H2 O4 6 . 1.18(3) 1.28(3) 2.450(10) 167.4(9) O5 H3 O7 5 5 1.12(2) 1.30(3) 2.410(10) 169.3(9) O8 H4 O6 7 . 0.97(2) 1.64(2) 2.606(9) 173.1(9) O16 H5 O12 . . 1.09(3) 1.42(3) 2.50(2) 170.9(9) O11 H6 O13 8 7 1.06(3) 1.52(3) 2.58(2) 172.6(3) O10 H7 O14 7 7 1.17(3) 1.32(2) 2.48(2) 168.8(6) O9 H8 O15 8 8 0.99(3) 1.53(3) 2.51(2) 173.9(2)