Li(3)Al(MoO(2))(2)O(2)(AsO(4))(2).

Single crystals of trilithium(I) aluminium(III) bis-[dioxidomolybdenum(VI)] dioxide bis-[arsenate(V)], Li(3)AlMo(2)As(2)O(14), have been prepared by solid-state reaction at 788 K. The structure consists of AsO(4) tetra-hedra, AlO(6) octa-hedra and Mo(2)O(10) groups sharing corners to form a three-dimensional framework containing channels running respectively along the [100] and [010] directions, where the Li(+) ions are located. This structure is compared with compounds having (MX(2)O(12))(n) chains (M = Mo, Al and X = P, As) and others containing M(2)O(10) (M = Mo, Fe) dimers.

Littérature assocíee

Pour le détail de la préparation, voir: Hajji et al. (2004 ▶, 2005 ▶); Zid et al. (1997 ▶, 1998 ▶). Pour le détail des composés avec structures reliées, voir: Lii et al. (1989 ▶); Leclaire et al. (1990 ▶); Driss & Jouini (1989 ▶); Guesdon et al. (1994 ▶); Borel et al. (1994 ▶); LeBail et al. (1995 ▶). Pour le détail des propriétés des composés reliés, voir: Manthiram & Goodenough, 1989 ▶; Tarascon et al., 1991 ▶; Sigala et al., 1997 ▶; Padhi et al., 1997 ▶; Masquelier et al., 1998 ▶. Pour le calcul des valences des liaisons, voir: Brown & Altermatt (1985 ▶)

Partie expérimentale

Données crystallines

Li3Al(MoO2)2O2(AsO4)2

M = 613.52

Triclinique,

a = 5.213 (1) Å

b = 5.426 (1) Å

c = 9.474 (2) Å

α = 95.98 (2)°

β = 102.25 (1)°

γ = 105.30 (1)°

V = 248.92 (9) Å3

Z = 1

Mo Kα radiation

μ = 9.29 mm−1

T = 298 K

0.20 × 0.15 × 0.12 mm

Collection des données

Diffractomètre Enraf–Nonius TurboCAD-4

Correction d’absorption: ψ scan (North et al., 1968 ▶) T min = 0.209, T max = 0.328

1663 réflexions mesurées

1084 réflexions independantes

1077 réflexions avec I > 2σ(I)

R int = 0.007

2 réflexions de référence fréquence: 120 min décroissance d’intensité: 1.1%

Affinement

R[F 2 > 2σ(F 2)] = 0.013

wR(F 2) = 0.039

S = 1.06

1084 réflexions

104 paramètres

Δρmax = 0.64 e Å−3

Δρmin = −0.41 e Å−3

Collection des données: CAD-4 EXPRESS (Duisenberg, 1992 ▶; Macíček & Yordanov, 1992 ▶); affinement des paramètres de la maille: CAD-4 EXPRESS; reduction des données: XCAD4 (Harms & Wocadlo, 1995 ▶); programme(s) pour la solution de la structure: SHELXS97 (Sheldrick, 2008 ▶); programme(s) pour l’affinement de la structure: SHELXL97 (Sheldrick, 2008 ▶); graphisme moléculaire: DIAMOND (Brandenburg, 1998 ▶); logiciel utilisé pour préparer le matériel pour publication: WinGX (Farrugia, 1999 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053680900631X/br2097sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053680900631X/br2097Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Li3Al(MoO2)2O2(AsO4)2	Z = 1
Mr = 613.52	F(000) = 284
Triclinic, P1	Dx = 4.093 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 5.213 (1) Å	Cell parameters from 25 reflections
b = 5.426 (1) Å	θ = 10–16°
c = 9.474 (2) Å	µ = 9.29 mm−1
α = 95.98 (2)°	T = 298 K
β = 102.25 (1)°	Prism, yellow
γ = 105.30 (1)°	0.20 × 0.15 × 0.12 mm
V = 248.92 (9) Å3

Enraf–Nonius TurboCAD-4 diffractometer	1077 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.007
graphite	θmax = 27.0°, θmin = 2.2°
ω/2θ scans	h = −2→6
Absorption correction: ψ scan (North et al., 1968)	k = −6→6
Tmin = 0.209, Tmax = 0.328	l = −12→12
1663 measured reflections	2 standard reflections every 120 min
1084 independent reflections	intensity decay: 1.1%

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)] = 0.013	w = 1/[σ2(Fo2) + (0.021P)2 + 0.6735P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.039	(Δ/σ)max = 0.001
S = 1.06	Δρmax = 0.64 e Å−3
1084 reflections	Δρmin = −0.41 e Å−3
104 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraints	Extinction coefficient: 0.0263 (14)

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
Mo	0.49876 (4)	0.84099 (4)	0.35495 (2)	0.00633 (9)
As	0.15020 (5)	0.23501 (5)	0.17692 (3)	0.00601 (10)
Al	0.5000	0.0000	0.0000	0.0026 (2)
Li1	0.0000	0.5000	0.5000	0.0225 (16)
Li2	0.8077 (14)	0.6121 (14)	0.1486 (9)	0.0392 (16)
O1	0.6756 (4)	0.1635 (4)	0.4618 (2)	0.0099 (4)
O2	0.7195 (4)	0.6684 (4)	0.4132 (2)	0.0132 (4)
O3	0.4158 (4)	0.2923 (4)	0.0959 (2)	0.0109 (4)
O4	0.8654 (4)	0.2067 (4)	0.0441 (2)	0.0110 (4)
O5	0.5596 (4)	0.8659 (4)	0.1781 (2)	0.0098 (4)
O6	0.1363 (4)	−0.0156 (4)	0.2672 (2)	0.0101 (4)
O7	0.1633 (4)	0.5095 (4)	0.2895 (2)	0.0106 (4)

	U11	U22	U33	U12	U13	U23
Mo	0.00695 (13)	0.00664 (13)	0.00518 (13)	0.00175 (8)	0.00146 (8)	0.00074 (8)
As	0.00626 (14)	0.00629 (14)	0.00524 (14)	0.00179 (10)	0.00123 (10)	0.00057 (9)
Al	0.0027 (5)	0.0038 (4)	0.0011 (4)	0.0005 (4)	0.0004 (3)	0.0002 (3)
Li1	0.018 (4)	0.018 (4)	0.031 (4)	0.007 (3)	−0.001 (3)	0.011 (3)
Li2	0.031 (3)	0.031 (3)	0.063 (5)	0.017 (3)	0.014 (3)	0.017 (3)
O1	0.0108 (9)	0.0086 (9)	0.0086 (8)	0.0001 (7)	0.0024 (7)	0.0012 (7)
O2	0.0137 (10)	0.0127 (9)	0.0146 (10)	0.0055 (8)	0.0035 (8)	0.0044 (8)
O3	0.0115 (9)	0.0094 (9)	0.0126 (9)	0.0020 (7)	0.0067 (7)	0.0010 (7)
O4	0.0086 (9)	0.0135 (9)	0.0092 (9)	0.0025 (7)	−0.0009 (7)	0.0025 (7)
O5	0.0093 (9)	0.0115 (9)	0.0083 (9)	0.0020 (7)	0.0025 (7)	0.0020 (7)
O6	0.0099 (9)	0.0110 (9)	0.0114 (9)	0.0044 (7)	0.0032 (7)	0.0061 (7)
O7	0.0109 (9)	0.0086 (9)	0.0108 (9)	0.0004 (7)	0.0048 (7)	−0.0023 (7)

Mo—O2	1.707 (2)	Al—O3v	1.942 (2)
Mo—O5	1.782 (2)	Al—O3	1.942 (2)
Mo—O1i	1.822 (2)	Li1—O2ii	2.000 (2)
Mo—O7	2.080 (2)	Li1—O2iv	2.000 (2)
Mo—O1ii	2.123 (2)	Li1—O1ii	2.073 (2)
Mo—O6i	2.261 (2)	Li1—O1iv	2.073 (2)
Mo—Moiii	3.0849 (8)	Li1—O7viii	2.328 (2)
As—O6	1.6737 (19)	Li1—O7	2.328 (2)
As—O4iv	1.6903 (19)	Li2—O5	2.159 (7)
As—O3	1.6960 (19)	Li2—O3	2.225 (7)
As—O7	1.7164 (19)	Li2—O6ix	2.272 (8)
Al—O4v	1.870 (2)	Li2—O7x	2.275 (7)
Al—O4	1.870 (2)	Li2—O4	2.435 (7)
Al—O5vi	1.905 (2)	Li2—O3vii	2.533 (8)
Al—O5vii	1.905 (2)	Li2—O2	2.645 (8)
O2—Mo—O5	98.47 (9)	O2ii—Li1—O2iv	180.000 (1)
O2—Mo—O1i	102.62 (9)	O2ii—Li1—O1ii	86.18 (8)
O5—Mo—O1i	104.19 (9)	O2iv—Li1—O1ii	93.82 (8)
O2—Mo—O7	92.53 (9)	O2ii—Li1—O1iv	93.82 (8)
O5—Mo—O7	96.70 (8)	O2iv—Li1—O1iv	86.18 (8)
O1i—Mo—O7	151.88 (8)	O1ii—Li1—O1iv	180.0
O2—Mo—O1ii	96.79 (9)	O2ii—Li1—O7viii	90.24 (8)
O5—Mo—O1ii	163.86 (8)	O2iv—Li1—O7viii	89.76 (8)
O1i—Mo—O1ii	77.39 (9)	O1ii—Li1—O7viii	106.95 (7)
O7—Mo—O1ii	77.39 (7)	O1iv—Li1—O7viii	73.05 (7)
O2—Mo—O6i	167.49 (8)	O2ii—Li1—O7	89.76 (8)
O5—Mo—O6i	83.83 (8)	O2iv—Li1—O7	90.24 (7)
O1i—Mo—O6i	88.62 (8)	O1ii—Li1—O7	73.05 (7)
O7—Mo—O6i	74.97 (8)	O1iv—Li1—O7	106.95 (7)
O1ii—Mo—O6i	80.14 (7)	O7viii—Li1—O7	180.0
O6—As—O4iv	115.31 (9)	O5—Li2—O3	85.6 (3)
O6—As—O3	112.28 (9)	O5—Li2—O6ix	79.0 (2)
O4iv—As—O3	106.27 (9)	O3—Li2—O6ix	158.9 (4)
O6—As—O7	111.28 (10)	O5—Li2—O7x	136.7 (4)
O4iv—As—O7	100.31 (10)	O3—Li2—O7x	112.7 (3)
O3—As—O7	110.70 (9)	O6ix—Li2—O7x	71.1 (2)
O4v—Al—O4	180.00 (15)	O5—Li2—O4	151.9 (4)
O4v—Al—O5vi	88.07 (8)	O3—Li2—O4	68.8 (2)
O4—Al—O5vi	91.93 (8)	O6ix—Li2—O4	128.6 (3)
O4v—Al—O5vii	91.93 (8)	O7x—Li2—O4	67.36 (19)
O4—Al—O5vii	88.07 (8)	O5—Li2—O3vii	69.4 (2)
O5vi—Al—O5vii	180.00 (10)	O3—Li2—O3vii	81.2 (3)
O4v—Al—O3v	87.61 (9)	O6ix—Li2—O3vii	106.3 (3)
O4—Al—O3v	92.39 (9)	O7x—Li2—O3vii	148.8 (4)
O5vi—Al—O3v	88.69 (8)	O4—Li2—O3vii	94.6 (3)
O5vii—Al—O3v	91.31 (8)	O5—Li2—O2	65.9 (2)
O4v—Al—O3	92.39 (9)	O3—Li2—O2	84.0 (2)
O4—Al—O3	87.61 (9)	O6ix—Li2—O2	76.6 (3)
O5vi—Al—O3	91.31 (8)	O7x—Li2—O2	77.0 (2)
O5vii—Al—O3	88.69 (8)	O4—Li2—O2	120.1 (3)
O3v—Al—O3	180.00 (12)	O3vii—Li2—O2	133.7 (3)