Poly[di-μ2-aqua-μ2-(5-methyl­pyrazine-2-carboxyl­ato)-(5-methyl­pyrazine-2-carboxyl­ato)-μ3-nitrato-trilithium]

Starosta, W.; Leciejewicz, J.

doi:10.1107/S1600536811024548

Volume 67
Part 7
Pages m1000-m1001
July 2011

Received 10 June 2011
Accepted 22 June 2011
Online 30 June 2011

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.002 Å
R = 0.040
wR = 0.122
Data-to-parameter ratio = 11.6
Details

Poly[di-₂-aqua-₂-(5-methylpyrazine-2-carboxylato)-(5-methylpyrazine-2-carboxylato)-₃-nitrato-trilithium]

Wojciech Starosta ^a and Janusz Leciejewicz ^a ^*

^aInstitute of Nuclear Chemistry and Technology, ul.Dorodna 16, 03-195 Warszawa, Poland
Correspondence e-mail: j.leciejewicz@ichtj.waw.pl

The asymmetric unit of the title compound, [Li₃(C₆H₅N₂O₂)₂(NO₃)(H₂O)₂]_n contains three Li^I ions, two ligand anions, two water molecules and a nitrate anion. Related by a centre of inversion, they form a centrosymmetric molecular cluster in which one of the Li^I ions shows trigonal-bipyramidal and the other two distorted tetrahedral coordination. Li^I ions are bridged by water O atoms and carboxylate O atoms donated by one of the ligands. The clusters, bridged by two nitrato O atoms, form molecular columns along [010], which are held together by O-HO and O-HN hydrogen bonds and [pi] - [pi] interactions [centroid-centroid distances = 3.694 (1) and 3.796 (1) Å].

Related literature

For the structure of a lithium complex with 3-aminopyrazine-2-carboxylate and aqua ligands, see: Starosta & Leciejewicz (2010). The structures of two complexes with pyridazine carboxylate ligands have been also determined, see: Starosta & Leciejewicz (2011a,b). For the structure of a Li^I complex with pyrimidine carboxylate and nitrate ligands, see: Starosta & Leciejewicz (2011c).

Experimental

Crystal data

[Li₃(C₆H₅N₂O₂)₂(NO₃)(H₂O)₂]
M_r = 393.10
Monoclinic, P 2₁ /c
a = 13.0222 (1) Å
b = 7.2288 (1) Å
c = 18.5819 (2) Å
= 100.760 (1)°
V = 1718.45 (3) Å³
Z = 4
Cu K radiation
= 1.10 mm^-1
T = 293 K
0.23 × 0.20 × 0.07 mm

Data collection

Oxford Diffraction Xcalibur Ruby diffractometer
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2010 $[Oxford Diffraction (2010). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.]$ ) T_min = 0.672, T_max = 1.000
15696 measured reflections
3215 independent reflections
2787 reflections with I > 2(I)
R_int = 0.026

Refinement

R[F² > 2(F²)] = 0.040
wR(F²) = 0.122
S = 1.07
3215 reflections
277 parameters
H atoms treated by a mixture of independent and constrained refinement
_max = 0.35 e Å^-3
_min = -0.31 e Å^-3

Table 1
Selected bond lengths (Å)

Li1-O11ⁱ	2.029 (3)
Li1-O11	2.039 (3)
Li1-O1	2.085 (3)
Li1-O4	2.114 (3)
Li1-N11	2.293 (3)
Li2-O12ⁱ	1.958 (3)
Li2-O4	1.965 (3)
Li2-O5	1.970 (3)
Li2-O2ⁱⁱ	2.163 (3)
Li3-O31	1.978 (3)
Li3-O5	2.025 (4)
Li3-O1	2.039 (3)
Li3-N31	2.117 (3)
Symmetry codes: (i) -x+2, -y, -z+2; (ii) x, y-1, z.

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O4-H41O32ⁱⁱⁱ	0.85 (2)	1.92 (2)	2.7449 (15)	165.3 (19)
O4-H42N12^iv	0.85 (2)	2.03 (2)	2.8414 (17)	159.0 (19)
O5-H52N32^v	0.84 (2)	2.05 (2)	2.8550 (17)	162 (2)
O5-H51O31ⁱⁱⁱ	0.86 (2)	1.85 (2)	2.7055 (15)	172 (2)
Symmetry codes: (iii) -x+1, -y, -z+2; (iv) $[-x+2, y-{\script{1\over 2}}, -z+{\script{5\over 2}}]$ ; (v) $[-x+1, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ .

Data collection: CrysAlis PRO (Oxford Diffraction, 2010 $[Oxford Diffraction (2010). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.]$ ); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: KP2334 ).

Acknowledgements

Thanks are due to Dr J. K. Maurin for collecting the diffraction data on the instrument at the Institute of Atomic Energy, Swierk.

References

Oxford Diffraction (2010). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Starosta, W. & Leciejewicz, J. (2010). Acta Cryst. E66, m744-m745.
Starosta, W. & Leciejewicz, J. (2011a). Acta Cryst. E67, m202.
Starosta, W. & Leciejewicz, J. (2011b). Acta Cryst. E67, m425-m426.
Starosta, W. & Leciejewicz, J. (2011c). Acta Cryst. E67, m818.

metal-organic compounds

Poly[di-2-aqua-2-(5-methylpyrazine-2-carboxylato)-(5-methylpyrazine-2-carboxylato)-3-nitrato-trilithium]