#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2012607.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_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)
_[local]_cod_data_source_file    ta1346.cif
_[local]_cod_data_source_block   I
_[local]_cod_cif_authors_sg_H-M  P_n_m_a
_[local]_cod_cif_authors_sg_Hall -p_2ac_2n
_cod_database_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_occupancy
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_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