Rare-earth(III) oxotellurates(IV) with the composition M2Te4O11 are known for yttrium and all lanthanides except promethium and lutetium from single-crystal X-ray structure determinations. Single crystals of the last missing non-radioactive isostructural compound, Lu2Te4O11, can now be obtained by modifying the common method of synthesis from the binary oxides (Lu2O3 and TeO2; 1:4 molar ratio) using torch-sealed non-evacuated silica ampoules as reaction containers. The structure contains layers of edge-sharing [LuO8] polyhedra connected by oxotellurate(IV) chains. These consist of [TeO3]2− and [Te2O5]2− anions (with ψ1-tetrahedral oxygen coordination for all central Te4+ cations) linked by strong secondary Te—O interactions.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (e-O) = 0.007 Å
- R factor = 0.034
- wR factor = 0.074
- Data-to-parameter ratio = 14.0
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
2 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
0 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
Data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: SHELXL97.
lutetium(III) oxotellurate(IV)
top
Crystal data top
Lu2Te4O11 | F(000) = 1752 |
Mr = 1036.34 | Dx = 7.241 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71069 Å |
Hall symbol: -C 2yc | Cell parameters from 3912 reflections |
a = 12.2953 (8) Å | θ = 1.0–27.5° |
b = 5.0596 (3) Å | µ = 32.74 mm−1 |
c = 15.9134 (9) Å | T = 293 K |
β = 106.202 (7)° | Spheroid, colourless |
V = 950.64 (10) Å3 | 0.04 × 0.03 × 0.02 × 0.02 (radius) mm |
Z = 4 | |
Data collection top
Nonius KappaCCD diffractometer | 1108 independent reflections |
Radiation source: fine-focus sealed tube | 791 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.096 |
Detector resolution: 9 pixels mm-1 | θmax = 27.6°, θmin = 2.7° |
φ and ω scans | h = −16→16 |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1998) | k = −6→6 |
Tmin = 0.320, Tmax = 0.539 | l = −20→20 |
10819 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.034 | w = 1/[σ2(Fo2) + (0.0272P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.074 | (Δ/σ)max = 0.001 |
S = 1.00 | Δρmax = 1.86 e Å−3 |
1108 reflections | Δρmin = −1.38 e Å−3 |
79 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00360 (11) |
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 | |
Lu | 0.11947 (4) | 0.25158 (8) | 0.03650 (3) | 0.01016 (19) | |
Te1 | 0.12680 (5) | 0.27753 (16) | 0.37376 (4) | 0.0092 (2) | |
Te2 | 0.12238 (6) | 0.72315 (17) | 0.19938 (5) | 0.0103 (2) | |
O1 | 0.2506 (6) | 0.0593 (13) | 0.3708 (5) | 0.0132 (16) | |
O2 | 0.2058 (6) | 0.5491 (13) | 0.4468 (5) | 0.0136 (16) | |
O3 | 0.0700 (6) | 0.1034 (13) | 0.4563 (5) | 0.0155 (16) | |
O4 | 0.4759 (6) | 0.0809 (13) | 0.4059 (5) | 0.0134 (16) | |
O5 | 0.3522 (6) | 0.5610 (13) | 0.3336 (5) | 0.0146 (16) | |
O6 | 0.0000 | 0.863 (2) | 0.2500 | 0.020 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Lu | 0.0104 (3) | 0.0107 (3) | 0.0096 (3) | 0.0002 (2) | 0.00312 (18) | 0.0003 (2) |
Te1 | 0.0089 (4) | 0.0103 (4) | 0.0086 (4) | 0.0000 (3) | 0.0026 (3) | −0.0008 (3) |
Te2 | 0.0108 (4) | 0.0112 (4) | 0.0089 (4) | −0.0003 (2) | 0.0027 (3) | 0.0020 (3) |
O1 | 0.013 (4) | 0.013 (4) | 0.015 (4) | −0.001 (3) | 0.006 (3) | 0.005 (3) |
O2 | 0.014 (4) | 0.015 (4) | 0.015 (4) | −0.001 (3) | 0.008 (3) | −0.001 (3) |
O3 | 0.021 (4) | 0.014 (4) | 0.010 (4) | 0.002 (3) | 0.002 (3) | 0.002 (3) |
O4 | 0.012 (4) | 0.011 (4) | 0.014 (4) | −0.001 (3) | −0.002 (3) | −0.001 (3) |
O5 | 0.026 (4) | 0.011 (3) | 0.010 (4) | 0.006 (3) | 0.010 (3) | 0.005 (3) |
O6 | 0.018 (6) | 0.025 (6) | 0.021 (7) | 0.000 | 0.013 (5) | 0.000 |
Geometric parameters (Å, º) top
Lu—O3i | 2.189 (7) | Te2—O5iv | 1.841 (7) |
Lu—O5ii | 2.218 (7) | Te2—O4iv | 1.912 (7) |
Lu—O2iii | 2.243 (7) | Te2—O6 | 2.023 (4) |
Lu—O2ii | 2.327 (7) | Te2—O1iv | 2.312 (7) |
Lu—O4iv | 2.365 (7) | O1—Te2ii | 2.312 (7) |
Lu—O1iv | 2.416 (7) | O1—Luii | 2.416 (7) |
Lu—O4v | 2.471 (7) | O2—Lux | 2.243 (7) |
Lu—O3vi | 2.480 (7) | O2—Luiv | 2.327 (7) |
Lu—Te2 | 3.5157 (10) | O3—Luxi | 2.189 (7) |
Lu—Te1iii | 3.5386 (9) | O3—Luvi | 2.480 (7) |
Lu—Luvii | 3.7058 (9) | O4—Te2ii | 1.912 (7) |
Lu—Luviii | 3.7942 (9) | O4—Luii | 2.365 (7) |
Te1—O3 | 1.871 (7) | O4—Luxii | 2.471 (7) |
Te1—O2 | 1.885 (7) | O5—Te2ii | 1.841 (7) |
Te1—O1 | 1.892 (7) | O5—Luiv | 2.218 (7) |
Te1—O4ix | 2.567 (7) | O6—Te2vi | 2.023 (4) |
Te1—Lux | 3.5385 (9) | | |
| | | |
O3i—Lu—O5ii | 97.6 (3) | O2iii—Lu—Luvii | 36.58 (17) |
O3i—Lu—O2iii | 95.8 (3) | O2ii—Lu—Luvii | 35.06 (16) |
O5ii—Lu—O2iii | 144.0 (3) | O4iv—Lu—Luvii | 133.73 (16) |
O3i—Lu—O2ii | 78.6 (3) | O1iv—Lu—Luvii | 73.23 (16) |
O5ii—Lu—O2ii | 78.6 (2) | O4v—Lu—Luvii | 102.45 (17) |
O2iii—Lu—O2ii | 71.6 (3) | O3vi—Lu—Luvii | 156.94 (16) |
O3i—Lu—O4iv | 135.8 (2) | Te2—Lu—Luvii | 113.74 (2) |
O5ii—Lu—O4iv | 84.9 (2) | Te1iii—Lu—Luvii | 64.681 (15) |
O2iii—Lu—O4iv | 107.7 (2) | O3i—Lu—Luviii | 107.42 (19) |
O2ii—Lu—O4iv | 143.9 (2) | O5ii—Lu—Luviii | 118.71 (18) |
O3i—Lu—O1iv | 156.0 (3) | O2iii—Lu—Luviii | 88.33 (17) |
O5ii—Lu—O1iv | 78.8 (2) | O2ii—Lu—Luviii | 159.70 (16) |
O2iii—Lu—O1iv | 75.5 (2) | O4iv—Lu—Luviii | 39.33 (17) |
O2ii—Lu—O1iv | 77.4 (2) | O1iv—Lu—Luviii | 94.79 (16) |
O4iv—Lu—O1iv | 67.9 (2) | O4v—Lu—Luviii | 37.33 (16) |
O3i—Lu—O4v | 76.9 (2) | O3vi—Lu—Luviii | 63.74 (16) |
O5ii—Lu—O4v | 145.3 (2) | Te2—Lu—Luviii | 67.902 (17) |
O2iii—Lu—O4v | 70.4 (2) | Te1iii—Lu—Luviii | 60.361 (17) |
O2ii—Lu—O4v | 131.8 (2) | Luvii—Lu—Luviii | 124.84 (2) |
O4iv—Lu—O4v | 76.7 (3) | O3—Te1—O2 | 98.1 (3) |
O1iv—Lu—O4v | 119.2 (2) | O3—Te1—O1 | 101.7 (3) |
O3i—Lu—O3vi | 70.5 (3) | O2—Te1—O1 | 99.2 (3) |
O5ii—Lu—O3vi | 74.4 (2) | O3—Te1—Lux | 73.3 (2) |
O2iii—Lu—O3vi | 141.6 (2) | O1—Te1—Lux | 126.6 (2) |
O2ii—Lu—O3vi | 135.3 (2) | O5iv—Te2—O4iv | 102.5 (3) |
O4iv—Lu—O3vi | 67.7 (2) | O5iv—Te2—O6 | 89.6 (3) |
O1iv—Lu—O3vi | 129.5 (2) | O4iv—Te2—O6 | 97.0 (2) |
O4v—Lu—O3vi | 71.5 (2) | O5iv—Te2—O1iv | 90.2 (3) |
O3i—Lu—Te2 | 158.54 (19) | O4iv—Te2—O1iv | 77.8 (3) |
O5ii—Lu—Te2 | 69.00 (17) | O6—Te2—O1iv | 174.65 (18) |
O2iii—Lu—Te2 | 104.77 (17) | O5iv—Te2—Lu | 112.8 (2) |
O2ii—Lu—Te2 | 113.29 (17) | O6—Te2—Lu | 132.52 (18) |
O4iv—Lu—Te2 | 30.70 (16) | Te1—O1—Te2ii | 117.3 (3) |
O1iv—Lu—Te2 | 40.84 (16) | Te1—O1—Luii | 139.5 (4) |
O4v—Lu—Te2 | 104.19 (16) | Te2ii—O1—Luii | 96.1 (2) |
O3vi—Lu—Te2 | 89.28 (16) | Te1—O2—Lux | 117.8 (3) |
O3i—Lu—Te1iii | 100.68 (19) | Te1—O2—Luiv | 133.8 (3) |
O5ii—Lu—Te1iii | 160.92 (17) | Lux—O2—Luiv | 108.4 (3) |
O2iii—Lu—Te1iii | 28.11 (17) | Te1—O3—Luxi | 134.3 (4) |
O2ii—Lu—Te1iii | 99.73 (17) | Te1—O3—Luvi | 115.4 (3) |
O4iv—Lu—Te1iii | 85.76 (17) | Luxi—O3—Luvi | 109.5 (3) |
O1iv—Lu—Te1iii | 82.28 (17) | Te2ii—O4—Luii | 110.1 (3) |
O4v—Lu—Te1iii | 46.49 (16) | Te2ii—O4—Luxii | 137.4 (3) |
O3vi—Lu—Te1iii | 116.97 (17) | Luii—O4—Luxii | 103.3 (3) |
Te2—Lu—Te1iii | 94.907 (18) | Te2ii—O5—Luiv | 132.4 (4) |
O3i—Lu—Luvii | 86.44 (19) | Te2vi—O6—Te2 | 138.9 (5) |
O5ii—Lu—Luvii | 111.43 (19) | | |
Symmetry codes: (i) x, −y, z−1/2; (ii) −x+1/2, y−1/2, −z+1/2; (iii) x, −y+1, z−1/2; (iv) −x+1/2, y+1/2, −z+1/2; (v) x−1/2, −y+1/2, z−1/2; (vi) −x, y, −z+1/2; (vii) −x+1/2, −y+1/2, −z; (viii) −x, −y+1, −z; (ix) x−1/2, y+1/2, z; (x) x, −y+1, z+1/2; (xi) x, −y, z+1/2; (xii) x+1/2, −y+1/2, z+1/2. |
Motifs of mutual adjunction and coordination numbers (CN) top | O1 | O2 | O3 | O4 | O5 | O6 | CN |
Lu | 1/1 | 2/2 | 2/2 | 2/2 | 1/1 | 0/0 | 8 |
Te1 | 1/1 | 1/1 | 1/1 | 0+1/0+1 | 0/0 | 0/0 | 3+1 |
Te2 | 0+1/0+1 | 0/0 | 0/0 | 1/1 | 1/1 | 1/2 | 3+1 |
CN | 2+1 | 3 | 3 | 3+1 | 2 | 2 | |