catena-Poly[[tetra­aqua-μ-aqua-bis­(μ4-pyrimidine-2-carboxyl­ato)tetra­lithium] dichloride]

Starosta, W.; Leciejewicz, J.

doi:10.1107/S1600536812041955

Volume 68
Part 11
Pages m1369-m1370
November 2012

Received 27 September 2012
Accepted 7 October 2012
Online 20 October 2012

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.003 Å
R = 0.044
wR = 0.147
Data-to-parameter ratio = 18.5
Details

catena-Poly[[tetraaqua--aqua-bis(₄-pyrimidine-2-carboxylato)tetralithium] dichloride]

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, [Li₄(C₅H₃N₂O₂)₂(H₂O)₅]Cl₂, contains two Li^I cations, one with a distorted trigonal-bipyramidal and the other with a distorted tetrahedral coordination geometry. Two symmetry-related asymmetric units constitute a building block of the structure, in which both ligand carboxylate O atoms are bidentate and bridge the metal ions, forming a divalent cation. Charge balance is maintained by two chloride anions. The building blocks, bridged by Li^I cations, form cationic ribbons with chloride anions in the space between them. The ribbons propagate in [010] and are held together by a network of weak O-HO hydrogen bonds which operate in the space between adjacent ribbons.

Related literature

For the structure of a Li complex with pyrimidine-2-carboxylate and nitrate ligands, see: Starosta & Leciejewicz (2011). The structure of a Li^I complex with pyrimidine-4-carboxylate and water ligands was reported recently by Starosta & Leciejewicz (2012).

Experimental

Crystal data

[Li₄(C₅H₃N₂O₂)₂(H₂O)₅]Cl₂
M_r = 434.93
Monoclinic, C 2/c
a = 22.084 (4) Å
b = 8.0773 (16) Å
c = 10.814 (2) Å
= 94.08 (3)°
V = 1924.1 (7) Å³
Z = 4
Mo K radiation
= 0.39 mm^-1
T = 293 K
0.37 × 0.24 × 0.18 mm

Data collection

Kuma KM4 four-circle diffractometer
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008 $[Oxford Diffraction (2008). CrysAlis RED. Oxford Diffraction Ltd., Yarnton, England.]$ ) T_min = 0.917, T_max = 0.935
2964 measured reflections
2819 independent reflections
1781 reflections with I > 2(I)
R_int = 0.029
3 standard reflections every 200 reflections intensity decay: 2.3%

Refinement

R[F² > 2(F²)] = 0.044
wR(F²) = 0.147
S = 1.02
2819 reflections
152 parameters
4 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 0.51 e Å^-3
_min = -0.36 e Å^-3

Table 1
Selected bond lengths (Å)

Li1-O1	2.069 (3)
Li1-N1	2.175 (4)
Li1-O3	1.987 (4)
Li1-O2ⁱ	2.029 (4)
Li1-N3ⁱ	2.221 (4)
Li2-O21	2.140 (6)
Li2-O22	1.915 (4)
Li2-O2ⁱⁱ	1.968 (4)
Li2-O1	1.993 (4)
Symmetry codes: (i) $[x, -y+2, z+{\script{1\over 2}}]$ ; (ii) $[-x, y, -z+{\script{1\over 2}}]$ .

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O22-H222O3	0.89 (2)	2.16 (3)	2.841 (3)	133 (3)
O22-H221Cl1ⁱⁱⁱ	0.87 (2)	2.36 (2)	3.212 (2)	167 (3)
O3-H31Cl1	0.83 (4)	2.35 (4)	3.1381 (19)	158 (3)
O3-H32Cl1^iv	0.86 (4)	2.29 (4)	3.1429 (19)	168 (4)
O21-H211Cl1^v	0.84 (3)	2.45 (3)	3.288 (2)	175 (3)
Symmetry codes: (iii) $[-x, y, -z+{\script{3\over 2}}]$ ; (iv) $[x, -y+1, z-{\script{1\over 2}}]$ ; (v) -x, -y+1, -z+1.

Data collection: KM-4 Software (Kuma, 1996 $[Kuma (1996). KM-4 Software. Kuma Diffraction Ltd. Wroclaw, Poland.]$ ); cell refinement: KM-4 Software; data reduction: DATAPROC (Kuma, 2001 $[Kuma (2001). DATAPROC. Kuma Diffraction Ltd. Wroclaw, Poland.]$ ); 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: QM2084 ).

References

Kuma (1996). KM-4 Software. Kuma Diffraction Ltd. Wroclaw, Poland.
Kuma (2001). DATAPROC. Kuma Diffraction Ltd. Wroclaw, Poland.
Oxford Diffraction (2008). CrysAlis RED. Oxford Diffraction Ltd., Yarnton, England.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Starosta, W. & Leciejewicz, J. (2011). Acta Cryst. E67, m818.
Starosta, W. & Leciejewicz, J. (2012). Acta Cryst. E68, m1065-m1066.

metal-organic compounds

catena-Poly[[tetraaqua--aqua-bis(4-pyrimidine-2-carboxylato)tetralithium] dichloride]