Redetermination of AgPO3

Terebilenko, K.V.; Zatovsky, I.V.; Ogorodnyk, I.V.; Baumer, V.N.; Slobodyanik, N.S.

doi:10.1107/S1600536811003977

Volume 67
Part 3
Page i22
March 2011

Received 19 January 2011
Accepted 31 January 2011
Online 9 February 2011

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (P-O) = 0.002 Å
R = 0.024
wR = 0.058
Data-to-parameter ratio = 25.4
Details

Redetermination of AgPO₃

Katherina V. Terebilenko,^a ^* Igor V. Zatovsky,^a Ivan V. Ogorodnyk,^a Vyacheslav N. Baumer ^b and Nikolay S. Slobodyanik ^a

^aDepartment of Inorganic Chemistry, Taras Shevchenko National University, 64 Volodymyrska Street, 01601 Kyiv, Ukraine, and ^bSTC `Institute for Single Crystals', NAS of Ukraine, 60 Lenin Avenue, 61001 Kharkiv, Ukraine
Correspondence e-mail: tereb@bigmir.ru

Single crystals of silver(I) polyphosphate(V), AgPO₃, were prepared via a phosphoric acid melt method using a solution of Ag₃PO₄ in H₃PO₄. In comparison with the previous study based on single-crystal Weissenberg photographs [Jost (1961). Acta Cryst. 14, 779-784], the results were mainly confirmed, but with much higher precision and with all displacement parameters refined anisotropically. The structure is built up from two types of distorted edge- and corner-sharing [AgO₅] polyhedra, giving rise to multidirectional ribbons, and from two types of PO₄ tetrahedra linked into meandering chains (PO₃)_n spreading parallel to the b axis with a repeat unit of four tetrahedra. The calculated bond-valence sum value of one of the two Ag^I ions indicates a significant strain of the structure.

Related literature

For a previous crystallographic study of AgPO₃, see: Jost (1961). For the isotypic A-form of the Kurrol salt NaPO₃, see: McAdam et al. (1968). Properties of glassy silver phosphates have been reported by Portier et al. (1990) and Novita et al. (2009). For long-chain polyphosphates AgM^III(PO₃)₄ (M^III = La, Gd, Eu), see: El Masloumi et al. (2005); Naili et al. (2006); Ayadi et al. (2009). For AgM^II (PO₃)₃ (M^II = Mg, Zn, Ba), see: Belharouak et al. (1999); for AgM^I(PO₃)₂ (M^I = K, Rb, Cs, Tl), see: Averbuch-Pouchot (1993). For background to the bond-valence method, see: Brown & Altermatt (1985).

Experimental

Crystal data

AgPO₃
M_r = 186.84
Monoclinic, P 2₁ /n
a = 11.9335 (3) Å
b = 6.0667 (1) Å
c = 7.3278 (2) Å
= 93.491 (2)°
V = 529.53 (2) Å³
Z = 8
Mo K radiation
= 7.96 mm^-1
T = 293 K
0.10 × 0.08 × 0.04 mm

Data collection

Oxford Diffraction Xcalibur-3 CCD diffractometer
Absorption correction: multi-scan (Blessing, 1995) T_min = 0.465, T_max = 0.733
22720 measured reflections
2333 independent reflections
2208 reflections with I > 2(I)
R_int = 0.042

Refinement

R[F² > 2(F²)] = 0.024
wR(F²) = 0.058
S = 1.08
2333 reflections
92 parameters
_max = 1.43 e Å^-3
_min = -1.86 e Å^-3

Table 1
Selected geometric parameters (Å, °)

Ag1-O3ⁱ	2.441 (2)
Ag1-O1	2.460 (2)
Ag1-O6ⁱⁱ	2.491 (2)
Ag1-O1ⁱⁱⁱ	2.511 (2)
Ag1-O6	2.540 (2)
Ag2-O5^iv	2.3708 (19)
Ag2-O5^v	2.3756 (19)
Ag2-O3	2.3968 (19)
Ag2-O6ⁱⁱ	2.487 (2)
Ag2-O3^iv	2.750 (2)
P1-O1	1.490 (2)
P1-O3	1.4952 (19)
P1-O4^vi	1.5889 (17)
P1-O2	1.6033 (17)
P2-O5	1.479 (2)
P2-O6	1.4924 (19)
P2-O4	1.5909 (17)
P2-O2	1.6074 (18)

P1-O2-P2	124.88 (11)
P1^vii-O4-P2	135.91 (11)
Symmetry codes: (i) x, y-1, z; (ii) -x, -y+1, -z+1; (iii) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (iv) -x, -y+2, -z+1; (v) x, y, z+1; (vi) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (vii) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

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).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2454 ).

References

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Ayadi, M., Férid, M. & Moine, B. (2009). Acta Cryst. E65, i13.
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Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
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Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.
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inorganic compounds