Literature DB >> 22807696

K₂V₂O₂(AsO₄)₂.

Sabrina Belkhiri¹, Djillali Mezaoui, Thierry Roisnel.

Abstract

The vanadium oxide arsenate with formula K₂V₂O₂(AsO₄)₂, dipotassium divanadium(IV) dioxide diarsenate, has been synthesized by solid-state reaction in an evacuated silica ampoule. Its structure is isotypic with K₂V₂O₂(PO₄)₂. The framework is built up from corner-sharing VO₆ octa-hedra and AsO₄ tetra-hedra, creating an infinite [VAsO₈](∞) chain running along the a- and c-axis directions. The K⁺ cations are located in hexa-gonal tunnels, which are delimited by the connection of the [VAsO₈](∞) chains.

Entities: Chemical Disease Species

Year: 2012 PMID： 22807696 PMCID： PMC3393139 DOI： 10.1107/S1600536812027183

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

Related literature

For the properties of the potassium titanyl phosphate KTiOPO4 (KTP) family, see: El Haidouri et al. (1990 ▶); Harrison & Phillips (1999 ▶); Phillips et al. (1990 ▶). For the structures of AMOXO4 compounds (A = K, Na, Li, M = transition metal and X = P, As) of the KTP family, see: Phillips et al. (1990 ▶); Harrison & Phillips (1999 ▶); El Haidouri et al. (1990 ▶). For the synthesis of K1.65V1.78W0.22O2(AsO4)2, see: Belkhiri et al. (2009 ▶). For the synthesis and structure of isotypic K2V2O2(PO4)2, see: Benhamada et al. (1991 ▶). For the effect on the electron transport properties caused by the distortion of the VIVO6 octahedra, see: El Haidouri et al. (1990 ▶); El Brahimi & Durand (1986 ▶); Nakagawa et al. (1999 ▶). For the hexagonal tungsten bronze structure, see: Magnéli (1953 ▶).

Experimental

Crystal data

K2V2O2(AsO4)2 M = 489.9 Orthorhombic, a = 6.5368 (2) Å b = 10.7228 (5) Å c = 13.0666 (4) Å V = 915.87 (6) Å3 Z = 4 Mo Kα radiation μ = 10.16 mm−1 T = 150 K 0.30 × 0.25 × 0.22 mm

Data collection

Bruker APEXII diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 2002 ▶) T min = 0.073, T max = 0.107 11866 measured reflections 4169 independent reflections 3805 reflections with I > 3σ(I) R int = 0.033

Refinement

R[F 2 > 2σ(F 2)] = 0.028 wR(F 2) = 0.034 S = 1.60 4169 reflections 139 parameters Δρmax = 0.94 e Å−3 Δρmin = −0.77 e Å−3 Absolute structure: Flack (1983 ▶), 1256 Friedel pairs Flack parameter: 0.387 (8) Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); data reduction: SAINT; program(s) used to solve structure: SuperFlip (Palatinus & Chapuis, 2007 ▶); program(s) used to refine structure: JANA2006 (Petříček et al., 2006 ▶); molecular graphics: ATOMS (Dowty, 1994 ▶) and GRETEP (Laugier & Bochu, 2002 ▶); software used to prepare material for publication: JANA2006. Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812027183/ru2035sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812027183/ru2035Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

K₂V₂O₂(AsO₄)₂	F(000) = 920
M_r = 489.9	D_x = 3.552 Mg m⁻³
Orthorhombic, Pc2₁n	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: P -2n -2ac	Cell parameters from 5952 reflections
a = 6.5368 (2) Å	θ = 3.5–40.2°
b = 10.7228 (5) Å	µ = 10.16 mm⁻¹
c = 13.0666 (4) Å	T = 150 K
V = 915.87 (6) Å³	Prism, black
Z = 4	0.3 × 0.25 × 0.22 mm

Bruker APEXII diffractometer	4169 independent reflections
Radiation source: fine-focus sealed tube	3805 reflections with I > 3σ(I)
Graphite monochromator	R_int = 0.033
CCD rotation images, thin slices scans	θ_max = 40.2°, θ_min = 3.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 2002)	h = −23→23
T_min = 0.073, T_max = 0.107	k = −11→10
11866 measured reflections	l = −19→15

Refinement on F	Weighting scheme based on measured s.u.'s w = 1/(σ²(F) + 0.000049F²)
R[F² > 2σ(F²)] = 0.028	(Δ/σ)_max = 0.003
wR(F²) = 0.034	Δρ_max = 0.94 e Å⁻³
S = 1.60	Δρ_min = −0.77 e Å⁻³
4169 reflections	Extinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)
139 parameters	Extinction coefficient: 970 (110)
0 restraints	Absolute structure: Flack (1983), 1256 Friedel pairs
0 constraints	Flack parameter: 0.387 (8)

	x	y	z	U_iso*/U_eq
As2	0.99887 (4)	0.333103	−0.18131 (2)	0.00293 (5)
V1	0.27644 (5)	0.59847 (6)	0.25107 (3)	0.00255 (8)
V2	0.49984 (6)	0.34895 (5)	−0.12277 (3)	0.00271 (8)
K1	−0.22511 (9)	0.53150 (8)	0.12103 (6)	0.01172 (15)
K2	0.79227 (10)	0.77688 (8)	−0.10496 (5)	0.01127 (15)
O1	−0.5484 (3)	0.4499 (2)	0.23637 (18)	0.0058 (5)
O2	0.7996 (3)	0.3653 (2)	−0.10470 (17)	0.0060 (3)
O3	0.1652 (3)	0.6001 (3)	−0.09922 (15)	0.0060 (4)
O4	0.4565 (3)	0.4521 (2)	−0.21415 (18)	0.0060 (5)
O5	0.4859 (3)	0.7051 (2)	0.01550 (19)	0.0061 (5)
O6	0.1747 (3)	0.5671 (2)	0.10771 (16)	0.0053 (4)
O7	0.4687 (4)	0.4564 (2)	−0.00520 (17)	0.0063 (5)
O8	1.2015 (3)	0.2971 (2)	−0.10749 (17)	0.0060 (3)
O9	0.9597 (3)	0.2103 (2)	−0.26290 (18)	0.0062 (5)
O10	0.4516 (3)	0.7042 (2)	0.22272 (18)	0.0061 (5)
As1	0.32206 (3)	0.58763 (5)	0.00215 (2)	0.00258 (5)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
As2	0.00216 (8)	0.00404 (10)	0.00258 (10)	−0.00032 (7)	−0.00002 (9)	0.00035 (10)
V1	0.00278 (13)	0.00322 (15)	0.00164 (15)	0.00008 (15)	0.00028 (13)	0.00010 (14)
V2	0.00261 (13)	0.00336 (17)	0.00216 (15)	0.00019 (13)	−0.00004 (13)	0.00031 (14)
K1	0.0052 (2)	0.0156 (3)	0.0144 (3)	−0.0015 (2)	−0.0016 (2)	0.0047 (3)
K2	0.0104 (2)	0.0171 (3)	0.0063 (2)	−0.0012 (2)	0.00160 (19)	−0.0001 (3)
O1	0.0065 (7)	0.0053 (8)	0.0057 (9)	0.0026 (6)	0.0020 (7)	0.0030 (7)
O2	0.0028 (4)	0.0093 (5)	0.0060 (5)	−0.0001 (4)	−0.0006 (5)	0.0005 (6)
O3	0.0046 (6)	0.0114 (9)	0.0020 (7)	0.0014 (7)	−0.0015 (5)	0.0004 (8)
O4	0.0046 (7)	0.0073 (8)	0.0063 (9)	0.0009 (6)	−0.0009 (6)	0.0011 (7)
O5	0.0062 (8)	0.0071 (8)	0.0049 (9)	−0.0031 (7)	0.0010 (6)	−0.0017 (7)
O6	0.0044 (7)	0.0088 (9)	0.0026 (7)	0.0013 (6)	0.0005 (6)	0.0012 (7)
O7	0.0069 (8)	0.0079 (8)	0.0043 (9)	0.0035 (7)	−0.0020 (6)	−0.0017 (7)
O8	0.0028 (4)	0.0093 (5)	0.0060 (5)	−0.0001 (4)	−0.0006 (5)	0.0005 (6)
O9	0.0066 (7)	0.0067 (8)	0.0052 (9)	−0.0025 (7)	0.0018 (7)	−0.0018 (8)
O10	0.0075 (8)	0.0070 (8)	0.0039 (8)	−0.0012 (7)	0.0011 (7)	0.0012 (7)
As1	0.00244 (8)	0.00385 (9)	0.00144 (9)	−0.00024 (9)	−0.00003 (8)	−0.00044 (9)

As2—O1ⁱ	1.682 (2)	V2—O2	1.9811 (19)
As2—O2	1.679 (2)	V2—O4	1.652 (2)
As2—O8	1.684 (2)	V2—O5^v	2.087 (2)
As2—O9	1.714 (2)	V2—O7	1.931 (2)
V1—O1ⁱⁱ	1.971 (2)	V2—O8^vi	2.0375 (19)
V1—O3ⁱⁱⁱ	1.993 (2)	V2—O10^v	2.053 (2)
V1—O4ⁱⁱⁱ	2.234 (2)	O3—As1	1.6805 (19)
V1—O6	2.016 (2)	O5—As1	1.662 (2)
V1—O9^iv	1.960 (2)	O6—As1	1.697 (2)
V1—O10	1.654 (2)	O7—As1	1.705 (2)

O1ⁱ—As2—O2	112.20 (11)	O4—V2—O5^v	171.20 (10)
O1ⁱ—As2—O8	112.68 (10)	O4—V2—O7	99.06 (11)
O1ⁱ—As2—O9	101.71 (11)	O4—V2—O8^vi	95.14 (10)
O2—As2—O8	108.44 (10)	O4—V2—O10^v	94.17 (10)
O2—As2—O9	114.38 (10)	O5^v—V2—O7	84.92 (10)
O8—As2—O9	107.32 (11)	O5^v—V2—O8^vi	77.00 (9)
O1ⁱⁱ—V1—O3ⁱⁱⁱ	89.52 (10)	O5^v—V2—O10^v	82.04 (9)
O1ⁱⁱ—V1—O4ⁱⁱⁱ	81.24 (9)	O7—V2—O8^vi	89.08 (10)
O1ⁱⁱ—V1—O6	88.06 (9)	O7—V2—O10^v	166.76 (10)
O1ⁱⁱ—V1—O9^iv	163.57 (9)	O8^vi—V2—O10^v	90.22 (9)
O1ⁱⁱ—V1—O10	97.49 (10)	As2ⁱⁱⁱ—O1—V1^vi	130.63 (13)
O3ⁱⁱⁱ—V1—O4ⁱⁱⁱ	86.39 (9)	As2—O2—V2	132.71 (13)
O3ⁱⁱⁱ—V1—O6	167.57 (9)	V1ⁱ—O3—As1	131.00 (10)
O3ⁱⁱⁱ—V1—O9^iv	93.90 (10)	V1ⁱ—O4—V2	137.25 (13)
O3ⁱⁱⁱ—V1—O10	94.66 (11)	V2^iv—O5—As1	131.25 (13)
O4ⁱⁱⁱ—V1—O6	81.19 (9)	V1—O6—As1	123.11 (10)
O4ⁱⁱⁱ—V1—O9^iv	82.94 (9)	V2—O7—As1	126.62 (13)
O4ⁱⁱⁱ—V1—O10	178.35 (10)	As2—O8—V2ⁱⁱ	129.37 (13)
O6—V1—O9^iv	85.16 (9)	As2—O9—V1^v	122.59 (12)
O6—V1—O10	97.74 (10)	V1—O10—V2^iv	140.17 (13)
O9^iv—V1—O10	98.24 (11)	O3—As1—O5	114.55 (12)
O2—V2—O4	101.33 (10)	O3—As1—O6	107.73 (9)
O2—V2—O5^v	86.62 (9)	O3—As1—O7	111.36 (12)
O2—V2—O7	87.53 (10)	O5—As1—O6	112.26 (11)
O2—V2—O8^vi	163.51 (9)	O5—As1—O7	105.60 (11)
O2—V2—O10^v	89.41 (9)	O6—As1—O7	104.94 (11)

1 in total

1. K(1.65)V(1.78)W(0.22)O(2)(AsO(4))(2).

Authors: Sabrina Belkhiri; Mohammed Kars; Djillali Mezaoui
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2009-08-29

1 in total

1. K0.78Na0.22MoO2AsO4.

Authors: Raja Jouini; Chahira Bouzidi; Mohamed Faouzi Zid; Ahmed Driss
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2013-07-10

1 in total