#------------------------------------------------------------------------------ #$Date: 2016-02-14 04:40:26 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176432 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/26/2012607.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_2012607 loop_ _publ_author_name 'du Boulay, Douglas' 'Yamashita, Reiko' 'Ishizawa, Nobuo' _publ_section_title ; Synchrotron X-ray study of orthorhombic Rb~3~Ta~5~O~14~ with a modified pyrochlore structure ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first i40 _journal_page_last i44 _journal_paper_doi 10.1107/S010827010101890X _journal_volume 58 _journal_year 2002 _chemical_formula_sum 'O14 Rb3 Ta5' _chemical_formula_weight 1385.13 _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _cell_angle_alpha 90.000(9) _cell_angle_beta 90.000(9) _cell_angle_gamma 90.000(9) _cell_formula_units_Z 8 _cell_length_a 7.3677(3) _cell_length_b 14.7904(19) _cell_length_c 25.379(3) _cell_measurement_reflns_used 10 _cell_measurement_temperature 298 _cell_measurement_theta_max 43.80 _cell_measurement_theta_min 21.61 _cell_volume 2765.6(5) _computing_cell_refinement 'Xtal LATCON (Hall, du Boulay & Olthof-Hazekamp, 2000)' _computing_data_collection 'Diff14A (Vaalsta & Hester, 1997' _computing_data_reduction 'Xtal DIFDAT SORTRF ABSORB ADDREF' _computing_molecular_graphics 'ATOMS (Dowty, 1995) and Xtal ORTEP (Hall, du Boulay & Olthof-Hazekamp, 2000)' _computing_publication_material 'Xtal BONDLA CIFIO (Hall, du Boulay & Olthof-Hazekamp, 2000)' _computing_structure_refinement 'Xtal CRYLSQ (Hall, du Boulay & Olthof-Hazekamp, 2000)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 298 _diffrn_measurement_device_type Tsukuba-BL14A _diffrn_measurement_method \w/2\q _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength .8499 _diffrn_reflns_av_R_equivalents .053 _diffrn_reflns_av_sigmaI/netI .037 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 35705 _diffrn_reflns_reduction_process 'equatorial monochr Lp' _diffrn_reflns_theta_max 50.01 _diffrn_reflns_theta_min 1.91 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 194 _diffrn_standards_number 6 _exptl_absorpt_coefficient_mu 62.9 _exptl_absorpt_correction_T_max .2195 _exptl_absorpt_correction_T_min .0926 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details 'Xtal ABSORB' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 6.653 _exptl_crystal_density_method none _exptl_crystal_description prism _exptl_crystal_F_000 4704 _exptl_crystal_size_max .066 _exptl_crystal_size_mid .037 _exptl_crystal_size_min .036 _refine_diff_density_max 7.299 _refine_diff_density_min -8.465 _refine_ls_extinction_coef 323E1(8) _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_extinction_method Zachariasen _refine_ls_goodness_of_fit_all 3.244 _refine_ls_goodness_of_fit_ref 3.275 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type atomblock _refine_ls_number_constraints 0 _refine_ls_number_parameters 219 _refine_ls_number_reflns 8498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all .044 _refine_ls_R_factor_gt .043 _refine_ls_shift/su_max .002 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_all .047 _refine_ls_wR_factor_ref .047 _reflns_number_gt 8498 _reflns_number_total 8727 _reflns_threshold_expression F>0.00\s(F) _cod_data_source_file ta1346.cif _cod_data_source_block I _cod_original_sg_symbol_Hall -p_2ac_2n _cod_original_sg_symbol_H-M P_n_m_a _cod_database_code 2012607 _cod_database_fobs_code 2012607 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,1/2-z -x,1/2+y,-z -x,-y,-z 1/2+x,+y,1/2-z 1/2-x,1/2+y,1/2+z +x,1/2-y,+z loop_ _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_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ta1 .59012(5) .25000 .055516(12) .00847(11) Uani ? ? 1.00000 ? ? Ta2 .56477(4) .75000 .056538(12) .00790(11) Uani ? ? 1.00000 ? ? Ta3 .87054(3) .122947(14) .153044(9) .00797(8) Uani ? ? 1.00000 ? ? Ta4 .86990(3) .619041(14) .143707(9) .00798(8) Uani ? ? 1.00000 ? ? Ta5 .10701(4) .25000 .055358(12) .00766(11) Uani ? ? 1.00000 ? ? Ta6 .08242(4) .75000 .061507(12) .00728(10) Uani ? ? 1.00000 ? ? Ta7 .14177(3) .510800(15) .244574(9) .00820(8) Uani ? ? 1.00000 ? ? Rb1 .3492(3) .25000 .20738(6) .0614(11) Uani ? ? 1.00000 ? ? Rb2 .3772(2) .75000 .20607(6) .0434(7) Uani ? ? 1.00000 ? ? Rb3 .77262(18) .48708(8) .01916(4) .0448(5) Uani ? ? 1.00000 ? ? Rb4 .3709(2) .49714(10) .11782(4) .0570(7) Uani ? ? 1.00000 ? ? O1 .8554(8) .25000 .0140(2) .009(2) Uani ? ? 1.00000 ? ? O2 .8292(9) .75000 .0189(2) .010(2) Uani ? ? 1.00000 ? ? O3 .6766(7) .1562(3) .10024(17) .0128(16) Uani ? ? 1.00000 ? ? O4 .6557(7) .6541(3) .10003(19) .0142(17) Uani ? ? 1.00000 ? ? O5 .3505(9) .25000 .0841(3) .014(2) Uani ? ? 1.00000 ? ? O6 .3275(9) .75000 .0881(3) .014(2) Uani ? ? 1.00000 ? ? O7 .0439(7) .1418(3) .08610(17) .0143(17) Uani ? ? 1.00000 ? ? O8 .0340(7) .6249(3) .07541(17) .0127(16) Uani ? ? 1.00000 ? ? O9 .9087(10) .25000 .1707(3) .014(2) Uani ? ? 1.00000 ? ? O10 .9497(10) .75000 .1378(2) .011(2) Uani ? ? 1.00000 ? ? O11 .7068(7) .0946(3) .20634(17) .0135(17) Uani ? ? 1.00000 ? ? O12 .7142(7) .6091(3) .20344(17) .0130(16) Uani ? ? 1.00000 ? ? O13 1.0823(6) .0851(3) .19225(17) .0113(15) Uani ? ? 1.00000 ? ? O14 1.0809(6) .5991(3) .19004(17) .0118(16) Uani ? ? 1.00000 ? ? O15 .4014(6) .5111(3) .22497(18) .0124(17) Uani ? ? 1.00000 ? ? O16 .8478(7) .0015(2) .12222(18) .0104(16) Uani ? ? 1.00000 ? ? O17 .5121(6) .1633(3) -.00075(16) .0119(16) Uani ? ? 1.00000 ? ? 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 Ta1 .00412(11) .01309(11) .00819(11) .00000 -.00125(10) .00000 Ta2 .00292(11) .01326(11) .00751(10) .00000 -.00061(9) .00000 Ta3 .00584(9) .00896(8) .00912(8) -.00045(6) -.00032(7) .00080(6) Ta4 .00563(9) .00884(8) .00945(8) -.00037(6) -.00032(7) .00086(6) Ta5 .00433(11) .01144(11) .00722(10) .00000 .00070(9) .00000 Ta6 .00347(11) .01085(10) .00752(10) .00000 .00033(9) .00000 Ta7 .00286(8) .01291(8) .00883(8) .00011(7) -.00047(7) .00035(7) Rb1 .0707(13) .0767(12) .0368(7) .00000 -.0074(9) .00000 Rb2 .0410(8) .0501(7) .0392(7) .00000 .0011(7) .00000 Rb3 .0415(6) .0664(6) .0265(3) -.0166(5) -.0049(5) .0027(4) Rb4 .0418(7) .1057(11) .0234(4) -.0116(6) .0050(5) -.0050(5) O1 .005(2) .011(2) .010(2) .00000 .000(2) .00000 O2 .009(2) .012(2) .010(2) .00000 .000(2) .00000 O3 .0111(18) .0141(15) .0131(16) -.0007(15) -.0046(16) .0019(14) O4 .0109(18) .0167(17) .0151(17) .0015(16) -.0037(17) .0044(15) O5 .010(2) .017(2) .016(2) .00000 .001(2) .00000 O6 .006(2) .020(2) .016(2) .00000 -.003(2) .00000 O7 .014(2) .0180(17) .0111(15) -.0004(17) .0028(17) -.0022(15) O8 .014(2) .0123(15) .0120(15) .0015(15) .0029(17) -.0001(13) O9 .015(3) .010(2) .016(2) .00000 -.005(3) .00000 O10 .013(3) .0061(18) .014(2) .00000 -.001(2) .00000 O11 .016(2) .0109(14) .0138(16) .0002(15) .0055(17) .0020(13) O12 .0113(18) .0151(16) .0125(16) -.0015(15) .0027(17) .0010(14) O13 .0081(16) .0130(15) .0127(15) .0004(14) -.0023(15) .0030(13) O14 .0070(16) .0144(15) .0139(16) -.0010(14) -.0040(15) .0034(14) O15 .0035(16) .0237(19) .0100(15) -.0001(15) -.0026(15) -.0032(15) O16 .012(2) .0092(14) .0095(15) .0028(13) -.0005(16) -.0001(11) O17 .0063(16) .0166(17) .0128(15) -.0022(14) -.0026(16) .0001(13) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O .013 .008972 'Int Tables Vol IV Tables 2.2B and 2.3.1' Rb -2.812 .547974 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ta -2.27 8.735 'Int Tables Vol IV Tables 2.2B and 2.3.1' 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 O3 Ta1 O3 8 . 93.62(19) O3 Ta1 O5 8 . 94.8(2) O3 Ta1 O17 8 8 93.15(18) O3 Ta1 O17 8 . 171.16(18) O3 Ta1 O1 8 . 89.31(18) O3 Ta1 O5 . . 94.8(2) O3 Ta1 O17 . 8 171.16(18) O3 Ta1 O17 . . 93.15(18) O3 Ta1 O1 . . 89.31(18) O5 Ta1 O17 . 8 90.3(2) O5 Ta1 O17 . . 90.3(2) O5 Ta1 O1 . . 174.1(3) O17 Ta1 O17 8 . 79.57(18) O17 Ta1 O1 8 . 85.10(17) O17 Ta1 O1 . . 85.10(17) O4 Ta2 O4 '8 565' . 95.4(2) O4 Ta2 O6 '8 565' . 94.4(2) O4 Ta2 O17 '8 565' '5 665' 91.85(19) O4 Ta2 O17 '8 565' '4 655' 169.78(19) O4 Ta2 O2 '8 565' . 86.57(18) O4 Ta2 O6 . . 94.4(2) O4 Ta2 O17 . '5 665' 169.78(19) O4 Ta2 O17 . '4 655' 91.85(19) O4 Ta2 O2 . . 86.57(18) O6 Ta2 O17 . '5 665' 92.2(2) O6 Ta2 O17 . '4 655' 92.2(2) O6 Ta2 O2 . . 178.5(3) O17 Ta2 O17 '5 665' '4 655' 80.11(18) O17 Ta2 O2 '5 665' . 86.68(17) O17 Ta2 O2 '4 655' . 86.68(17) O11 Ta3 O13 . . 94.8(2) O11 Ta3 O9 . . 98.3(2) O11 Ta3 O16 . . 91.62(19) O11 Ta3 O3 . . 94.5(2) O11 Ta3 O7 . '1 655' 172.72(18) O13 Ta3 O9 . . 92.6(2) O13 Ta3 O16 . . 90.51(19) O13 Ta3 O3 . . 169.39(18) O13 Ta3 O7 . '1 655' 87.97(18) O9 Ta3 O16 . . 169.4(2) O9 Ta3 O3 . . 91.1(2) O9 Ta3 O7 . '1 655' 88.3(2) O16 Ta3 O3 . . 84.18(18) O16 Ta3 O7 . '1 655' 81.62(18) O3 Ta3 O7 . '1 655' 82.18(18) O16 Ta4 O12 8 . 96.1(2) O16 Ta4 O14 8 . 95.7(2) O16 Ta4 O4 8 . 91.0(2) O16 Ta4 O10 8 . 155.9(2) O16 Ta4 O8 8 '1 655' 81.36(18) O12 Ta4 O14 . . 89.4(2) O12 Ta4 O4 . . 89.2(2) O12 Ta4 O10 . . 107.9(2) O12 Ta4 O8 . '1 655' 176.97(18) O14 Ta4 O4 . . 173.25(18) O14 Ta4 O10 . . 87.6(2) O14 Ta4 O8 . '1 655' 92.52(18) O4 Ta4 O10 . . 86.5(2) O4 Ta4 O8 . '1 655' 89.22(19) O10 Ta4 O8 . '1 655' 74.6(2) O7 Ta5 O7 . 8 120.9(2) O7 Ta5 O5 . . 94.25(18) O7 Ta5 O2 . '4 645' 118.20(14) O7 Ta5 O1 . '1 455' 89.37(17) O7 Ta5 O5 8 . 94.25(18) O7 Ta5 O2 8 '4 645' 118.20(14) O7 Ta5 O1 8 '1 455' 89.37(17) O5 Ta5 O2 . '4 645' 98.1(3) O5 Ta5 O1 . '1 455' 172.6(3) O2 Ta5 O1 '4 645' '1 455' 74.5(2) O8 Ta6 O8 '8 565' . 149.7(2) O8 Ta6 O6 '8 565' . 96.29(16) O8 Ta6 O1 '8 565' '4 655' 102.84(13) O8 Ta6 O2 '8 565' '1 455' 86.07(15) O8 Ta6 O10 '8 565' '1 455' 75.63(13) O8 Ta6 O6 . . 96.29(16) O8 Ta6 O1 . '4 655' 102.84(13) O8 Ta6 O2 . '1 455' 86.07(15) O8 Ta6 O10 . '1 455' 75.63(13) O6 Ta6 O1 . '4 655' 97.1(3) O6 Ta6 O2 . '1 455' 170.4(3) O6 Ta6 O10 . '1 455' 96.3(3) O1 Ta6 O2 '4 655' '1 455' 73.3(2) O1 Ta6 O10 '4 655' '1 455' 166.6(2) O2 Ta6 O10 '1 455' '1 455' 93.3(2) O15 Ta7 O14 '6 455' '1 455' 94.1(2) O15 Ta7 O15 '6 455' . 171.00(19) O15 Ta7 O13 '6 455' '8 455' 93.83(19) O15 Ta7 O12 '6 455' '6 455' 88.8(2) O15 Ta7 O11 '6 455' '3 455' 88.4(2) O15 Ta7 Rb4 '6 455' . 141.17(14) O14 Ta7 O15 '1 455' . 92.42(19) O14 Ta7 O13 '1 455' '8 455' 87.33(18) O14 Ta7 O12 '1 455' '6 455' 92.39(18) O14 Ta7 O11 '1 455' '3 455' 172.18(18) O14 Ta7 Rb4 '1 455' . 61.16(13) O15 Ta7 O13 . '8 455' 92.66(19) O15 Ta7 O12 . '6 455' 84.7(2) O15 Ta7 O11 . '3 455' 85.9(2) O15 Ta7 Rb4 . . 47.82(13) O13 Ta7 O12 '8 455' '6 455' 177.35(19) O13 Ta7 O11 '8 455' '3 455' 85.12(17) O13 Ta7 Rb4 '8 455' . 58.20(13) O12 Ta7 O11 '6 455' '3 455' 95.06(17) O12 Ta7 Rb4 '6 455' . 119.43(13) O11 Ta7 Rb4 '3 455' . 112.71(13) 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 Ta1 O3 . 8_555 1.902(4) no Ta1 O3 . . 1.902(4) y Ta1 O5 . . 1.909(7) y Ta1 O17 . 8_555 2.003(4) no Ta1 O17 . . 2.003(4) y Ta1 O1 . . 2.220(6) y Ta2 O4 . 8_565 1.918(5) no Ta2 O4 . . 1.918(5) y Ta2 O6 . . 1.923(7) y Ta2 O17 . 5_665 1.992(4) no Ta2 O17 . 4_655 1.992(4) y Ta2 O2 . . 2.170(6) y Ta3 O11 . . 1.860(5) y Ta3 O13 . . 1.934(4) y Ta3 O9 . . 1.9519(18) y Ta3 O16 . . 1.967(4) y Ta3 O3 . . 2.020(5) y Ta3 O7 . 1_655 2.144(5) y Ta4 O16 . 8_555 1.871(4) y Ta4 O12 . . 1.907(5) y Ta4 O14 . . 1.972(4) y Ta4 O4 . . 1.997(5) y Ta4 O10 . . 2.030(2) y Ta4 O8 . 1_655 2.115(5) y Ta5 O7 . . 1.840(5) y Ta5 O7 . 8_555 1.840(5) no Ta5 O5 . . 1.937(7) y Ta5 O2 . 4_645 1.941(6) y Ta5 O1 . 1_455 2.130(6) y Ta6 O8 . 8_565 1.917(4) no Ta6 O8 . . 1.917(4) y Ta6 O6 . . 1.928(7) y Ta6 O1 . 4_655 1.971(6) y Ta6 O2 . 1_455 2.157(6) y Ta6 O10 . 1_455 2.168(6) y Ta7 O15 . 6_455 1.932(5) y Ta7 O14 . 1_455 1.955(4) y Ta7 O15 . . 1.977(5) y Ta7 O13 . 8_455 1.992(4) y Ta7 O12 . 6_455 2.035(4) y Ta7 O11 . 3_455 2.052(4) y Ta7 Rb4 . . 3.6385(13) y Rb1 O9 . 3_455 3.126(7) y Rb1 O5 . . 3.128(7) y Rb1 O13 . 8_455 3.156(5) no Rb1 O13 . 1_455 3.156(5) y Rb1 O11 . 6_455 3.343(4) no Rb1 O11 . 3_455 3.343(4) y Rb1 O9 . 1_455 3.377(8) y Rb1 O11 . 8_555 3.496(5) no Rb1 O11 . . 3.496(5) y Rb1 O3 . 8_555 3.891(5) no Rb1 O3 . . 3.891(5) y Rb1 O15 . 8_555 3.906(5) no Rb1 O15 . . 3.906(5) y Rb1 O13 . 6_455 3.923(5) no Rb1 O13 . 3_455 3.923(5) y Rb1 O7 . 8_555 4.134(5) no Rb1 O7 . . 4.134(5) y Rb1 O9 . . 4.226(8) y Rb1 Rb1 . 3_555 4.272(3) no Rb1 Rb1 . 3_455 4.272(3) y Rb1 Rb4 . 8_555 4.3072(17) no Rb1 Rb4 . . 4.3072(17) y Rb2 O6 . . 3.016(7) y Rb2 O14 . 8_465 3.148(5) no Rb2 O14 . 1_455 3.148(5) y Rb2 O12 . 8_565 3.242(5) no Rb2 O12 . . 3.242(5) y Rb2 O12 . 6_455 3.325(5) no Rb2 O12 . 3_465 3.325(5) y Rb2 O15 . 8_565 3.571(5) no Rb2 O15 . . 3.571(5) y Rb2 O10 . 1_455 3.595(7) y Rb2 O4 . 8_565 3.669(5) no Rb2 O4 . . 3.669(5) y Rb2 O14 . 6_455 3.766(5) no Rb2 O14 . 3_465 3.766(5) y Rb2 O10 . 3_465 3.999(6) y Rb2 Rb2 . 3_465 4.306(2) no Rb2 Rb2 . 3_565 4.306(2) y Rb2 Rb4 . 8_565 4.3595(17) no Rb2 Rb4 . . 4.3595(17) y Rb3 O16 . 8_555 2.679(5) y Rb3 O17 . 8_555 2.981(5) y Rb3 O3 . 8_555 3.038(5) y Rb3 O8 . 1_655 3.147(5) y Rb3 O7 . 8_655 3.243(5) y Rb3 O8 . 5_665 3.245(5) y Rb3 O4 . . 3.325(5) y Rb3 O17 . 4_655 3.378(5) y Rb3 Rb3 . 5_765 3.5097(19) y Rb3 O1 . . 3.5615(16) y Rb3 Rb4 . 5_665 3.6412(16) y Rb3 O7 . 4_655 3.768(5) y Rb3 Rb4 . . 3.8796(18) y Rb3 O2 . . 3.9110(15) y Rb3 Rb3 . 5_665 4.1508(19) y Rb3 Rb4 . 1_655 5.072(2) y Rb4 O15 . . 2.736(5) y Rb4 O13 . 8_455 3.093(5) y Rb4 O4 . . 3.162(5) y Rb4 O14 . 1_455 3.193(5) y Rb4 O3 . 8_555 3.228(5) y Rb4 O7 . 8_555 3.267(5) y Rb4 O8 . . 3.300(5) y Rb4 O16 . 8_555 3.515(5) y Rb4 O11 . 8_555 3.607(5) y Rb4 O12 . . 3.723(5) y Rb4 O5 . . 3.757(2) y Rb4 O6 . . 3.829(2) y Rb4 O16 . 8_455 3.856(5) y Rb4 O17 . 4_655 3.951(4) y Rb4 O17 . 8_555 3.971(4) y