Poly[[[μ3-(E)-N-(pyridin-4-yl­methyl­idene)hy­droxy­laminato-κ3O:N:N′][μ2-(E)-N-(pyridin-4-yl­methyl­idene)hydroxyl­amine-κ2N:N′][(E)-N-(pyridin-4-yl­methyl­idene-κN)hydroxyl­amine]­disilver(I)] nitrate]

Gao, S.; Ng, S.W.

doi:10.1107/S1600536812046090

Volume 68
Part 12
Pages m1540-m1541
December 2012

Received 4 November 2012
Accepted 7 November 2012
Online 28 November 2012

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.006 Å
Disorder in solvent or counterion
R = 0.042
wR = 0.119
Data-to-parameter ratio = 16.5
Details

Poly[[[₃-(E)-N-(pyridin-4-ylmethylidene)hydroxylaminato-³O:N:N'][₂-(E)-N-(pyridin-4-ylmethylidene)hydroxylamine-²N:N'][(E)-N-(pyridin-4-ylmethylidene-N)hydroxylamine]disilver(I)] nitrate]

Shan Gao ^a and Seik Weng Ng ^b,^c ^*

^aKey Laboratory of Functional Inorganic Material Chemistry, Ministry of Education, Heilongjiang University, Harbin 150080, People's Republic of China,^bDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia, and ^cChemistry Department, Faculty of Science, King Abdulaziz University, PO Box 80203 Jeddah, Saudi Arabia
Correspondence e-mail: seikweng@um.edu.my

The title coordination polymer, {[Ag₂(C₆H₅N₂O)(C₆H₆N₂O)₂]NO₃}_n, features a deprotonated N-(pyridin-4-ylmethylidene)hydroxylaminate anion and two neutral N-(pyridin-4-ylmethylidene)hydroxylamine molecules in the asymmetric unit. The anion connects three Ag^I atoms through its O and two N-donor atoms. One neutral ligand functions in a monodentate mode; the other functions in a bridging mode, binding though its two N atoms. The coordination geometry of the two independent metal atoms is T-shaped; the manner of bridging gives rise to a layer motif parallel to (100). In the crystal, the nitrate ion is disordered over two positions in a 1:1 ratio, and is sandwiched between adjacent layers. O-HO hydrogen bonding is present between nitrate ions and layers, and also between adjacent layers.

Related literature

For mononuclear (Nitrato- [kappa] ²O,O')bis[(E)-N-(pyridin-4-ylmethylidene- [kappa] N)hydroxyamine]silver(I), see: Gao & Ng (2012).

Experimental

Crystal data

[Ag₂(C₆H₅N₂O)(C₆H₆N₂O)₂]NO₃
M_r = 643.13
Monoclinic, P 2₁ /c
a = 13.1628 (18) Å
b = 10.9926 (18) Å
c = 16.315 (2) Å
= 110.412 (4)°
V = 2212.4 (6) Å³
Z = 4
Mo K radiation
= 1.82 mm^-1
T = 293 K
0.20 × 0.12 × 0.12 mm

Data collection

Rigaku R-AXIS RAPID IP diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) T_min = 0.712, T_max = 0.811
21226 measured reflections
5047 independent reflections
3355 reflections with I > 2(I)
R_int = 0.047

Refinement

R[F² > 2(F²)] = 0.042
wR(F²) = 0.119
S = 1.07
5047 reflections
306 parameters
26 restraints
H-atom parameters constrained
_max = 0.77 e Å^-3
_min = -0.43 e Å^-3

Table 1
Selected bond lengths (Å)

Ag1-O1	2.612 (3)
Ag1-N3	2.151 (3)
Ag1-N5	2.158 (3)
Ag2-O1ⁱ	2.546 (2)
Ag2-N1	2.161 (3)
Ag2-N2ⁱⁱ	2.183 (3)
Symmetry codes: (i) $[x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (ii) $[-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O2-H2O4	0.84	1.81	2.642 (9)	169
O2-H2O4'	0.84	2.21	2.997 (14)	156
O3-H3O1ⁱⁱⁱ	0.84	1.69	2.527 (4)	174
Symmetry code: (iii) $[x, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ .

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalClear (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: XU5648 ).

Acknowledgements

We thank the Key Project of the Natural Science Foundation of Heilongjiang Province (No. ZD200903), the Key Project of the Education Bureau of Heilongjiang Province (Nos. 12511z023 and 2011CJHB006), the Innovation Team of the Education Bureau of Heilongjiang Province (No. 2010 t d03), Heilongjiang University (Hdtd2010-04) and the Ministry of Higher Education of Malaysia (grant No. UM.C/HIR/MOHE/SC/12) for supporting this study.

References

Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.
Gao, S. & Ng, S. W. (2012). Acta Cryst. E68, m1542.
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Rigaku (1998). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.
Rigaku/MSC (2002). CrystalClear. Rigaku/MSC Inc., The Woodlands, Texas, USA.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.

metal-organic compounds

Poly[[[3-(E)-N-(pyridin-4-ylmethylidene)hydroxylaminato-3O:N:N'][2-(E)-N-(pyridin-4-ylmethylidene)hydroxylamine-2N:N'][(E)-N-(pyridin-4-ylmethylidene-N)hydroxylamine]disilver(I)] nitrate]