Poly[(μ₅-3-carb­oxy­benzene-1,2-di­carboxyl­ato)lead(II)]: a helical lead(II) coordination polymer

In the title polymer, [Pb(C₉H₄O₆)]_n, the asymmetric unit con­tains a monomer of a Pb^II cation with a doubly de­pro­tonated 3-carb­oxy­benzene-1,2-di­carboxyl­ate dianion (1,2,3-Hbtc²⁻). Each Pb^II centre is seven-coordinated by seven O atoms of bridging carboxy/carboxyl­ate groups from five 1,2,3-Hbtc²⁻ ligands, forming a distorted penta­gonal bipyramid. The Pb^II cations are bridged by 1,2,3-Hbtc²⁻ anions, yielding two-dimensional chiral layers. The layers are stacked above each other to generate a three-dimensional supra­molecular architecture via a combination of C—H...O inter­actions. The thermogravimetric and optical properties are also reported.

Computing details

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXL2013 (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: SHELXL2013 (Sheldrick, 2008) and PLATON (Spek, 2009).

Poly[(µ₅-3-carboxybenzene-1,2-dicarboxylato)lead(II)]

Crystal data

[Pb(C9H4O6)]	Dx = 3.033 Mg m^−3
Mr = 415.31	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121	Cell parameters from 2173 reflections
a = 4.7900 (8) Å	θ = 2.8–23.4°
b = 7.7306 (12) Å	µ = 18.56 mm^−1
c = 24.562 (4) Å	T = 296 K
V = 909.5 (3) Å^3	Block, colourless
Z = 4	0.08 × 0.07 × 0.07 mm
F(000) = 752

Data collection

Bruker APEXII CCD area-detector diffractometer	1920 reflections with I > 2σ(I)
φ and ω scans	Rint = 0.062
Absorption correction: multi-scan (SADABS; Bruker, 2003)	θmax = 27.6°, θmin = 2.8°
Tmin = 0.318, Tmax = 0.357	h = −6→6
7913 measured reflections	k = −10→10
2091 independent reflections	l = −31→30

Refinement

Refinement on F^2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.030	w = 1/[σ^2(Fo^2) + (0.0002P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.055	(Δ/σ)max < 0.001
S = 0.95	Δρmax = 0.92 e Å^−3
2091 reflections	Δρmin = −1.89 e Å^−3
146 parameters	Absolute structure: Flack x parameter determined using 712 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons & Flack, 2004)
0 restraints	Absolute structure parameter: 0.006 (13)

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	0.57304 (7)	0.31544 (5)	0.22456 (2)	0.01720 (11)
C1	0.3478 (18)	0.2908 (14)	0.3850 (4)	0.015 (2)
C2	0.193 (2)	0.4305 (15)	0.3657 (4)	0.019 (2)
C3	0.148 (2)	0.5760 (15)	0.4001 (4)	0.020 (2)
C4	0.269 (2)	0.5808 (15)	0.4512 (4)	0.022 (2)
H4	0.2386	0.6760	0.4736	0.027*
C5	0.435 (3)	0.4448 (15)	0.4695 (4)	0.029 (3)
H5	0.5232	0.4517	0.5031	0.035*
C6	0.467 (2)	0.2998 (16)	0.4374 (4)	0.026 (2)
H6	0.5685	0.2063	0.4506	0.031*
C7	0.386 (2)	0.1275 (14)	0.3530 (5)	0.024 (3)
C8	0.063 (2)	0.4280 (12)	0.3089 (4)	0.015 (2)
C9	−0.030 (2)	0.7199 (12)	0.3813 (4)	0.018 (2)
O1	0.4579 (19)	−0.0059 (10)	0.3788 (3)	0.034 (2)
O2	0.3343 (15)	0.1268 (9)	0.3024 (3)	0.0226 (18)
O3	0.2079 (13)	0.4809 (8)	0.2693 (3)	0.0187 (15)
O4	−0.1825 (15)	0.3759 (11)	0.3067 (3)	0.027 (2)
O5	−0.0725 (17)	0.7543 (9)	0.3338 (3)	0.0260 (17)
O6	−0.1500 (15)	0.8067 (11)	0.4213 (3)	0.0292 (18)
H6A	−0.2515	0.8818	0.4085	0.044*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pb1	0.01956 (16)	0.01638 (18)	0.01564 (18)	0.00080 (18)	0.00175 (18)	−0.00035 (18)
C1	0.017 (5)	0.015 (6)	0.014 (5)	−0.001 (4)	0.001 (4)	−0.003 (4)
C2	0.013 (4)	0.027 (6)	0.018 (6)	−0.001 (5)	0.004 (4)	0.008 (5)
C3	0.025 (6)	0.018 (6)	0.016 (6)	0.005 (4)	0.000 (4)	0.001 (5)
C4	0.033 (6)	0.022 (6)	0.012 (6)	0.005 (5)	−0.003 (5)	−0.005 (5)
C5	0.036 (6)	0.031 (6)	0.020 (6)	0.012 (6)	−0.014 (6)	−0.002 (5)
C6	0.029 (5)	0.025 (6)	0.023 (6)	0.006 (5)	−0.005 (5)	0.009 (5)
C7	0.022 (6)	0.021 (6)	0.030 (7)	0.001 (4)	0.001 (5)	0.003 (5)
C8	0.023 (5)	0.005 (4)	0.018 (5)	0.002 (5)	0.001 (5)	0.001 (4)
C9	0.023 (5)	0.012 (5)	0.019 (5)	0.004 (4)	0.004 (4)	−0.002 (4)
O1	0.045 (5)	0.022 (4)	0.035 (5)	0.011 (4)	−0.007 (4)	−0.001 (4)
O2	0.028 (4)	0.018 (4)	0.021 (4)	−0.002 (3)	−0.002 (3)	−0.003 (3)
O3	0.021 (3)	0.020 (4)	0.015 (4)	0.004 (3)	0.009 (3)	0.001 (3)
O4	0.023 (4)	0.042 (5)	0.017 (4)	−0.006 (3)	−0.003 (3)	−0.003 (4)
O5	0.030 (4)	0.037 (4)	0.011 (4)	0.016 (4)	−0.003 (4)	0.004 (3)
O6	0.041 (5)	0.023 (4)	0.023 (4)	0.018 (4)	0.001 (3)	−0.001 (4)

Geometric parameters (Å, º)

Pb1—O4^i	2.379 (7)	C4—C5	1.393 (15)
Pb1—O3	2.430 (6)	C4—H4	0.9300
Pb1—O2^ii	2.535 (7)	C5—C6	1.379 (15)
Pb1—O2	2.663 (8)	C5—H5	0.9300
Pb1—O5^iii	2.833 (8)	C6—H6	0.9300
Pb1—O3^iv	2.795 (6)	C7—O1	1.257 (13)
Pb1—O5^iv	2.829 (8)	C7—O2	1.269 (13)
C1—C2	1.393 (14)	C8—O4	1.246 (12)
C1—C6	1.409 (14)	C8—O3	1.262 (12)
C1—C7	1.498 (15)	C9—O5	1.215 (12)
C2—C3	1.423 (15)	C9—O6	1.321 (12)
C2—C8	1.527 (15)	O2—Pb1^iv	2.535 (7)
C3—C4	1.382 (13)	O4—Pb1^v	2.379 (7)
C3—C9	1.475 (14)	O6—H6A	0.8200
O4^i—Pb1—O3	82.4 (3)	C4—C5—H5	120.2
O4^i—Pb1—O2^ii	87.1 (3)	C5—C6—C1	121.2 (10)
O3—Pb1—O2^ii	75.2 (2)	C5—C6—H6	119.4
O4^i—Pb1—O2	73.2 (2)	C1—C6—H6	119.4
O3—Pb1—O2	69.8 (2)	O1—C7—O2	122.9 (11)
O2^ii—Pb1—O2	141.5 (2)	O1—C7—C1	117.4 (11)
C2—C1—C6	119.2 (10)	O2—C7—C1	119.6 (10)
C2—C1—C7	122.7 (9)	O4—C8—O3	126.2 (10)
C6—C1—C7	118.1 (10)	O4—C8—C2	115.4 (9)
C1—C2—C3	119.4 (9)	O3—C8—C2	118.4 (10)
C1—C2—C8	121.2 (10)	O5—C9—O6	121.9 (9)
C3—C2—C8	119.4 (9)	O5—C9—C3	124.3 (9)
C4—C3—C2	119.9 (10)	O6—C9—C3	113.8 (9)
C4—C3—C9	120.3 (10)	C7—O2—Pb1^iv	103.0 (7)
C2—C3—C9	119.8 (9)	C7—O2—Pb1	128.1 (7)
C3—C4—C5	120.7 (11)	Pb1^iv—O2—Pb1	104.9 (3)
C3—C4—H4	119.6	C8—O3—Pb1	124.9 (6)
C5—C4—H4	119.6	C8—O4—Pb1^v	124.4 (7)
C6—C5—C4	119.5 (10)	C9—O6—H6A	109.5
C6—C5—H5	120.2

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6A···O1^vi	0.82	1.80	2.592 (11)	163

Symmetry code: (vi) x−1, y+1, z.