A three-dimensional Pb^II coordination framework: poly[[[mu]₄-(E)-2,2'-(diazene-1,2-di­yl)dibenzoato]di­methanol­lead(II)]

In the title coordination polymer, [Pb(C₁₄H₈N₂O₄)(CH₃OH)₂]_n, the asymmetric unit contains half of a Pb^II cation, half of a 2,2'-(diazene-1,2-di­yl)dibenzoate dianionic ligand (denoted L^2-) and one methanol ligand. Each Pb^II centre is eight-coordinated by six O atoms of chelating/bridging carboxyl­ate groups from four L^2- ligands and two O atoms from two terminal methanol ligands, forming a distorted dodeca­hedron. The [PbL₂(MeOH)₂] subunits are inter­linked via the sharing of two carboxyl­ate O atoms to form a one-dimensional [PbL₂(MeOH)₂]_n chain. Adjacent chains are further connected by L^2- ligands, giving rise to a two-dimensional layer, and these layers are bridged by L^2- linkers to afford a three-dimensional framework with a 4¹²6³ topology.

Computing details

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXS2013 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008); molecular graphics: XP (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).

Poly[[µ₄-(E)-2,2'-(diazene-1,2-diyl)dibenzoato]dimethanollead(II)]

Crystal data

[Pb(C14H8N2O4)(CH4O)2]	F(000) = 1024
Mr = 539.50	Dx = 2.059 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 20.508 (4) Å	Cell parameters from 2584 reflections
b = 10.899 (2) Å	θ = 3.7–26.8°
c = 8.2818 (17) Å	µ = 9.73 mm^−1
β = 109.90 (3)°	T = 296 K
V = 1740.5 (7) Å^3	Block, yellow
Z = 4	0.28 × 0.25 × 0.15 mm

Data collection

Bruker APEXII CCD area-detector diffractometer	1446 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.044
φ and ω scans	θmax = 25.3°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Bruker, 2003)	h = −17→24
Tmin = 0.082, Tmax = 0.232	k = −12→13
4608 measured reflections	l = −9→8
1571 independent reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.028	Hydrogen site location: mixed
wR(F^2) = 0.067	H-atom parameters constrained
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0354P)^2] where P = (Fo^2 + 2Fc^2)/3
1571 reflections	(Δ/σ)max = 0.001
115 parameters	Δρmax = 1.57 e Å^−3
0 restraints	Δρmin = −1.52 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Pb1	0.5000	0.55017 (2)	0.7500	0.03200 (7)
C1	0.41692 (19)	0.3406 (4)	0.5626 (5)	0.0354 (10)
C2	0.3883 (2)	0.2213 (4)	0.4781 (5)	0.0344 (10)
C3	0.4313 (2)	0.1452 (4)	0.4251 (6)	0.0474 (12)
H3	0.4765	0.1692	0.4403	0.057*
C4	0.4066 (3)	0.0331 (5)	0.3492 (8)	0.0593 (16)
H4	0.4356	−0.0178	0.3137	0.071*
C5	0.3402 (3)	−0.0031 (5)	0.3261 (7)	0.0560 (15)
H5	0.3246	−0.0792	0.2775	0.067*
C6	0.2959 (3)	0.0728 (4)	0.3746 (7)	0.0486 (14)
H6	0.2504	0.0488	0.3565	0.058*
C7	0.3200 (2)	0.1851 (4)	0.4502 (5)	0.0357 (11)
C8	0.6640 (3)	0.6853 (7)	0.9810 (8)	0.078 (2)
H8A	0.6808	0.6038	1.0151	0.094*
H8B	0.6931	0.7436	1.0601	0.094*
H8C	0.6647	0.7014	0.8677	0.094*
N1	0.27692 (17)	0.2721 (3)	0.4925 (5)	0.0407 (9)
O1	0.44550 (17)	0.4094 (3)	0.4864 (4)	0.0481 (8)
O2	0.41432 (17)	0.3673 (3)	0.7057 (4)	0.0549 (9)
O3	0.59552 (17)	0.6959 (4)	0.9811 (5)	0.0610 (11)
H3A	0.6047	0.6754	1.0856	0.073*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb1	0.02566 (10)	0.03958 (12)	0.03090 (11)	0.000	0.00982 (8)	0.000
C1	0.0239 (18)	0.045 (2)	0.037 (2)	−0.0059 (17)	0.0093 (15)	0.0007 (19)
C2	0.0322 (19)	0.042 (2)	0.0292 (19)	−0.0040 (17)	0.0107 (16)	0.0029 (18)
C3	0.037 (2)	0.051 (3)	0.056 (3)	0.007 (2)	0.0178 (19)	0.003 (2)
C4	0.067 (3)	0.055 (3)	0.061 (3)	0.005 (2)	0.029 (3)	−0.005 (2)
C5	0.069 (3)	0.041 (2)	0.057 (3)	−0.008 (3)	0.020 (3)	−0.008 (3)
C6	0.044 (3)	0.049 (3)	0.049 (3)	−0.014 (2)	0.012 (2)	−0.003 (2)
C7	0.031 (2)	0.041 (2)	0.033 (2)	−0.0041 (17)	0.0074 (17)	0.0051 (18)
C8	0.051 (3)	0.114 (5)	0.063 (3)	−0.009 (3)	0.012 (3)	0.004 (4)
N1	0.0290 (15)	0.045 (2)	0.0476 (19)	−0.0076 (14)	0.0122 (15)	−0.0003 (17)
O1	0.0532 (18)	0.0523 (16)	0.0464 (17)	−0.0205 (15)	0.0267 (14)	−0.0068 (16)
O2	0.0608 (19)	0.069 (2)	0.0392 (16)	−0.0251 (16)	0.0229 (14)	−0.0137 (16)
O3	0.0488 (19)	0.085 (3)	0.0480 (18)	−0.0177 (17)	0.0145 (15)	0.0050 (18)

Geometric parameters (Å, º)

Pb1—O1^i	2.590 (3)	C4—C5	1.368 (9)
Pb1—O1	2.590 (3)	C4—H4	0.9300
Pb1—O2	2.599 (3)	C5—C6	1.386 (9)
Pb1—O2^i	2.599 (3)	C5—H5	0.9300
Pb1—O1^ii	2.601 (4)	C6—C7	1.387 (6)
Pb1—O1^iii	2.601 (4)	C6—H6	0.9300
Pb1—O3	2.733 (3)	C7—N1	1.418 (6)
Pb1—O3^i	2.733 (3)	C8—O3	1.409 (7)
C1—O2	1.239 (5)	C8—H8A	0.9600
C1—O1	1.248 (6)	C8—H8B	0.9600
C1—C2	1.498 (6)	C8—H8C	0.9600
C2—C3	1.386 (7)	N1—N1^iv	1.249 (7)
C2—C7	1.396 (6)	O1—Pb1^iii	2.601 (4)
C3—C4	1.388 (7)	O3—H3A	0.8500
C3—H3	0.9300
O1^i—Pb1—O1	107.34 (15)	C3—C2—C1	118.5 (4)
O1^i—Pb1—O2	75.03 (11)	C7—C2—C1	122.3 (4)
O1—Pb1—O2	49.45 (11)	C2—C3—C4	119.8 (5)
O1^i—Pb1—O2^i	49.45 (11)	C2—C3—H3	120.1
O1—Pb1—O2^i	75.03 (11)	C4—C3—H3	120.1
O2—Pb1—O2^i	79.88 (16)	C5—C4—C3	120.6 (6)
O1^i—Pb1—O1^ii	68.82 (12)	C5—C4—H4	119.7
O1—Pb1—O1^ii	124.21 (13)	C3—C4—H4	119.7
O2—Pb1—O1^ii	78.05 (11)	C4—C5—C6	120.5 (5)
O2^i—Pb1—O1^ii	117.84 (10)	C4—C5—H5	119.7
O1^i—Pb1—O1^iii	124.21 (13)	C6—C5—H5	119.7
O1—Pb1—O1^iii	68.82 (12)	C5—C6—C7	119.3 (5)
O2—Pb1—O1^iii	117.84 (10)	C5—C6—H6	120.4
O2^i—Pb1—O1^iii	78.05 (11)	C7—C6—H6	120.4
O1^ii—Pb1—O1^iii	160.48 (15)	C6—C7—C2	120.5 (4)
O1^i—Pb1—O3	75.71 (11)	C6—C7—N1	123.0 (4)
O1—Pb1—O3	159.27 (12)	C2—C7—N1	116.4 (4)
O2—Pb1—O3	146.44 (11)	O3—C8—H8A	109.5
O2^i—Pb1—O3	93.31 (11)	O3—C8—H8B	109.5
O1^ii—Pb1—O3	76.32 (11)	H8A—C8—H8B	109.5
O1^iii—Pb1—O3	92.26 (10)	O3—C8—H8C	109.5
O1^i—Pb1—O3^i	159.27 (12)	H8A—C8—H8C	109.5
O1—Pb1—O3^i	75.71 (11)	H8B—C8—H8C	109.5
O2—Pb1—O3^i	93.31 (11)	N1^iv—N1—C7	114.4 (5)
O2^i—Pb1—O3^i	146.44 (11)	C1—O1—Pb1	94.1 (3)
O1^ii—Pb1—O3^i	92.26 (10)	C1—O1—Pb1^iii	151.5 (3)
O1^iii—Pb1—O3^i	76.32 (11)	Pb1—O1—Pb1^iii	111.18 (12)
O3—Pb1—O3^i	108.94 (16)	C1—O2—Pb1	93.9 (3)
O2—C1—O1	121.5 (4)	C8—O3—Pb1	115.4 (4)
O2—C1—C2	120.9 (4)	C8—O3—H3A	96.0
O1—C1—C2	117.5 (4)	Pb1—O3—H3A	114.7
C3—C2—C7	119.2 (4)
O2—C1—C2—C3	−125.5 (5)	C1—C2—C7—C6	−178.7 (4)
O1—C1—C2—C3	52.0 (5)	C3—C2—C7—N1	−174.2 (4)
O2—C1—C2—C7	54.9 (6)	C1—C2—C7—N1	5.4 (6)
O1—C1—C2—C7	−127.6 (5)	C6—C7—N1—N1^iv	21.3 (7)
C7—C2—C3—C4	−1.6 (7)	C2—C7—N1—N1^iv	−162.9 (5)
C1—C2—C3—C4	178.8 (4)	O2—C1—O1—Pb1	10.3 (4)
C2—C3—C4—C5	0.0 (8)	C2—C1—O1—Pb1	−167.2 (3)
C3—C4—C5—C6	1.5 (9)	O2—C1—O1—Pb1^iii	163.5 (4)
C4—C5—C6—C7	−1.4 (8)	C2—C1—O1—Pb1^iii	−14.0 (8)
C5—C6—C7—C2	−0.3 (7)	O1—C1—O2—Pb1	−10.2 (4)
C5—C6—C7—N1	175.4 (5)	C2—C1—O2—Pb1	167.2 (3)
C3—C2—C7—C6	1.7 (6)

Symmetry codes: (i) −x+1, y, −z+3/2; (ii) x, −y+1, z+1/2; (iii) −x+1, −y+1, −z+1; (iv) −x+1/2, −y+1/2, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3A···O2^v	0.85	1.95	2.756 (5)	157

Symmetry code: (v) −x+1, −y+1, −z+2.