K(3)Al(2)As(3)O(12).

Single crystals of K(3)Al(2)As(3)O(12), tripotassium dialuminotriarsenate(V), were obtained unintentionally by the reaction of KAsO(3) with a corundum crucible at 973 K. The asymmetric unit contains three K, two Al, three As and 12 O atoms. The structure of the title compound is isotypic with those of other K(3)M'(2)X(3)O(12) (M' = Al, Ga; X = P, As) structures and is made up of a three-dimensional network of corner-sharing [AlO(4)] and [AsO(4)] tetra-hedra. The three K(+) cations are located in channels running along the [100], [001], [101] and [10[Formula: see text]] directions, exhibiting different coordination numbers of 9, 8 and 6, respectively. All corresponding [KO(x)] polyhedra are considerably distorted.

Related literature

For a recent review on NASICON-type materials, see: Anantharamulu et al. (2011 ▶). For isotypic K3 M′2 X 3O12 structures, see: Beaurain et al. (2008 ▶) and Yakubovich et al. (2008 ▶) for K3Ga2P3O12; Boughzala et al. (1997 ▶) for the solid solution K3Al2(As1.92P1.08)O12; Devi & Vidyasagar (2000 ▶) for K3Al2P3O12. For the isopointal structure of Tl3Al2P3O12, see: Devi & Vidyasagar (2000 ▶). For background to the bond-valence method, see: Brown & Altermatt (1985 ▶).

Experimental

Crystal data

K3Al2As3O12

M = 588

Orthorhombic,

a = 8.7943 (2) Å

b = 17.4400 (2) Å

c = 8.6610 (3) Å

V = 1328.36 (6) Å3

Z = 4

Mo Kα radiation

μ = 8.63 mm−1

T = 100 K

0.10 × 0.06 × 0.01 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2008 ▶) T min = 0.49, T max = 0.92

52293 measured reflections

9623 independent reflections

8606 reflections with I > 3σ(I)

R int = 0.038

Refinement

R[F 2 > 3σ(F 2)] = 0.018

wR(F 2) = 0.039

S = 0.80

9623 reflections

181 parameters

Δρmax = 0.33 e Å−3

Δρmin = −0.31 e Å−3

Absolute structure: Flack (1983 ▶), 3882 Friedel pairs

Flack parameter: 0.008 (3)

Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT-Plus (Bruker, 2008 ▶); data reduction: SAINT-Plus; method used to solve structure: coordinates taken from an isotypic structure; program(s) used to refine structure: JANA2006 (Petříček et al., 2006 ▶); molecular graphics: ATOMS (Dowty, 2006 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812000438/gw2112sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812000438/gw2112Isup2.hkl

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

K3Al2As3O12	F(000) = 1112
Mr = 588	Dx = 2.939 Mg m−3
Orthorhombic, Pna21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2n	Cell parameters from 54411 reflections
a = 8.7943 (2) Å	θ = 3.3–44.8°
b = 17.4400 (2) Å	µ = 8.63 mm−1
c = 8.6610 (3) Å	T = 100 K
V = 1328.36 (6) Å3	Plate, colourless
Z = 4	0.10 × 0.06 × 0.01 mm

Bruker APEXII CCD diffractometer	9623 independent reflections
Radiation source: X-ray tube	8606 reflections with I > 3σ(I)
graphite	Rint = 0.038
ω and φ scans	θmax = 45.1°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Bruker, 2008)	h = −17→17
Tmin = 0.49, Tmax = 0.92	k = −34→34
52293 measured reflections	l = −15→17

Refinement on F2	Primary atom site location: isomorphous structure methods
R[F2 > 2σ(F2)] = 0.018	Weighting scheme based on measured s.u.'s w = 1/(σ2(I) + 0.0004I2)
wR(F2) = 0.039	(Δ/σ)max = 0.003
S = 0.80	Δρmax = 0.33 e Å−3
9623 reflections	Δρmin = −0.31 e Å−3
181 parameters	Absolute structure: Flack (1983), 3882 Friedel pairs
0 restraints	Flack parameter: 0.008 (3)
1 constraint

	x	y	z	Uiso*/Ueq
As1	0.156896 (11)	0.215743 (6)	0.0009	0.004155 (18)
As2	0.293241 (12)	0.313601 (6)	0.511929 (16)	0.004909 (19)
As3	0.236068 (12)	0.502941 (6)	0.085202 (18)	0.005355 (19)
K1	0.01017 (3)	0.402188 (14)	0.84037 (3)	0.00837 (4)
K2	0.95033 (3)	0.354962 (14)	0.30906 (3)	0.00818 (4)
K3	0.68161 (3)	0.488891 (15)	0.11580 (3)	0.01179 (5)
Al1	0.34851 (4)	0.34012 (2)	0.14668 (4)	0.00492 (7)
Al2	0.13204 (4)	0.16767 (2)	0.65562 (4)	0.00520 (7)
O1	0.29089 (10)	0.15184 (5)	0.03110 (9)	0.00824 (17)
O2	0.02014 (10)	0.20900 (5)	0.13689 (9)	0.00746 (16)
O3	0.21755 (9)	0.30785 (4)	0.00781 (10)	0.00643 (14)
O4	0.06929 (10)	0.20939 (5)	0.82779 (9)	0.00730 (16)
O5	0.17013 (13)	0.37287 (6)	0.58794 (12)	0.0139 (2)
O6	0.47459 (12)	0.34183 (7)	0.53518 (11)	0.0168 (2)
O7	0.27956 (11)	0.22138 (5)	0.57055 (11)	0.01044 (18)
O8	0.26654 (10)	0.30933 (6)	0.31927 (9)	0.00936 (18)
O9	0.07409 (11)	0.46866 (6)	0.15273 (11)	0.01076 (18)
O10	0.29028 (11)	0.57855 (5)	0.19818 (10)	0.00894 (17)
O11	0.23407 (11)	0.52699 (6)	0.90078 (10)	0.01074 (19)
O12	0.37999 (10)	0.43772 (5)	0.12022 (10)	0.00883 (16)

	U11	U22	U33	U12	U13	U23
As1	0.00437 (3)	0.00356 (3)	0.00453 (3)	0.00007 (3)	−0.00035 (3)	−0.00027 (3)
As2	0.00554 (3)	0.00472 (4)	0.00447 (3)	−0.00042 (3)	0.00028 (3)	0.00036 (3)
As3	0.00642 (4)	0.00336 (3)	0.00628 (3)	−0.00018 (3)	−0.00018 (3)	−0.00019 (3)
K1	0.00698 (7)	0.01015 (8)	0.00797 (6)	−0.00039 (6)	0.00040 (5)	0.00102 (6)
K2	0.00765 (8)	0.00734 (8)	0.00955 (7)	0.00014 (6)	0.00017 (6)	0.00078 (6)
K3	0.01516 (10)	0.00792 (9)	0.01230 (8)	−0.00147 (7)	−0.00295 (7)	−0.00020 (6)
Al1	0.00487 (12)	0.00439 (12)	0.00550 (10)	−0.00023 (9)	−0.00019 (9)	−0.00024 (9)
Al2	0.00592 (12)	0.00438 (12)	0.00532 (10)	0.00071 (10)	−0.00068 (9)	−0.00031 (9)
O1	0.0078 (3)	0.0069 (3)	0.0101 (3)	0.0029 (2)	−0.0011 (2)	−0.0004 (2)
O2	0.0062 (3)	0.0094 (3)	0.0067 (2)	−0.0020 (2)	0.0017 (2)	−0.0006 (2)
O3	0.0075 (2)	0.0046 (2)	0.0072 (2)	−0.0014 (2)	−0.0019 (2)	0.0005 (2)
O4	0.0078 (3)	0.0089 (3)	0.0052 (2)	0.0016 (2)	−0.0019 (2)	−0.0019 (2)
O5	0.0193 (4)	0.0088 (3)	0.0138 (3)	0.0037 (3)	0.0083 (3)	−0.0016 (3)
O6	0.0101 (3)	0.0274 (5)	0.0130 (3)	−0.0102 (3)	−0.0069 (3)	0.0108 (3)
O7	0.0121 (3)	0.0056 (3)	0.0136 (3)	0.0006 (2)	0.0041 (2)	0.0026 (2)
O8	0.0094 (3)	0.0144 (4)	0.0043 (2)	−0.0031 (3)	−0.0001 (2)	0.0002 (2)
O9	0.0084 (3)	0.0083 (3)	0.0155 (3)	−0.0023 (2)	0.0031 (2)	0.0001 (3)
O10	0.0131 (3)	0.0043 (3)	0.0094 (3)	−0.0018 (2)	0.0003 (2)	−0.0010 (2)
O11	0.0138 (3)	0.0121 (4)	0.0063 (3)	0.0010 (3)	−0.0004 (2)	0.0016 (2)
O12	0.0085 (3)	0.0044 (3)	0.0136 (3)	0.0006 (2)	−0.0019 (2)	0.0002 (2)

K1—O1i	2.7084 (9)	Al1—O8	1.7443 (9)
K1—O3ii	2.8524 (8)	Al1—O12	1.7396 (9)
K1—O5	2.6496 (11)	Al2—O4	1.7485 (9)
K1—O9ii	2.9964 (10)	Al2—O6vii	1.7415 (11)
K1—O9iii	2.8747 (10)	Al2—O7	1.7616 (10)
K1—O10iii	2.9344 (10)	Al2—O10viii	1.7373 (10)
K1—O11	2.9814 (10)	As1—O1	1.6429 (9)
K2—O1iv	2.7885 (9)	As1—O2	1.6875 (8)
K2—O2v	3.0134 (9)	As1—O3	1.6936 (8)
K2—O7iv	3.0260 (10)	As1—O4ix	1.6893 (8)
K2—O8v	2.8939 (10)	As2—O5	1.6352 (10)
K2—O9v	2.6362 (10)	As2—O6	1.6812 (11)
K2—O11vi	2.7384 (10)	As2—O7	1.6909 (9)
K3—O1iv	2.7360 (9)	As2—O8	1.6867 (8)
K3—O5vi	2.7515 (10)	As3—O9	1.6519 (9)
K3—O11vi	2.5921 (9)	As3—O10	1.7098 (9)
K3—O12	2.7989 (10)	As3—O11ix	1.6515 (9)
Al1—O2iv	1.7376 (9)	As3—O12	1.7285 (9)
Al1—O3	1.7578 (9)
O1i—K1—O3ii	86.82 (3)	O1iv—K3—O5vi	126.59 (3)
O1i—K1—O5	144.51 (3)	O1iv—K3—O11vi	93.38 (3)
O1i—K1—O9ii	73.59 (3)	O1iv—K3—O12	92.90 (3)
O1i—K1—O9iii	115.72 (3)	O5vi—K3—O11vi	92.38 (3)
O1i—K1—O10iii	69.80 (3)	O5vi—K3—O12	136.86 (3)
O1i—K1—O11	128.11 (3)	O11vi—K3—O12	102.95 (3)
O3ii—K1—O5	88.21 (3)	O2iv—Al1—O3	112.21 (4)
O3ii—K1—O9ii	69.16 (3)	O2iv—Al1—O8	104.42 (4)
O3ii—K1—O9iii	154.71 (3)	O2iv—Al1—O12	109.74 (5)
O3ii—K1—O10iii	148.77 (2)	O3—Al1—O8	102.53 (4)
O3ii—K1—O11	84.81 (2)	O3—Al1—O12	109.11 (4)
O5—K1—O9ii	136.06 (3)	O8—Al1—O12	118.68 (5)
O5—K1—O9iii	79.72 (3)	O4—Al2—O6vii	107.43 (5)
O5—K1—O10iii	98.85 (3)	O4—Al2—O7	111.59 (4)
O5—K1—O11	86.28 (3)	O4—Al2—O10viii	108.39 (4)
O9ii—K1—O9iii	104.81 (3)	O6vii—Al2—O7	112.68 (5)
O9ii—K1—O10iii	120.24 (3)	O6vii—Al2—O10viii	110.77 (6)
O9ii—K1—O11	55.61 (2)	O7—Al2—O10viii	105.95 (5)
O9iii—K1—O10iii	56.01 (3)	O1—As1—O2	110.66 (4)
O9iii—K1—O11	72.39 (3)	O1—As1—O3	114.32 (4)
O10iii—K1—O11	125.79 (3)	O1—As1—O4ix	115.08 (4)
O1iv—K2—O2v	68.86 (2)	O2—As1—O3	105.42 (4)
O1iv—K2—O7iv	112.20 (3)	O2—As1—O4ix	106.85 (4)
O1iv—K2—O8v	119.86 (2)	O3—As1—O4ix	103.72 (4)
O1iv—K2—O9v	78.24 (3)	O5—As2—O6	113.25 (6)
O1iv—K2—O11vi	89.12 (3)	O5—As2—O7	115.67 (5)
O2v—K2—O7iv	95.73 (2)	O5—As2—O8	109.52 (5)
O2v—K2—O8v	65.61 (2)	O6—As2—O7	108.07 (5)
O2v—K2—O9v	107.28 (3)	O6—As2—O8	105.28 (4)
O2v—K2—O11vi	154.06 (3)	O7—As2—O8	104.19 (5)
O7iv—K2—O8v	109.45 (3)	O9—As3—O10	108.48 (5)
O7iv—K2—O9v	156.96 (3)	O9—As3—O11ix	115.16 (5)
O7iv—K2—O11vi	79.62 (3)	O9—As3—O12	109.34 (4)
O8v—K2—O9v	79.97 (3)	O10—As3—O11ix	111.13 (5)
O8v—K2—O11vi	140.08 (3)	O10—As3—O12	101.71 (4)
O9v—K2—O11vi	80.10 (3)	O11ix—As3—O12	110.16 (5)