Literature DB >> 24109253

K0.78Na0.22MoO2AsO4.

Raja Jouini¹, Chahira Bouzidi, Mohamed Faouzi Zid, Ahmed Driss.

Abstract

The title compound, potassium sodium dioxidomolybden-um(VI) arsenate, K0.78Na0.22MoO2AsO4, was synthesized by a solid-state reaction route. The structure is built up from corner-sharing MoO6 octa-hedra and AsO4 tetra-hedra, creating infinite [MoAsO8]∞ chains running along the b-axis direction. As, Mo and all but one O atom are on special positions (4c) with m symmetry and K (occupancy 0.78) is on a position (4a) of -1 in the tunnels. The possible motion of the alkali cations has been investigated by means of the bond-valance sum (BVS) model. The simulation shows that the Na(+) motion appears to be easier mainly along the b-axis direction. Structural relationships between the different compounds of the AMoO2AsO4 (A = Ag, Li, Na, K, Rb) series and MXO8 (M = V; X = P, As) chains are discussed.

Entities: Chemical Disease Gene

Year: 2013 PMID： 24109253 PMCID： PMC3793666 DOI： 10.1107/S1600536813018540

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

Related literature

For background to the physico-chemical properties of related compounds, see: Gueho et al. (1993 ▶); Piffard et al. (1985 ▶). For details of structurally related compounds, see: Zid & Jouini (1996 ▶, 1999 ▶); Ben Hlila et al. (2009 ▶); Hajji & Zid (2006 ▶); Linnros (1970 ▶); Zid et al. (1997 ▶); Hajji et al. (2004 ▶); Belkhiri et al. (2012 ▶); Benhamada et al. (1991 ▶); Boudin et al. (1995 ▶). For the preparation, see: Jouini et al. (2012 ▶, 2013 ▶). For BVS pathway simulation, see: Ouerfelli et al. (2007 ▶); Ben Smida et al. (2013 ▶); Ben Amor et al. (2008 ▶). For bond-valence-sum calculations, see: Brown & Altermatt (1985 ▶).

Experimental

Crystal data

K0.78Na0.22MoO2AsO4 M = 302.47 Orthorhombic, a = 10.5672 (9) Å b = 6.6323 (8) Å c = 6.9621 (8) Å V = 487.94 (9) Å3 Z = 4 Mo Kα radiation μ = 10.05 mm−1 T = 298 K 0.45 × 0.33 × 0.23 mm

Data collection

Enraf–Nonius CAD-4 diffractometer Absorption correction: ψ scan (North et al., 1968 ▶) T min = 0.025, T max = 0.098 1413 measured reflections 576 independent reflections 553 reflections with I > 2σ(I) R int = 0.037 2 standard reflections every 120 min intensity decay: 1.2%

Refinement

R[F 2 > 2σ(F 2)] = 0.025 wR(F 2) = 0.067 S = 1.17 576 reflections 64 parameters 1 restraint Δρmax = 0.64 e Å−3 Δρmin = −1.13 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 publication routines (Farrugia, 2012 ▶). Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536813018540/br2228sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813018540/br2228Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

K_0.78Na_0.22MoO₂AsO₄	F(000) = 561
M_r = 302.47	D_x = 4.117 Mg m⁻³
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 25 reflections
a = 10.5672 (9) Å	θ = 10–15°
b = 6.6323 (8) Å	µ = 10.05 mm⁻¹
c = 6.9621 (8) Å	T = 298 K
V = 487.94 (9) Å³	Prism, yellow
Z = 4	0.45 × 0.33 × 0.23 mm

Enraf–Nonius CAD-4 diffractometer	553 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.037
Graphite monochromator	θ_max = 27.0°, θ_min = 3.5°
ω/2θ scans	h = −1→13
Absorption correction: ψ scan (North et al., 1968)	k = −1→8
T_min = 0.025, T_max = 0.098	l = −8→8
1413 measured reflections	2 standard reflections every 120 min
576 independent reflections	intensity decay: 1.2%

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(F_o²) + (0.0355P)² + 0.6861P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.067	(Δ/σ)_max < 0.001
S = 1.17	Δρ_max = 0.64 e Å⁻³
576 reflections	Δρ_min = −1.13 e Å⁻³
64 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
1 restraint	Extinction coefficient: 0.041 (2)

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	U_iso*/U_eq	Occ. (<1)
Mo1	0.33773 (3)	0.2500	0.04848 (5)	0.0073 (2)
As1	0.15597 (4)	0.2500	0.46230 (6)	0.0063 (2)
K1	0.0000	0.0000	1.0000	0.026 (2)	0.78 (4)
Na1	0.019 (4)	0.004 (7)	0.909 (13)	0.045 (8)	0.11 (2)
O1	0.4059 (3)	0.2500	0.8266 (5)	0.0162 (7)
O2	0.5287 (3)	0.2500	0.1823 (5)	0.0112 (6)
O3	0.1832 (3)	0.2500	0.9890 (5)	0.0221 (8)
O4	0.1507 (2)	0.0449 (4)	0.6066 (3)	0.0135 (5)
O5	0.2973 (3)	0.2500	0.3516 (4)	0.0108 (6)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.0091 (3)	0.0092 (3)	0.0037 (3)	0.000	−0.00043 (12)	0.000
As1	0.0082 (3)	0.0069 (3)	0.0038 (3)	0.000	0.00037 (14)	0.000
K1	0.0228 (19)	0.0218 (13)	0.034 (5)	−0.0057 (8)	0.0014 (16)	−0.0102 (19)
Na1	0.050 (17)	0.039 (15)	0.05 (2)	−0.019 (11)	0.011 (16)	−0.025 (18)
O1	0.0176 (15)	0.0227 (17)	0.0082 (15)	0.000	0.0042 (12)	0.000
O2	0.0107 (12)	0.0181 (16)	0.0047 (14)	0.000	0.0007 (13)	0.000
O3	0.0126 (14)	0.042 (2)	0.0118 (16)	0.000	−0.0015 (14)	0.000
O4	0.0235 (13)	0.0091 (10)	0.0079 (10)	−0.0024 (8)	0.0005 (9)	0.0024 (8)
O5	0.0081 (13)	0.0167 (15)	0.0076 (14)	0.000	0.0014 (11)	0.000

Mo1—O3ⁱ	1.685 (3)	K1—O2^viii	2.781 (3)
Mo1—O1ⁱ	1.704 (3)	K1—O5^vii	2.899 (2)
Mo1—O4ⁱⁱ	2.001 (2)	K1—O5^viii	2.899 (2)
Mo1—O4ⁱⁱⁱ	2.001 (2)	K1—O1^viii	2.985 (3)
Mo1—O5	2.153 (3)	K1—O1^vii	2.985 (3)
Mo1—O2	2.223 (3)	K1—O4^vi	3.182 (2)
As1—O2^iv	1.680 (3)	K1—O4	3.182 (2)
As1—O5	1.681 (3)	Na1—O2^viii	2.36 (5)
As1—O4^v	1.692 (2)	Na1—O3	2.45 (3)
As1—O4	1.692 (2)	Na1—O4	2.54 (9)
K1—O3^vi	2.550 (3)	Na1—O5^viii	2.60 (4)
K1—O3	2.550 (3)	Na1—O1^vii	2.61 (7)
K1—O2^vii	2.781 (3)	Na1—O3^vi	2.81 (6)

O3ⁱ—Mo1—O1ⁱ	100.77 (16)	O5^viii—K1—O1^viii	73.00 (8)
O3ⁱ—Mo1—O4ⁱⁱ	96.26 (7)	O3^vi—K1—O1^vii	97.53 (8)
O1ⁱ—Mo1—O4ⁱⁱ	99.06 (7)	O3—K1—O1^vii	82.47 (8)
O3ⁱ—Mo1—O4ⁱⁱⁱ	96.26 (7)	O2^vii—K1—O1^vii	108.13 (6)
O1ⁱ—Mo1—O4ⁱⁱⁱ	99.06 (7)	O2^viii—K1—O1^vii	71.87 (6)
O4ⁱⁱ—Mo1—O4ⁱⁱⁱ	155.61 (13)	O5^vii—K1—O1^vii	73.00 (8)
O3ⁱ—Mo1—O5	92.79 (14)	O5^viii—K1—O1^vii	107.00 (8)
O1ⁱ—Mo1—O5	166.44 (13)	O3^vi—K1—O4^vi	62.19 (9)
O4ⁱⁱ—Mo1—O5	79.28 (7)	O3—K1—O4^vi	117.81 (9)
O4ⁱⁱⁱ—Mo1—O5	79.28 (7)	O2^vii—K1—O4^vi	54.95 (7)
O3ⁱ—Mo1—O2	169.45 (15)	O2^viii—K1—O4^vi	125.05 (7)
O1ⁱ—Mo1—O2	89.78 (14)	O5^vii—K1—O4^vi	51.47 (6)
O4ⁱⁱ—Mo1—O2	81.94 (6)	O5^viii—K1—O4^vi	128.53 (6)
O4ⁱⁱⁱ—Mo1—O2	81.94 (6)	O1^viii—K1—O4^vi	57.25 (7)
O5—Mo1—O2	76.66 (12)	O1^vii—K1—O4^vi	122.75 (7)
O2^iv—As1—O5	115.90 (16)	O3^vi—K1—O4	117.81 (9)
O2^iv—As1—O4^v	109.23 (9)	O3—K1—O4	62.19 (9)
O5—As1—O4^v	107.55 (9)	O2^vii—K1—O4	125.05 (7)
O2^iv—As1—O4	109.23 (10)	O2^viii—K1—O4	54.95 (7)
O5—As1—O4	107.55 (9)	O5^vii—K1—O4	128.53 (6)
O4^v—As1—O4	107.03 (16)	O5^viii—K1—O4	51.47 (6)
O3^vi—K1—O2^vii	116.53 (10)	O1^viii—K1—O4	122.75 (7)
O3—K1—O2^vii	63.47 (10)	O1^vii—K1—O4	57.25 (7)
O3^vi—K1—O2^viii	63.47 (10)	O2^viii—Na1—O3	141 (4)
O3—K1—O2^viii	116.53 (10)	O2^viii—Na1—O4	69 (2)
O3^vi—K1—O5^vii	78.48 (7)	O3—Na1—O4	74.2 (19)
O3—K1—O5^vii	101.52 (7)	O2^viii—Na1—O5^viii	66.1 (13)
O2^vii—K1—O5^vii	57.05 (9)	O3—Na1—O5^viii	86.5 (11)
O2^viii—K1—O5^vii	122.95 (9)	O4—Na1—O5^viii	62.1 (16)
O3^vi—K1—O5^viii	101.52 (7)	O2^viii—Na1—O1^vii	86 (2)
O3—K1—O5^viii	78.48 (7)	O3—Na1—O1^vii	93 (2)
O2^vii—K1—O5^viii	122.95 (9)	O4—Na1—O1^vii	70 (2)
O2^viii—K1—O5^viii	57.05 (9)	O5^viii—Na1—O1^vii	131 (4)
O3^vi—K1—O1^viii	82.47 (8)	O2^viii—Na1—O3^vi	65.1 (9)
O3—K1—O1^viii	97.53 (8)	O3—Na1—O3^vi	152 (4)
O2^vii—K1—O1^viii	71.87 (6)	O4—Na1—O3^vi	134 (2)
O2^viii—K1—O1^viii	108.13 (6)	O5^viii—Na1—O3^vi	102.7 (16)
O5^vii—K1—O1^viii	107.00 (8)	O1^vii—Na1—O3^vi	100.6 (10)

7 in total

K0.78Na0.22MoO2AsO4.

Related literature

Experimental

Crystal data

Data collection

Refinement

1. A short history of SHELX.

2. La variété β-NaMoO(2)(AsO(4)).

3. [Beta-LiMoO2(AsO4)].

4. LiCo2As3O10: une nouvelle structure à tunnels inter-connectés.

5. K(MoO2)4O3(AsO4).

6. K₂V₂O₂(AsO₄)₂.

7. Na2MoO2As2O7.