Download citation
Download citation
link to html
The structure of penta­barium ditantalum dichloride nona­oxide, Ba5Ta2Cl2O9, is isotypic with Ba5Ru1.6W0.4Cl2O9 and with one polymorph of Ba5Ru2Cl2O9. It is related to the perovskite structure and shows a ten-layer stacking of BaO3 and BaCl blocks along the c axis. The Ta cations occupy octa­hedral inter­stices, forming Ta2O9 dimers of distorted face-shared TaO6 octa­hedra. Except for one O atom, all atoms are situated on special positions: Ba1 (Wyckoff position \overline 6m2), Ba2 and Ba3 (3m.), Ta (3m.), Cl (3m.) and O1 (mm2).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807016790/wm2105sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807016790/wm2105Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal synchrotron study
  • T = 150 K
  • Mean [sigma](a-O) = 0.014 Å
  • R factor = 0.035
  • wR factor = 0.088
  • Data-to-parameter ratio = 17.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 37.00 A   3 PLAT732_ALERT_1_C Angle Calc 92.8(5), Rep 92.8(2) ...... 2.50 su-Ra TA -O1 -BA1 1.555 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 57.10(13), Rep 57.10(6) ...... 2.17 su-Ra TA -O1 -BA3 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: WinGX (Farrugia, 1999); software used to prepare material for publication: SHELXL97.

Pentabarium ditantalum dichloride nonaoxide top
Crystal data top
Ba5Ta2Cl2O9Dx = 5.467 Mg m3
Mr = 1263.50Synchrotron radiation, λ = 0.78480 Å
Hexagonal, P63/mmcCell parameters from 1215 reflections
Hall symbol: -P 6c 2cθ = 4.7–31.7°
a = 5.9787 (3) ŵ = 27.18 mm1
c = 24.796 (3) ÅT = 150 K
V = 767.59 (10) Å3Block, yellow
Z = 20.04 × 0.02 × 0.02 mm
F(000) = 1064
Data collection top
Bruker APEXII CCD area-detector
diffractometer
351 independent reflections
Radiation source: Daresbury SRS Station 16.2SMX317 reflections with I > 2σ(I)
Silicon 111 monochromatorRint = 0.093
ω scansθmax = 29.3°, θmin = 4.4°
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
h = 77
Tmin = 0.337, Tmax = 0.665k = 77
5409 measured reflectionsl = 3030
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.035Secondary atom site location: difference Fourier map
wR(F2) = 0.088 w = 1/[σ2(Fo2) + (0.018P)2 + 39.7853P]
where P = (Fo2 + 2Fc2)/3
S = 1.12(Δ/σ)max < 0.001
351 reflectionsΔρmax = 1.93 e Å3
20 parametersΔρmin = 2.88 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ba10.33330.66670.25000.0060 (5)
Ba20.66670.33330.17192 (5)0.0060 (4)
Ba30.33330.66670.08105 (6)0.0085 (4)
Ta0.00000.00000.18941 (4)0.0047 (3)
Cl0.66670.33330.0464 (3)0.032 (2)
O10.294 (3)0.1470 (15)0.25000.015 (3)*
O20.1613 (13)0.323 (3)0.1552 (5)0.023 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ba10.0044 (6)0.0044 (6)0.0090 (9)0.0022 (3)0.0000.000
Ba20.0050 (5)0.0050 (5)0.0081 (7)0.0025 (2)0.0000.000
Ba30.0092 (5)0.0092 (5)0.0070 (7)0.0046 (2)0.0000.000
Ta10.0032 (4)0.0032 (4)0.0079 (6)0.00159 (18)0.0000.000
Cl10.044 (3)0.044 (3)0.009 (3)0.0220 (16)0.0000.000
Geometric parameters (Å, º) top
O1—Ta2.139 (11)Ba2—O1x2.734 (11)
O1—Tai2.139 (11)Ba2—O2xii3.018 (16)
O1—Ba2i2.734 (11)Ba2—O2xiii3.018 (17)
O1—Ba22.734 (11)Ba2—O2xi3.018 (16)
O1—Ba1ii2.996 (11)Ba2—O2vii3.018 (16)
O1—Ba12.996 (11)Ba2—O2x3.018 (17)
O2—Ta1.873 (13)Ba2—Cl3.113 (7)
O2—Ba32.561 (12)Ta—O2ix1.873 (13)
O2—Ba12.949 (12)Ta—O2xii1.873 (13)
O2—Ba2iii3.018 (16)Ta—O1ix2.139 (11)
O2—Ba23.018 (16)Ta—O1xii2.139 (11)
Ba1—O2iv2.949 (12)Ta—Tai3.0046 (19)
Ba1—O2v2.949 (12)Ba3—O2vi2.561 (12)
Ba1—O2vi2.949 (12)Ba3—O2vii2.561 (12)
Ba1—O2i2.949 (12)Ba3—Clxiv3.159 (7)
Ba1—O2vii2.949 (12)Ba3—Cliii3.5574 (17)
Ba1—O1viii2.996 (11)Ba3—Clviii3.5574 (17)
Ba1—O1ix2.996 (11)Ba3—Cl3.5574 (17)
Ba1—O1vi2.996 (11)Cl—Ba3xiv3.159 (7)
Ba1—O1vii2.996 (11)Cl—Ba3xiii3.5574 (17)
Ba1—O1x2.996 (10)Cl—Ba3ii3.5574 (17)
Ba2—O1xi2.734 (11)
Ta—O1—Tai89.2 (6)O1xi—Ba2—O2xii96.3 (2)
Ta—O1—Ba2i179.5 (6)O1x—Ba2—O2xii134.1 (3)
Tai—O1—Ba2i90.28 (7)O1—Ba2—O2xii59.0 (3)
Ta—O1—Ba290.28 (7)O1xi—Ba2—O2xiii59.0 (3)
Tai—O1—Ba2179.5 (6)O1x—Ba2—O2xiii96.3 (2)
Ba2i—O1—Ba290.2 (5)O1—Ba2—O2xiii134.1 (3)
Ta—O1—Ba1ii92.8 (2)O2xii—Ba2—O2xiii118.15 (10)
Tai—O1—Ba1ii92.8 (2)O1xi—Ba2—O2xi59.0 (3)
Ba2i—O1—Ba1ii87.2 (2)O1x—Ba2—O2xi134.1 (3)
Ba2—O1—Ba1ii87.2 (2)O1—Ba2—O2xi96.3 (2)
Ta—O1—Ba192.8 (2)O2xii—Ba2—O2xi61.5 (5)
Tai—O1—Ba192.8 (2)O2xiii—Ba2—O2xi57.3 (5)
Ba2i—O1—Ba187.2 (2)O1xi—Ba2—O2vii134.1 (3)
Ba2—O1—Ba187.2 (2)O1x—Ba2—O2vii59.0 (3)
Ba1ii—O1—Ba1172.2 (6)O1—Ba2—O2vii96.3 (2)
Ta—O1—Ba357.10 (6)O2xii—Ba2—O2vii118.15 (10)
Tai—O1—Ba3126.8 (4)O2xiii—Ba2—O2vii118.15 (10)
Ba2i—O1—Ba3123.2 (3)O2xi—Ba2—O2vii164.1 (4)
Ba2—O1—Ba352.84 (18)O1xi—Ba2—O2x96.3 (2)
Ba1ii—O1—Ba3125.20 (5)O1x—Ba2—O2x59.0 (3)
Ta—O2—Ba3161.0 (6)O1—Ba2—O2x134.1 (3)
Ta—O2—Ba1100.3 (5)O2xii—Ba2—O2x164.1 (4)
Ba3—O2—Ba198.7 (4)O2xiii—Ba2—O2x61.5 (5)
Ta—O2—Ba2iii87.4 (2)O2xi—Ba2—O2x118.15 (10)
Ba3—O2—Ba2iii94.9 (2)O2vii—Ba2—O2x57.3 (5)
Ba1—O2—Ba2iii83.1 (2)O1xi—Ba2—O2134.1 (3)
Ta—O2—Ba287.4 (2)O1x—Ba2—O296.3 (2)
Ba3—O2—Ba294.9 (2)O1—Ba2—O259.0 (3)
Ba1—O2—Ba283.1 (2)O2xii—Ba2—O257.3 (5)
Ba2iii—O2—Ba2164.1 (4)O2xiii—Ba2—O2164.1 (4)
O2iv—Ba1—O2v63.1 (4)O2xi—Ba2—O2118.15 (10)
O2iv—Ba1—O2144.8 (2)O2vii—Ba2—O261.5 (5)
O2v—Ba1—O2144.8 (2)O2x—Ba2—O2118.15 (10)
O2iv—Ba1—O2vi105.7 (5)O1xi—Ba2—Cl135.1 (2)
O2v—Ba1—O2vi144.8 (2)O1x—Ba2—Cl135.1 (2)
O2—Ba1—O2vi63.1 (4)O1—Ba2—Cl135.1 (2)
O2iv—Ba1—O2i63.1 (4)O2xii—Ba2—Cl82.1 (2)
O2v—Ba1—O2i63.1 (4)O2xiii—Ba2—Cl82.1 (2)
O2—Ba1—O2i105.7 (5)O2xi—Ba2—Cl82.1 (2)
O2vi—Ba1—O2i144.8 (2)O2vii—Ba2—Cl82.1 (2)
O2iv—Ba1—O2vii144.8 (2)O2x—Ba2—Cl82.1 (2)
O2v—Ba1—O2vii105.7 (5)O2—Ba2—Cl82.1 (2)
O2—Ba1—O2vii63.1 (4)O2ix—Ta—O2101.1 (5)
O2vi—Ba1—O2vii63.1 (4)O2ix—Ta—O2xii101.1 (5)
O2i—Ba1—O2vii144.8 (2)O2—Ta—O2xii101.1 (5)
O2iv—Ba1—O1viii57.1 (2)O2ix—Ta—O1162.3 (5)
O2v—Ba1—O1viii92.36 (19)O2—Ta—O190.0 (3)
O2—Ba1—O1viii120.1 (2)O2xii—Ta—O190.0 (3)
O2vi—Ba1—O1viii57.1 (2)O2ix—Ta—O1ix90.0 (3)
O2i—Ba1—O1viii120.1 (2)O2—Ta—O1ix90.0 (3)
O2vii—Ba1—O1viii92.36 (19)O2xii—Ta—O1ix162.3 (5)
O2iv—Ba1—O1ix92.36 (18)O1—Ta—O1ix76.1 (5)
O2v—Ba1—O1ix120.1 (2)O2ix—Ta—O1xii90.0 (3)
O2—Ba1—O1ix57.1 (2)O2—Ta—O1xii162.3 (5)
O2vi—Ba1—O1ix92.36 (18)O2xii—Ta—O1xii90.0 (3)
O2i—Ba1—O1ix57.1 (2)O1—Ta—O1xii76.1 (5)
O2vii—Ba1—O1ix120.1 (2)O1ix—Ta—O1xii76.1 (5)
O1viii—Ba1—O1ix120.000 (2)O2vi—Ba3—O2vii74.1 (4)
O2iv—Ba1—O1vi57.1 (2)O2vi—Ba3—O274.1 (4)
O2v—Ba1—O1vi120.1 (2)O2vii—Ba3—O274.1 (4)
O2—Ba1—O1vi92.36 (19)O2vi—Ba3—Clxiv135.9 (3)
O2vi—Ba1—O1vi57.1 (2)O2vii—Ba3—Clxiv135.9 (3)
O2i—Ba1—O1vi92.36 (19)O2—Ba3—Clxiv135.9 (3)
O2vii—Ba1—O1vi120.1 (2)O2vi—Ba3—Cliii80.57 (17)
O1viii—Ba1—O1vi52.2 (6)O2vii—Ba3—Cliii148.1 (3)
O1ix—Ba1—O1vi67.8 (6)O2—Ba3—Cliii80.57 (17)
O2iv—Ba1—O1vii92.36 (18)Clxiv—Ba3—Cliii76.01 (11)
O2v—Ba1—O1vii57.1 (2)O2vi—Ba3—Clviii80.57 (17)
O2—Ba1—O1vii120.1 (2)O2vii—Ba3—Clviii80.57 (17)
O2vi—Ba1—O1vii92.36 (18)O2—Ba3—Clviii148.1 (3)
O2i—Ba1—O1vii120.1 (2)Clxiv—Ba3—Clviii76.01 (11)
O2vii—Ba1—O1vii57.1 (2)Cliii—Ba3—Clviii114.35 (8)
O1viii—Ba1—O1vii67.8 (6)O2vi—Ba3—Cl148.1 (3)
O1ix—Ba1—O1vii172.2 (6)O2vii—Ba3—Cl80.57 (17)
O1vi—Ba1—O1vii120.000 (2)O2—Ba3—Cl80.57 (17)
O2iv—Ba1—O1x120.1 (2)Clxiv—Ba3—Cl76.01 (11)
O2v—Ba1—O1x57.1 (2)Cliii—Ba3—Cl114.35 (8)
O2—Ba1—O1x92.36 (18)Clviii—Ba3—Cl114.35 (8)
O2vi—Ba1—O1x120.1 (2)O2vi—Ba3—O175.6 (3)
O2i—Ba1—O1x92.36 (18)O2vii—Ba3—O156.2 (3)
O2vii—Ba1—O1x57.1 (2)O2—Ba3—O118.6 (2)
O1viii—Ba1—O1x120.000 (2)Clxiv—Ba3—O1144.427 (13)
O1ix—Ba1—O1x120.0Cliii—Ba3—O199.1 (2)
O1vi—Ba1—O1x172.2 (6)Clviii—Ba3—O1134.72 (15)
O1vii—Ba1—O1x52.2 (6)Cl—Ba3—O174.23 (13)
O2iv—Ba1—O1120.1 (2)Ba2—Cl—Ba3xiv180.0
O2v—Ba1—O192.36 (18)Ba2—Cl—Ba3xiii76.01 (11)
O2—Ba1—O157.1 (2)Ba3xiv—Cl—Ba3xiii103.99 (11)
O2vi—Ba1—O1120.1 (2)Ba2—Cl—Ba3ii76.01 (11)
O2i—Ba1—O157.1 (2)Ba3xiv—Cl—Ba3ii103.99 (11)
O2vii—Ba1—O192.36 (18)Ba3xiii—Cl—Ba3ii114.35 (8)
O1viii—Ba1—O1172.2 (6)Ba2—Cl—Ba376.01 (11)
O1ix—Ba1—O152.2 (6)Ba3xiv—Cl—Ba3103.99 (11)
O1vi—Ba1—O1120.000 (2)Ba3xiii—Cl—Ba3114.35 (8)
O1vii—Ba1—O1120.000 (1)Ba3ii—Cl—Ba3114.35 (8)
O1x—Ba1—O167.8 (6)Ba3xiv—Cl—Ba1145.64 (4)
O1xi—Ba2—O1x75.4 (4)Ba3xiii—Cl—Ba194.25 (11)
O1xi—Ba2—O175.4 (4)Ba3ii—Cl—Ba194.25 (11)
O1x—Ba2—O175.4 (4)
Symmetry codes: (i) x, y, z+1/2; (ii) x, y1, z; (iii) x1, y, z; (iv) x+y, x+1, z+1/2; (v) y+1, xy+1, z+1/2; (vi) x+y, x+1, z; (vii) y+1, xy+1, z; (viii) x, y+1, z; (ix) y, xy, z; (x) x+y+1, x+1, z; (xi) y+1, xy, z; (xii) x+y, x, z; (xiii) x+1, y, z; (xiv) x+1, y+1, z.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds