Poly[aqua-(μ-pyrazine-2-carboxyl-ato-κN,O:O)(μ-pyrazine-2-carboxyl-ato-κN,O:O')lead(II)].

The polymeric structure of the title compound, [Pb(C(5)H(3)N(2)O(2))(2)(H(2)O)](n), is built up from centrosymmetric [Pb(C(5)H(3)N(2)O(2))(2)(H(2)O)](2) dimers, which are bridged by ligand carboxyl-ate O atoms. The Pb(II) ion adopts an irregular PbN(2)O(5) coordination polyhedron; it is chelated by one N,O-bidentate ligand and also bonds to a water O atom. A second N,O-bidentate ligand forms the dimer bridge and another bridging O atom from a nearby dimer also bonds to the Pb(II) ion, leading to layers propagating in (100). A network of O-H⋯O hydrogen bonds operates between water O atoms (donors) and carboxyl-ate O atoms (acceptors).

Related literature

For the crystal structures of divalent metal ions with pyrazine-2-carboxyl­ate and water ligands, see, for example: Alcock et al. (1996 ▶); Ptasiewicz-Bąk et al. (1995 ▶, 1998 ▶). The structures of lead(II) complexes with pyrazine-4-carboxyl­ate (Starosta & Leciejewicz, 2009 ▶) and pyrazine-3-carboxyl­ate ligands (Starosta & Leciejewicz, 2010 ▶) have also been reported.

Experimental

Crystal data

[Pb(C5H3N2O2)2(H2O)]

M = 471.39

Monoclinic,

a = 11.098 (2) Å

b = 10.382 (2) Å

c = 11.678 (2) Å

β = 114.13 (3)°

V = 1228.0 (4) Å3

Z = 4

Mo Kα radiation

μ = 13.77 mm−1

T = 293 K

0.29 × 0.16 × 0.12 mm

Data collection

Kuma KM-4 four-circle diffractometer

Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008 ▶) T min = 0.135, T max = 0.251

3579 measured reflections

3411 independent reflections

2230 reflections with I > 2σ(I)

R int = 0.051

3 standard reflections every 200 reflections intensity decay: 20.2%

Refinement

R[F 2 > 2σ(F 2)] = 0.058

wR(F 2) = 0.163

S = 1.02

3411 reflections

188 parameters

5 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 6.45 e Å−3

Δρmin = −5.86 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: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810013188/hb5383sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810013188/hb5383Isup2.hkl

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

[Pb(C5H3N2O2)2(H2O)]	F(000) = 872
Mr = 471.39	Dx = 2.550 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 25 reflections
a = 11.098 (2) Å	θ = 6–15°
b = 10.382 (2) Å	µ = 13.77 mm−1
c = 11.678 (2) Å	T = 293 K
β = 114.13 (3)°	Blocks, colourless
V = 1228.0 (4) Å3	0.29 × 0.16 × 0.12 mm
Z = 4

Kuma KM-4 four-circle diffractometer	2230 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.051
graphite	θmax = 30.1°, θmin = 2.0°
profile data from ω/2θ scans	h = 0→14
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008)	k = −14→0
Tmin = 0.135, Tmax = 0.251	l = −15→14
3579 measured reflections	3 standard reflections every 200 reflections
3411 independent reflections	intensity decay: 20.2%

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.058	H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.163	w = 1/[σ2(Fo2) + (0.1217P)2] where P = (Fo2 + 2Fc2)/3
S = 1.02	(Δ/σ)max < 0.001
3411 reflections	Δρmax = 6.45 e Å−3
188 parameters	Δρmin = −5.86 e Å−3
5 restraints	Extinction correction: SHELXTL (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0154 (12)

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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
Pb1	0.47863 (3)	0.12876 (4)	0.35712 (3)	0.02848 (19)
O11	0.3570 (7)	−0.0031 (8)	0.4636 (8)	0.0413 (18)
C22	0.6620 (9)	0.3784 (10)	0.5171 (10)	0.034 (2)
O21	0.4811 (9)	0.2586 (8)	0.5220 (8)	0.0399 (18)
N21	0.6655 (8)	0.2972 (9)	0.4344 (8)	0.0327 (18)
C12	0.1581 (9)	0.1152 (9)	0.3625 (10)	0.0299 (19)
C13	0.0296 (11)	0.1383 (11)	0.3473 (11)	0.039 (2)
H13	−0.0039	0.0957	0.3980	0.047*
C27	0.5599 (12)	0.3532 (11)	0.5717 (12)	0.040 (2)
N22	0.8312 (12)	0.5089 (11)	0.5106 (13)	0.059 (3)
C26	0.7546 (11)	0.3203 (12)	0.3893 (12)	0.039 (2)
H26	0.7616	0.2642	0.3303	0.047*
N11	0.2083 (9)	0.1695 (10)	0.2906 (9)	0.0362 (19)
C16	0.1307 (12)	0.2491 (12)	0.2013 (12)	0.045 (3)
H16	0.1628	0.2889	0.1481	0.054*
C23	0.7440 (13)	0.4853 (12)	0.5559 (14)	0.050 (3)
H23	0.7365	0.5409	0.6151	0.060*
O1	0.4080 (11)	0.3287 (10)	0.2149 (9)	0.056 (2)
H1	0.378 (11)	0.402 (7)	0.218 (10)	0.084*
H2	0.385 (8)	0.312 (13)	0.138 (3)	0.084*
O12	0.2045 (8)	−0.0170 (9)	0.5394 (8)	0.0445 (19)
C17	0.2455 (9)	0.0251 (9)	0.4646 (9)	0.0275 (18)
N12	−0.0479 (10)	0.2225 (11)	0.2591 (11)	0.050 (3)
C15	0.0023 (12)	0.2730 (13)	0.1871 (12)	0.047 (3)
H15	−0.0500	0.3278	0.1230	0.056*
C25	0.8376 (14)	0.4253 (14)	0.4272 (15)	0.055 (3)
H25	0.8995	0.4379	0.3935	0.066*
O22	0.5643 (12)	0.4168 (10)	0.6610 (9)	0.054 (2)

	U11	U22	U33	U12	U13	U23
Pb1	0.0271 (2)	0.0296 (2)	0.0327 (3)	0.00255 (14)	0.01621 (15)	0.00445 (14)
O11	0.024 (3)	0.044 (4)	0.060 (5)	0.005 (3)	0.020 (3)	0.021 (4)
C22	0.019 (4)	0.039 (5)	0.041 (5)	−0.002 (4)	0.010 (4)	0.008 (4)
O21	0.045 (4)	0.035 (4)	0.058 (5)	−0.011 (3)	0.040 (4)	−0.012 (3)
N21	0.024 (4)	0.044 (5)	0.038 (5)	−0.005 (4)	0.021 (3)	−0.002 (4)
C12	0.018 (4)	0.035 (5)	0.038 (5)	−0.002 (3)	0.012 (3)	−0.003 (4)
C13	0.031 (5)	0.048 (7)	0.041 (6)	0.009 (4)	0.019 (4)	−0.001 (4)
C27	0.038 (6)	0.039 (6)	0.047 (6)	−0.005 (4)	0.020 (5)	−0.001 (4)
N22	0.048 (6)	0.050 (6)	0.091 (9)	−0.021 (5)	0.042 (6)	−0.007 (6)
C26	0.034 (5)	0.050 (6)	0.050 (6)	−0.004 (5)	0.032 (5)	−0.003 (5)
N11	0.027 (4)	0.043 (5)	0.040 (5)	0.001 (4)	0.016 (4)	0.009 (4)
C16	0.039 (7)	0.046 (6)	0.051 (7)	0.008 (5)	0.018 (6)	0.021 (5)
C23	0.042 (6)	0.040 (6)	0.077 (9)	−0.017 (5)	0.032 (6)	−0.012 (6)
O1	0.072 (7)	0.052 (5)	0.042 (5)	0.009 (5)	0.022 (5)	0.013 (4)
O12	0.040 (4)	0.056 (5)	0.044 (4)	0.002 (4)	0.024 (3)	0.011 (4)
C17	0.022 (4)	0.027 (4)	0.033 (5)	−0.007 (3)	0.011 (3)	−0.003 (3)
N12	0.031 (5)	0.064 (7)	0.054 (6)	0.018 (5)	0.016 (5)	−0.003 (5)
C15	0.030 (6)	0.057 (8)	0.045 (7)	0.011 (5)	0.008 (5)	0.012 (5)
C25	0.044 (7)	0.055 (8)	0.081 (10)	−0.015 (6)	0.041 (7)	0.003 (7)
O22	0.077 (6)	0.062 (6)	0.042 (5)	−0.030 (5)	0.043 (4)	−0.017 (4)

Pb1—O21	2.341 (7)	C13—N12	1.357 (15)
Pb1—O11i	2.508 (7)	C13—H13	0.9300
Pb1—O1	2.573 (9)	C27—O22	1.217 (15)
Pb1—O11	2.572 (8)	N22—C23	1.302 (17)
Pb1—N21	2.577 (9)	N22—C25	1.328 (19)
Pb1—N11	2.807 (9)	C26—C25	1.378 (18)
Pb1—O22ii	2.856 (8)	C26—H26	0.9300
O11—C17	1.277 (12)	N11—C16	1.334 (14)
O11—Pb1i	2.508 (7)	C16—C15	1.388 (17)
C22—N21	1.295 (14)	C16—H16	0.9300
C22—C23	1.389 (15)	C23—H23	0.9300
C22—C27	1.532 (16)	O1—H1	0.84 (2)
O21—C27	1.285 (14)	O1—H2	0.84 (2)
N21—C26	1.318 (12)	O12—C17	1.219 (12)
C12—N11	1.310 (13)	N12—C15	1.295 (17)
C12—C13	1.385 (13)	C15—H15	0.9300
C12—C17	1.513 (13)	C25—H25	0.9300
O21—Pb1—O11i	81.6 (3)	C13—C12—C17	120.2 (9)
O21—Pb1—O1	88.0 (3)	N12—C13—C12	120.6 (11)
O11i—Pb1—O1	152.2 (3)	N12—C13—H13	119.7
O21—Pb1—O11	75.0 (3)	C12—C13—H13	119.7
O11i—Pb1—O11	70.5 (3)	O22—C27—O21	125.7 (12)
O1—Pb1—O11	131.3 (3)	O22—C27—C22	119.1 (10)
O21—Pb1—N21	65.4 (3)	O21—C27—C22	115.1 (10)
O11i—Pb1—N21	81.6 (3)	C23—N22—C25	116.5 (11)
O1—Pb1—N21	70.6 (3)	N21—C26—C25	121.9 (11)
O11—Pb1—N21	134.3 (3)	N21—C26—H26	119.0
O21—Pb1—N11	78.0 (3)	C25—C26—H26	119.0
O11i—Pb1—N11	129.8 (3)	C12—N11—C16	117.4 (10)
O1—Pb1—N11	72.0 (3)	C12—N11—Pb1	116.4 (6)
O11—Pb1—N11	60.1 (3)	C16—N11—Pb1	125.8 (8)
N21—Pb1—N11	127.6 (3)	N11—C16—C15	120.5 (11)
O21—Pb1—O22ii	149.2 (3)	N11—C16—H16	119.8
O11i—Pb1—O22ii	102.5 (3)	C15—C16—H16	119.8
O1—Pb1—O22ii	74.3 (3)	N22—C23—C22	121.0 (13)
O11—Pb1—O22ii	135.4 (3)	N22—C23—H23	119.5
N21—Pb1—O22ii	84.8 (3)	C22—C23—H23	119.5
N11—Pb1—O22ii	118.2 (3)	Pb1—O1—H1	137 (10)
C17—O11—Pb1i	119.3 (6)	Pb1—O1—H2	113 (9)
C17—O11—Pb1	125.8 (6)	H1—O1—H2	106 (3)
Pb1i—O11—Pb1	109.5 (3)	O12—C17—O11	124.8 (9)
N21—C22—C23	123.2 (11)	O12—C17—C12	118.7 (9)
N21—C22—C27	116.9 (9)	O11—C17—C12	116.5 (8)
C23—C22—C27	119.9 (11)	C15—N12—C13	116.5 (10)
C27—O21—Pb1	126.1 (7)	N12—C15—C16	122.9 (11)
C22—N21—C26	115.8 (10)	N12—C15—H15	118.5
C22—N21—Pb1	116.0 (6)	C16—C15—H15	118.5
C26—N21—Pb1	127.7 (8)	N22—C25—C26	121.5 (11)
N11—C12—C13	121.9 (10)	N22—C25—H25	119.2
N11—C12—C17	117.9 (8)	C26—C25—H25	119.2

D—H···A	D—H	H···A	D···A	D—H···A
O1—H2···O21ii	0.84 (2)	2.17 (5)	2.837 (13)	136 (7)
O1—H1···O22iii	0.84 (2)	2.29 (5)	2.969 (15)	139 (7)
O1—H1···O12ii	0.84 (2)	2.49 (7)	3.056 (13)	126 (7)

Table 1

Selected bond lengths (Å)

Pb1—O21	2.341 (7)
Pb1—O11i	2.508 (7)
Pb1—O1	2.573 (9)
Pb1—O11	2.572 (8)
Pb1—N21	2.577 (9)
Pb1—N11	2.807 (9)
Pb1—O22ii	2.856 (8)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H2⋯O21ii	0.84 (2)	2.17 (5)	2.837 (13)	136 (7)
O1—H1⋯O22iii	0.84 (2)	2.29 (5)	2.969 (15)	139 (7)
O1—H1⋯O12ii	0.84 (2)	2.49 (7)	3.056 (13)	126 (7)

Symmetry codes: (ii) ; (iii) .