#------------------------------------------------------------------------------ #$Date: 2009-11-18 14:56:34 +0000 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003007.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003007 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 54 _journal_year 1998 _journal_page_first 790 _journal_page_last 797 _publ_section_title ; Isotope effect in TlH2PO4 and TlD2PO4 ; loop_ _publ_author_name "R\'ios, Susana" 'Paulus, Werner' 'Cousson, Alain' 'Quilichini, Marguerite' 'Heger, Gernot' _chemical_name_systematic 'thallium dideuterium phosphate' _chemical_formula_sum 'D2 O4 P Tl' _[local]_cod_chemical_formula_sum_orig 'Tl D2 PO4' _chemical_formula_weight 303.3 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 1 21/b ' _symmetry_space_group_name_Hall '-P 2bc' loop_ _symmetry_equiv_pos_as_xyz 'X,Y,Z' '-X,-Y,-Z' '-X,-Y+1/2,Z+1/2' 'X,Y+1/2,-Z+1/2' _cell_length_a 9.070(6) _cell_length_b 15.000(10) _cell_length_c 6.575(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 106.92(5) _cell_volume 856.0(10) _cell_formula_units_Z 8 _cell_measurement_reflns_used 13 _cell_measurement_theta_min 13 _cell_measurement_theta_max 22 _cell_measurement_temperature 300 _exptl_crystal_description ' no special shape ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 4.51 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 40.37 _exptl_absorpt_coefficient_mu 0.0015 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_radiation_type neutron _diffrn_radiation_wavelength 0.8308 _diffrn_radiation_source "Hot neutron beamline at Reactor Orph\'ee" _diffrn_radiation_monochromator ' Cu (220) ' _diffrn_measurement_device ' 5C.2 four-circle diffractometer ' _diffrn_measurement_method w _diffrn_reflns_number 4811 _diffrn_reflns_av_R_equivalents 0.015 _diffrn_reflns_theta_max 37.33 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 6 _diffrn_standards_number 2 _diffrn_standards_interval_time 450 _diffrn_standards_decay_% 2 _reflns_number_total 2594 _reflns_number_observed 1878 _reflns_observed_criterion F>3\s(F) _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.040 _refine_ls_wR_factor_obs 0.038 _refine_ls_goodness_of_fit_obs 1.2 _refine_ls_number_reflns 1878 _refine_ls_number_parameters 146 _refine_ls_hydrogen_treatment H_atoms_refined_anisotropically _refine_ls_weighting_scheme 'w=1/\s^2^(F)' _refine_ls_shift/esd_max 0.009 _refine_diff_density_max 0.115 _refine_diff_density_min -0.0903 _refine_ls_extinction_method 'Type I, Lorentzian (Larson, 1970)' _refine_ls_extinction_coef 1745.1(3) loop_ _atom_type_symbol 'TL' 'P' 'O' 'D' _atom_type_scat_source ; Sears (1992) CRYSTALS (Watkin, Carruthers & Betteridge, 1985) CAMERON (Pearce, Watkin & Prout, 1994: CAMERON. Program for Plotting Molecular Structures. Chemical Crystallography Laboratory, University of Oxford, England.) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy Tl1 0.06040(10) 0.11848(6) 0.2281(2) 0.0280(4) Uani 1.00 Tl2 0.56310(10) 0.13608(6) 0.2770(2) 0.0292(5) Uani 1.00 P1 0.1789(2) 0.37445(9) 0.2450(3) 0.0204(7) Uani 1.00 P2 0.68130(10) 0.37506(9) 0.2526(3) 0.0186(7) Uani 1.00 O11 0.2601(2) 0.42350(10) 0.0587(3) 0.0540(10) Uani 1.00 O12 0.0208(2) 0.30480(10) 0.1816(3) 0.0316(9) Uani 1.00 O13 0.1506(2) 0.43760(10) 0.4085(3) 0.0386(9) Uani 1.00 O14 0.2720(2) 0.30920(10) 0.3296(3) 0.0287(8) Uani 1.00 O21 0.7901(2) 0.43620(10) 0.0900(3) 0.0440(10) Uani 1.00 O22 0.5319(2) 0.31700(10) 0.1626(2) 0.0294(8) Uani 1.00 O23 0.6371(2) 0.44400(10) 0.4034(3) 0.0356(9) Uani 1.00 O24 0.7735(2) 0.31870(10) 0.3547(2) 0.0283(8) Uani 1.00 D11 0.7233(2) 0.49093(9) 0.4782(2) 0.0336(8) Uani 1.00 D12 0.7626(2) 0.49230(10) 0.0275(2) 0.0348(8) Uani 1.00 D21 0.37540(10) 0.31525(9) 0.2632(2) 0.0324(7) Uani 1.00 D22 -0.0754(2) 0.31290(10) 0.2506(3) 0.0349(8) 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 Tl1 0.0298(5) 0.0264(5) 0.0277(4) 0.0075(4) -0.0070(5) 0.0008(4) Tl2 0.0345(5) 0.0274(5) 0.0257(6) 0.0119(4) -0.0069(5) -0.0013(4) P1 0.0215(7) 0.0182(6) 0.0214(8) 0.0079(5) 0.0072(6) 0.0007(6) P2 0.0160(6) 0.0190(6) 0.0208(8) 0.0057(5) 0.0053(6) 0.0008(6) O11 0.0640(10) 0.0430(10) 0.0540(10) 0.0380(10) 0.0410(10) 0.0330(10) O12 0.0228(7) 0.0350(9) 0.0370(10) 0.0149(6) -0.0073(7) -0.0161(8) O13 0.0269(8) 0.0370(10) 0.0520(10) -0.0003(7) 0.0110(8) -0.0278(9) O14 0.0182(7) 0.0355(8) 0.0324(9) 0.0084(6) 0.0026(6) 0.0135(7) O21 0.0440(10) 0.0356(9) 0.0540(10) 0.0259(8) 0.0330(10) 0.0263(9) O22 0.0216(7) 0.0352(8) 0.0313(9) 0.0129(6) -0.0075(6) -0.0093(7) O23 0.0235(8) 0.0364(9) 0.0470(10) 0.0036(7) 0.0089(8) -0.0204(9) O24 0.0197(7) 0.0337(8) 0.0315(9) 0.0085(6) -0.0024(6) 0.0094(7) D11 0.0341(8) 0.0280(7) 0.0388(9) 0.0086(6) 0.0070(7) -0.0035(7) D12 0.0322(7) 0.0351(8) 0.0372(9) 0.0089(6) 0.0096(7) 0.0009(7) D21 0.0257(6) 0.0352(7) 0.0364(9) 0.0099(5) 0.0035(6) -0.0024(7) D22 0.0300(7) 0.0351(7) 0.0395(9) 0.0119(6) 0.0062(7) 0.0034(7)