AgNa(2)Mo(3)O(9)AsO(4).

The title compound, silver disodium trimolybdenum(VI) nonaoxide arsenate, AgNa(2)Mo(3)O(9)AsO(4), was prepared by a solid-state reaction at 808 K. The structure consists of an infinite (Mo(3)AsO(13))(n) ribbon, parallel to the c axis, composed of AsO(4) tetra-hedra and MoO(6) octa-hedra sharing edges and corners. The Na and Ag ions partially occupy several independent close positions, with various occupancies, in the inter-ribbon space delimited by the one-dimensional framework. The composition was refined to Ag(1.06(1))Na(1.94(1))Mo(3)O(9)AsO(4).

Related literature

For framework structures containing MO6 and XO4 (M = transition metal, X = P, As) building blocks, see: Benhamada et al. (1992 ▶); Harrison et al. (1994 ▶); Guyomard et al. (1999 ▶); Ben Smail et al. (1999 ▶); Ben Amor & Zid (2006 ▶). For a similar one-dimensional structure, see: Hamza et al. (2010 ▶). For details of the synthesis, see: Hajji et al. (2004 ▶, 2005 ▶); Ben Hlila et al. (2009 ▶); Zid & Jouini (1996 ▶); Zid et al. (1998 ▶). For the bond-valence model, see: Brown & Altermatt (1985 ▶). For physical properties of related compounds, see: Daidouh et al. (1997 ▶); Ouerfelli et al. (2004 ▶, 2007 ▶); Piffard et al. (1985 ▶); Oyetola et al. (1988 ▶); Goubitz et al. (2001 ▶); Ledain et al. (1997 ▶); Harrison et al. (1998 ▶); Hajji & Zid (2006 ▶); Ruiz et al. (2002 ▶).

Experimental

Crystal data

AgNa2Mo3O9AsO4

M = 729.68

Triclinic,

a = 8.1767 (8) Å

b = 9.7687 (9) Å

c = 8.0451 (8) Å

α = 99.49 (2)°

β = 106.07 (2)°

γ = 113.29 (2)°

V = 539.14 (19) Å3

Z = 2

Mo Kα radiation

μ = 8.50 mm−1

T = 298 K

0.36 × 0.24 × 0.16 mm

Data collection

Enraf–Nonius CAD-4 diffractometer

Absorption correction: ψ scan (North et al., 1968 ▶) T min = 0.098, T max = 0.247

2853 measured reflections

2355 independent reflections

2047 reflections with I > 2σ(I)

R int = 0.023

2 standard reflections every 120 min intensity decay: 1.1%

Refinement

R[F 2 > 2σ(F 2)] = 0.024

wR(F 2) = 0.063

S = 1.09

2355 reflections

188 parameters

3 restraints

Δρmax = 0.95 e Å−3

Δρmin = −0.76 e Å−3

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994 ▶); 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 datablock(s) I, global. DOI: 10.1107/S1600536811041961/br2178sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811041961/br2178Isup2.hkl

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

AgNa2Mo3O9AsO4	Z = 2
Mr = 729.68	F(000) = 668
Triclinic, P1	Dx = 4.495 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.1767 (8) Å	Cell parameters from 25 reflections
b = 9.7687 (9) Å	θ = 10–15°
c = 8.0451 (8) Å	µ = 8.50 mm−1
α = 99.49 (2)°	T = 298 K
β = 106.07 (2)°	Prism, yellow
γ = 113.29 (2)°	0.36 × 0.24 × 0.16 mm
V = 539.14 (19) Å3

Enraf–Nonius CAD-4 diffractometer	2047 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.023
graphite	θmax = 27.0°, θmin = 2.4°
ω/2θ scans	h = −10→1
Absorption correction: ψ scan (North et al., 1968)	k = −11→12
Tmin = 0.098, Tmax = 0.247	l = −10→10
2853 measured reflections	2 standard reflections every 120 min
2355 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)] = 0.024	w = 1/[σ2(Fo2) + (0.0204P)2 + 1.4359P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.063	(Δ/σ)max < 0.001
S = 1.09	Δρmax = 0.95 e Å−3
2355 reflections	Δρmin = −0.76 e Å−3
188 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
3 restraints	Extinction coefficient: 0.00141 (17)

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)
Mo1	0.71234 (5)	0.14251 (5)	0.48605 (5)	0.00818 (11)
Mo2	0.58834 (6)	0.75426 (5)	0.30104 (5)	0.00827 (11)
Mo3	0.43503 (6)	0.22968 (5)	0.11436 (5)	0.00868 (11)
As1	0.22233 (7)	0.82953 (5)	0.04824 (6)	0.00761 (12)
Ag1	0.14302 (10)	0.43681 (8)	−0.09577 (9)	0.0213 (3)	0.524 (3)
Na1	0.14302 (10)	0.43681 (8)	−0.09577 (9)	0.0213 (3)	0.476 (4)
Ag2	0.84335 (15)	0.57626 (11)	0.60990 (13)	0.0320 (4)	0.391 (3)
Na2	0.84335 (15)	0.57626 (11)	0.60990 (13)	0.0320 (4)	0.609 (4)
Ag3	0.97290 (18)	−0.02400 (16)	0.74218 (18)	0.0194 (5)	0.147 (3)
Na3	0.97290 (18)	−0.02400 (16)	0.74218 (18)	0.0194 (5)	0.853 (4)
O1	0.2244 (5)	−0.0212 (4)	0.9676 (5)	0.0135 (7)
O2	0.8795 (5)	0.3378 (4)	0.5567 (5)	0.0173 (8)
O3	0.0460 (5)	0.6539 (4)	0.9111 (5)	0.0168 (8)
O4	0.6979 (5)	0.7508 (4)	0.1170 (4)	0.0120 (7)
O5	0.3912 (5)	0.5759 (4)	0.2330 (5)	0.0202 (8)
O6	0.4357 (5)	0.8235 (4)	0.0849 (4)	0.0114 (7)
O7	0.5640 (5)	0.1338 (4)	0.2611 (5)	0.0139 (7)
O8	0.5097 (5)	0.8757 (4)	0.4424 (5)	0.0130 (7)
O9	0.6297 (5)	0.4137 (4)	0.2142 (5)	0.0177 (8)
O10	0.2813 (5)	0.2401 (5)	0.2173 (5)	0.0196 (8)
O11	0.8223 (5)	0.0337 (4)	0.4165 (5)	0.0152 (7)
O12	0.8183 (5)	0.1370 (4)	0.7539 (4)	0.0133 (7)
O13	0.7650 (5)	0.7405 (4)	0.4636 (5)	0.0146 (7)

	U11	U22	U33	U12	U13	U23
Mo1	0.0074 (2)	0.0088 (2)	0.0082 (2)	0.00380 (16)	0.00317 (15)	0.00218 (15)
Mo2	0.0096 (2)	0.0090 (2)	0.00853 (19)	0.00560 (16)	0.00429 (15)	0.00358 (15)
Mo3	0.0106 (2)	0.0086 (2)	0.0085 (2)	0.00513 (16)	0.00467 (16)	0.00320 (15)
As1	0.0071 (2)	0.0071 (2)	0.0090 (2)	0.00346 (18)	0.00316 (18)	0.00267 (18)
Ag1	0.0186 (4)	0.0182 (4)	0.0256 (4)	0.0050 (3)	0.0110 (3)	0.0074 (3)
Na1	0.0186 (4)	0.0182 (4)	0.0256 (4)	0.0050 (3)	0.0110 (3)	0.0074 (3)
Ag2	0.0444 (7)	0.0255 (5)	0.0269 (5)	0.0217 (5)	0.0045 (4)	0.0116 (4)
Na2	0.0444 (7)	0.0255 (5)	0.0269 (5)	0.0217 (5)	0.0045 (4)	0.0116 (4)
Ag3	0.0142 (7)	0.0231 (8)	0.0215 (8)	0.0102 (6)	0.0056 (5)	0.0060 (6)
Na3	0.0142 (7)	0.0231 (8)	0.0215 (8)	0.0102 (6)	0.0056 (5)	0.0060 (6)
O1	0.0152 (17)	0.0105 (17)	0.0143 (17)	0.0060 (14)	0.0036 (14)	0.0065 (14)
O2	0.0177 (18)	0.0111 (17)	0.0166 (18)	0.0035 (15)	0.0031 (15)	0.0026 (14)
O3	0.0119 (17)	0.0117 (17)	0.0181 (18)	0.0012 (14)	0.0014 (15)	0.0015 (14)
O4	0.0155 (17)	0.0157 (17)	0.0116 (16)	0.0120 (15)	0.0062 (14)	0.0066 (14)
O5	0.0182 (19)	0.0136 (19)	0.027 (2)	0.0057 (16)	0.0079 (16)	0.0069 (16)
O6	0.0118 (16)	0.0171 (17)	0.0100 (16)	0.0093 (14)	0.0054 (14)	0.0066 (14)
O7	0.0164 (18)	0.0140 (17)	0.0117 (16)	0.0088 (15)	0.0035 (14)	0.0032 (14)
O8	0.0119 (17)	0.0153 (17)	0.0123 (16)	0.0067 (14)	0.0054 (14)	0.0037 (14)
O9	0.0188 (18)	0.0132 (18)	0.0201 (19)	0.0065 (15)	0.0087 (16)	0.0028 (15)
O10	0.024 (2)	0.025 (2)	0.0181 (19)	0.0152 (17)	0.0126 (16)	0.0087 (16)
O11	0.0165 (18)	0.0140 (18)	0.0186 (18)	0.0079 (15)	0.0102 (15)	0.0053 (15)
O12	0.0140 (17)	0.0224 (19)	0.0102 (16)	0.0129 (15)	0.0060 (14)	0.0071 (14)
O13	0.0159 (18)	0.0184 (19)	0.0119 (17)	0.0113 (16)	0.0035 (14)	0.0054 (14)

Mo1—O2	1.727 (4)	Mo3—O6iv	2.249 (3)
Mo1—O11	1.758 (3)	As1—O3v	1.667 (4)
Mo1—O7	1.845 (3)	As1—O1vi	1.687 (3)
Mo1—O8i	2.004 (3)	As1—O6	1.713 (3)
Mo1—O12	2.107 (3)	As1—O12i	1.720 (3)
Mo1—O8ii	2.371 (4)	Ag1—O9iv	2.405 (4)
Mo2—O5	1.706 (4)	Ag1—O3vii	2.450 (4)
Mo2—O13	1.727 (3)	Ag1—O3v	2.539 (4)
Mo2—O8	1.917 (3)	Ag1—O5	2.574 (4)
Mo2—O4	1.933 (3)	Ag2—O3viii	2.318 (4)
Mo2—O6	2.212 (3)	Ag2—O13	2.321 (3)
Mo2—O11iii	2.455 (4)	Ag2—O2	2.446 (4)
Mo3—O10	1.710 (4)	Ag3—O1viii	2.322 (4)
Mo3—O9	1.722 (4)	Ag3—O12	2.381 (4)
Mo3—O7	1.959 (3)	Ag3—O11ix	2.390 (4)
Mo3—O4iv	1.961 (3)	Ag3—O10x	2.453 (4)
Mo3—O1v	2.225 (4)	Ag3—O13ii	2.511 (4)
O2—Mo1—O11	106.77 (17)	O13—Mo2—O11iii	82.93 (15)
O2—Mo1—O7	97.84 (16)	O8—Mo2—O11iii	68.41 (13)
O11—Mo1—O7	99.39 (16)	O4—Mo2—O11iii	83.59 (13)
O2—Mo1—O8i	108.96 (16)	O6—Mo2—O11iii	83.66 (13)
O11—Mo1—O8i	142.78 (15)	O10—Mo3—O9	103.12 (18)
O7—Mo1—O8i	85.84 (15)	O10—Mo3—O7	101.59 (16)
O2—Mo1—O12	89.08 (16)	O9—Mo3—O7	93.33 (16)
O11—Mo1—O12	90.26 (15)	O10—Mo3—O4iv	97.04 (16)
O7—Mo1—O12	165.90 (14)	O9—Mo3—O4iv	100.96 (16)
O8i—Mo1—O12	80.29 (13)	O7—Mo3—O4iv	153.26 (14)
O2—Mo1—O8ii	169.84 (14)	O10—Mo3—O1v	88.09 (16)
O11—Mo1—O8ii	72.75 (14)	O9—Mo3—O1v	168.35 (15)
O7—Mo1—O8ii	92.22 (14)	O7—Mo3—O1v	81.16 (13)
O8i—Mo1—O8ii	70.24 (15)	O4iv—Mo3—O1v	80.47 (14)
O12—Mo1—O8ii	80.79 (13)	O10—Mo3—O6iv	164.85 (16)
O5—Mo2—O13	104.45 (18)	O9—Mo3—O6iv	89.22 (15)
O5—Mo2—O8	98.74 (17)	O7—Mo3—O6iv	86.19 (13)
O13—Mo2—O8	103.37 (15)	O4iv—Mo3—O6iv	71.67 (12)
O5—Mo2—O4	106.41 (17)	O1v—Mo3—O6iv	80.22 (13)
O13—Mo2—O4	95.64 (15)	O3v—As1—O1vi	113.92 (17)
O8—Mo2—O4	143.46 (14)	O3v—As1—O6	107.68 (17)
O5—Mo2—O6	90.71 (16)	O1vi—As1—O6	110.61 (17)
O13—Mo2—O6	163.30 (15)	O3v—As1—O12i	106.89 (18)
O8—Mo2—O6	80.74 (13)	O1vi—As1—O12i	105.76 (17)
O4—Mo2—O6	72.99 (12)	O6—As1—O12i	111.99 (15)
O5—Mo2—O11iii	166.61 (15)