Di-μ-benzoato-κO,O':O;κO:O,O'-bis-[(acetato-κO)(1,10-phenanthroline-κN,N')lead(II)] dihydrate.

The title compound, [Pb(2)(CH(3)COO)(2)(C(7)H(5)O(2))(2)(C(12)H(8)N(2))(2)]·2H(2)O, consists of dimeric units built up around a crystallographic centre of symmetry and two non-coordinating water mol-ecules. Each Pb(II) unit is six-coordinated by a bidentate 1,10-phenanthroline (phen) ligand, a monodentate acetate anion and a bidentate benzoate anion, which also acts as a bridge linking the two Pb(II) atoms. The crystal packing is stabilized by O-H⋯O hydrogen bonds and by π-π inter-actions between the phen rings of neighboring mol-ecules, with a centroid-centroid distance of 3.577 (3) Å.

Related literature

For information on the coordination chemistry of lead, see: Shimoni-Livny et al. (1998 ▶). For related structures, see: Li & Yang (2004 ▶); Xuan et al. (2008 ▶); Xuan & Zhao (2007 ▶); Zhao et al. (2007 ▶); Zhu et al. (2004 ▶).

Experimental

Crystal data

[Pb2(C2H3O2)2(C7H5O2)2(C12H8N2)2]·2H2O

M = 1171.15

Monoclinic,

a = 11.809 (4) Å

b = 13.910 (5) Å

c = 12.290 (4) Å

β = 107.392 (4)°

V = 1926.5 (11) Å3

Z = 2

Mo Kα radiation

μ = 8.79 mm−1

T = 294 K

0.11 × 0.07 × 0.05 mm

Data collection

Bruker SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 1997 ▶) T min = 0.445, T max = 0.668

16820 measured reflections

4417 independent reflections

3343 reflections with I > 2σ(I)

R int = 0.044

Refinement

R[F 2 > 2σ(F 2)] = 0.029

wR(F 2) = 0.057

S = 1.03

4417 reflections

263 parameters

18 restraints

H-atom parameters constrained

Δρmax = 0.73 e Å−3

Δρmin = −0.85 e Å−3

Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); 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: publCIF (Westrip, 2009 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809025896/sj2634sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809025896/sj2634Isup2.hkl

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

[Pb2(C2H3O2)2(C7H5O2)2(C12H8N2)2]·2H2O	F(000) = 1120
Mr = 1171.15	Dx = 2.019 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 3638 reflections
a = 11.809 (4) Å	θ = 2.3–23.1°
b = 13.910 (5) Å	µ = 8.79 mm−1
c = 12.290 (4) Å	T = 294 K
β = 107.392 (4)°	Block, colourless
V = 1926.5 (11) Å3	0.11 × 0.07 × 0.05 mm
Z = 2

Bruker SMART CCD area-detector diffractometer	4417 independent reflections
Radiation source: fine-focus sealed tube	3343 reflections with I > 2σ(I)
graphite	Rint = 0.044
φ and ω scans	θmax = 27.5°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Bruker, 1997)	h = −15→15
Tmin = 0.445, Tmax = 0.668	k = −18→18
16820 measured reflections	l = −15→15

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)] = 0.029	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.057	H-atom parameters constrained
S = 1.03	w = 1/[σ2(Fo2) + (0.0213P)2] where P = (Fo2 + 2Fc2)/3
4417 reflections	(Δ/σ)max = 0.001
263 parameters	Δρmax = 0.73 e Å−3
18 restraints	Δρmin = −0.85 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 takeninto account individually in the estimation of e.s.d.'s in distances, anglesand torsion angles; correlations between e.s.d.'s in cell parameters are onlyused 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
Pb1	0.173727 (14)	0.043850 (12)	0.498903 (14)	0.03372 (6)
N1	0.2720 (3)	−0.0825 (3)	0.3883 (3)	0.0359 (9)
N2	0.3507 (3)	0.1041 (3)	0.4296 (3)	0.0311 (8)
O1	−0.0112 (3)	−0.0419 (2)	0.3725 (3)	0.0457 (8)
O2	0.0805 (3)	0.0648 (2)	0.2958 (3)	0.0423 (8)
O3	0.0861 (3)	0.2009 (2)	0.4678 (3)	0.0518 (7)
O4	0.2321 (3)	0.2249 (2)	0.6272 (3)	0.0544 (8)
O5	0.3305 (3)	0.3221 (3)	0.8466 (3)	0.0727 (12)
H1W	0.3119	0.2922	0.7852	0.109*
H2W	0.4037	0.3247	0.8745	0.109*
C1	−0.0917 (4)	−0.0099 (3)	0.1737 (4)	0.0316 (10)
C2	−0.0902 (4)	0.0467 (4)	0.0825 (4)	0.0496 (13)
H2	−0.0340	0.0953	0.0923	0.059*
C3	−0.1716 (5)	0.0322 (4)	−0.0240 (4)	0.0610 (16)
H3	−0.1702	0.0710	−0.0852	0.073*
C4	−0.2551 (5)	−0.0405 (4)	−0.0383 (5)	0.0591 (15)
H4	−0.3101	−0.0508	−0.1094	0.071*
C5	−0.2564 (4)	−0.0974 (4)	0.0529 (4)	0.0517 (14)
H5	−0.3130	−0.1457	0.0433	0.062*
C6	−0.1751 (4)	−0.0836 (3)	0.1580 (4)	0.0408 (12)
H6	−0.1757	−0.1233	0.2187	0.049*
C7	−0.0022 (4)	0.0053 (3)	0.2875 (4)	0.0358 (11)
C8	0.2340 (5)	−0.1718 (4)	0.3670 (4)	0.0478 (13)
H8	0.1693	−0.1909	0.3903	0.057*
C9	0.2844 (5)	−0.2388 (4)	0.3123 (4)	0.0555 (15)
H9	0.2538	−0.3008	0.2992	0.067*
C10	0.3789 (5)	−0.2130 (4)	0.2779 (4)	0.0510 (14)
H10	0.4144	−0.2572	0.2415	0.061*
C11	0.4235 (4)	−0.1176 (4)	0.2979 (4)	0.0408 (12)
C12	0.5245 (5)	−0.0854 (4)	0.2670 (4)	0.0493 (14)
H12	0.5628	−0.1274	0.2307	0.059*
C13	0.5649 (4)	0.0053 (4)	0.2898 (4)	0.0467 (13)
H13	0.6318	0.0242	0.2703	0.056*
C14	0.5072 (4)	0.0736 (3)	0.3438 (4)	0.0342 (11)
C15	0.5469 (4)	0.1678 (4)	0.3670 (4)	0.0426 (12)
H15	0.6125	0.1896	0.3471	0.051*
C16	0.4878 (4)	0.2280 (4)	0.4197 (4)	0.0429 (12)
H16	0.5116	0.2917	0.4345	0.051*
C17	0.3918 (4)	0.1927 (3)	0.4507 (4)	0.0367 (11)
H17	0.3542	0.2338	0.4885	0.044*
C18	0.4080 (4)	0.0436 (3)	0.3760 (4)	0.0306 (10)
C19	0.3653 (4)	−0.0553 (3)	0.3537 (4)	0.0329 (10)
C20	0.1402 (5)	0.2519 (4)	0.5538 (4)	0.0513 (7)
C21	0.0877 (5)	0.3482 (4)	0.5642 (4)	0.0572 (11)
H21A	0.0272	0.3411	0.6012	0.086*
H21B	0.0535	0.3751	0.4896	0.086*
H21C	0.1487	0.3902	0.6084	0.086*

	U11	U22	U33	U12	U13	U23
Pb1	0.02875 (9)	0.04061 (11)	0.03074 (10)	−0.00348 (9)	0.00726 (7)	−0.00015 (9)
N1	0.036 (2)	0.031 (2)	0.038 (2)	−0.0030 (17)	0.0064 (18)	−0.0009 (17)
N2	0.030 (2)	0.033 (2)	0.030 (2)	−0.0017 (17)	0.0089 (16)	0.0002 (16)
O1	0.0395 (19)	0.065 (2)	0.0321 (18)	−0.0089 (17)	0.0104 (15)	0.0032 (17)
O2	0.043 (2)	0.039 (2)	0.0392 (19)	−0.0107 (15)	0.0051 (16)	0.0036 (15)
O3	0.0595 (17)	0.0502 (16)	0.0416 (15)	0.0045 (13)	0.0091 (13)	−0.0036 (13)
O4	0.0521 (18)	0.0559 (18)	0.0500 (17)	0.0017 (15)	0.0074 (14)	0.0008 (15)
O5	0.052 (2)	0.087 (3)	0.085 (3)	−0.006 (2)	0.029 (2)	−0.008 (2)
C1	0.028 (2)	0.035 (2)	0.030 (2)	0.004 (2)	0.007 (2)	−0.001 (2)
C2	0.046 (3)	0.056 (3)	0.040 (3)	−0.010 (3)	0.004 (2)	0.007 (3)
C3	0.067 (4)	0.073 (4)	0.037 (3)	−0.004 (3)	0.007 (3)	0.010 (3)
C4	0.058 (4)	0.062 (4)	0.041 (3)	0.003 (3)	−0.010 (3)	−0.006 (3)
C5	0.041 (3)	0.047 (3)	0.055 (3)	−0.005 (2)	−0.004 (3)	−0.007 (3)
C6	0.039 (3)	0.038 (3)	0.043 (3)	0.000 (2)	0.009 (2)	0.003 (2)
C7	0.036 (3)	0.038 (3)	0.034 (3)	0.004 (2)	0.011 (2)	−0.004 (2)
C8	0.050 (3)	0.043 (3)	0.045 (3)	−0.011 (3)	0.007 (3)	0.000 (2)
C9	0.075 (4)	0.033 (3)	0.048 (3)	−0.002 (3)	0.002 (3)	−0.007 (3)
C10	0.071 (4)	0.045 (3)	0.031 (3)	0.013 (3)	0.007 (3)	−0.008 (2)
C11	0.047 (3)	0.046 (3)	0.025 (2)	0.015 (2)	0.005 (2)	0.002 (2)
C12	0.051 (3)	0.059 (4)	0.040 (3)	0.025 (3)	0.017 (3)	0.005 (3)
C13	0.039 (3)	0.068 (4)	0.038 (3)	0.018 (3)	0.019 (2)	0.017 (3)
C14	0.024 (2)	0.050 (3)	0.027 (2)	0.006 (2)	0.0062 (19)	0.013 (2)
C15	0.029 (3)	0.057 (3)	0.039 (3)	−0.007 (2)	0.007 (2)	0.013 (2)
C16	0.038 (3)	0.043 (3)	0.047 (3)	−0.012 (2)	0.011 (2)	0.000 (2)
C17	0.034 (3)	0.039 (3)	0.036 (3)	−0.004 (2)	0.009 (2)	−0.002 (2)
C18	0.027 (2)	0.034 (2)	0.027 (2)	0.003 (2)	0.0023 (18)	0.002 (2)
C19	0.035 (2)	0.035 (3)	0.023 (2)	0.007 (2)	−0.0002 (19)	0.005 (2)
C20	0.0571 (16)	0.0509 (16)	0.0431 (15)	0.0041 (13)	0.0105 (13)	−0.0033 (12)
C21	0.062 (2)	0.055 (2)	0.049 (2)	0.0080 (19)	0.0087 (18)	−0.0094 (18)

Pb1—O3	2.399 (3)	C5—H5	0.9300
Pb1—O2	2.426 (3)	C6—H6	0.9300
Pb1—O1	2.565 (3)	C8—C9	1.384 (7)
Pb1—O1i	2.828 (3)	C8—H8	0.9300
Pb1—N2	2.619 (4)	C9—C10	1.355 (7)
Pb1—N1	2.688 (4)	C9—H9	0.9300
Pb1—C7	2.851 (5)	C10—C11	1.421 (7)
N1—C8	1.320 (6)	C10—H10	0.9300
N1—C19	1.349 (6)	C11—C19	1.405 (6)
N2—C17	1.321 (5)	C11—C12	1.428 (7)
N2—C18	1.366 (5)	C12—C13	1.348 (7)
O1—C7	1.264 (5)	C12—H12	0.9300
O2—C7	1.261 (5)	C13—C14	1.442 (7)
O3—C20	1.273 (6)	C13—H13	0.9300
O4—C20	1.244 (6)	C14—C15	1.393 (6)
O5—H1W	0.8317	C14—C18	1.407 (6)
O5—H2W	0.8295	C15—C16	1.370 (6)
C1—C2	1.375 (6)	C15—H15	0.9300
C1—C6	1.394 (6)	C16—C17	1.390 (6)
C1—C7	1.495 (6)	C16—H16	0.9300
C2—C3	1.387 (7)	C17—H17	0.9300
C2—H2	0.9300	C18—C19	1.463 (6)
C3—C4	1.387 (7)	C20—C21	1.498 (7)
C3—H3	0.9300	C21—H21A	0.9600
C4—C5	1.377 (7)	C21—H21B	0.9600
C4—H4	0.9300	C21—H21C	0.9600
C5—C6	1.373 (6)
O3—Pb1—O2	71.68 (11)	O1—C7—Pb1	64.1 (2)
O3—Pb1—O1	94.51 (11)	C1—C7—Pb1	176.6 (4)
O2—Pb1—O1	52.41 (10)	N1—C8—C9	124.1 (5)
O3—Pb1—N2	90.27 (12)	N1—C8—H8	118.0
O2—Pb1—N2	77.74 (11)	C9—C8—H8	118.0
O1—Pb1—N2	124.72 (10)	C10—C9—C8	119.2 (5)
O3—Pb1—N1	138.24 (11)	C10—C9—H9	120.4
O2—Pb1—N1	71.93 (11)	C8—C9—H9	120.4
O1—Pb1—N1	78.91 (11)	C9—C10—C11	119.3 (5)
N2—Pb1—N1	62.48 (11)	C9—C10—H10	120.3
O3—Pb1—C7	82.19 (12)	C11—C10—H10	120.3
O2—Pb1—C7	26.08 (12)	C19—C11—C10	116.8 (5)
O1—Pb1—C7	26.33 (11)	C19—C11—C12	120.4 (5)
N2—Pb1—C7	101.47 (13)	C10—C11—C12	122.8 (5)
N1—Pb1—C7	73.94 (12)	C13—C12—C11	120.7 (5)
C8—N1—C19	117.6 (4)	C13—C12—H12	119.7
C8—N1—Pb1	122.9 (3)	C11—C12—H12	119.7
C19—N1—Pb1	119.5 (3)	C12—C13—C14	121.8 (5)
C17—N2—C18	117.6 (4)	C12—C13—H13	119.1
C17—N2—Pb1	121.1 (3)	C14—C13—H13	119.1
C18—N2—Pb1	121.2 (3)	C15—C14—C18	118.6 (4)
C7—O1—Pb1	89.6 (3)	C15—C14—C13	122.6 (5)
C7—O2—Pb1	96.1 (3)	C18—C14—C13	118.8 (5)
C20—O3—Pb1	106.8 (3)	C16—C15—C14	119.0 (4)
H1W—O5—H2W	110.9	C16—C15—H15	120.5
C2—C1—C6	119.3 (4)	C14—C15—H15	120.5
C2—C1—C7	120.2 (4)	C15—C16—C17	119.1 (5)
C6—C1—C7	120.5 (4)	C15—C16—H16	120.5
C1—C2—C3	120.8 (5)	C17—C16—H16	120.5
C1—C2—H2	119.6	N2—C17—C16	124.0 (4)
C3—C2—H2	119.6	N2—C17—H17	118.0
C4—C3—C2	119.4 (5)	C16—C17—H17	118.0
C4—C3—H3	120.3	N2—C18—C14	121.8 (4)
C2—C3—H3	120.3	N2—C18—C19	118.5 (4)
C5—C4—C3	119.7 (5)	C14—C18—C19	119.7 (4)
C5—C4—H4	120.1	N1—C19—C11	123.1 (4)
C3—C4—H4	120.1	N1—C19—C18	118.2 (4)
C6—C5—C4	120.8 (5)	C11—C19—C18	118.7 (4)
C6—C5—H5	119.6	O4—C20—O3	123.1 (5)
C4—C5—H5	119.6	O4—C20—C21	120.1 (5)
C5—C6—C1	119.9 (5)	O3—C20—C21	116.8 (5)
C5—C6—H6	120.0	C20—C21—H21A	109.5
C1—C6—H6	120.0	C20—C21—H21B	109.5
O2—C7—O1	121.9 (4)	H21A—C21—H21B	109.5
O2—C7—C1	118.9 (4)	C20—C21—H21C	109.5
O1—C7—C1	119.2 (4)	H21A—C21—H21C	109.5
O2—C7—Pb1	57.8 (2)	H21B—C21—H21C	109.5
O3—Pb1—N1—C8	−124.4 (3)	C6—C1—C7—O1	−8.0 (7)
O2—Pb1—N1—C8	−93.9 (4)	O3—Pb1—C7—O2	63.8 (3)
O1—Pb1—N1—C8	−40.1 (3)	O1—Pb1—C7—O2	−179.1 (5)
N2—Pb1—N1—C8	−179.2 (4)	N2—Pb1—C7—O2	−24.9 (3)
C7—Pb1—N1—C8	−66.7 (4)	N1—Pb1—C7—O2	−81.6 (3)
O3—Pb1—N1—C19	56.5 (4)	O3—Pb1—C7—O1	−117.1 (3)
O2—Pb1—N1—C19	87.0 (3)	O2—Pb1—C7—O1	179.1 (5)
O1—Pb1—N1—C19	140.8 (3)	N2—Pb1—C7—O1	154.2 (3)
N2—Pb1—N1—C19	1.7 (3)	N1—Pb1—C7—O1	97.5 (3)
C7—Pb1—N1—C19	114.2 (3)	C19—N1—C8—C9	0.4 (7)
O3—Pb1—N2—C17	34.5 (3)	Pb1—N1—C8—C9	−178.7 (4)
O2—Pb1—N2—C17	105.7 (3)	N1—C8—C9—C10	0.2 (8)
O1—Pb1—N2—C17	130.2 (3)	C8—C9—C10—C11	−0.5 (7)
N1—Pb1—N2—C17	−178.5 (3)	C9—C10—C11—C19	0.2 (7)
C7—Pb1—N2—C17	116.6 (3)	C9—C10—C11—C12	178.4 (5)
O3—Pb1—N2—C18	−149.1 (3)	C19—C11—C12—C13	−0.6 (7)
O2—Pb1—N2—C18	−77.9 (3)	C10—C11—C12—C13	−178.6 (4)
O1—Pb1—N2—C18	−53.4 (3)	C11—C12—C13—C14	−1.3 (7)
N1—Pb1—N2—C18	−2.1 (3)	C12—C13—C14—C15	−179.3 (4)
C7—Pb1—N2—C18	−67.0 (3)	C12—C13—C14—C18	1.7 (7)
O3—Pb1—O1—C7	62.2 (3)	C18—C14—C15—C16	−0.3 (6)
O2—Pb1—O1—C7	−0.5 (3)	C13—C14—C15—C16	−179.3 (4)
N2—Pb1—O1—C7	−31.3 (3)	C14—C15—C16—C17	1.5 (7)
N1—Pb1—O1—C7	−76.1 (3)	C18—N2—C17—C16	1.3 (6)
O3—Pb1—O2—C7	−110.5 (3)	Pb1—N2—C17—C16	177.8 (3)
O1—Pb1—O2—C7	0.5 (3)	C15—C16—C17—N2	−2.0 (7)
N2—Pb1—O2—C7	155.0 (3)	C17—N2—C18—C14	−0.1 (6)
N1—Pb1—O2—C7	90.3 (3)	Pb1—N2—C18—C14	−176.5 (3)
O2—Pb1—O3—C20	−157.3 (4)	C17—N2—C18—C19	178.9 (4)
O1—Pb1—O3—C20	154.8 (3)	Pb1—N2—C18—C19	2.5 (5)
N2—Pb1—O3—C20	−80.3 (3)	C15—C14—C18—N2	−0.4 (6)
N1—Pb1—O3—C20	−126.8 (3)	C13—C14—C18—N2	178.6 (4)
C7—Pb1—O3—C20	178.1 (4)	C15—C14—C18—C19	−179.4 (4)
C6—C1—C2—C3	1.0 (8)	C13—C14—C18—C19	−0.3 (6)
C7—C1—C2—C3	178.9 (5)	C8—N1—C19—C11	−0.7 (6)
C1—C2—C3—C4	−0.2 (9)	Pb1—N1—C19—C11	178.4 (3)
C2—C3—C4—C5	0.0 (9)	C8—N1—C19—C18	179.6 (4)
C3—C4—C5—C6	−0.6 (9)	Pb1—N1—C19—C18	−1.2 (5)
C4—C5—C6—C1	1.4 (8)	C10—C11—C19—N1	0.4 (6)
C2—C1—C6—C5	−1.6 (7)	C12—C11—C19—N1	−177.7 (4)
C7—C1—C6—C5	−179.5 (4)	C10—C11—C19—C18	−180.0 (4)
Pb1—O2—C7—O1	−1.0 (5)	C12—C11—C19—C18	1.9 (6)
Pb1—O2—C7—C1	179.3 (4)	N2—C18—C19—N1	−0.8 (6)
Pb1—O1—C7—O2	0.9 (5)	C14—C18—C19—N1	178.2 (4)
Pb1—O1—C7—C1	−179.4 (4)	N2—C18—C19—C11	179.6 (4)
C2—C1—C7—O2	−6.3 (7)	C14—C18—C19—C11	−1.4 (6)
C6—C1—C7—O2	171.7 (4)	Pb1—O3—C20—O4	10.0 (7)
C2—C1—C7—O1	174.0 (4)	Pb1—O3—C20—C21	−169.7 (4)

D—H···A	D—H	H···A	D···A	D—H···A
O5—H2W···O3ii	0.83	2.15	2.958 (5)	166
O5—H1W···O4	0.83	2.11	2.928 (5)	169

Table 1

Selected bond lengths (Å)

Pb1—O3	2.399 (3)
Pb1—O2	2.426 (3)
Pb1—O1	2.565 (3)
Pb1—O1i	2.828 (3)
Pb1—N2	2.619 (4)
Pb1—N1	2.688 (4)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H2W⋯O3ii	0.83	2.15	2.958 (5)	166
O5—H1W⋯O4	0.83	2.11	2.928 (5)	169

Symmetry code: (ii) .