μ-Oxalato-κ(4)O(1),O(2):O(1'),O(2')-bis-[aqua-(2,2'-bipyridine-κN)(nitrato-κ(2)O,O')lead(II)].

The title compound, [Pb(2)(C(2)O(4))(NO(3))(2)(C(10)H(8)N(2))(2)(H(2)O)(2)], was synthesized hydro-thermally. The binuclear complex mol-ecule is centrosymmetric, the inversion centre being located at the mid-point of the oxalate C-C bond. The Pb(II) ion is hepta-coordinated by the O atom of one water mol-ecule, two oxalate O atoms, two nitrate O atoms and two 2,2'-bipyridine N atoms, forming an irregular coordination environemnt. Inter-molecular O-H⋯O hydrogen bonds between water mol-ecules and oxalate and nitrate ions result in the formation of layers parallel to (010). π-π inter-actions between pyridine rings in adjacent layers, with centroid-centroid distances of 3.584 (2) Å, stabilize the structural set-up.

Related literature

For general background to this class of compounds, see: Fan & Zhu (2006 ▶); Hamilton et al. (2004 ▶); Hagrman & Zubieta (2000 ▶); Li et al. (2002 ▶).

Experimental

Crystal data

[Pb2(C2O4)(NO3)2(C10H8N2)2(H2O)2]

M = 974.82

Monoclinic,

a = 9.5791 (19) Å

b = 20.6330 (14) Å

c = 6.7649 (15) Å

β = 91.687 (1)°

V = 1336.5 (4) Å3

Z = 2

Mo Kα radiation

μ = 12.66 mm−1

T = 296 K

0.29 × 0.28 × 0.26 mm

Data collection

Bruker SMART CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2003 ▶) T min = 0.120, T max = 0.137

7096 measured reflections

2336 independent reflections

2082 reflections with I > 2σ(I)

R int = 0.038

Refinement

R[F 2 > 2σ(F 2)] = 0.031

wR(F 2) = 0.082

S = 1.07

2336 reflections

190 parameters

H-atom parameters constrained

Δρmax = 2.68 e Å−3

Δρmin = −1.19 e Å−3

Data collection: SMART (Bruker, 2003 ▶); cell refinement: SAINT (Bruker, 2003 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2009 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶).

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812040196/wm2667sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812040196/wm2667Isup2.hkl

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

[Pb2(C2O4)(NO3)2(C10H8N2)2(H2O)2]	F(000) = 908
Mr = 974.82	Dx = 2.422 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 3490 reflections
a = 9.5791 (19) Å	θ = 2.3–28.3°
b = 20.6330 (14) Å	µ = 12.66 mm−1
c = 6.7649 (15) Å	T = 296 K
β = 91.687 (1)°	Block, colorless
V = 1336.5 (4) Å3	0.29 × 0.28 × 0.26 mm
Z = 2

Bruker SMART CCD diffractometer	2336 independent reflections
Radiation source: fine-focus sealed tube	2082 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.038
phi and ω scans	θmax = 25.0°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2003)	h = −11→10
Tmin = 0.120, Tmax = 0.137	k = −24→24
7096 measured reflections	l = −7→8

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)] = 0.031	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.082	H-atom parameters constrained
S = 1.07	w = 1/[σ2(Fo2) + (0.035P)2 + 5.1328P] where P = (Fo2 + 2Fc2)/3
2336 reflections	(Δ/σ)max = 0.001
190 parameters	Δρmax = 2.68 e Å−3
0 restraints	Δρmin = −1.19 e Å−3

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 > 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.

	x	y	z	Uiso*/Ueq
Pb1	0.68880 (3)	0.537173 (12)	0.87652 (4)	0.03036 (13)
N1	0.7954 (9)	0.3925 (3)	0.8164 (10)	0.0504 (18)
N2	0.6271 (6)	0.6548 (3)	0.8129 (9)	0.0345 (14)
N3	0.8863 (6)	0.6061 (3)	0.7555 (8)	0.0317 (13)
O1	0.6656 (8)	0.4032 (3)	0.7926 (12)	0.0678 (18)
O2	0.8406 (9)	0.3377 (3)	0.8302 (12)	0.084 (2)
O3	0.8765 (6)	0.4408 (3)	0.8182 (10)	0.0563 (16)
O5	0.6731 (5)	0.5291 (2)	0.5190 (8)	0.0393 (13)
O6	0.5602 (5)	0.4830 (3)	0.2626 (7)	0.0411 (12)
O7	0.8279 (6)	0.5894 (3)	1.2112 (8)	0.0463 (13)
H7A	0.8289	0.5600	1.2993	0.056*
H7B	0.9123	0.5956	1.1805	0.056*
C1	0.4989 (8)	0.6777 (4)	0.8412 (12)	0.0449 (19)
H1	0.4275	0.6480	0.8607	0.054*
C2	0.4664 (9)	0.7424 (4)	0.8432 (13)	0.052 (2)
H2	0.3755	0.7562	0.8633	0.062*
C3	0.5712 (9)	0.7861 (4)	0.8148 (12)	0.049 (2)
H3	0.5521	0.8303	0.8155	0.058*
C4	0.7051 (9)	0.7647 (4)	0.7851 (12)	0.0408 (18)
H4	0.7772	0.7940	0.7661	0.049*
C5	0.7308 (8)	0.6978 (3)	0.7841 (10)	0.0332 (16)
C6	0.8707 (7)	0.6707 (3)	0.7405 (10)	0.0294 (15)
C7	0.9824 (8)	0.7097 (4)	0.6843 (12)	0.0425 (18)
H7	0.9715	0.7544	0.6737	0.051*
C8	1.1074 (8)	0.6813 (4)	0.6453 (13)	0.051 (2)
H8	1.1828	0.7067	0.6091	0.061*
C9	1.1214 (8)	0.6160 (4)	0.6595 (13)	0.047 (2)
H9	1.2056	0.5961	0.6315	0.057*
C10	1.0100 (8)	0.5801 (4)	0.7156 (11)	0.0384 (17)
H10	1.0206	0.5354	0.7267	0.046*
C11	0.5660 (7)	0.5032 (3)	0.4367 (11)	0.0319 (15)

	U11	U22	U33	U12	U13	U23
Pb1	0.02946 (19)	0.03118 (19)	0.03045 (19)	−0.00956 (10)	0.00100 (11)	0.00129 (10)
N1	0.066 (5)	0.037 (4)	0.048 (4)	0.001 (4)	0.006 (3)	0.002 (3)
N2	0.032 (3)	0.036 (3)	0.035 (3)	0.003 (3)	0.002 (3)	−0.002 (3)
N3	0.031 (3)	0.029 (3)	0.035 (3)	−0.007 (2)	0.002 (2)	−0.001 (3)
O1	0.063 (5)	0.044 (4)	0.097 (5)	−0.009 (3)	−0.001 (4)	0.006 (4)
O2	0.119 (7)	0.032 (4)	0.101 (6)	0.018 (4)	0.009 (5)	0.004 (4)
O3	0.043 (3)	0.042 (3)	0.083 (5)	−0.008 (3)	−0.005 (3)	0.006 (3)
O5	0.027 (3)	0.051 (3)	0.040 (3)	−0.011 (2)	0.003 (2)	−0.001 (2)
O6	0.029 (3)	0.065 (3)	0.030 (3)	−0.013 (2)	0.004 (2)	−0.012 (3)
O7	0.040 (3)	0.055 (3)	0.044 (3)	−0.005 (3)	0.003 (2)	0.006 (3)
C1	0.032 (4)	0.062 (6)	0.041 (5)	0.001 (4)	0.005 (3)	−0.001 (4)
C2	0.043 (5)	0.066 (6)	0.047 (5)	0.023 (4)	0.005 (4)	−0.008 (4)
C3	0.065 (6)	0.039 (5)	0.041 (5)	0.017 (4)	−0.007 (4)	−0.005 (4)
C4	0.049 (5)	0.038 (4)	0.035 (4)	0.006 (4)	−0.001 (3)	−0.002 (3)
C5	0.041 (4)	0.030 (4)	0.028 (4)	0.000 (3)	0.001 (3)	−0.005 (3)
C6	0.034 (4)	0.028 (4)	0.026 (4)	−0.005 (3)	0.000 (3)	0.000 (3)
C7	0.042 (4)	0.036 (4)	0.050 (5)	−0.016 (3)	0.004 (3)	0.004 (3)
C8	0.034 (4)	0.061 (6)	0.058 (6)	−0.019 (4)	0.011 (4)	0.001 (4)
C9	0.035 (4)	0.057 (5)	0.051 (5)	0.000 (4)	0.015 (3)	−0.003 (4)
C10	0.037 (4)	0.036 (4)	0.042 (5)	0.000 (3)	0.006 (3)	−0.004 (3)
C11	0.026 (4)	0.033 (4)	0.037 (4)	−0.001 (3)	0.003 (3)	−0.001 (3)

Pb1—O5	2.425 (5)	C1—C2	1.371 (12)
Pb1—N3	2.522 (5)	C1—H1	0.9300
Pb1—N2	2.532 (6)	C2—C3	1.368 (12)
Pb1—O6i	2.572 (5)	C2—H2	0.9300
Pb1—O3	2.718 (6)	C3—C4	1.377 (11)
Pb1—O7	2.809 (6)	C3—H3	0.9300
N1—O2	1.214 (9)	C4—C5	1.401 (10)
N1—O3	1.263 (9)	C4—H4	0.9300
N1—O1	1.269 (10)	C5—C6	1.490 (10)
N2—C1	1.334 (9)	C6—C7	1.401 (9)
N2—C5	1.351 (9)	C7—C8	1.366 (11)
N3—C10	1.336 (9)	C7—H7	0.9300
N3—C6	1.344 (9)	C8—C9	1.358 (12)
O5—C11	1.270 (9)	C8—H8	0.9300
O6—C11	1.249 (9)	C9—C10	1.362 (11)
O6—Pb1i	2.572 (5)	C9—H9	0.9300
O7—H7A	0.8500	C10—H10	0.9300
O7—H7B	0.8499	C11—C11i	1.554 (13)
O5—Pb1—N3	74.93 (17)	C2—C1—H1	118.1
O5—Pb1—N2	83.62 (18)	C3—C2—C1	118.2 (8)
N3—Pb1—N2	65.04 (19)	C3—C2—H2	120.9
O5—Pb1—O6i	66.07 (16)	C1—C2—H2	120.9
N3—Pb1—O6i	131.97 (18)	C2—C3—C4	120.0 (8)
N2—Pb1—O6i	83.30 (19)	C2—C3—H3	120.0
O5—Pb1—O3	80.03 (19)	C4—C3—H3	120.0
N3—Pb1—O3	81.95 (18)	C3—C4—C5	118.8 (8)
N2—Pb1—O3	146.01 (19)	C3—C4—H4	120.6
O6i—Pb1—O3	116.03 (18)	C5—C4—H4	120.6
O5—Pb1—O7	147.62 (16)	N2—C5—C4	121.1 (7)
N3—Pb1—O7	72.69 (17)	N2—C5—C6	116.8 (6)
N2—Pb1—O7	82.64 (18)	C4—C5—C6	122.0 (7)
O6i—Pb1—O7	140.35 (16)	N3—C6—C7	120.5 (7)
O3—Pb1—O7	95.61 (18)	N3—C6—C5	117.1 (6)
O2—N1—O3	121.0 (8)	C7—C6—C5	122.4 (6)
O2—N1—O1	121.2 (8)	C8—C7—C6	119.1 (7)
O3—N1—O1	117.7 (7)	C8—C7—H7	120.4
C1—N2—C5	118.2 (7)	C6—C7—H7	120.4
C1—N2—Pb1	121.7 (5)	C9—C8—C7	119.8 (7)
C5—N2—Pb1	119.0 (5)	C9—C8—H8	120.1
C10—N3—C6	118.7 (6)	C7—C8—H8	120.1
C10—N3—Pb1	121.2 (5)	C8—C9—C10	118.9 (8)
C6—N3—Pb1	120.0 (4)	C8—C9—H9	120.5
N1—O3—Pb1	99.7 (5)	C10—C9—H9	120.5
C11—O5—Pb1	119.4 (4)	N3—C10—C9	123.0 (7)
C11—O6—Pb1i	114.5 (4)	N3—C10—H10	118.5
Pb1—O7—H7A	106.6	C9—C10—H10	118.5
Pb1—O7—H7B	107.0	O6—C11—O5	124.5 (6)
H7A—O7—H7B	106.7	O6—C11—C11i	118.5 (8)
N2—C1—C2	123.8 (8)	O5—C11—C11i	117.0 (8)
N2—C1—H1	118.1

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O5ii	0.85	2.23	2.875 (7)	133
O7—H7B···O3iii	0.85	2.16	2.912 (8)	148

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7A⋯O5i	0.85	2.23	2.875 (7)	133
O7—H7B⋯O3ii	0.85	2.16	2.912 (8)	148

Symmetry codes: (i) ; (ii) .