Lutetium(III) oxotellurate(IV), Lu₂Te₄O₁₁

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.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](e-O) = 0.007 Å
• R factor = 0.034
• wR factor = 0.074
• Data-to-parameter ratio = 14.0

checkCIF/PLATON results

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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

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Computing details

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)

Crystal data

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) Å^3	0.04 × 0.03 × 0.02 × 0.02 (radius) mm
Z = 4

Data collection

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

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.034	w = 1/[σ^2(Fo^2) + (0.0272P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00360 (11)

Special details

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Lu—O3^i	2.189 (7)	Te2—O5^iv	1.841 (7)
Lu—O5^ii	2.218 (7)	Te2—O4^iv	1.912 (7)
Lu—O2^iii	2.243 (7)	Te2—O6	2.023 (4)
Lu—O2^ii	2.327 (7)	Te2—O1^iv	2.312 (7)
Lu—O4^iv	2.365 (7)	O1—Te2^ii	2.312 (7)
Lu—O1^iv	2.416 (7)	O1—Lu^ii	2.416 (7)
Lu—O4^v	2.471 (7)	O2—Lu^x	2.243 (7)
Lu—O3^vi	2.480 (7)	O2—Lu^iv	2.327 (7)
Lu—Te2	3.5157 (10)	O3—Lu^xi	2.189 (7)
Lu—Te1^iii	3.5386 (9)	O3—Lu^vi	2.480 (7)
Lu—Lu^vii	3.7058 (9)	O4—Te2^ii	1.912 (7)
Lu—Lu^viii	3.7942 (9)	O4—Lu^ii	2.365 (7)
Te1—O3	1.871 (7)	O4—Lu^xii	2.471 (7)
Te1—O2	1.885 (7)	O5—Te2^ii	1.841 (7)
Te1—O1	1.892 (7)	O5—Lu^iv	2.218 (7)
Te1—O4^ix	2.567 (7)	O6—Te2^vi	2.023 (4)
Te1—Lu^x	3.5385 (9)
O3^i—Lu—O5^ii	97.6 (3)	O2^iii—Lu—Lu^vii	36.58 (17)
O3^i—Lu—O2^iii	95.8 (3)	O2^ii—Lu—Lu^vii	35.06 (16)
O5^ii—Lu—O2^iii	144.0 (3)	O4^iv—Lu—Lu^vii	133.73 (16)
O3^i—Lu—O2^ii	78.6 (3)	O1^iv—Lu—Lu^vii	73.23 (16)
O5^ii—Lu—O2^ii	78.6 (2)	O4^v—Lu—Lu^vii	102.45 (17)
O2^iii—Lu—O2^ii	71.6 (3)	O3^vi—Lu—Lu^vii	156.94 (16)
O3^i—Lu—O4^iv	135.8 (2)	Te2—Lu—Lu^vii	113.74 (2)
O5^ii—Lu—O4^iv	84.9 (2)	Te1^iii—Lu—Lu^vii	64.681 (15)
O2^iii—Lu—O4^iv	107.7 (2)	O3^i—Lu—Lu^viii	107.42 (19)
O2^ii—Lu—O4^iv	143.9 (2)	O5^ii—Lu—Lu^viii	118.71 (18)
O3^i—Lu—O1^iv	156.0 (3)	O2^iii—Lu—Lu^viii	88.33 (17)
O5^ii—Lu—O1^iv	78.8 (2)	O2^ii—Lu—Lu^viii	159.70 (16)
O2^iii—Lu—O1^iv	75.5 (2)	O4^iv—Lu—Lu^viii	39.33 (17)
O2^ii—Lu—O1^iv	77.4 (2)	O1^iv—Lu—Lu^viii	94.79 (16)
O4^iv—Lu—O1^iv	67.9 (2)	O4^v—Lu—Lu^viii	37.33 (16)
O3^i—Lu—O4^v	76.9 (2)	O3^vi—Lu—Lu^viii	63.74 (16)
O5^ii—Lu—O4^v	145.3 (2)	Te2—Lu—Lu^viii	67.902 (17)
O2^iii—Lu—O4^v	70.4 (2)	Te1^iii—Lu—Lu^viii	60.361 (17)
O2^ii—Lu—O4^v	131.8 (2)	Lu^vii—Lu—Lu^viii	124.84 (2)
O4^iv—Lu—O4^v	76.7 (3)	O3—Te1—O2	98.1 (3)
O1^iv—Lu—O4^v	119.2 (2)	O3—Te1—O1	101.7 (3)
O3^i—Lu—O3^vi	70.5 (3)	O2—Te1—O1	99.2 (3)
O5^ii—Lu—O3^vi	74.4 (2)	O3—Te1—Lu^x	73.3 (2)
O2^iii—Lu—O3^vi	141.6 (2)	O1—Te1—Lu^x	126.6 (2)
O2^ii—Lu—O3^vi	135.3 (2)	O5^iv—Te2—O4^iv	102.5 (3)
O4^iv—Lu—O3^vi	67.7 (2)	O5^iv—Te2—O6	89.6 (3)
O1^iv—Lu—O3^vi	129.5 (2)	O4^iv—Te2—O6	97.0 (2)
O4^v—Lu—O3^vi	71.5 (2)	O5^iv—Te2—O1^iv	90.2 (3)
O3^i—Lu—Te2	158.54 (19)	O4^iv—Te2—O1^iv	77.8 (3)
O5^ii—Lu—Te2	69.00 (17)	O6—Te2—O1^iv	174.65 (18)
O2^iii—Lu—Te2	104.77 (17)	O5^iv—Te2—Lu	112.8 (2)
O2^ii—Lu—Te2	113.29 (17)	O6—Te2—Lu	132.52 (18)
O4^iv—Lu—Te2	30.70 (16)	Te1—O1—Te2^ii	117.3 (3)
O1^iv—Lu—Te2	40.84 (16)	Te1—O1—Lu^ii	139.5 (4)
O4^v—Lu—Te2	104.19 (16)	Te2^ii—O1—Lu^ii	96.1 (2)
O3^vi—Lu—Te2	89.28 (16)	Te1—O2—Lu^x	117.8 (3)
O3^i—Lu—Te1^iii	100.68 (19)	Te1—O2—Lu^iv	133.8 (3)
O5^ii—Lu—Te1^iii	160.92 (17)	Lu^x—O2—Lu^iv	108.4 (3)
O2^iii—Lu—Te1^iii	28.11 (17)	Te1—O3—Lu^xi	134.3 (4)
O2^ii—Lu—Te1^iii	99.73 (17)	Te1—O3—Lu^vi	115.4 (3)
O4^iv—Lu—Te1^iii	85.76 (17)	Lu^xi—O3—Lu^vi	109.5 (3)
O1^iv—Lu—Te1^iii	82.28 (17)	Te2^ii—O4—Lu^ii	110.1 (3)
O4^v—Lu—Te1^iii	46.49 (16)	Te2^ii—O4—Lu^xii	137.4 (3)
O3^vi—Lu—Te1^iii	116.97 (17)	Lu^ii—O4—Lu^xii	103.3 (3)
Te2—Lu—Te1^iii	94.907 (18)	Te2^ii—O5—Lu^iv	132.4 (4)
O3^i—Lu—Lu^vii	86.44 (19)	Te2^vi—O6—Te2	138.9 (5)
O5^ii—Lu—Lu^vii	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.