Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807016790/wm2105sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807016790/wm2105Isup2.hkl |
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.
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 |
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 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 |
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. |
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)* |
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 |
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. |
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