The structure of pentabarium ditantalum dichloride nonaoxide, Ba
5Ta
2Cl
2O
9, is isotypic with Ba
5Ru
1.6W
0.4Cl
2O
9 and with one polymorph of Ba
5Ru
2Cl
2O
9. It is related to the perovskite structure and shows a ten-layer stacking of BaO
3 and BaCl blocks along the
c axis. The Ta cations occupy octahedral interstices, forming Ta
2O
9 dimers of distorted face-shared TaO
6 octahedra. Except for one O atom, all atoms are situated on special positions: Ba1 (Wyckoff position
m2), Ba2 and Ba3 (3
m.), Ta (3
m.), Cl (3
m.) and O1 (
mm2).
Supporting information
Key indicators
- Single-crystal synchrotron study
- T = 150 K
- Mean (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
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
Ba5Ta2Cl2O9 | Dx = 5.467 Mg m−3 |
Mr = 1263.50 | Synchrotron radiation, λ = 0.78480 Å |
Hexagonal, P63/mmc | Cell parameters from 1215 reflections |
Hall symbol: -P 6c 2c | θ = 4.7–31.7° |
a = 5.9787 (3) Å | µ = 27.18 mm−1 |
c = 24.796 (3) Å | T = 150 K |
V = 767.59 (10) Å3 | Block, yellow |
Z = 2 | 0.04 × 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 16.2SMX | 317 reflections with I > 2σ(I) |
Silicon 111 monochromator | Rint = 0.093 |
ω scans | θmax = 29.3°, θmin = 4.4° |
Absorption correction: multi-scan (SADABS; Bruker, 2004) | h = −7→7 |
Tmin = 0.337, Tmax = 0.665 | k = −7→7 |
5409 measured reflections | l = −30→30 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.035 | Secondary 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 reflections | Δρmax = 1.93 e Å−3 |
20 parameters | Δρmin = −2.88 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Ba1 | 0.3333 | 0.6667 | 0.2500 | 0.0060 (5) | |
Ba2 | 0.6667 | 0.3333 | 0.17192 (5) | 0.0060 (4) | |
Ba3 | 0.3333 | 0.6667 | 0.08105 (6) | 0.0085 (4) | |
Ta | 0.0000 | 0.0000 | 0.18941 (4) | 0.0047 (3) | |
Cl | 0.6667 | 0.3333 | 0.0464 (3) | 0.032 (2) | |
O1 | 0.294 (3) | 0.1470 (15) | 0.2500 | 0.015 (3)* | |
O2 | 0.1613 (13) | 0.323 (3) | 0.1552 (5) | 0.023 (2)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ba1 | 0.0044 (6) | 0.0044 (6) | 0.0090 (9) | 0.0022 (3) | 0.000 | 0.000 |
Ba2 | 0.0050 (5) | 0.0050 (5) | 0.0081 (7) | 0.0025 (2) | 0.000 | 0.000 |
Ba3 | 0.0092 (5) | 0.0092 (5) | 0.0070 (7) | 0.0046 (2) | 0.000 | 0.000 |
Ta1 | 0.0032 (4) | 0.0032 (4) | 0.0079 (6) | 0.00159 (18) | 0.000 | 0.000 |
Cl1 | 0.044 (3) | 0.044 (3) | 0.009 (3) | 0.0220 (16) | 0.000 | 0.000 |
Geometric parameters (Å, º) top
O1—Ta | 2.139 (11) | Ba2—O1x | 2.734 (11) |
O1—Tai | 2.139 (11) | Ba2—O2xii | 3.018 (16) |
O1—Ba2i | 2.734 (11) | Ba2—O2xiii | 3.018 (17) |
O1—Ba2 | 2.734 (11) | Ba2—O2xi | 3.018 (16) |
O1—Ba1ii | 2.996 (11) | Ba2—O2vii | 3.018 (16) |
O1—Ba1 | 2.996 (11) | Ba2—O2x | 3.018 (17) |
O2—Ta | 1.873 (13) | Ba2—Cl | 3.113 (7) |
O2—Ba3 | 2.561 (12) | Ta—O2ix | 1.873 (13) |
O2—Ba1 | 2.949 (12) | Ta—O2xii | 1.873 (13) |
O2—Ba2iii | 3.018 (16) | Ta—O1ix | 2.139 (11) |
O2—Ba2 | 3.018 (16) | Ta—O1xii | 2.139 (11) |
Ba1—O2iv | 2.949 (12) | Ta—Tai | 3.0046 (19) |
Ba1—O2v | 2.949 (12) | Ba3—O2vi | 2.561 (12) |
Ba1—O2vi | 2.949 (12) | Ba3—O2vii | 2.561 (12) |
Ba1—O2i | 2.949 (12) | Ba3—Clxiv | 3.159 (7) |
Ba1—O2vii | 2.949 (12) | Ba3—Cliii | 3.5574 (17) |
Ba1—O1viii | 2.996 (11) | Ba3—Clviii | 3.5574 (17) |
Ba1—O1ix | 2.996 (11) | Ba3—Cl | 3.5574 (17) |
Ba1—O1vi | 2.996 (11) | Cl—Ba3xiv | 3.159 (7) |
Ba1—O1vii | 2.996 (11) | Cl—Ba3xiii | 3.5574 (17) |
Ba1—O1x | 2.996 (10) | Cl—Ba3ii | 3.5574 (17) |
Ba2—O1xi | 2.734 (11) | | |
| | | |
Ta—O1—Tai | 89.2 (6) | O1xi—Ba2—O2xii | 96.3 (2) |
Ta—O1—Ba2i | 179.5 (6) | O1x—Ba2—O2xii | 134.1 (3) |
Tai—O1—Ba2i | 90.28 (7) | O1—Ba2—O2xii | 59.0 (3) |
Ta—O1—Ba2 | 90.28 (7) | O1xi—Ba2—O2xiii | 59.0 (3) |
Tai—O1—Ba2 | 179.5 (6) | O1x—Ba2—O2xiii | 96.3 (2) |
Ba2i—O1—Ba2 | 90.2 (5) | O1—Ba2—O2xiii | 134.1 (3) |
Ta—O1—Ba1ii | 92.8 (2) | O2xii—Ba2—O2xiii | 118.15 (10) |
Tai—O1—Ba1ii | 92.8 (2) | O1xi—Ba2—O2xi | 59.0 (3) |
Ba2i—O1—Ba1ii | 87.2 (2) | O1x—Ba2—O2xi | 134.1 (3) |
Ba2—O1—Ba1ii | 87.2 (2) | O1—Ba2—O2xi | 96.3 (2) |
Ta—O1—Ba1 | 92.8 (2) | O2xii—Ba2—O2xi | 61.5 (5) |
Tai—O1—Ba1 | 92.8 (2) | O2xiii—Ba2—O2xi | 57.3 (5) |
Ba2i—O1—Ba1 | 87.2 (2) | O1xi—Ba2—O2vii | 134.1 (3) |
Ba2—O1—Ba1 | 87.2 (2) | O1x—Ba2—O2vii | 59.0 (3) |
Ba1ii—O1—Ba1 | 172.2 (6) | O1—Ba2—O2vii | 96.3 (2) |
Ta—O1—Ba3 | 57.10 (6) | O2xii—Ba2—O2vii | 118.15 (10) |
Tai—O1—Ba3 | 126.8 (4) | O2xiii—Ba2—O2vii | 118.15 (10) |
Ba2i—O1—Ba3 | 123.2 (3) | O2xi—Ba2—O2vii | 164.1 (4) |
Ba2—O1—Ba3 | 52.84 (18) | O1xi—Ba2—O2x | 96.3 (2) |
Ba1ii—O1—Ba3 | 125.20 (5) | O1x—Ba2—O2x | 59.0 (3) |
Ta—O2—Ba3 | 161.0 (6) | O1—Ba2—O2x | 134.1 (3) |
Ta—O2—Ba1 | 100.3 (5) | O2xii—Ba2—O2x | 164.1 (4) |
Ba3—O2—Ba1 | 98.7 (4) | O2xiii—Ba2—O2x | 61.5 (5) |
Ta—O2—Ba2iii | 87.4 (2) | O2xi—Ba2—O2x | 118.15 (10) |
Ba3—O2—Ba2iii | 94.9 (2) | O2vii—Ba2—O2x | 57.3 (5) |
Ba1—O2—Ba2iii | 83.1 (2) | O1xi—Ba2—O2 | 134.1 (3) |
Ta—O2—Ba2 | 87.4 (2) | O1x—Ba2—O2 | 96.3 (2) |
Ba3—O2—Ba2 | 94.9 (2) | O1—Ba2—O2 | 59.0 (3) |
Ba1—O2—Ba2 | 83.1 (2) | O2xii—Ba2—O2 | 57.3 (5) |
Ba2iii—O2—Ba2 | 164.1 (4) | O2xiii—Ba2—O2 | 164.1 (4) |
O2iv—Ba1—O2v | 63.1 (4) | O2xi—Ba2—O2 | 118.15 (10) |
O2iv—Ba1—O2 | 144.8 (2) | O2vii—Ba2—O2 | 61.5 (5) |
O2v—Ba1—O2 | 144.8 (2) | O2x—Ba2—O2 | 118.15 (10) |
O2iv—Ba1—O2vi | 105.7 (5) | O1xi—Ba2—Cl | 135.1 (2) |
O2v—Ba1—O2vi | 144.8 (2) | O1x—Ba2—Cl | 135.1 (2) |
O2—Ba1—O2vi | 63.1 (4) | O1—Ba2—Cl | 135.1 (2) |
O2iv—Ba1—O2i | 63.1 (4) | O2xii—Ba2—Cl | 82.1 (2) |
O2v—Ba1—O2i | 63.1 (4) | O2xiii—Ba2—Cl | 82.1 (2) |
O2—Ba1—O2i | 105.7 (5) | O2xi—Ba2—Cl | 82.1 (2) |
O2vi—Ba1—O2i | 144.8 (2) | O2vii—Ba2—Cl | 82.1 (2) |
O2iv—Ba1—O2vii | 144.8 (2) | O2x—Ba2—Cl | 82.1 (2) |
O2v—Ba1—O2vii | 105.7 (5) | O2—Ba2—Cl | 82.1 (2) |
O2—Ba1—O2vii | 63.1 (4) | O2ix—Ta—O2 | 101.1 (5) |
O2vi—Ba1—O2vii | 63.1 (4) | O2ix—Ta—O2xii | 101.1 (5) |
O2i—Ba1—O2vii | 144.8 (2) | O2—Ta—O2xii | 101.1 (5) |
O2iv—Ba1—O1viii | 57.1 (2) | O2ix—Ta—O1 | 162.3 (5) |
O2v—Ba1—O1viii | 92.36 (19) | O2—Ta—O1 | 90.0 (3) |
O2—Ba1—O1viii | 120.1 (2) | O2xii—Ta—O1 | 90.0 (3) |
O2vi—Ba1—O1viii | 57.1 (2) | O2ix—Ta—O1ix | 90.0 (3) |
O2i—Ba1—O1viii | 120.1 (2) | O2—Ta—O1ix | 90.0 (3) |
O2vii—Ba1—O1viii | 92.36 (19) | O2xii—Ta—O1ix | 162.3 (5) |
O2iv—Ba1—O1ix | 92.36 (18) | O1—Ta—O1ix | 76.1 (5) |
O2v—Ba1—O1ix | 120.1 (2) | O2ix—Ta—O1xii | 90.0 (3) |
O2—Ba1—O1ix | 57.1 (2) | O2—Ta—O1xii | 162.3 (5) |
O2vi—Ba1—O1ix | 92.36 (18) | O2xii—Ta—O1xii | 90.0 (3) |
O2i—Ba1—O1ix | 57.1 (2) | O1—Ta—O1xii | 76.1 (5) |
O2vii—Ba1—O1ix | 120.1 (2) | O1ix—Ta—O1xii | 76.1 (5) |
O1viii—Ba1—O1ix | 120.000 (2) | O2vi—Ba3—O2vii | 74.1 (4) |
O2iv—Ba1—O1vi | 57.1 (2) | O2vi—Ba3—O2 | 74.1 (4) |
O2v—Ba1—O1vi | 120.1 (2) | O2vii—Ba3—O2 | 74.1 (4) |
O2—Ba1—O1vi | 92.36 (19) | O2vi—Ba3—Clxiv | 135.9 (3) |
O2vi—Ba1—O1vi | 57.1 (2) | O2vii—Ba3—Clxiv | 135.9 (3) |
O2i—Ba1—O1vi | 92.36 (19) | O2—Ba3—Clxiv | 135.9 (3) |
O2vii—Ba1—O1vi | 120.1 (2) | O2vi—Ba3—Cliii | 80.57 (17) |
O1viii—Ba1—O1vi | 52.2 (6) | O2vii—Ba3—Cliii | 148.1 (3) |
O1ix—Ba1—O1vi | 67.8 (6) | O2—Ba3—Cliii | 80.57 (17) |
O2iv—Ba1—O1vii | 92.36 (18) | Clxiv—Ba3—Cliii | 76.01 (11) |
O2v—Ba1—O1vii | 57.1 (2) | O2vi—Ba3—Clviii | 80.57 (17) |
O2—Ba1—O1vii | 120.1 (2) | O2vii—Ba3—Clviii | 80.57 (17) |
O2vi—Ba1—O1vii | 92.36 (18) | O2—Ba3—Clviii | 148.1 (3) |
O2i—Ba1—O1vii | 120.1 (2) | Clxiv—Ba3—Clviii | 76.01 (11) |
O2vii—Ba1—O1vii | 57.1 (2) | Cliii—Ba3—Clviii | 114.35 (8) |
O1viii—Ba1—O1vii | 67.8 (6) | O2vi—Ba3—Cl | 148.1 (3) |
O1ix—Ba1—O1vii | 172.2 (6) | O2vii—Ba3—Cl | 80.57 (17) |
O1vi—Ba1—O1vii | 120.000 (2) | O2—Ba3—Cl | 80.57 (17) |
O2iv—Ba1—O1x | 120.1 (2) | Clxiv—Ba3—Cl | 76.01 (11) |
O2v—Ba1—O1x | 57.1 (2) | Cliii—Ba3—Cl | 114.35 (8) |
O2—Ba1—O1x | 92.36 (18) | Clviii—Ba3—Cl | 114.35 (8) |
O2vi—Ba1—O1x | 120.1 (2) | O2vi—Ba3—O1 | 75.6 (3) |
O2i—Ba1—O1x | 92.36 (18) | O2vii—Ba3—O1 | 56.2 (3) |
O2vii—Ba1—O1x | 57.1 (2) | O2—Ba3—O1 | 18.6 (2) |
O1viii—Ba1—O1x | 120.000 (2) | Clxiv—Ba3—O1 | 144.427 (13) |
O1ix—Ba1—O1x | 120.0 | Cliii—Ba3—O1 | 99.1 (2) |
O1vi—Ba1—O1x | 172.2 (6) | Clviii—Ba3—O1 | 134.72 (15) |
O1vii—Ba1—O1x | 52.2 (6) | Cl—Ba3—O1 | 74.23 (13) |
O2iv—Ba1—O1 | 120.1 (2) | Ba2—Cl—Ba3xiv | 180.0 |
O2v—Ba1—O1 | 92.36 (18) | Ba2—Cl—Ba3xiii | 76.01 (11) |
O2—Ba1—O1 | 57.1 (2) | Ba3xiv—Cl—Ba3xiii | 103.99 (11) |
O2vi—Ba1—O1 | 120.1 (2) | Ba2—Cl—Ba3ii | 76.01 (11) |
O2i—Ba1—O1 | 57.1 (2) | Ba3xiv—Cl—Ba3ii | 103.99 (11) |
O2vii—Ba1—O1 | 92.36 (18) | Ba3xiii—Cl—Ba3ii | 114.35 (8) |
O1viii—Ba1—O1 | 172.2 (6) | Ba2—Cl—Ba3 | 76.01 (11) |
O1ix—Ba1—O1 | 52.2 (6) | Ba3xiv—Cl—Ba3 | 103.99 (11) |
O1vi—Ba1—O1 | 120.000 (2) | Ba3xiii—Cl—Ba3 | 114.35 (8) |
O1vii—Ba1—O1 | 120.000 (1) | Ba3ii—Cl—Ba3 | 114.35 (8) |
O1x—Ba1—O1 | 67.8 (6) | Ba3xiv—Cl—Ba1 | 145.64 (4) |
O1xi—Ba2—O1x | 75.4 (4) | Ba3xiii—Cl—Ba1 | 94.25 (11) |
O1xi—Ba2—O1 | 75.4 (4) | Ba3ii—Cl—Ba1 | 94.25 (11) |
O1x—Ba2—O1 | 75.4 (4) | | |
Symmetry codes: (i) x, y, −z+1/2; (ii) x, y−1, z; (iii) x−1, y, z; (iv) −x+y, −x+1, −z+1/2; (v) −y+1, x−y+1, −z+1/2; (vi) −x+y, −x+1, z; (vii) −y+1, x−y+1, z; (viii) x, y+1, z; (ix) −y, x−y, z; (x) −x+y+1, −x+1, z; (xi) −y+1, x−y, z; (xii) −x+y, −x, z; (xiii) x+1, y, z; (xiv) −x+1, −y+1, −z. |