NASICON-type Na3V2(PO4)3

Zatovsky, I.V.

doi:10.1107/S1600536810002801

inorganic compounds

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Volume 66| Part 2| February 2010| Page i12

https://doi.org/10.1107/S1600536810002801

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NASICON-type Na₃V₂(PO₄)₃

Igor V. Zatovsky ^a ^*

^aDepartment of Inorganic Chemistry, Taras Shevchenko National University, 64 Volodymyrska str., 01601 Kyiv, Ukraine
^*Correspondence e-mail: zvigo@yandex.ru

(Received 19 December 2009; accepted 22 January 2010; online 27 January 2010)

Single crystals of the title compound, trisodium divanadium(III) tris(orthophosphate), were grown from a self-flux in the system Na₄P₂O₇–NaVP₂O₇. Na₃V₂(PO₄)₃ belongs to the family of NASICON-related structures and is built up from isolated [VO₆] octahedra (3. symmetry) and [PO₄] tetrahedra (.2 symmetry) interlinked via corners to establish the framework anion [V₂(PO₄)₃]³⁻. The two independent Na⁺ cations are partially occupied [site-occupancy factors = 0.805 (18) and 0.731 (7)] and are located in channels with two different oxygen environments, viz sixfold coordination for the first ( $[\overline{3}]$ . symmetry) and eightfold for the second (.2 symmetry) Na⁺ cation.

Related literature

For structures and properties of complex phosphates with general formula Na₃M^III₂(PO₄)₃ (M^III = Sc, Fe, Cr), see: Collin et al. (1986 ); Genkina et al. (1991 ); Lazoryak et al. (1980 ); Lucazeau et al. (1986 ); Masquelier et al. (1992 ); Susman et al. (1983 ). For preparation of NaVP₂O₇ which was used as an educt for crystal growth of the title compound, see: Zatovsky et al. (1999 ).

Experimental

Crystal data

Na₃V₂(PO₄)₃
M_r = 455.76
Trigonal, $[R \overline 3c ]$
a = 8.7288 (2) Å
c = 21.8042 (7) Å
V = 1438.73 (7) Å³
Z = 6
Mo Kα radiation
μ = 2.66 mm⁻¹
T = 293 K
0.20 × 0.15 × 0.10 mm

Data collection

Oxford Diffraction Xcalibur-3 CCD diffractometer
Absorption correction: multi-scan (Blessing, 1995 ) T_min = 0.635, T_max = 0.780
12580 measured reflections
1331 independent reflections
1153 reflections with I > 2σ(I)
R_int = 0.063

Refinement

R[F² > 2σ(F²)] = 0.032
wR(F²) = 0.075
S = 1.1
1331 reflections
37 parameters
Δρ_max = 1.12 e Å⁻³
Δρ_min = −0.74 e Å⁻³

Table 1
Selected bond lengths (Å)

V1—O2ⁱ	1.9693 (10)
V1—O1ⁱⁱ	2.0271 (9)
Na1—O1	2.5045 (11)
Na2—O1ⁱⁱ	2.3883 (12)
Na2—O1ⁱ	2.4448 (19)
Na2—O2ⁱⁱⁱ	2.6280 (16)
Na2—O2^iv	2.8352 (19)
P1—O2^v	1.5227 (12)
P1—O1	1.5358 (10)
Symmetry codes: (i) -y+1, x-y+1, z; (ii) -x+y, -x+1, z; (iii) $[-x+{\script{4\over 3}}, -x+y+{\script{2\over 3}}, -z+{\script{1\over 6}}]$ ; (iv) $[-y+{\script{4\over 3}}, -x+{\script{5\over 3}}, z+{\script{1\over 6}}]$ ; (v) $[x-{\script{2\over 3}}, x-y+{\script{2\over 3}}, z+{\script{1\over 6}}]$ .

Data collection: CrysAlis CCD (Oxford Diffraction, 2006 $[Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2006 $[Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999 ); software used to prepare material for publication: WinGX (Farrugia, 1999 ) and enCIFer (Allen et al., 2004 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536810002801/wm2293sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810002801/wm2293Isup2.hkl

checkCIF report

Comment top

The structures and properties of complex phosphates with general formula Na₃M^III₂(PO₄)₃ (M^III - Sc, Fe, Cr) have been intensively investigated, for instance: (Collin et al., 1986; Genkina et al., 1991; Lazoryak et al., 1980; Lucazeau et al., 1986; Masquelier et al., 1992; Susman et al., 1983). The structure of NASICON-type Na₃V₂(PO₄)₃, (I), is reported here.

In the asymmetric unit of (I) (Fig. 1) there is one V and one P atom, while other,atoms (Na and O) are represented in two distinct positions each. The main building block of (I) (Fig. 2) involves two VO₆ octahedra interlinked by three phosphate groups lying along the c axis. As a result of the block aggregation, a three-dimensional framework with an overall composition of [V₂(PO₄)₃]^3- is organized (Fig. 3).

Sodium atoms are located in the voids of the framework with six- (position 6b) and eightfold (18b) coordination when a cut-off distance of 2.9 Å is considered.

Related literature top

For structures and properties of complex phosphates with general formula Na₃M^III₂(PO₄)₃ (M^III = Sc, Fe, Cr), see: Collin et al. (1986); Genkina et al. (1991); Lazoryak et al. (1980); Lucazeau et al. (1986); Masquelier et al. (1992); Susman et al. (1983). For preparation of NaVP₂O₇ which was used as an educt for crystal growth of the title compound, see: Zatovsky et al. (1999).

Experimental top

Crystals of (I) were obtained in the system Na₄P₂O₇—NaVP₂O₇ using a high-temperature crystallization technique. Initial NaVP₂O₇ was prepared in accordance to Zatovsky et al. (1999). A thoroughly ground mixture of Na₄P₂O₇ and NaVP₂O₇ (ratio 1:3) was heated up to 1343 K and then kept for 2 h in a sealed silica tube under vacuum. Then it was cooled down to 823 K with a rate of 5 K/h and left in the furnace to reach room temperature. The final product, green prismatic crystals, was leached out from the solidified melt with boiling water.

Structure description top

Sodium atoms are located in the voids of the framework with six- (position 6b) and eightfold (18b) coordination when a cut-off distance of 2.9 Å is considered.

For structures and properties of complex phosphates with general formula Na₃M^III₂(PO₄)₃ (M^III = Sc, Fe, Cr), see: Collin et al. (1986); Genkina et al. (1991); Lazoryak et al. (1980); Lucazeau et al. (1986); Masquelier et al. (1992); Susman et al. (1983). For preparation of NaVP₂O₇ which was used as an educt for crystal growth of the title compound, see: Zatovsky et al. (1999).

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis CCD (Oxford Diffraction, 2006); data reduction: CrysAlis RED (Oxford Diffraction, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).

Figures top

	Fig. 1. The asymmetric unit of Na₃V₂(PO₄)₃ with displacement ellipsoids at the 50% probability level.
	Fig. 2. The central building block [V₂(PO₄)₃] in the structure of compound (I).
	Fig. 3. The view of the structure of compound (I) on the ab plane.

trisodium divanadium(III) tris(orthophosphate) top

Crystal data top

Na₃V₂(PO₄)₃	D_x = 3.156 Mg m⁻³
M_r = 455.76	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3c	Cell parameters from 12580 reflections
Hall symbol: -R 3 2"c	θ = 3.3–45.0°
a = 8.7288 (2) Å	µ = 2.66 mm⁻¹
c = 21.8042 (7) Å	T = 293 K
V = 1438.73 (7) Å³	Prism, green
Z = 6	0.20 × 0.15 × 0.10 mm
F(000) = 1320

Data collection top

Oxford Diffraction Xcalibur-3 CCD diffractometer	1331 independent reflections
Radiation source: fine-focus sealed tube	1153 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.063
φ and ω scans	θ_max = 45°, θ_min = 3.3°
Absorption correction: multi-scan (Blessing, 1995)	h = −17→16
T_min = 0.635, T_max = 0.780	k = −17→17
12580 measured reflections	l = −43→41

Refinement top

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)] = 0.032	w = 1/[σ²(F_o²) + (0.0264P)² + 5.1429P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.075	(Δ/σ)_max < 0.001
S = 1.1	Δρ_max = 1.12 e Å⁻³
1331 reflections	Δρ_min = −0.74 e Å⁻³
37 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008)
0 restraints	Extinction coefficient: 0.0056 (4)

Crystal data top

Na₃V₂(PO₄)₃	Z = 6
M_r = 455.76	Mo Kα radiation
Trigonal, R3c	µ = 2.66 mm⁻¹
a = 8.7288 (2) Å	T = 293 K
c = 21.8042 (7) Å	0.20 × 0.15 × 0.10 mm
V = 1438.73 (7) Å³

Data collection top

Oxford Diffraction Xcalibur-3 CCD diffractometer	1331 independent reflections
Absorption correction: multi-scan (Blessing, 1995)	1153 reflections with I > 2σ(I)
T_min = 0.635, T_max = 0.780	R_int = 0.063
12580 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.032	37 parameters
wR(F²) = 0.075	0 restraints
S = 1.1	Δρ_max = 1.12 e Å⁻³
1331 reflections	Δρ_min = −0.74 e Å⁻³

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
V1	0.3333	0.6667	0.019498 (13)	0.00690 (6)
Na1	0.3333	0.6667	0.1667	0.149 (5)	0.805 (18)
Na2	0.6667	0.96726 (19)	0.0833	0.0522 (10)	0.731 (7)
P1	−0.04273 (5)	0.3333	0.0833	0.00866 (8)
O1	0.14193 (13)	0.49765 (14)	0.07762 (5)	0.01643 (16)
O2	0.54047 (16)	0.84480 (17)	−0.02643 (7)	0.0259 (2)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
V1	0.00643 (7)	0.00643 (7)	0.00784 (10)	0.00321 (4)	0	0
Na1	0.218 (8)	0.218 (8)	0.0111 (14)	0.109 (4)	0	0
Na2	0.0224 (8)	0.0170 (5)	0.119 (2)	0.0112 (4)	−0.0354 (11)	−0.0177 (5)
P1	0.00635 (10)	0.00714 (14)	0.01276 (15)	0.00357 (7)	0.00152 (5)	0.00305 (11)
O1	0.0089 (3)	0.0130 (3)	0.0220 (4)	0.0015 (3)	0.0048 (3)	0.0057 (3)
O2	0.0185 (4)	0.0223 (5)	0.0322 (6)	0.0067 (4)	0.0143 (4)	0.0151 (4)

Geometric parameters (Å, º) top

V1—O2ⁱ	1.9693 (10)	Na2—O1ⁱⁱ	2.3883 (12)
V1—O2	1.9693 (11)	Na2—O1^vi	2.3883 (12)
V1—O2ⁱⁱ	1.9693 (10)	Na2—O1ⁱ	2.4448 (19)
V1—O1ⁱⁱ	2.0271 (9)	Na2—O1^vii	2.4449 (19)
V1—O1	2.0271 (9)	Na2—O2^viii	2.6280 (16)
V1—O1ⁱ	2.0271 (9)	Na2—O2	2.6281 (16)
V1—Na2ⁱ	3.1070 (6)	Na2—O2^ix	2.8352 (19)
V1—Na2	3.1070 (7)	Na2—O2^x	2.8352 (19)
V1—Na2ⁱⁱ	3.1070 (6)	Na2—P1^xi	2.9222 (11)
V1—Na1	3.2096 (3)	Na2—P1ⁱⁱ	2.9222 (11)
Na1—O1	2.5045 (11)	Na2—P1ⁱ	2.9968 (17)
Na1—O1ⁱⁱ	2.5045 (11)	P1—O2^xii	1.5227 (12)
Na1—O1ⁱ	2.5045 (11)	P1—O2^xiii	1.5227 (12)
Na1—O1ⁱⁱⁱ	2.5045 (11)	P1—O1	1.5358 (10)
Na1—O1^iv	2.5045 (11)	P1—O1^xiv	1.5359 (10)
Na1—O1^v	2.5046 (11)	P1—Na2^xv	2.9222 (11)
Na1—V1^iv	3.2081 (2)	P1—Na2ⁱ	2.9222 (11)
Na1—Na2ⁱ	3.3193 (6)	P1—Na2ⁱⁱ	2.9968 (17)
Na1—Na2^v	3.3193 (6)	O1—Na2ⁱ	2.3883 (12)
Na1—Na2	3.3193 (6)	O1—Na2ⁱⁱ	2.4448 (19)
Na1—Na2ⁱⁱ	3.3205 (6)

O2ⁱ—V1—O2	96.44 (6)	O1ⁱⁱ—Na2—O2	68.20 (4)
O2ⁱ—V1—O2ⁱⁱ	96.44 (6)	O1^vi—Na2—O2	115.98 (4)
O2—V1—O2ⁱⁱ	96.44 (6)	O1ⁱ—Na2—O2	66.40 (4)
O2ⁱ—V1—O1ⁱⁱ	88.22 (5)	O1^vii—Na2—O2	93.51 (6)
O2—V1—O1ⁱⁱ	89.72 (5)	O2^viii—Na2—O2	157.25 (9)
O2ⁱⁱ—V1—O1ⁱⁱ	171.80 (6)	O1ⁱⁱ—Na2—O2^ix	54.99 (4)
O2ⁱ—V1—O1	89.72 (5)	O1^vi—Na2—O2^ix	108.39 (6)
O2—V1—O1	171.80 (6)	O1ⁱ—Na2—O2^ix	115.94 (4)
O2ⁱⁱ—V1—O1	88.22 (5)	O1^vii—Na2—O2^ix	151.11 (4)
O1ⁱⁱ—V1—O1	85.05 (5)	O2^viii—Na2—O2^ix	85.67 (3)
O2ⁱ—V1—O1ⁱ	171.80 (6)	O2—Na2—O2^ix	112.13 (5)
O2—V1—O1ⁱ	88.22 (5)	O1ⁱⁱ—Na2—O2^x	108.39 (6)
O2ⁱⁱ—V1—O1ⁱ	89.72 (5)	O1^vi—Na2—O2^x	54.99 (4)
O1ⁱⁱ—V1—O1ⁱ	85.05 (5)	O1ⁱ—Na2—O2^x	151.10 (4)
O1—V1—O1ⁱ	85.05 (5)	O1^vii—Na2—O2^x	115.94 (4)
O1—Na1—O1ⁱⁱ	66.33 (3)	O2^viii—Na2—O2^x	112.13 (5)
O1—Na1—O1ⁱ	66.33 (3)	O2—Na2—O2^x	85.67 (3)
O1ⁱⁱ—Na1—O1ⁱ	66.33 (3)	O2^ix—Na2—O2^x	80.45 (7)
O1—Na1—O1ⁱⁱⁱ	113.67 (3)	O2^xii—P1—O2^xiii	111.67 (12)
O1ⁱⁱ—Na1—O1ⁱⁱⁱ	180	O2^xii—P1—O1	106.07 (7)
O1ⁱ—Na1—O1ⁱⁱⁱ	113.67 (3)	O2^xiii—P1—O1	112.18 (7)
O1—Na1—O1^iv	180	O2^xii—P1—O1^xiv	112.19 (7)
O1ⁱⁱ—Na1—O1^iv	113.67 (3)	O2^xiii—P1—O1^xiv	106.07 (7)
O1ⁱ—Na1—O1^iv	113.67 (3)	O1—P1—O1^xiv	108.74 (9)
O1ⁱⁱⁱ—Na1—O1^iv	66.33 (3)	P1—O1—V1	145.95 (7)
O1—Na1—O1^v	113.67 (3)	P1—O1—Na2ⁱ	93.73 (6)
O1ⁱⁱ—Na1—O1^v	113.67 (3)	V1—O1—Na2ⁱ	89.05 (5)
O1ⁱ—Na1—O1^v	180	P1—O1—Na2ⁱⁱ	94.93 (5)
O1ⁱⁱⁱ—Na1—O1^v	66.33 (3)	V1—O1—Na2ⁱⁱ	87.50 (4)
O1^iv—Na1—O1^v	66.33 (3)	Na2ⁱ—O1—Na2ⁱⁱ	169.09 (5)
O1ⁱⁱ—Na2—O1^vi	160.52 (9)	P1—O1—Na1	124.53 (6)
O1ⁱⁱ—Na2—O1ⁱ	69.07 (5)	V1—O1—Na1	89.52 (4)
O1^vi—Na2—O1ⁱ	130.40 (6)	Na2ⁱ—O1—Na1	85.40 (5)
O1ⁱⁱ—Na2—O1^vii	130.40 (6)	Na2ⁱⁱ—O1—Na1	84.23 (4)
O1^vi—Na2—O1^vii	69.07 (5)	P1^xvi—O2—V1	151.38 (10)
O1ⁱ—Na2—O1^vii	61.41 (6)	P1^xvi—O2—Na2	120.77 (8)
O1ⁱⁱ—Na2—O2^viii	115.98 (4)	V1—O2—Na2	83.72 (5)
O1^vi—Na2—O2^viii	68.20 (4)	P1^xvi—O2—Na2^xvii	77.85 (5)
O1ⁱ—Na2—O2^viii	93.51 (6)	V1—O2—Na2^xvii	107.30 (6)
O1^vii—Na2—O2^viii	66.40 (4)	Na2—O2—Na2^xvii	113.64 (7)

Symmetry codes: (i) −y+1, x−y+1, z; (ii) −x+y, −x+1, z; (iii) x−y+2/3, x+1/3, −z+1/3; (iv) −x+2/3, −y+4/3, −z+1/3; (v) y−1/3, −x+y+1/3, −z+1/3; (vi) x−y+4/3, −y+5/3, −z+1/6; (vii) y+1/3, x+2/3, −z+1/6; (viii) −x+4/3, −x+y+2/3, −z+1/6; (ix) −y+4/3, −x+5/3, z+1/6; (x) y, −x+y+1, −z; (xi) x+1, y+1, z; (xii) x−2/3, x−y+2/3, z+1/6; (xiii) y−1, −x+y, −z; (xiv) x−y+1/3, −y+2/3, −z+1/6; (xv) x−1, y−1, z; (xvi) x−y+1, x+1, −z; (xvii) x−y+1, x, −z.

Experimental details

Crystal data
Chemical formula	Na₃V₂(PO₄)₃
M_r	455.76
Crystal system, space group	Trigonal, R3c
Temperature (K)	293
a, c (Å)	8.7288 (2), 21.8042 (7)
V (Å³)	1438.73 (7)
Z	6
Radiation type	Mo Kα
µ (mm⁻¹)	2.66
Crystal size (mm)	0.20 × 0.15 × 0.10

Data collection
Diffractometer	Oxford Diffraction Xcalibur-3 CCD
Absorption correction	Multi-scan (Blessing, 1995)
T_min, T_max	0.635, 0.780
No. of measured, independent and observed [I > 2σ(I)] reflections	12580, 1331, 1153
R_int	0.063
(sin θ/λ)_max (Å⁻¹)	0.995

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.032, 0.075, 1.1
No. of reflections	1331
No. of parameters	37
Δρ_max, Δρ_min (e Å⁻³)	1.12, −0.74

Computer programs: CrysAlis CCD (Oxford Diffraction, 2006), CrysAlis RED (Oxford Diffraction, 2006), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 1999), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).

Selected bond lengths (Å) top

V1—O2ⁱ	1.9693 (10)	Na2—O2ⁱⁱⁱ	2.6280 (16)
V1—O1ⁱⁱ	2.0271 (9)	Na2—O2^iv	2.8352 (19)
Na1—O1	2.5045 (11)	P1—O2^v	1.5227 (12)
Na2—O1ⁱⁱ	2.3883 (12)	P1—O1	1.5358 (10)
Na2—O1ⁱ	2.4448 (19)

Symmetry codes: (i) −y+1, x−y+1, z; (ii) −x+y, −x+1, z; (iii) −x+4/3, −x+y+2/3, −z+1/6; (iv) −y+4/3, −x+5/3, z+1/6; (v) x−2/3, x−y+2/3, z+1/6.

Acknowledgements

The author is grateful to Professor Vyacheslav N. Baumer from STC "Institute for Single Crystals", NAS of Ukraine, Kharkiv, Ukraine, for the single-crystal measurements.

References

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