catena-Poly[[(benzoato-κ2O,O′)(2,2′-bipyridine-κ2N,N′)lead(II)]-μ3-nitrato-κ4O:O,O′:O′′]

Yang, J.; Dai, J.; Wang, X.

doi:10.1107/S160053681004907X

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 12| December 2010| Page m1686

https://doi.org/10.1107/S160053681004907X

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catena-Poly[[(benzoato-κ²O,O′)(2,2′-bipyridine-κ²N,N′)lead(II)]-μ₃-nitrato-κ⁴O:O,O′:O′′]

Juan Yang,^a ^* Jun Dai ^b and Xiaohan Wang ^b

^aDepartment of Physical Chemistry, Henan Polytechnic University, Jiaozuo 454003, People's Republic of China, and ^bInstitute of Safety Science and Engineering, Henan Polytechnic University, Jiaozuo 454003, People's Republic of China
^*Correspondence e-mail: yangjuan0302@yahoo.cn

(Received 16 November 2010; accepted 23 November 2010; online 27 November 2010)

In the title coordination polymer, [Pb(C₇H₅O₂)(NO₃)(C₁₀H₈N₂)]_n, the Pb^II ion is eight-coordinated by two N atoms from one 2,2′-bipyridine ligand, two O atoms from one benzoate anion and four O atoms from three nitrate groups (one chelating, two bridging) in a distorted dodecahedral geometry. Adjacent Pb^II ions are linked by bridging nitrate O atoms through the central Pb₂O₂ and Pb₂O₄N₂ cores, resulting in an infinite chain structure along the b axis. The crystal structure is stabilized by π–π stacking interactions between 2,2′-bipyridine and benzoate ligands belonging to neighboring chains, with shortest centroid–centroid distances of 3.685 (8) and 3.564 (8) Å.

Related literature

For applications of complexes containing Pb(II), see: Fan & Zhu (2006 ); Hamilton et al. (2004 ); Alvarado et al. (2005 ). For the use of aromatic carboxylate and 2,2′-bipyridine-like ligands in the preparation of metal-organic complexes, see: Wang et al. (2006 ); Masaoka et al. (2001 ); Hagrman & Zubieta (2000 ); Li et al. (2002 ).

Experimental

Crystal data

[Pb(C₇H₅O₂)(NO₃)(C₁₀H₈N₂)]
M_r = 546.49
Triclinic, $[P \overline 1]$
a = 6.5389 (11) Å
b = 8.5052 (14) Å
c = 15.548 (3) Å
α = 84.566 (3)°
β = 86.593 (3)°
γ = 83.729 (2)°
V = 854.6 (3) Å³
Z = 2
Mo Kα radiation
μ = 9.91 mm⁻¹
T = 296 K
0.23 × 0.21 × 0.15 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2007 ) T_min = 0.118, T_max = 0.226
4385 measured reflections
2981 independent reflections
2769 reflections with I > 2σ(I)
R_int = 0.030

Refinement

R[F² > 2σ(F²)] = 0.037
wR(F²) = 0.099
S = 1.02
2981 reflections
235 parameters
H-atom parameters constrained
Δρ_max = 2.70 e Å⁻³
Δρ_min = −2.79 e Å⁻³

Table 1
Selected bond lengths (Å)

Pb1—O1	2.432 (5)
Pb1—N2	2.441 (6)
Pb1—N1	2.471 (5)
Pb1—O2	2.619 (6)
Pb1—O4	2.871 (6)
Pb1—O3	2.928 (6)
Pb1—O3ⁱ	2.893 (6)
Pb1—O5ⁱⁱ	2.887 (7)
Symmetry codes: (i) -x+1, -y, -z+1; (ii) -x, -y, -z+1.

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; 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.

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S160053681004907X/gk2325sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S160053681004907X/gk2325Isup2.hkl

checkCIF report

Comment top

Complexes containing Pb(II) ion have recently attracted considerable interest not only because of the variety of their architectures, but also because of their potential applications, especially in environmental protection and in systems with different biological properties (Fan & Zhu, 2006; Hamilton et al., 2004; Alvarado et al., 2005). As an important family of multidentate O-donor ligands, aromatic carboxylate ligands have been extensively employed in the preparation of metal-organic complexes because of their potential properties and intriguing structural topologies (Wang et al., 2006; Masaoka et al., 2001). To our knowledge, carboxylate coordinates metal in various ways, for example, in the mode of monodentate, bidentate chelating, bidentate bridging or chelating-bridging. It is well known that the introduction of chelate ligands such as 2,2'-bipyridine are capable of passivating metal sites via the N donors of the organic groups and may induce new structural evolution (Hagrman et al., 2000; Li et al., 2002). Herein, we report the structure of the title polymer.

The asymmetric unit of the title compound, [Pb(C₁₀H₈N₂)(C₇H₅O₂)(NO₃)], contains a Pb^II cation, one 2,2'-bipyridine ligand, one benzoate and one nitrate ligand, as illustrated in in Fig.1. The Pb^II atom is eight-coordinated by two N atoms from one 2,2'-bipyridine ligand, two O atoms from one benzoate anion and four O atoms from three chelating-bridging nitrate ligands in a distorted dodecahedron geometry. The O3 and O5 atoms of bridging nitrato ligands link the adjacent Pb^II ions through the central Pb₂O₂ and Pb₂O₄N₂ cores, resulting in an infinite chain structure along the b axis (Fig.2). The excellent coordinating ability and large conjugated systems of 2,2'-bipyridine and benzoato ligands allow to form π..π interactions. The chains are extended into the framework through π..π stacking interactions between the ligands belonging to the neighboring chains, with the shortest centroid-centroid distance of 3.685 (8) and 3.564 (8)Å.

Related literature top

For applications of complexes containing Pb(II) ion, see: Fan & Zhu (2006); Hamilton et al. (2004); Alvarado et al. (2005). For the use of aromatic carboxylate and 2,2'-bipyridine-like ligands in the preparation of metal-organic complexes, see: Wang et al. (2006); Masaoka et al. (2001); Hagrman & Zubieta (2000); Li et al. (2002).

Experimental top

A mixture of Pb(NO₃)₂ (0.09 g, 0.27 mmol), benzoic acid (0.102 g, 0.84 mmol), 2,2'-bipyridine (0.065 g, 0.41 mmol) and distilled water (10 ml) was sealed in a 25 ml Teflon-lined stainless autoclave. The mixture was heated at 403 K for 6 days to give the colorless crystals suitable for X-ray diffraction analysis.

Structure description top

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); 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 (Sheldrick, 2008).

Figures top

	Fig. 1. The coordination environment around Pb^II in the title compound with the atom-labeling scheme. Displacement ellipsoids for non-hydrogen atoms are drawn at the 30% probability level. Symmetry codes: (i) 1-x, -y, 1-z; (ii) -x, -y, 1-z.
	Fig. 2. The chain of the title polymer viewed down the b axis.; H atoms are omitted for clarity.

catena-Poly[[(benzoato-κ²O,O')(2,2'-bipyridine- κ²N,N')lead(II)]-µ₃-nitrato- κ⁴O:O,O':O''] top

Crystal data top

[Pb(C₇H₅O₂)(NO₃)(C₁₀H₈N₂)]	Z = 2
M_r = 546.49	F(000) = 516
Triclinic, P1	D_x = 2.124 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.5389 (11) Å	Cell parameters from 3772 reflections
b = 8.5052 (14) Å	θ = 2.6–28.2°
c = 15.548 (3) Å	µ = 9.91 mm⁻¹
α = 84.566 (3)°	T = 296 K
β = 86.593 (3)°	Column, colorless
γ = 83.729 (2)°	0.23 × 0.21 × 0.15 mm
V = 854.6 (3) Å³

Data collection top

Bruker APEXII CCD area-detector diffractometer	2981 independent reflections
Radiation source: fine-focus sealed tube	2769 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.030
φ and ω scans	θ_max = 25.0°, θ_min = 2.7°
Absorption correction: multi-scan (SADABS; Bruker, 2007)	h = −7→7
T_min = 0.118, T_max = 0.226	k = −9→10
4385 measured reflections	l = −18→15

Refinement top

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)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.099	H-atom parameters constrained
S = 1.02	w = 1/[σ²(F_o²) + (0.0675P)²] where P = (F_o² + 2F_c²)/3
2981 reflections	(Δ/σ)_max = 0.001
235 parameters	Δρ_max = 2.70 e Å⁻³
0 restraints	Δρ_min = −2.79 e Å⁻³

Crystal data top

[Pb(C₇H₅O₂)(NO₃)(C₁₀H₈N₂)]	γ = 83.729 (2)°
M_r = 546.49	V = 854.6 (3) Å³
Triclinic, P1	Z = 2
a = 6.5389 (11) Å	Mo Kα radiation
b = 8.5052 (14) Å	µ = 9.91 mm⁻¹
c = 15.548 (3) Å	T = 296 K
α = 84.566 (3)°	0.23 × 0.21 × 0.15 mm
β = 86.593 (3)°

Data collection top

Bruker APEXII CCD area-detector diffractometer	2981 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2007)	2769 reflections with I > 2σ(I)
T_min = 0.118, T_max = 0.226	R_int = 0.030
4385 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	0 restraints
wR(F²) = 0.099	H-atom parameters constrained
S = 1.02	Δρ_max = 2.70 e Å⁻³
2981 reflections	Δρ_min = −2.79 e Å⁻³
235 parameters

Special details top

Experimental. 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 > 2sigma(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. 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Pb1	0.31380 (3)	0.02444 (2)	0.362929 (15)	0.02612 (13)
O3	0.3180 (9)	0.0845 (7)	0.5451 (4)	0.0433 (14)
O2	0.2641 (8)	−0.0974 (7)	0.2180 (4)	0.0409 (13)
O4	0.0370 (9)	0.1789 (8)	0.4866 (4)	0.0546 (16)
O1	0.5402 (9)	0.0249 (7)	0.2331 (4)	0.0443 (14)
O5	0.0478 (10)	0.1446 (10)	0.6257 (5)	0.064 (2)
N3	0.1340 (9)	0.1372 (8)	0.5520 (5)	0.0339 (15)
N1	0.4378 (8)	0.2885 (6)	0.3637 (4)	0.0278 (13)
N2	0.1021 (8)	0.2377 (6)	0.2836 (4)	0.0282 (12)
C1	0.6040 (10)	0.3077 (9)	0.4070 (5)	0.0351 (17)
H1	0.6739	0.2188	0.4357	0.042*
C16	0.5298 (18)	−0.2934 (13)	−0.0021 (7)	0.064 (3)
H16	0.4584	−0.3589	−0.0314	0.076*
C11	0.4407 (11)	−0.0630 (9)	0.1930 (5)	0.0328 (17)
C14	0.8340 (17)	−0.1765 (12)	0.0162 (8)	0.067 (3)
H14	0.9697	−0.1615	−0.0009	0.081*
C10	−0.0635 (12)	0.2054 (10)	0.2451 (5)	0.0349 (18)
H10	−0.0986	0.1017	0.2507	0.042*
C8	−0.1339 (12)	0.4738 (10)	0.1900 (6)	0.045 (2)
H8	−0.2144	0.5531	0.1583	0.054*
C9	−0.1831 (11)	0.3195 (10)	0.1977 (6)	0.0412 (18)
H9	−0.2966	0.2933	0.1709	0.049*
C12	0.5419 (13)	−0.1335 (9)	0.1145 (5)	0.0360 (18)
C15	0.7274 (19)	−0.2662 (12)	−0.0304 (7)	0.067 (3)
H15	0.7873	−0.3080	−0.0802	0.080*
C3	0.5708 (13)	0.5819 (10)	0.3691 (7)	0.050 (2)
H3	0.6165	0.6812	0.3708	0.060*
C2	0.6744 (12)	0.4517 (10)	0.4106 (6)	0.0420 (19)
H2	0.7907	0.4609	0.4406	0.050*
C13	0.7444 (14)	−0.1082 (10)	0.0878 (6)	0.049 (2)
H13	0.8178	−0.0458	0.1181	0.058*
C17	0.4357 (15)	−0.2243 (11)	0.0694 (6)	0.049 (2)
H17	0.3002	−0.2400	0.0864	0.058*
C6	0.1514 (10)	0.3891 (7)	0.2771 (5)	0.0268 (14)
C7	0.0347 (11)	0.5089 (9)	0.2296 (5)	0.0395 (18)
H7	0.0708	0.6123	0.2246	0.047*
C5	0.3344 (10)	0.4157 (7)	0.3236 (5)	0.0275 (14)
C4	0.3976 (13)	0.5674 (9)	0.3244 (7)	0.047 (2)
H4	0.3258	0.6557	0.2959	0.057*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.02844 (18)	0.01828 (18)	0.0322 (2)	−0.00253 (11)	−0.00343 (11)	−0.00370 (12)
O3	0.039 (3)	0.049 (4)	0.041 (3)	0.004 (3)	−0.007 (2)	−0.008 (3)
O2	0.030 (3)	0.042 (3)	0.053 (4)	−0.014 (2)	0.003 (2)	−0.010 (3)
O4	0.041 (3)	0.060 (4)	0.060 (4)	0.015 (3)	−0.022 (3)	−0.004 (3)
O1	0.048 (3)	0.047 (3)	0.043 (3)	−0.023 (3)	0.007 (3)	−0.019 (3)
O5	0.050 (4)	0.093 (6)	0.056 (4)	−0.025 (4)	0.012 (3)	−0.025 (4)
N3	0.031 (3)	0.029 (3)	0.043 (4)	−0.006 (3)	−0.002 (3)	−0.007 (3)
N1	0.028 (3)	0.020 (3)	0.036 (3)	−0.003 (2)	−0.005 (2)	−0.004 (3)
N2	0.029 (3)	0.024 (3)	0.032 (3)	−0.004 (2)	−0.003 (2)	−0.004 (3)
C1	0.027 (3)	0.033 (4)	0.046 (5)	−0.005 (3)	−0.010 (3)	−0.004 (4)
C16	0.089 (8)	0.062 (7)	0.043 (6)	0.003 (6)	−0.014 (5)	−0.023 (5)
C11	0.034 (4)	0.032 (4)	0.031 (4)	0.006 (3)	0.002 (3)	−0.006 (3)
C14	0.067 (6)	0.055 (6)	0.073 (8)	0.000 (5)	0.030 (6)	0.001 (6)
C10	0.039 (4)	0.032 (4)	0.035 (4)	−0.002 (3)	−0.007 (3)	−0.010 (3)
C8	0.040 (4)	0.040 (5)	0.051 (5)	0.005 (3)	−0.011 (4)	0.008 (4)
C9	0.033 (4)	0.048 (5)	0.044 (5)	−0.005 (3)	−0.011 (3)	−0.006 (4)
C12	0.050 (5)	0.026 (4)	0.031 (4)	0.004 (3)	−0.002 (3)	−0.002 (3)
C15	0.102 (8)	0.057 (6)	0.038 (6)	0.012 (6)	0.012 (5)	−0.022 (5)
C3	0.050 (5)	0.028 (4)	0.076 (7)	−0.010 (4)	−0.017 (4)	−0.013 (4)
C2	0.040 (4)	0.041 (5)	0.051 (5)	−0.012 (4)	−0.008 (4)	−0.019 (4)
C13	0.051 (5)	0.040 (5)	0.056 (6)	−0.008 (4)	0.009 (4)	−0.018 (4)
C17	0.056 (5)	0.050 (5)	0.042 (5)	−0.004 (4)	−0.009 (4)	−0.012 (4)
C6	0.027 (3)	0.021 (3)	0.032 (4)	0.003 (3)	−0.003 (3)	−0.003 (3)
C7	0.042 (4)	0.027 (4)	0.048 (5)	0.000 (3)	−0.004 (4)	0.004 (4)
C5	0.031 (3)	0.022 (3)	0.029 (4)	−0.003 (3)	−0.001 (3)	−0.006 (3)
C4	0.050 (5)	0.023 (4)	0.070 (6)	−0.002 (3)	−0.013 (4)	−0.007 (4)

Geometric parameters (Å, º) top

Pb1—O1	2.432 (5)	C16—C17	1.387 (13)
Pb1—N2	2.441 (6)	C11—C12	1.498 (11)
Pb1—N1	2.471 (5)	C13—H13	0.9300
Pb1—O2	2.619 (6)	C14—H14	0.9300
Pb1—C11	2.863 (7)	C14—C13	1.375 (13)
Pb1—O4	2.871 (6)	C14—C15	1.368 (16)
Pb1—O3	2.928 (6)	C10—C9	1.365 (12)
Pb1—O3ⁱ	2.893 (6)	C8—H8	0.9300
Pb1—O5ⁱⁱ	2.887 (7)	C9—H9	0.9300
O3—N3	1.239 (9)	C10—H10	0.9300
O2—C11	1.252 (9)	C8—C7	1.368 (12)
O4—N3	1.234 (9)	C8—C9	1.378 (11)
O1—C11	1.270 (10)	C12—C17	1.359 (12)
O5—N3	1.251 (9)	C17—H17	0.9300
N1—C5	1.333 (9)	C12—C13	1.397 (12)
N1—C1	1.344 (9)	C3—C4	1.386 (12)
N2—C10	1.334 (10)	C3—C2	1.361 (12)
N2—C6	1.355 (8)	C6—C7	1.386 (10)
C1—C2	1.362 (10)	C7—H7	0.9300
C1—H1	0.9300	C6—C5	1.483 (9)
C2—H2	0.9300	C5—C4	1.399 (10)
C16—C15	1.376 (16)	C3—H3	0.9300
C16—H16	0.9300	C4—H4	0.9300
C15—H15	0.9300

O1—Pb1—N2	85.6 (2)	O2—C11—C12	118.6 (7)
O1—Pb1—N1	80.21 (18)	O1—C11—C12	118.6 (7)
N2—Pb1—N1	66.18 (18)	O2—C11—Pb1	66.1 (4)
O1—Pb1—O2	51.83 (16)	O1—C11—Pb1	57.6 (4)
N2—Pb1—O2	77.48 (18)	C12—C11—Pb1	167.3 (6)
N1—Pb1—O2	121.47 (18)	C15—C14—C13	121.3 (10)
O1—Pb1—C11	26.2 (2)	N2—C10—C9	122.2 (7)
N2—Pb1—C11	83.2 (2)	C7—C8—C9	119.2 (8)
N1—Pb1—C11	102.9 (2)	C10—C9—C8	119.3 (7)
O2—Pb1—C11	25.91 (19)	C17—C12—C13	119.8 (8)
O1—Pb1—O4	152.8 (2)	C17—C12—C11	119.5 (8)
N2—Pb1—O4	72.48 (18)	C13—C12—C11	120.7 (8)
N1—Pb1—O4	76.30 (19)	C14—C15—C16	118.7 (9)
O2—Pb1—O4	133.87 (16)	C2—C3—C4	120.5 (7)
C11—Pb1—O4	153.8 (2)	C3—C2—C1	118.5 (7)
O1—Pb1—O3	139.88 (17)	C14—C13—C12	119.3 (9)
N2—Pb1—O3	110.35 (18)	C12—C17—C16	119.9 (9)
N1—Pb1—O3	73.97 (19)	N2—C6—C7	120.8 (6)
O2—Pb1—O3	164.48 (18)	N2—C6—C5	115.7 (6)
C11—Pb1—O3	162.4 (2)	C7—C6—C5	123.5 (6)
O4—Pb1—O3	43.33 (16)	C8—C7—C6	119.4 (7)
O1—Pb1—O5ⁱⁱ	120.1 (2)	N1—C5—C4	121.4 (7)
N2—Pb1—O5ⁱⁱ	85.50 (19)	N1—C5—C6	117.2 (5)
N1—Pb1—O5ⁱⁱ	144.52 (19)	C4—C5—C6	121.4 (7)
O2—Pb1—O5ⁱⁱ	68.42 (19)	C3—C4—C5	117.8 (8)
C11—Pb1—O5ⁱⁱ	94.0 (2)	N1—C1—H1	118.6
O4—Pb1—O5ⁱⁱ	74.99 (19)	C2—C1—H1	118.6
O3—Pb1—O5ⁱⁱ	98.23 (19)	C1—C2—H2	120.8
O1—Pb1—O3ⁱ	85.60 (19)	C3—C2—H2	120.7
N2—Pb1—O3ⁱ	149.75 (17)	C2—C3—H3	120.0
N1—Pb1—O3ⁱ	83.81 (17)	C4—C3—H3	120.0
O2—Pb1—O3ⁱ	118.16 (17)	H4—C4—C3	121.1
C11—Pb1—O3ⁱ	100.76 (19)	H4—C4—C5	121.1
O4—Pb1—O3ⁱ	105.12 (17)	C6—C7—H7	120.3
O3—Pb1—O3ⁱ	61.80 (17)	H7—C7—C8	120.3
O5ⁱⁱ—Pb1—O3ⁱ	123.69 (18)	H8—C8—C7	120.4
N3—O3—Pb1	95.6 (5)	H8—C8—C9	120.4
C11—O2—Pb1	88.0 (5)	C8—C9—H9	120.4
N3—O4—Pb1	98.6 (4)	H9—C9—C10	120.3
C11—O1—Pb1	96.2 (4)	C9—C10—H10	118.9
O4—N3—O3	120.0 (7)	H10—C10—N2	118.9
O4—N3—O5	120.7 (7)	C12—C13—H13	120.4
O3—N3—O5	119.3 (7)	H13—C13—C14	120.3
C5—N1—C1	119.0 (6)	H14—C14—C13	119.4
C5—N1—Pb1	119.9 (4)	H14—C14—C15	119.3
C1—N1—Pb1	121.0 (5)	H15—C15—C14	120.7
C10—N2—C6	119.1 (6)	H15—C15—C16	120.6
C10—N2—Pb1	119.9 (5)	C15—C16—H16	119.5
C6—N2—Pb1	121.0 (4)	C17—C16—H16	119.6
N1—C1—C2	122.8 (7)	H17—C17—C12	120.1
C15—C16—C17	120.9 (10)	H17—C17—C16	120.0
O2—C11—O1	122.8 (7)

Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x, −y, −z+1.

Experimental details

Crystal data
Chemical formula	[Pb(C₇H₅O₂)(NO₃)(C₁₀H₈N₂)]
M_r	546.49
Crystal system, space group	Triclinic, P1
Temperature (K)	296
a, b, c (Å)	6.5389 (11), 8.5052 (14), 15.548 (3)
α, β, γ (°)	84.566 (3), 86.593 (3), 83.729 (2)
V (Å³)	854.6 (3)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	9.91
Crystal size (mm)	0.23 × 0.21 × 0.15

Data collection
Diffractometer	Bruker APEXII CCD area-detector
Absorption correction	Multi-scan (SADABS; Bruker, 2007)
T_min, T_max	0.118, 0.226
No. of measured, independent and observed [I > 2σ(I)] reflections	4385, 2981, 2769
R_int	0.030
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.099, 1.02
No. of reflections	2981
No. of parameters	235
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	2.70, −2.79

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Pb1—O1	2.432 (5)	Pb1—O4	2.871 (6)
Pb1—N2	2.441 (6)	Pb1—O3	2.928 (6)
Pb1—N1	2.471 (5)	Pb1—O3ⁱ	2.893 (6)
Pb1—O2	2.619 (6)	Pb1—O5ⁱⁱ	2.887 (7)

Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x, −y, −z+1.

Acknowledgements

The authors acknowledge financial support by the Doctoral Foundation of Henan Polytechnic University (B2008-58 648265).

References

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