K(0.12)Na(0.54)Ag(0.34)Nb(4)O(9)AsO(4).

Potassium sodium silver tetra-niobium nona-oxide arsenate, K(0.12)Na(0.54)Ag(0.34)Nb(4)AsO(13), synthesized by solid-state reaction at 1123 K, adopts a three-dimensional framework delimiting tunnels running along [001] in which occupationally disordered sodium, silver, and potassium ions are located. Of the 11 atoms in the asymmetric unit (two Nb, one As, one Ag, one K, one Na and fiveO), nine are located on special positions: one Nb and the K, Ag, Na and two O atoms are situated on mirror planes, the other Nb is on a twofold rotation axis, and the As atom and one O atom are on sites of m2m symmetry.

Related literature

For physical properties, see: Piffard et al. (1985 ▶); Lachgar et al. (1986 ▶); Harrison et al. (1994 ▶); Ledain et al. (1997 ▶); Hizaoui et al. (1999 ▶); Zid et al. (2003 ▶); Hajji et al. (2004 ▶). For synthetic details, see: Zid et al. (1988 ▶, 1989 ▶); Haddad et al. (1988 ▶); Ben Amor & Zid (2006 ▶). For structural relationships, see: Ben Amor et al. (2008 ▶); Bestaoui et al. (1998 ▶); Haddad et al. (1988 ▶). For bond-valence sums, see: Brown & Altermatt (1985 ▶).

Experimental

Crystal data

K0.12Na0.54Ag0.34Nb4AsO13

M = 708.82

Orthorhombic,

a = 10.412 (2) Å

b = 10.452 (2) Å

c = 10.009 (4) Å

V = 1089.2 (5) Å3

Z = 4

Mo Kα radiation

μ = 7.86 mm−1

T = 298 K

0.22 × 0.16 × 0.10 mm

Data collection

Enraf–Nonius CAD-4 diffractometer

Absorption correction: ψ scan (North et al., 1968 ▶) T min = 0.239, T max = 0.452

1550 measured reflections

667 independent reflections

642 reflections with I > 2σ(I)

R int = 0.014

2 standard reflections every 120 min intensity decay: 1.1%

Refinement

R[F 2 > 2σ(F 2)] = 0.013

wR(F 2) = 0.035

S = 1.14

667 reflections

72 parameters

1 restraint

Δρmax = 0.42 e Å−3

Δρmin = −0.57 e Å−3

Data collection: CAD-4 EXPRESS (Duisenberg, 1992 ▶; Macíček & Yordanov, 1992 ▶); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 1998 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811000055/mg2111sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811000055/mg2111Isup2.hkl

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

K0.12Na0.54Ag0.34Nb4AsO13	F(000) = 1302
Mr = 708.82	Dx = 4.322 Mg m−3
Orthorhombic, Cmcm	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2c 2	Cell parameters from 25 reflections
a = 10.412 (2) Å	θ = 10–15°
b = 10.452 (2) Å	µ = 7.86 mm−1
c = 10.009 (4) Å	T = 298 K
V = 1089.2 (5) Å3	Prism, colourless
Z = 4	0.22 × 0.16 × 0.10 mm

Enraf–Nonius CAD-4 diffractometer	642 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.014
graphite	θmax = 26.9°, θmin = 2.8°
ω/2θ scans	h = −13→13
Absorption correction: ψ scan (North et al., 1968)	k = −1→13
Tmin = 0.239, Tmax = 0.452	l = −1→12
1550 measured reflections	2 standard reflections every 120 min
667 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) + (0.0164P)2 + 2.8925P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.035	(Δ/σ)max = 0.001
S = 1.14	Δρmax = 0.42 e Å−3
667 reflections	Δρmin = −0.57 e Å−3
72 parameters	Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
1 restraint	Extinction coefficient: 0.00226 (10)

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	Occ. (<1)
Nb1	0.17145 (3)	0.23034 (3)	0.2500	0.00637 (11)
Nb2	0.17813 (3)	0.5000	0.0000	0.00638 (11)
As1	0.0000	0.65963 (5)	0.2500	0.00553 (13)
Ag1	0.0000	−0.0486 (8)	0.2165 (6)	0.044 (13)	0.173 (4)
K1	0.0000	−0.057 (3)	0.067 (9)	0.047 (13)	0.059 (13)
Na1	0.0000	−0.0472 (18)	0.160 (3)	0.012 (12)	0.268 (13)
O1	0.15106 (17)	0.34333 (17)	0.11032 (18)	0.0131 (4)
O2	0.0000	0.1632 (3)	0.2500	0.0090 (7)
O3	0.0000	0.5664 (2)	0.1105 (2)	0.0095 (5)
O4	0.21550 (16)	0.07889 (17)	0.11618 (17)	0.0127 (4)
O5	0.8731 (2)	0.7580 (2)	0.2500	0.0110 (5)

	U11	U22	U33	U12	U13	U23
Nb1	0.00591 (16)	0.00475 (17)	0.00844 (16)	0.00075 (10)	0.000	0.000
Nb2	0.00670 (16)	0.00656 (17)	0.00588 (16)	0.000	0.000	−0.00138 (10)
As1	0.0053 (2)	0.0051 (2)	0.0062 (2)	0.000	0.000	0.000
Ag1	0.054 (2)	0.0075 (11)	0.07 (4)	0.000	0.000	0.001 (3)
K1	0.034 (11)	0.048 (14)	0.06 (4)	0.000	0.000	0.007 (18)
Na1	0.012 (4)	0.002 (4)	0.02 (4)	0.000	0.000	0.001 (7)
O1	0.0133 (8)	0.0111 (8)	0.0149 (9)	0.0001 (7)	0.0002 (7)	0.0043 (7)
O2	0.0056 (15)	0.0086 (16)	0.0128 (17)	0.000	0.000	0.000
O3	0.0092 (10)	0.0117 (11)	0.0077 (11)	0.000	0.000	−0.0043 (10)
O4	0.0143 (8)	0.0116 (8)	0.0121 (8)	0.0022 (7)	0.0021 (7)	−0.0026 (7)
O5	0.0068 (11)	0.0090 (11)	0.0173 (13)	0.0010 (9)	0.000	0.000

Nb1—O1i	1.8424 (18)	As1—O3i	1.703 (2)
Nb1—O1	1.8424 (18)	Ag1—O2	2.239 (9)
Nb1—O2	1.9180 (14)	Ag1—O5ix	2.439 (7)
Nb1—O5ii	2.119 (3)	Ag1—O5x	2.439 (7)
Nb1—O4	2.1236 (18)	K1—O4	2.70 (3)
Nb1—O4i	2.1236 (18)	K1—O4xi	2.70 (3)
Nb2—O4iii	1.8052 (17)	K1—O4xii	2.91 (6)
Nb2—O4iv	1.8052 (17)	K1—O4xiii	2.91 (6)
Nb2—O1	1.9950 (17)	K1—O2	2.94 (8)
Nb2—O1v	1.9950 (17)	K1—O5ix	2.97 (5)
Nb2—O3vi	2.2681 (14)	Na1—O2	2.37 (2)
Nb2—O3	2.2681 (14)	Na1—O5ix	2.588 (18)
As1—O5vii	1.674 (2)	Na1—O5x	2.588 (18)
As1—O5viii	1.674 (2)	Na1—O4	2.640 (11)
As1—O3	1.703 (2)	Na1—O4xi	2.640 (11)
O1i—Nb1—O1	98.72 (12)	O4iii—Nb2—O1v	93.92 (8)
O1i—Nb1—O2	97.31 (8)	O4iv—Nb2—O1v	96.03 (8)
O1—Nb1—O2	97.31 (8)	O1—Nb2—O1v	163.76 (10)
O1i—Nb1—O5ii	91.53 (7)	O4iii—Nb2—O3vi	162.84 (8)
O1—Nb1—O5ii	91.53 (7)	O4iv—Nb2—O3vi	92.74 (7)
O2—Nb1—O5ii	166.39 (12)	O1—Nb2—O3vi	84.44 (8)
O1i—Nb1—O4	168.89 (8)	O1v—Nb2—O3vi	82.29 (8)
O1—Nb1—O4	91.38 (8)	O4iii—Nb2—O3	92.74 (7)
O2—Nb1—O4	85.90 (9)	O4iv—Nb2—O3	162.84 (8)
O5ii—Nb1—O4	83.55 (7)	O1—Nb2—O3	82.29 (8)
O1i—Nb1—O4i	91.38 (8)	O1v—Nb2—O3	84.44 (8)
O1—Nb1—O4i	168.89 (8)	O3vi—Nb2—O3	70.28 (10)
O2—Nb1—O4i	85.90 (9)	O5vii—As1—O5viii	104.25 (17)
O5ii—Nb1—O4i	83.55 (7)	O5vii—As1—O3	110.57 (6)
O4—Nb1—O4i	78.20 (10)	O5viii—As1—O3	110.57 (6)
O4iii—Nb2—O4iv	104.31 (11)	O5vii—As1—O3i	110.57 (6)
O4iii—Nb2—O1	96.03 (8)	O5viii—As1—O3i	110.57 (6)
O4iv—Nb2—O1	93.92 (8)	O3—As1—O3i	110.19 (17)