Disodium tris-(dioxidomolybdenum) bis-(diarsenate).

The asymmetric unit of the title compound, Na(2)(MoO(2))(3)(As(2)O(7))(2), is composed of two cyclic MoAs(2)O(11) units and an MoO(6) corner-sharing octa-hedron. The anionic framework can be decomposed into two types of layers, viz. MoO(2)As(2)O(7) and Mo(2)As(2)O(14), which use mixed Mo-O-As and As-O-Mo bridges to achieve a new three-dimensional structure with two types of large channels in which the Na(+) cations are located. Two O atoms are disordered and are located in two positions close to their initial positions with occupancy ratios of 0.612 (17):0.388 (17) and 0.703 (12):0.298 (12).

Related literature

For background to the search for new materials with open structures, see: Kierkegaard & Westerlund (1964 ▶); Lii et al. (1987 ▶); Guesdon et al. (1994 ▶); Masquelier et al. (1995 ▶). In these materials, the association of XO4 (X = P, As) tetra­hedra and MO6 (M = transition metal) octa­hedra forms covalent hybrid structures that delimit tunnels, see: Linnros (1970 ▶); Hammond & Barbier (1996 ▶). For details of the preparation, see: Zid & Jouini (1996a ▶,b ▶); Zid et al. (1997 ▶, 1998 ▶); Hajji et al. (2004 ▶); Hajji & Zid (2006 ▶); Ben Hlila et al. (2009 ▶). For related structures, see: Averbuch-Pouchot (1988 ▶, 1989 ▶); Zid et al. (2003 ▶); Lii & Wang (1989 ▶); Benhamada et al. (1992 ▶). For the properties of related compounds, see: Marzouki et al. (2010 ▶); Ouerfelli et al. (2007 ▶). For background to the bond-valence method, see: Brown & Altermatt (1985 ▶).

Experimental

Crystal data

Na2(MoO2)3(As2O7)2

M = 953.48

Monoclinic,

a = 14.571 (3) Å

b = 12.580 (2) Å

c = 9.258 (2) Å

β = 94.51 (2)°

V = 1691.9 (6) Å3

Z = 4

Mo Kα radiation

μ = 10.11 mm−1

T = 298 K

0.26 × 0.18 × 0.14 mm

Data collection

Enraf–Nonius CAD-4 diffractometer

Absorption correction: ψ scan (North et al., 1968 ▶) T min = 0.133, T max = 0.246

4271 measured reflections

3676 independent reflections

3128 reflections with I > 2σ(I)

R int = 0.022

2 standard reflections every 120 min intensity decay: 1.1%

Refinement

R[F 2 > 2σ(F 2)] = 0.025

wR(F 2) = 0.060

S = 1.06

3676 reflections

273 parameters

2 restraints

Δρmax = 0.98 e Å−3

Δρmin = −0.75 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 datablock(s) I, global. DOI: 10.1107/S1600536812010069/fj2524sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812010069/fj2524Isup2.hkl

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

Na2(MoO2)3(As2O7)2	F(000) = 1760
Mr = 953.48	Dx = 3.743 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 25 reflections
a = 14.571 (3) Å	θ = 10–15°
b = 12.580 (2) Å	µ = 10.11 mm−1
c = 9.258 (2) Å	T = 298 K
β = 94.51 (2)°	Prism, yellow
V = 1691.9 (6) Å3	0.26 × 0.18 × 0.14 mm
Z = 4

Enraf–Nonius CAD-4 diffractometer	3128 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.022
Graphite monochromator	θmax = 27.0°, θmin = 2.1°
ω/2θ scans	h = −18→18
Absorption correction: ψ scan (North et al., 1968)	k = −1→16
Tmin = 0.133, Tmax = 0.246	l = −11→1
4271 measured reflections	2 standard reflections every 120 min
3676 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)] = 0.025	w = 1/[σ2(Fo2) + (0.0188P)2 + 7.737P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.060	(Δ/σ)max = 0.001
S = 1.06	Δρmax = 0.98 e Å−3
3676 reflections	Δρmin = −0.75 e Å−3
273 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
2 restraints	Extinction coefficient: 0.00106 (6)

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	0.31869 (3)	0.06243 (4)	0.05295 (4)	0.01284 (10)
Mo2	0.02062 (3)	0.37400 (3)	0.26296 (5)	0.01470 (11)
Mo3	0.70516 (3)	0.12821 (3)	0.42003 (4)	0.00864 (10)
As1	0.53859 (3)	0.00042 (4)	0.20483 (5)	0.00852 (11)
As2	0.60470 (3)	0.33825 (4)	0.24714 (5)	0.00885 (11)
As3	0.00777 (3)	0.62745 (4)	0.12380 (6)	0.01163 (11)
As4	0.81642 (3)	0.53068 (4)	0.18604 (5)	0.00924 (11)
Na1	0.4171 (2)	0.1428 (2)	0.4537 (3)	0.0381 (7)
Na2	0.13444 (18)	0.8679 (2)	0.9496 (3)	0.0343 (6)
O1	0.6093 (2)	0.0020 (3)	0.3549 (4)	0.0129 (7)
O2	0.5933 (2)	0.0231 (3)	0.0556 (4)	0.0146 (7)
O3	0.7475 (2)	0.6100 (3)	0.2769 (4)	0.0150 (7)
O4	0.1230 (3)	0.3287 (3)	0.2208 (5)	0.0291 (10)
O5	0.5893 (2)	0.3594 (3)	0.0702 (4)	0.0163 (7)
O6	0.7499 (3)	0.4947 (3)	0.0395 (4)	0.0189 (8)
O7	0.3449 (3)	0.1862 (3)	0.9950 (4)	0.0276 (9)
O8	0.7566 (3)	0.2271 (3)	0.5219 (4)	0.0225 (8)
O9	0.6874 (2)	0.4098 (3)	0.3346 (4)	0.0136 (7)
O10	0.8787 (2)	0.4405 (3)	0.2789 (4)	0.0161 (7)
O11	0.4431 (2)	0.0715 (3)	0.2150 (4)	0.0125 (7)
O12	0.0325 (3)	0.3820 (4)	0.4454 (5)	0.0425 (12)
O13	0.2237 (3)	0.0292 (4)	0.9471 (4)	0.0259 (9)
O14	0.8884 (2)	0.6242 (3)	0.1131 (4)	0.0149 (7)
O15	0.7762 (2)	0.1145 (3)	0.2859 (4)	0.0222 (9)
O16	0.5032 (2)	0.8672 (3)	0.1910 (4)	0.0123 (7)
O17	0.6118 (2)	0.2098 (3)	0.2942 (4)	0.0147 (7)
O18	0.0423 (3)	0.7296 (3)	0.2295 (5)	0.0366 (12)
O19	0.0424 (7)	0.6173 (10)	0.9610 (11)	0.0191 (19)	0.612 (17)
O191	0.0395 (12)	0.6633 (14)	0.9569 (19)	0.0191 (19)	0.388 (17)
O20	0.0489 (4)	0.5281 (5)	0.2364 (9)	0.0181 (15)	0.703 (12)
O201	0.0481 (10)	0.5117 (13)	0.164 (2)	0.0181 (15)	0.298 (12)

	U11	U22	U33	U12	U13	U23
Mo1	0.00827 (19)	0.0211 (2)	0.0093 (2)	0.00355 (16)	0.00231 (15)	0.00338 (16)
Mo2	0.0095 (2)	0.0139 (2)	0.0205 (2)	−0.00034 (16)	0.00001 (17)	0.00670 (17)
Mo3	0.00620 (19)	0.0103 (2)	0.0094 (2)	0.00053 (15)	0.00019 (14)	0.00045 (15)
As1	0.0061 (2)	0.0123 (2)	0.0073 (2)	−0.00051 (17)	0.00123 (17)	−0.00062 (17)
As2	0.0072 (2)	0.0101 (2)	0.0095 (2)	0.00085 (17)	0.00259 (17)	0.00266 (18)
As3	0.0083 (2)	0.0091 (2)	0.0182 (3)	−0.00207 (18)	0.00470 (19)	−0.00203 (19)
As4	0.0057 (2)	0.0116 (2)	0.0105 (2)	−0.00142 (17)	0.00102 (17)	−0.00197 (18)
Na1	0.0537 (17)	0.0409 (15)	0.0194 (12)	0.0219 (13)	−0.0001 (11)	−0.0080 (11)
Na2	0.0316 (14)	0.0373 (15)	0.0341 (14)	0.0110 (11)	0.0024 (11)	0.0004 (11)
O1	0.0126 (17)	0.0139 (17)	0.0115 (17)	−0.0014 (14)	−0.0039 (13)	−0.0012 (13)
O2	0.0116 (17)	0.0240 (19)	0.0091 (17)	0.0022 (14)	0.0064 (13)	0.0021 (14)
O3	0.0155 (17)	0.0130 (17)	0.0179 (18)	−0.0009 (14)	0.0091 (14)	−0.0030 (14)
O4	0.017 (2)	0.023 (2)	0.048 (3)	0.0010 (17)	0.0076 (19)	0.0048 (19)
O5	0.0149 (18)	0.0234 (19)	0.0107 (17)	−0.0006 (15)	0.0011 (14)	0.0043 (14)
O6	0.023 (2)	0.0188 (19)	0.0137 (18)	−0.0089 (15)	−0.0053 (15)	−0.0032 (15)
O7	0.028 (2)	0.027 (2)	0.029 (2)	0.0067 (18)	0.0126 (18)	0.0129 (18)
O8	0.0198 (19)	0.021 (2)	0.025 (2)	−0.0005 (15)	−0.0092 (16)	−0.0054 (16)
O9	0.0109 (16)	0.0136 (17)	0.0163 (18)	0.0005 (13)	0.0003 (14)	0.0004 (14)
O10	0.0095 (16)	0.0187 (18)	0.0203 (19)	0.0036 (14)	0.0024 (14)	0.0041 (15)
O11	0.0084 (16)	0.0156 (18)	0.0135 (17)	0.0012 (13)	0.0012 (13)	−0.0039 (14)
O12	0.029 (2)	0.068 (4)	0.029 (3)	0.002 (2)	−0.001 (2)	0.003 (2)
O13	0.0128 (18)	0.047 (3)	0.017 (2)	0.0070 (18)	−0.0025 (15)	−0.0025 (18)
O14	0.0055 (16)	0.0152 (18)	0.025 (2)	−0.0020 (13)	0.0052 (14)	0.0046 (15)
O15	0.0131 (18)	0.032 (2)	0.023 (2)	0.0060 (16)	0.0096 (15)	0.0064 (17)
O16	0.0087 (16)	0.0129 (17)	0.0159 (17)	−0.0016 (13)	0.0049 (13)	−0.0016 (13)
O17	0.0126 (17)	0.0088 (16)	0.0218 (19)	0.0015 (13)	−0.0041 (14)	0.0032 (14)
O18	0.015 (2)	0.024 (2)	0.069 (3)	0.0017 (17)	−0.004 (2)	−0.030 (2)
O19	0.012 (2)	0.030 (6)	0.017 (2)	0.006 (5)	0.0075 (17)	0.005 (5)
O191	0.012 (2)	0.030 (6)	0.017 (2)	0.006 (5)	0.0075 (17)	0.005 (5)
O20	0.013 (2)	0.019 (3)	0.021 (4)	−0.0069 (19)	−0.009 (3)	0.009 (3)
O201	0.013 (2)	0.019 (3)	0.021 (4)	−0.0069 (19)	−0.009 (3)	0.009 (3)

Mo1—O13i	1.684 (4)	As2—O9	1.663 (3)
Mo1—O7i	1.700 (4)	As2—O17	1.675 (3)
Mo1—O3ii	2.002 (3)	As2—O16ii	1.753 (3)
Mo1—O2iii	2.003 (3)	As3—O19i	1.631 (10)
Mo1—O9ii	2.189 (3)	As3—O18	1.669 (4)
Mo1—O11	2.264 (3)	As3—O20	1.706 (6)
Mo2—O4	1.672 (4)	As3—O14vi	1.735 (3)
Mo2—O12	1.688 (5)	As4—O10	1.651 (3)
Mo2—O20	2.002 (6)	As4—O6	1.666 (3)
Mo2—O18iv	2.038 (4)	As4—O3	1.686 (3)
Mo2—O19v	2.204 (10)	As4—O14	1.747 (3)
Mo2—O10vi	2.246 (3)	Na1—O7ix	2.438 (5)
Mo3—O15	1.686 (4)	Na1—O11	2.442 (4)
Mo3—O8	1.699 (4)	Na1—O1x	2.592 (4)
Mo3—O6vii	1.982 (3)	Na1—O5vii	2.652 (4)
Mo3—O17	2.003 (3)	Na2—O8xi	2.379 (5)
Mo3—O1	2.168 (3)	Na2—O13xii	2.412 (5)
Mo3—O5vii	2.275 (4)	Na2—O20xiii	2.603 (8)
As1—O11	1.663 (3)	Na2—O15xiv	2.636 (5)
As1—O1	1.664 (3)	Na2—O18xiii	2.651 (6)
As1—O2	1.673 (3)	Na2—O10xi	2.695 (4)
As1—O16viii	1.755 (3)	Na2—O12xv	2.695 (5)
As2—O5	1.657 (3)
O13i—Mo1—O7i	103.8 (2)	O11—As1—O16viii	105.99 (16)
O13i—Mo1—O3ii	96.13 (17)	O1—As1—O16viii	103.40 (16)
O7i—Mo1—O3ii	96.25 (17)	O2—As1—O16viii	105.00 (17)
O13i—Mo1—O2iii	95.99 (17)	O5—As2—O9	115.52 (17)
O7i—Mo1—O2iii	99.49 (17)	O5—As2—O17	114.38 (18)
O3ii—Mo1—O2iii	157.22 (14)	O9—As2—O17	111.62 (17)
O13i—Mo1—O9ii	89.84 (17)	O5—As2—O16ii	103.55 (17)
O7i—Mo1—O9ii	166.34 (17)	O9—As2—O16ii	111.25 (16)
O3ii—Mo1—O9ii	81.23 (13)	O17—As2—O16ii	98.86 (16)
O2iii—Mo1—O9ii	79.59 (13)	O19i—As3—O18	120.1 (5)
O13i—Mo1—O11	167.66 (18)	O19i—As3—O20	112.8 (5)
O7i—Mo1—O11	88.54 (17)	O18—As3—O20	97.5 (3)
O3ii—Mo1—O11	82.75 (13)	O19i—As3—O14vi	109.1 (4)
O2iii—Mo1—O11	81.30 (13)	O18—As3—O14vi	107.80 (18)
O9ii—Mo1—O11	77.84 (12)	O20—As3—O14vi	108.7 (2)
O4—Mo2—O12	103.3 (2)	O10—As4—O6	119.85 (18)
O4—Mo2—O20	96.0 (2)	O10—As4—O3	118.10 (18)
O12—Mo2—O20	93.4 (3)	O6—As4—O3	103.65 (18)
O4—Mo2—O18iv	96.68 (19)	O10—As4—O14	110.01 (17)
O12—Mo2—O18iv	91.7 (2)	O6—As4—O14	101.34 (18)
O20—Mo2—O18iv	164.8 (2)	O3—As4—O14	101.14 (16)
O4—Mo2—O19v	96.4 (3)	O7ix—Na1—O11	124.45 (17)
O12—Mo2—O19v	160.3 (3)	O7ix—Na1—O1x	115.09 (16)
O20—Mo2—O19v	84.9 (4)	O11—Na1—O1x	113.72 (15)
O18iv—Mo2—O19v	85.5 (3)	O7ix—Na1—O5vii	110.59 (16)
O4—Mo2—O10vi	170.19 (18)	O11—Na1—O5vii	98.91 (14)
O12—Mo2—O10vi	86.26 (19)	O1x—Na1—O5vii	84.34 (13)
O20—Mo2—O10vi	81.20 (19)	O8xi—Na2—O13xii	105.79 (16)
O18iv—Mo2—O10vi	84.89 (15)	O8xi—Na2—O20xiii	137.2 (2)
O19v—Mo2—O10vi	74.1 (3)	O13xii—Na2—O20xiii	78.22 (17)
O15—Mo3—O8	102.3 (2)	O8xi—Na2—O15xiv	77.62 (15)
O15—Mo3—O6vii	97.89 (17)	O13xii—Na2—O15xiv	67.62 (15)
O8—Mo3—O6vii	98.61 (17)	O20xiii—Na2—O15xiv	64.43 (18)
O15—Mo3—O17	93.01 (17)	O8xi—Na2—O18xiii	91.96 (15)
O8—Mo3—O17	101.38 (16)	O13xii—Na2—O18xiii	128.51 (16)
O6vii—Mo3—O17	154.59 (15)	O20xiii—Na2—O18xiii	57.74 (16)
O15—Mo3—O1	98.02 (17)	O15xiv—Na2—O18xiii	69.91 (14)
O8—Mo3—O1	159.50 (17)	O8xi—Na2—O10xi	104.17 (15)
O6vii—Mo3—O1	76.15 (14)	O13xii—Na2—O10xi	78.55 (14)
O17—Mo3—O1	79.65 (13)	O20xiii—Na2—O10xi	118.17 (18)
O15—Mo3—O5vii	169.94 (16)	O15xiv—Na2—O10xi	144.98 (16)
O8—Mo3—O5vii	85.81 (16)	O18xiii—Na2—O10xi	143.58 (16)
O6vii—Mo3—O5vii	86.56 (15)	O8xi—Na2—O12xv	128.48 (19)
O17—Mo3—O5vii	79.47 (14)	O13xii—Na2—O12xv	116.79 (18)
O1—Mo3—O5vii	74.19 (13)	O20xiii—Na2—O12xv	81.29 (19)
O11—As1—O1	114.32 (17)	O15xiv—Na2—O12xv	144.23 (17)
O11—As1—O2	114.23 (17)	O18xiii—Na2—O12xv	83.71 (16)
O1—As1—O2	112.56 (17)	O10xi—Na2—O12xv	60.61 (13)