Poly[(μ(4)-pyridine-2,3-dicarboxyl-ato)lead(II)].

In the title coordination polymer, [Pb(C(7)H(3)NO(4))](n), the Pb(II) ion is eight-coordinated in a distorted square-anti-prismatic geometry formed by one pyridine N atom and seven carboxyl-ate O atoms from four pyridine-2,3-dicarboxyl-ate (pda) anions. In the pda anion, the dihedral angles between the pyridine ring and carboxyl-ate groups are 19.5 (6) and 73.3 (6)°. The carboxyl-ate groups of the pda anions bridge the Pb ions, forming a two-dimensional coordination polymer parallel to (100). Weak inter-molecular C-H⋯O hydrogen boning is present in the crystal structure.

Related literature

For the coordination modes of the pyridine-2,3-dicarboxyl­ate anion, see: Aghabozorg et al. (2007 ▶); Baruah et al. (2007 ▶); Li et al. (2006 ▶). For the biological activity of n class="Chemical">pyridine-2,3-dicarb­oxy­lic acid, see: Xiang et al. (2006 ▶); Yang et al. (2006 ▶); Zhang et al. (2008 ▶). For the inert lone-pair effect, see: Liat et al. (1998 ▶). For longer Pb—O bonds, see: Mao et al. (2006 ▶); Yang et al. (2010 ▶).

Experimental

Crystal data

[Pb(C7H3NO4)]

M = 372.30

Monoclinic,

a = 11.6943 (9) Å

b = 4.5392 (4) Å

c = 14.1636 (12) Å

β = 90.046 (2)°

V = 751.84 (11) Å3

Z = 4

Mo Kα radiation

μ = 22.42 mm−1

T = 297 K

0.54 × 0.23 × 0.04 mm

Data collection

Bruker SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.659, T max = 1.000

4013 measured reflections

1484 independent reflections

1336 reflections with I > 2σ(I)

R int = 0.125

Refinement

R[F 2 > 2σ(F 2)] = 0.073

wR(F 2) = 0.204

S = 1.13

1484 reflections

118 parameters

H-atom parameters constrained

Δρmax = 4.56 e Å−3

Δρmin = −5.06 e Å−3

Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 1999 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: PLATON (Spek, 2009 ▶); software used to prepare material for publication: PLATON.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811000419/xu5124sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811000419/xu5124Isup2.hkl

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

[Pb(C7H3NO4)]	F(000) = 664
Mr = 372.30	Dx = 3.289 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2856 reflections
a = 11.6943 (9) Å	θ = 2.3–26.0°
b = 4.5392 (4) Å	µ = 22.42 mm−1
c = 14.1636 (12) Å	T = 297 K
β = 90.046 (2)°	Parallelepiped, colorless
V = 751.84 (11) Å3	0.54 × 0.23 × 0.04 mm
Z = 4

Bruker SMART CCD area-detector diffractometer	1484 independent reflections
Radiation source: fine-focus sealed tube	1336 reflections with I > 2σ(I)
graphite	Rint = 0.125
Detector resolution: 9 pixels mm-1	θmax = 26.0°, θmin = 1.7°
ω scan	h = −14→10
Absorption correction: multi-scan (SADABS; Bruker, 2001)	k = −5→5
Tmin = 0.659, Tmax = 1.000	l = −17→17
4013 measured reflections

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)] = 0.073	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.204	H-atom parameters constrained
S = 1.13	w = 1/[σ2(Fo2) + (0.1477P)2] where P = (Fo2 + 2Fc2)/3
1484 reflections	(Δ/σ)max = 0.001
118 parameters	Δρmax = 4.56 e Å−3
0 restraints	Δρmin = −5.06 e Å−3

Experimental. Elemental analysis: calculated for C7H3NO4Pb: (Mr=372.29) C, 22.56; H, 0.81; N, 3.76%. Found:C,22.47; H, 0.89; N, 3.85%. IR data (cm-1): 3429(s), 1602(s), 1579(s), 1551(s), 1459(w), 1385(s), 1276(w), 1236(w), 1105(m), 871(m), 825(m), 779(m), 711(s), 700(m), 660(m), 603(w), 534(w), 443(w).

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Refinement. Refinement on F2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating -R-factor-obs 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
Pb	0.60762 (4)	0.01636 (10)	0.85892 (3)	0.0213 (3)
O1	0.6007 (6)	0.3400 (19)	0.5591 (4)	0.035 (2)
O2	0.5381 (7)	0.120 (2)	0.6883 (5)	0.037 (3)
O3	0.6905 (9)	−0.061 (2)	0.4106 (6)	0.032 (3)
O4	0.8222 (6)	0.2863 (17)	0.4294 (4)	0.038 (2)
N	0.7437 (6)	−0.1315 (19)	0.7170 (5)	0.024 (2)
C1	0.7208 (12)	−0.0178 (18)	0.6321 (9)	0.021 (4)
C2	0.7951 (11)	−0.058 (3)	0.5526 (9)	0.021 (3)
C3	0.8932 (8)	−0.216 (2)	0.5715 (6)	0.027 (3)
C4	0.9192 (9)	−0.325 (3)	0.6603 (7)	0.038 (4)
C5	0.8383 (9)	−0.288 (3)	0.7300 (6)	0.036 (3)
C6	0.6141 (8)	0.163 (3)	0.6231 (6)	0.023 (3)
C7	0.7687 (9)	0.068 (2)	0.4580 (7)	0.019 (3)
H3A	0.94410	−0.25180	0.52240	0.0320*
H4A	0.98820	−0.41980	0.67230	0.0450*
H5A	0.85060	−0.37490	0.78850	0.0430*

	U11	U22	U33	U12	U13	U23
Pb	0.0207 (5)	0.0242 (5)	0.0189 (5)	−0.0031 (1)	−0.0051 (3)	−0.0016 (1)
O1	0.035 (4)	0.045 (5)	0.026 (3)	0.015 (4)	0.007 (3)	0.012 (3)
O2	0.027 (4)	0.061 (6)	0.024 (3)	0.017 (5)	0.001 (3)	0.013 (4)
O3	0.039 (5)	0.031 (4)	0.027 (4)	0.006 (4)	−0.022 (4)	−0.013 (4)
O4	0.044 (4)	0.041 (5)	0.030 (3)	−0.007 (4)	−0.010 (3)	0.009 (3)
N	0.018 (4)	0.032 (5)	0.021 (3)	0.004 (3)	−0.003 (3)	0.004 (3)
C1	0.018 (7)	0.028 (6)	0.017 (6)	−0.002 (3)	0.000 (5)	−0.001 (3)
C2	0.006 (5)	0.037 (5)	0.021 (5)	0.002 (4)	−0.004 (4)	−0.010 (5)
C3	0.023 (5)	0.032 (6)	0.026 (4)	0.006 (4)	0.003 (4)	0.003 (4)
C4	0.029 (6)	0.054 (8)	0.031 (5)	0.018 (6)	−0.013 (4)	0.010 (5)
C5	0.041 (6)	0.046 (7)	0.021 (4)	0.009 (5)	−0.009 (4)	0.011 (4)
C6	0.018 (5)	0.031 (5)	0.021 (4)	0.006 (4)	−0.005 (3)	0.002 (4)
C7	0.008 (5)	0.030 (5)	0.019 (4)	0.006 (4)	−0.007 (4)	0.004 (4)

Pb—N	2.651 (7)	N—C1	1.336 (14)
Pb—O1i	2.816 (7)	N—C5	1.327 (14)
Pb—O1ii	2.911 (6)	C1—C2	1.435 (18)
Pb—O2	2.592 (7)	C1—C6	1.499 (17)
Pb—O2i	2.566 (9)	C2—C3	1.379 (16)
Pb—O3iii	2.397 (9)	C2—C7	1.489 (16)
Pb—O3ii	2.754 (9)	C3—C4	1.385 (14)
Pb—O4ii	2.845 (7)	C4—C5	1.378 (14)
O1—C6	1.221 (13)	C3—H3A	0.9300
O2—C6	1.297 (12)	C4—H4A	0.9300
O3—C7	1.276 (14)	C5—H5A	0.9300
O4—C7	1.240 (12)
O2—Pb—N	61.8 (2)	Pbv—O1—C6	150.1 (7)
O1i—Pb—O2	99.5 (2)	Pbiv—O1—Pbv	111.3 (2)
O2—Pb—O2i	71.1 (3)	Pb—O2—C6	118.5 (6)
O2—Pb—O3iii	124.6 (3)	Pb—O2—Pbiv	125.3 (3)
O1ii—Pb—O2	149.2 (2)	Pbiv—O2—C6	99.5 (7)
O2—Pb—O3ii	101.2 (3)	Pbvi—O3—C7	147.7 (8)
O2—Pb—O4ii	123.1 (2)	Pbv—O3—C7	88.8 (6)
O2—Pb—C7ii	121.1 (3)	Pbvi—O3—Pbv	123.4 (4)
O1i—Pb—N	139.5 (2)	Pbv—O4—C7	85.5 (6)
O2i—Pb—N	91.4 (2)	Pb—N—C1	117.7 (7)
O3iii—Pb—N	76.7 (3)	Pb—N—C5	122.1 (6)
O1ii—Pb—N	144.3 (2)	C1—N—C5	119.9 (9)
O3ii—Pb—N	102.6 (3)	N—C1—C2	122.4 (11)
O4ii—Pb—N	79.4 (2)	N—C1—C6	117.0 (10)
N—Pb—C7ii	97.8 (3)	C2—C1—C6	120.5 (10)
O1i—Pb—O2i	48.2 (2)	C1—C2—C3	114.7 (11)
O1i—Pb—O3iii	88.8 (3)	C1—C2—C7	122.2 (11)
O1i—Pb—O1ii	68.73 (19)	C3—C2—C7	123.1 (10)
O1i—Pb—O3ii	116.7 (3)	C2—C3—C4	123.0 (10)
O1i—Pb—O4ii	135.08 (17)	C3—C4—C5	117.2 (10)
O1i—Pb—C7ii	121.8 (2)	N—C5—C4	122.6 (9)
O2i—Pb—O3iii	75.1 (3)	O1—C6—O2	122.7 (10)
O1ii—Pb—O2i	113.1 (2)	O1—C6—C1	122.0 (9)
O2i—Pb—O3ii	158.7 (3)	O2—C6—C1	115.3 (10)
O2i—Pb—O4ii	153.8 (2)	O3—C7—O4	123.8 (9)
O2i—Pb—C7ii	167.3 (2)	O3—C7—C2	116.4 (9)
O1ii—Pb—O3iii	84.7 (3)	Pbv—C7—O3	66.1 (6)
O3iii—Pb—O3ii	123.4 (3)	O4—C7—C2	119.8 (9)
O3iii—Pb—O4ii	78.9 (3)	Pbv—C7—O4	70.3 (5)
O3iii—Pb—C7ii	98.4 (3)	Pbv—C7—C2	142.1 (7)
O1ii—Pb—O3ii	63.3 (2)	C2—C3—H3A	119.00
O1ii—Pb—O4ii	67.22 (18)	C4—C3—H3A	118.00
O1ii—Pb—C7ii	54.8 (2)	C3—C4—H4A	121.00
O3ii—Pb—O4ii	46.7 (3)	C5—C4—H4A	121.00
O3ii—Pb—C7ii	25.1 (3)	N—C5—H5A	119.00
O4ii—Pb—C7ii	24.2 (2)	C4—C5—H5A	119.00
Pbiv—O1—C6	89.5 (6)
N—Pb—O2—C6	−27.3 (8)	O2—Pb—O4ii—C7ii	93.1 (6)
N—Pb—O2—Pbiv	−155.1 (5)	N—Pb—O4ii—C7ii	138.9 (6)
O1i—Pb—O2—C6	−169.0 (9)	O2—Pb—C7ii—O3ii	41.3 (7)
O1i—Pb—O2—Pbiv	63.2 (4)	O2—Pb—C7ii—O4ii	−102.4 (5)
O2i—Pb—O2—C6	−129.5 (9)	O2—Pb—C7ii—C2ii	144.2 (11)
O2i—Pb—O2—Pbiv	102.7 (4)	N—Pb—C7ii—O3ii	102.9 (6)
O3iii—Pb—O2—C6	−73.9 (10)	N—Pb—C7ii—O4ii	−40.7 (6)
O3iii—Pb—O2—Pbiv	158.3 (4)	N—Pb—C7ii—C2ii	−154.2 (12)
O1ii—Pb—O2—C6	126.9 (9)	Pbv—O1—C6—O2	−131.7 (11)
O1ii—Pb—O2—Pbiv	−0.9 (7)	Pbiv—O1—C6—C1	−175.5 (10)
O3ii—Pb—O2—C6	71.1 (9)	Pbiv—O1—C6—O2	3.8 (11)
O3ii—Pb—O2—Pbiv	−56.7 (4)	Pbv—O1—C6—C1	49.0 (19)
O4ii—Pb—O2—C6	25.9 (10)	Pbiv—O2—C6—C1	175.1 (8)
O4ii—Pb—O2—Pbiv	−101.9 (4)	Pb—O2—C6—C1	36.0 (13)
C7ii—Pb—O2—C6	54.5 (10)	Pb—O2—C6—O1	−143.4 (9)
C7ii—Pb—O2—Pbiv	−73.3 (5)	Pbiv—O2—C6—O1	−4.2 (12)
O2—Pb—N—C1	15.4 (7)	Pbvi—O3—C7—O4	136.7 (11)
O2—Pb—N—C5	−171.4 (9)	Pbv—O3—C7—O4	−42.2 (10)
O1i—Pb—N—C1	85.5 (8)	Pbvi—O3—C7—C2	−43.1 (19)
O1i—Pb—N—C5	−101.3 (8)	Pbv—O3—C7—C2	138.0 (9)
O2i—Pb—N—C1	83.0 (7)	Pbvi—O3—C7—Pbv	178.9 (15)
O2i—Pb—N—C5	−103.8 (9)	Pbv—O4—C7—O3	40.7 (10)
O3iii—Pb—N—C1	157.4 (8)	Pbv—O4—C7—C2	−139.5 (9)
O3iii—Pb—N—C5	−29.4 (9)	C5—N—C1—C2	0.1 (16)
O1ii—Pb—N—C1	−142.1 (7)	Pb—N—C1—C2	173.5 (8)
O1ii—Pb—N—C5	31.1 (10)	Pb—N—C1—C6	−5.1 (12)
O3ii—Pb—N—C1	−80.8 (7)	C1—N—C5—C4	4.1 (17)
O3ii—Pb—N—C5	92.4 (9)	C5—N—C1—C6	−178.5 (10)
O4ii—Pb—N—C1	−121.6 (7)	Pb—N—C5—C4	−169.0 (9)
O4ii—Pb—N—C5	51.6 (8)	C6—C1—C2—C3	176.8 (10)
C7ii—Pb—N—C1	−105.8 (7)	N—C1—C2—C3	−1.7 (16)
C7ii—Pb—N—C5	67.4 (9)	N—C1—C2—C7	179.7 (10)
O2—Pb—O1i—C6i	51.7 (7)	C6—C1—C2—C7	−1.9 (17)
O2—Pb—O1i—Pbvii	−150.3 (3)	N—C1—C6—O1	159.4 (10)
N—Pb—O1i—C6i	−5.4 (8)	N—C1—C6—O2	−20.0 (15)
N—Pb—O1i—Pbvii	152.5 (3)	C2—C1—C6—O1	−19.2 (17)
O2—Pb—O2i—Pbi	14.6 (4)	C2—C1—C6—O2	161.5 (10)
O2—Pb—O2i—C6i	−120.6 (7)	C1—C2—C3—C4	−0.7 (17)
N—Pb—O2i—Pbi	−44.8 (4)	C7—C2—C3—C4	177.9 (11)
N—Pb—O2i—C6i	179.9 (7)	C1—C2—C7—O3	−74.7 (15)
O2—Pb—O3iii—C7iii	136.3 (13)	C1—C2—C7—O4	105.5 (13)
N—Pb—O3iii—C7iii	95.1 (14)	C1—C2—C7—Pbv	10 (2)
O2—Pb—O1ii—Pbvii	72.2 (6)	C3—C2—C7—O3	106.7 (13)
O2—Pb—O1ii—C6ii	−59.0 (14)	C3—C2—C7—O4	−73.0 (15)
N—Pb—O1ii—Pbvii	−149.1 (3)	C3—C2—C7—Pbv	−168.9 (8)
N—Pb—O1ii—C6ii	79.8 (14)	C2—C3—C4—C5	4.5 (18)
O2—Pb—O3ii—C7ii	−144.8 (6)	C3—C4—C5—N	−6.3 (18)
N—Pb—O3ii—C7ii	−81.6 (6)

D—H···A	D—H	H···A	D···A	D—H···A
C5—H5A···O3iii	0.93	2.57	3.164 (13)	122

Table 1

Selected bond lengths (Å)

Pb—N	2.651 (7)
Pb—O1i	2.816 (7)
Pb—O1ii	2.911 (6)
Pb—O2	2.592 (7)
Pb—O2i	2.566 (9)
Pb—O3iii	2.397 (9)
Pb—O3ii	2.754 (9)
Pb—O4ii	2.845 (7)

Symmetry codes: (i) ; (ii) ; (iii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C5—H5A⋯O3iii	0.93	2.57	3.164 (13)	122

Symmetry code: (iii) .