catena-Poly[[(3,5-dicarb-oxy-pyrazine-2,6-dicarboxyl-ato-κO,N,O)lithium(I)]-μ-aqua-[triaqua-lithium(I)]-μ-aqua].

The title coordination polymer, [Li(2)(C(8)H(2)N(2)O(8))(H(2)O)(5)](n) contains two symmetry-independent Li(+) ions; one is coordin-ated by five water O atoms, the other by an O,N,O'-tridentate doubly deprotonated pyrazine-2,3,5,6-tetra-carboxyl-ate ligand and two water O atoms. Water mol-ecules bridge adjacent Li(+) ions into ribbons propagating in [100]; an alternative analysis of the structure considers it to contain alternating [Li(C(8)H(2)N(2)O(8))(H(2)O)(2)](-) anions and [Li(H(2)O)(3)](+) cations. In the polymeric model, both lithium ions show distorted trigonal-bipyramidal coordination geometries. Within the ligand, the carboxyl H atoms participate in short, almost symmetric O⋯H⋯O hydrogen bonds in which the non-coordinated carboxyl-ate O atoms are donors and acceptors. In the crystal, the ribbons inter-act via a network of O-H⋯O hydrogen bonds in which the coordinated water mol-ecules act as donors and ligand carboxyl-ate O atoms as acceptors.

Related literature

For the crystal structures of 3d transition metal complexes with pyrazine-2,3,5,6-tetra­carboxyl­ate and water ligands, see: Alfonso et al. (2001 ▶); Graf et al. (1993 ▶); Marioni et al. (1986 ▶); Marioni et al. (1994 ▶). For the structure of a Ca(II) complex, see: Starosta & Leciejewicz (2008 ▶). For the structure of a Li complex with pyrazine-2,3-dicarboxyl­ate and water ligands, see: Tombul et al. (2008 ▶). For a review on metal organic frameworks (MOFs), see: MacGillivray (2010 ▶).

Experimental

Crystal data

[Li2(C8H2N2O8)(H2O)5]

M = 358.08

Monoclinic,

a = 6.8806 (14) Å

b = 11.767 (2) Å

c = 8.8082 (18) Å

β = 103.59 (3)°

V = 693.2 (2) Å3

Z = 2

Mo Kα radiation

μ = 0.16 mm−1

T = 293 K

0.23 × 0.21 × 0.17 mm

Data collection

Kuma KM-4 four-circle diffractometer

Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008) ▶ T min = 0.971, T max = 0.975

2291 measured reflections

2136 independent reflections

1459 reflections with I > 2σ(I)

R int = 0.012

3 standard reflections every 200 reflections intensity decay: 0.5%

Refinement

R[F 2 > 2σ(F 2)] = 0.039

wR(F 2) = 0.127

S = 1.03

2136 reflections

148 parameters

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.42 e Å−3

Δρmin = −0.32 e Å−3

Data collection: KM-4 Software (Kuma, 1996 ▶); cell refinement: KM-4 Software; data reduction: DATAPROC (Kuma, 2001 ▶); 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.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810045903/hb5710sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810045903/hb5710Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Li2(C8H2N2O8)(H2O)5]	F(000) = 368
Mr = 358.08	Dx = 1.716 Mg m−3
Monoclinic, P21/m	Mo Kα radiation, λ = 0.71073 Å
a = 6.8806 (14) Å	Cell parameters from 25 reflections
b = 11.767 (2) Å	θ = 6–15°
c = 8.8082 (18) Å	µ = 0.16 mm−1
β = 103.59 (3)°	T = 293 K
V = 693.2 (2) Å3	Blocks, colourless
Z = 2	0.23 × 0.21 × 0.17 mm

Kuma KM-4 four-circle diffractometer	1459 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.012
graphite	θmax = 30.1°, θmin = 2.4°
profile data from ω/2θ scans	h = 0→9
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008)	k = 0→16
Tmin = 0.971, Tmax = 0.975	l = −12→12
2291 measured reflections	3 standard reflections every 200 reflections
2136 independent reflections	intensity decay: 0.5%

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.039	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.127	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	w = 1/[σ2(Fo2) + (0.0886P)2 + 0.040P] where P = (Fo2 + 2Fc2)/3
2136 reflections	(Δ/σ)max < 0.001
148 parameters	Δρmax = 0.42 e Å−3
0 restraints	Δρmin = −0.32 e Å−3

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

	x	y	z	Uiso*/Ueq
N1	0.4556 (2)	0.7500	0.72520 (15)	0.0184 (3)
N2	0.1994 (2)	0.7500	0.44032 (15)	0.0197 (3)
O4	0.61711 (14)	0.92277 (7)	0.87982 (11)	0.0287 (2)
O2	0.06363 (16)	0.93417 (8)	0.28320 (11)	0.0354 (3)
O1	0.21919 (16)	1.05057 (7)	0.46536 (10)	0.0315 (3)
O3	0.44557 (15)	1.04935 (7)	0.71677 (11)	0.0296 (2)
C5	0.49353 (17)	0.94719 (9)	0.76029 (13)	0.0207 (2)
C3	0.26124 (16)	0.84858 (8)	0.50943 (12)	0.0178 (2)
C2	0.39451 (16)	0.84873 (8)	0.65765 (12)	0.0176 (2)
C6	0.17301 (17)	0.95080 (10)	0.41030 (13)	0.0220 (2)
O6	0.16203 (15)	0.91197 (8)	0.92116 (12)	0.0334 (3)
O8	0.9298 (2)	0.7500	1.09008 (14)	0.0276 (3)
O7	0.4555 (2)	0.7500	1.09036 (16)	0.0338 (3)
O5	−0.0754 (3)	0.7500	0.72326 (19)	0.0438 (4)
Li2	0.1189 (6)	0.7500	0.9392 (4)	0.0332 (7)
Li1	0.6568 (5)	0.7500	0.9480 (4)	0.0347 (7)
H61	0.071 (3)	0.9536 (18)	0.853 (2)	0.051 (6)*
H62	0.230 (4)	0.962 (2)	0.992 (3)	0.079 (8)*
H81	0.976 (3)	0.8072 (17)	1.148 (2)	0.054 (6)*
H71	0.484 (3)	0.8066 (16)	1.154 (2)	0.044 (5)*
H51	−0.125 (3)	0.8094 (16)	0.661 (2)	0.044 (5)*
H32	0.336 (3)	1.055 (2)	0.588 (2)	0.061 (7)*

	U11	U22	U33	U12	U13	U23
N1	0.0231 (6)	0.0119 (5)	0.0173 (5)	0.000	−0.0007 (5)	0.000
N2	0.0242 (7)	0.0148 (6)	0.0177 (6)	0.000	0.0002 (5)	0.000
O4	0.0329 (5)	0.0198 (4)	0.0261 (4)	−0.0035 (3)	−0.0079 (4)	−0.0019 (3)
O2	0.0486 (6)	0.0218 (4)	0.0254 (4)	0.0038 (4)	−0.0124 (4)	0.0033 (3)
O1	0.0485 (6)	0.0135 (4)	0.0257 (4)	0.0029 (4)	−0.0046 (4)	0.0017 (3)
O3	0.0409 (5)	0.0126 (4)	0.0290 (4)	−0.0016 (3)	−0.0047 (4)	−0.0019 (3)
C5	0.0244 (5)	0.0145 (5)	0.0211 (5)	−0.0031 (4)	0.0008 (4)	−0.0018 (4)
C3	0.0220 (5)	0.0130 (5)	0.0166 (4)	0.0011 (4)	0.0011 (4)	0.0014 (4)
C2	0.0212 (5)	0.0130 (4)	0.0168 (4)	−0.0008 (4)	0.0010 (4)	−0.0005 (3)
C6	0.0282 (6)	0.0155 (5)	0.0201 (5)	0.0029 (4)	0.0011 (4)	0.0033 (4)
O6	0.0373 (5)	0.0181 (4)	0.0354 (5)	−0.0004 (4)	−0.0104 (4)	0.0004 (4)
O8	0.0340 (7)	0.0225 (6)	0.0212 (6)	0.000	−0.0037 (5)	0.000
O7	0.0486 (9)	0.0199 (6)	0.0288 (6)	0.000	0.0005 (6)	0.000
O5	0.0585 (10)	0.0214 (7)	0.0379 (8)	0.000	−0.0160 (7)	0.000
Li2	0.0433 (18)	0.0236 (15)	0.0341 (16)	0.000	0.0117 (14)	0.000
Li1	0.0393 (17)	0.0264 (15)	0.0295 (15)	0.000	−0.0099 (13)	0.000

Li1—N1	2.119 (4)	N2—C3i	1.3324 (12)
Li1—O4	2.1194 (13)	O4—C5	1.2221 (15)
Li1—O8	1.997 (4)	O2—C6	1.2091 (15)
Li1—O7	2.075 (5)	O1—C6	1.2815 (15)
Li1—O4i	2.1194 (13)	O1—H32	1.19 (2)
Li2—O6	1.9412 (12)	O3—C5	1.2811 (14)
Li2—O7	2.385 (4)	O3—H32	1.21 (2)
Li2—O5	2.052 (4)	C5—C2	1.5279 (15)
Li2—O6i	1.9412 (12)	C3—C2	1.4081 (15)
Li2—O8ii	2.067 (4)	C3—C6	1.5260 (14)
Li2—Li1ii	3.199 (5)	O6—H61	0.90 (2)
Li1—Li2iii	3.199 (5)	O6—H62	0.91 (3)
O8—Li2iii	2.067 (4)	O8—H81	0.86 (2)
N1—C2i	1.3277 (12)	O7—H71	0.862 (19)
N1—C2	1.3277 (12)	O5—H51	0.903 (19)
N2—C3	1.3324 (12)
C2i—N1—C2	122.10 (13)	O6—Li2—O5	90.18 (11)
C2i—N1—Li1	118.95 (6)	O6i—Li2—O5	90.18 (11)
C2—N1—Li1	118.95 (6)	O6—Li2—O8ii	100.61 (11)
C3—N2—C3i	121.05 (13)	O6i—Li2—O8ii	100.61 (11)
C5—O4—Li1	119.15 (11)	O5—Li2—O8ii	102.98 (18)
C6—O1—H32	116.2 (12)	O6—Li2—O7	84.17 (12)
C5—O3—H32	113.3 (11)	O6i—Li2—O7	84.17 (12)
O4—C5—O3	123.82 (10)	O5—Li2—O7	148.57 (19)
O4—C5—C2	117.04 (10)	O8ii—Li2—O7	108.45 (15)
O3—C5—C2	119.13 (9)	O6—Li2—Li1ii	100.02 (12)
N2—C3—C2	119.55 (9)	O6i—Li2—Li1ii	100.02 (12)
N2—C3—C6	112.55 (9)	O5—Li2—Li1ii	65.66 (13)
C2—C3—C6	127.91 (9)	O8ii—Li2—Li1ii	37.32 (10)
N1—C2—C3	118.88 (9)	O7—Li2—Li1ii	145.77 (15)
N1—C2—C5	110.38 (9)	O8—Li1—O7	106.53 (16)
C3—C2—C5	130.71 (9)	O8—Li1—O4i	102.54 (10)
O2—C6—O1	122.94 (11)	O7—Li1—O4i	96.41 (12)
O2—C6—C3	118.66 (10)	O8—Li1—O4	102.54 (10)
O1—C6—C3	118.40 (9)	O7—Li1—O4	96.40 (12)
Li2—O6—H61	119.4 (14)	O4i—Li1—O4	147.18 (17)
Li2—O6—H62	130.5 (17)	O8—Li1—N1	153.3 (2)
H61—O6—H62	106 (2)	O7—Li1—N1	100.14 (17)
Li1—O8—Li2iii	103.81 (16)	O4i—Li1—N1	74.03 (9)
Li1—O8—H81	122.3 (13)	O4—Li1—N1	74.03 (9)
Li2iii—O8—H81	100.2 (14)	O8—Li1—Li2iii	38.87 (10)
Li1—O7—Li2	111.17 (14)	O7—Li1—Li2iii	145.40 (16)
Li1—O7—H71	107.9 (13)	O4i—Li1—Li2iii	93.19 (12)
Li2—O7—H71	114.0 (13)	O4—Li1—Li2iii	93.19 (12)
Li2—O5—H51	129.1 (12)	N1—Li1—Li2iii	114.46 (17)
O6—Li2—O6i	158.1 (2)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H61···O2iv	0.90 (2)	1.87 (2)	2.7597 (14)	165.4 (19)
O6—H62···O4v	0.91 (3)	1.91 (3)	2.8129 (14)	173 (2)
O8—H81···O2vi	0.86 (2)	1.92 (2)	2.7753 (13)	175.9 (19)
O7—H71···O3v	0.862 (19)	2.037 (19)	2.8950 (12)	173.8 (17)
O5—H51···O1iv	0.903 (19)	2.010 (19)	2.9110 (13)	175.4 (17)
O1—H32···O3	1.19 (2)	1.21 (2)	2.3894 (15)	173 (2)

Table 1

Selected bond lengths (Å)

Li1—N1	2.119 (4)
Li1—O4	2.1194 (13)
Li1—O8	1.997 (4)
Li1—O7	2.075 (5)
Li1—O4i	2.1194 (13)
Li2—O6	1.9412 (12)
Li2—O7	2.385 (4)
Li2—O5	2.052 (4)
Li2—O6i	1.9412 (12)
Li2—O8ii	2.067 (4)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O6—H61⋯O2iii	0.90 (2)	1.87 (2)	2.7597 (14)	165.4 (19)
O6—H62⋯O4iv	0.91 (3)	1.91 (3)	2.8129 (14)	173 (2)
O8—H81⋯O2v	0.86 (2)	1.92 (2)	2.7753 (13)	175.9 (19)
O7—H71⋯O3iv	0.862 (19)	2.037 (19)	2.8950 (12)	173.8 (17)
O5—H51⋯O1iii	0.903 (19)	2.010 (19)	2.9110 (13)	175.4 (17)
O1—H32⋯O3	1.19 (2)	1.21 (2)	2.3894 (15)	173 (2)

Symmetry codes: (iii) ; (iv) ; (v) .