Poly[diaqua­bis(μ2-5-carb­oxy-2-propyl-1H-imidazole-4-carboxyl­ato-κ3N3,O4:O5)lead(II)]

Chen, X.; Liu, H.-C.

doi:10.1107/S1600536810013735

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 5| May 2010| Page m543

https://doi.org/10.1107/S1600536810013735

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Poly[diaquabis(μ₂-5-carboxy-2-propyl-1H-imidazole-4-carboxylato-κ³N³,O⁴:O⁵)lead(II)]

Xiang Chen ^a ^* and Hai-Cheng Liu ^b

^aDepartment of Chemistry and Chemical Engineering, Henan University of Urban Construction, Pingdingshan 467044, People's Republic of China, and ^bDepartment of Environmental and Municipal Engineering, Henan University of Urban Construction, Pingdingshan 467044, People's Republic of China
^*Correspondence e-mail: chenxiangdl2008@163.com

(Received 12 April 2010; accepted 14 April 2010; online 21 April 2010)

In the title complex, [Pb(C₈H₉N₂O₄)₂(H₂O)₂]_n, the eight-coordinate Pb^II atom lies on a twofold rotation axis and adopts a slightly distorted square-antiprismatic N₂O₆ coordination geometry. The ligand donor atoms are the tertiary N atoms of the imidazole rings and the carboxylate O atoms of two chelating 5-carboxy-2-propyl-1H-imidazole-4-carboxylate ligands, the carboxy O atoms of two additional imidazole ligands and two water O atoms. The carboxy O and the N,O-chelate systems also link adjacent Pb^II atoms, forming a two-dimensional layer structure, with four individual Pb^II atoms located at the corners of a square. These layers are further interconnected by an extensive array of O—H⋯O and N—H⋯O hydrogen bonds into a three-dimensional network.

Related literature

For the properties and uses of imidazoledicarboxylate complexes, see: Cao et al. (2002 ); Rajendiran et al. (2003 ).

Experimental

Crystal data

[Pb(C₈H₉N₂O₄)₂(H₂O)₂]
M_r = 637.57
Monoclinic, C 2/c
a = 13.1201 (15) Å
b = 13.2929 (16) Å
c = 11.5910 (13) Å
β = 98.531 (2)°
V = 1999.2 (4) Å³
Z = 4
Mo Kα radiation
μ = 8.50 mm⁻¹
T = 293 K
0.45 × 0.17 × 0.13 mm

Data collection

Bruker SMART 1000 CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2007 ) T_min = 0.114, T_max = 0.404
4884 measured reflections
1751 independent reflections
1640 reflections with I > 2σ(I)
R_int = 0.048

Refinement

R[F² > 2σ(F²)] = 0.019
wR(F²) = 0.039
S = 1.02
1751 reflections
143 parameters
H-atom parameters constrained
Δρ_max = 0.82 e Å⁻³
Δρ_min = −0.69 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5D⋯O4ⁱ	0.85	2.58	3.182 (4)	129
O5—H5D⋯O3ⁱ	0.85	2.16	3.004 (3)	176
O5—H5C⋯O1ⁱⁱ	0.85	2.19	3.035 (3)	176
O3—H3⋯O2	0.82	1.64	2.459 (3)	178
N2—H2⋯O1ⁱⁱⁱ	0.86	2.05	2.909 (4)	172
Symmetry codes: (i) $[x+{\script{1\over 2}}, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (ii) $[x, -y+1, z-{\script{1\over 2}}]$ ; (iii) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ .

Data collection: SMART (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) and DIAMOND (Brandenburg, 1999 ); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810013735/sj2771sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810013735/sj2771Isup2.hkl

checkCIF report

Comment top

It is well known that 4,5-imidazoledicarboxylic acid, a rigid N-heterocyclic dicarboxylic acid has great potential as a ligand in coordination complexes and for hydrogen bond formation. Imidazoledicarboxylate complexes have been found to exhibit useful properties, such as magnetism and porosity (Cao et al., 2002; Rajendiran et al., 2003). We have therefore reacted the 2-propyl-1H-imidazole-4,5 dicarboxylic acid ligand with Pb(NO₃)₂ under hydrothermal conditions to obtain a new Pb^II complex and its structure is reported here.

In the title complex, [Pb(C₈H₉N₂O₄)₂(H₂O)₂]_n, the eight coordinate Pb^II atom lies on a two-fold rotation axis and adopts a slightly distorted square-antiprismatic N₂O₆ coordination geometry. The ligand donor atoms are the N1 atoms of the imidazole rings and the carboxylate O1 atoms of two chelating 5-carboxy-2-propyl-1H-imidazole-4- carboxylato ligands, the O4 carboxy oxygen atoms of two additional imidazole ligands and two O5 water molecules. The O1 and N1 atoms of the chelate systems also link adjacent Pb^II centres forming a two-dimensional layer structure, with four individual Pb^II atoms located at the corners of a square. These layers are further interconnected by an extensive array of O—H···O and N—H···O hydrogen bonds into a three-dimensional network.

Related literature top

For the properties and uses of imidazoledicarboxylate complexes, see: Cao et al. (2002); Rajendiran et al. (2003).

Experimental top

A mixture of Pb(NO₃)₂ (0.5 mmol, 0.07 g) and 2-propyl-1H-imidazole-4,5-dicarboxylic acid(0.5 mmol, 0.99 g) in 15 ml of H₂O solution was sealed in an autoclave equipped with a Teflon liner (25 ml) and then heated at 373k for 3 days. Crystals of the title compound were obtained by slow evaporation of the solvent at room temperature.

Structure description top

For the properties and uses of imidazoledicarboxylate complexes, see: Cao et al. (2002); Rajendiran et al. (2003).

Computing details top

Data collection: SMART (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) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. The structure of the title compound, showing the atomic numbering scheme. Non-H atoms are shown with 30% probability displacement ellipsoids(H atoms are omitted for clarity). [Symmetry codes: (i) 1-x, y, 1.5-z; (ii) -0.5+x, 0.5+y, z; (iii) 0.5+x, 0.5+y, z; (iv) 0.5+x, -0.5+y, z; (v) 0.5-x, -0.5+y, 1.5-z]
	Fig. 2. A two-dimensional layer constructed of Pb₄ squares
	Fig. 3. Crystal packing of the title compound

Poly[diaquabis(µ₂-5-carboxy-2-propyl-1H-imidazole-4-carboxylato- κ³N³,O⁴:O⁵)lead(II)] top

Crystal data top

[Pb(C₈H₉N₂O₄)₂(H₂O)₂]	F(000) = 1232
M_r = 637.57	D_x = 2.118 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 2051 reflections
a = 13.1201 (15) Å	θ = 2.5–23.9°
b = 13.2929 (16) Å	µ = 8.50 mm⁻¹
c = 11.5910 (13) Å	T = 293 K
β = 98.531 (2)°	Block, colorless
V = 1999.2 (4) Å³	0.45 × 0.17 × 0.13 mm
Z = 4

Data collection top

Bruker SMART 1000 CCD area-detector diffractometer	1751 independent reflections
Radiation source: fine-focus sealed tube	1640 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.048
φ and ω scans	θ_max = 25.0°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2007)	h = −13→15
T_min = 0.114, T_max = 0.404	k = −15→15
4884 measured reflections	l = −10→13

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.019	H-atom parameters constrained
wR(F²) = 0.039	w = 1/[σ²(F_o²) + 0.170P] where P = (F_o² + 2F_c²)/3
S = 1.02	(Δ/σ)_max = 0.002
1751 reflections	Δρ_max = 0.82 e Å⁻³
143 parameters	Δρ_min = −0.69 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00501 (14)

Crystal data top

[Pb(C₈H₉N₂O₄)₂(H₂O)₂]	V = 1999.2 (4) Å³
M_r = 637.57	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 13.1201 (15) Å	µ = 8.50 mm⁻¹
b = 13.2929 (16) Å	T = 293 K
c = 11.5910 (13) Å	0.45 × 0.17 × 0.13 mm
β = 98.531 (2)°

Data collection top

Bruker SMART 1000 CCD area-detector diffractometer	1751 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2007)	1640 reflections with I > 2σ(I)
T_min = 0.114, T_max = 0.404	R_int = 0.048
4884 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.019	0 restraints
wR(F²) = 0.039	H-atom parameters constrained
S = 1.02	Δρ_max = 0.82 e Å⁻³
1751 reflections	Δρ_min = −0.69 e Å⁻³
143 parameters

Special details top

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 > 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.

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

	x	y	z	U_iso*/U_eq
Pb1	0.5000	0.585420 (12)	0.7500	0.02187 (10)
N1	0.36101 (17)	0.72953 (19)	0.7416 (2)	0.0206 (6)
N2	0.26176 (19)	0.8636 (2)	0.7255 (2)	0.0245 (6)
H2	0.2380	0.9221	0.7040	0.029*
O1	0.33533 (16)	0.55121 (18)	0.8607 (2)	0.0288 (6)
O2	0.20043 (17)	0.61233 (19)	0.9317 (2)	0.0346 (6)
O3	0.09662 (17)	0.7669 (2)	0.9230 (2)	0.0400 (7)
H3	0.1304	0.7149	0.9245	0.060*
O4	0.0980 (2)	0.9168 (2)	0.8428 (3)	0.0521 (9)
O5	0.43915 (18)	0.6096 (2)	0.5232 (2)	0.0374 (6)
H5C	0.4120	0.5656	0.4750	0.045*
H5D	0.4830	0.6427	0.4915	0.045*
C1	0.2736 (2)	0.6209 (3)	0.8716 (3)	0.0240 (7)
C2	0.2842 (2)	0.7169 (2)	0.8095 (3)	0.0204 (7)
C3	0.2221 (2)	0.8003 (3)	0.7997 (3)	0.0228 (8)
C4	0.1323 (3)	0.8316 (3)	0.8572 (3)	0.0314 (9)
C5	0.3450 (2)	0.8188 (2)	0.6912 (3)	0.0230 (8)
C6	0.4039 (2)	0.8661 (3)	0.6046 (3)	0.0285 (8)
H6A	0.4688	0.8309	0.6062	0.034*
H6B	0.4193	0.9353	0.6274	0.034*
C7	0.3461 (3)	0.8646 (3)	0.4806 (3)	0.0355 (9)
H7A	0.3380	0.7954	0.4541	0.043*
H7B	0.2779	0.8928	0.4803	0.043*
C8	0.4016 (3)	0.9236 (3)	0.3967 (4)	0.0408 (10)
H8A	0.4129	0.9913	0.4246	0.061*
H8B	0.3604	0.9245	0.3210	0.061*
H8C	0.4667	0.8923	0.3914	0.061*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.02470 (12)	0.01520 (13)	0.02690 (14)	0.000	0.00777 (7)	0.000
N1	0.0251 (13)	0.0146 (16)	0.0229 (15)	0.0002 (11)	0.0059 (11)	0.0026 (13)
N2	0.0337 (15)	0.0126 (15)	0.0273 (16)	0.0049 (12)	0.0047 (12)	0.0059 (14)
O1	0.0343 (13)	0.0162 (13)	0.0375 (15)	0.0015 (10)	0.0110 (10)	0.0029 (12)
O2	0.0376 (14)	0.0306 (14)	0.0396 (16)	−0.0018 (11)	0.0191 (11)	0.0072 (13)
O3	0.0354 (13)	0.0414 (18)	0.0474 (17)	0.0086 (12)	0.0203 (11)	0.0008 (15)
O4	0.0632 (18)	0.046 (2)	0.051 (2)	0.0373 (14)	0.0236 (15)	0.0114 (15)
O5	0.0407 (14)	0.0395 (16)	0.0338 (16)	−0.0070 (12)	0.0115 (11)	−0.0025 (13)
C1	0.0266 (17)	0.0222 (19)	0.0236 (19)	−0.0044 (15)	0.0049 (14)	−0.0031 (17)
C2	0.0235 (15)	0.0163 (18)	0.0212 (18)	−0.0013 (13)	0.0026 (13)	−0.0018 (15)
C3	0.0264 (16)	0.022 (2)	0.0198 (18)	0.0019 (14)	0.0022 (13)	−0.0012 (16)
C4	0.0335 (19)	0.035 (2)	0.027 (2)	0.0074 (17)	0.0083 (15)	−0.0017 (19)
C5	0.0244 (16)	0.0178 (19)	0.0266 (19)	−0.0001 (14)	0.0030 (13)	0.0008 (16)
C6	0.0286 (18)	0.025 (2)	0.033 (2)	−0.0009 (15)	0.0050 (14)	0.0066 (18)
C7	0.0365 (19)	0.037 (2)	0.033 (2)	−0.0111 (17)	0.0026 (15)	0.003 (2)
C8	0.049 (2)	0.042 (3)	0.031 (2)	−0.0065 (18)	0.0058 (18)	0.0088 (19)

Geometric parameters (Å, º) top

Pb1—N1	2.637 (2)	O4—C4	1.221 (4)
Pb1—N1ⁱ	2.637 (2)	O4—Pb1^iv	2.725 (3)
Pb1—O5ⁱ	2.651 (3)	O5—H5C	0.8500
Pb1—O5	2.652 (3)	O5—H5D	0.8500
Pb1—O1	2.710 (2)	C1—C2	1.481 (5)
Pb1—O1ⁱ	2.710 (2)	C2—C3	1.370 (4)
Pb1—O4ⁱⁱ	2.725 (3)	C3—C4	1.496 (5)
Pb1—O4ⁱⁱⁱ	2.725 (3)	C5—C6	1.494 (5)
N1—C5	1.326 (4)	C6—C7	1.522 (4)
N1—C2	1.377 (4)	C6—H6A	0.9700
N2—C5	1.354 (4)	C6—H6B	0.9700
N2—C3	1.361 (5)	C7—C8	1.517 (5)
N2—H2	0.8600	C7—H7A	0.9700
O1—C1	1.249 (4)	C7—H7B	0.9700
O2—C1	1.273 (4)	C8—H8A	0.9600
O3—C4	1.284 (4)	C8—H8B	0.9600
O3—H3	0.8200	C8—H8C	0.9600

N1—Pb1—N1ⁱ	86.81 (11)	Pb1—O5—H5C	127.1
N1—Pb1—O5ⁱ	93.06 (8)	Pb1—O5—H5D	111.6
N1ⁱ—Pb1—O5ⁱ	76.75 (8)	H5C—O5—H5D	108.5
N1—Pb1—O5	76.75 (8)	O1—C1—O2	122.8 (3)
N1ⁱ—Pb1—O5	93.06 (8)	O1—C1—C2	118.7 (3)
O5ⁱ—Pb1—O5	166.09 (11)	O2—C1—C2	118.4 (3)
N1—Pb1—O1	62.85 (7)	C3—C2—N1	109.3 (3)
N1ⁱ—Pb1—O1	134.44 (7)	C3—C2—C1	129.8 (3)
O5ⁱ—Pb1—O1	72.23 (7)	N1—C2—C1	120.8 (3)
O5—Pb1—O1	110.24 (7)	N2—C3—C2	106.0 (3)
N1—Pb1—O1ⁱ	134.44 (7)	N2—C3—C4	120.6 (3)
N1ⁱ—Pb1—O1ⁱ	62.85 (7)	C2—C3—C4	133.3 (3)
O5ⁱ—Pb1—O1ⁱ	110.23 (7)	O4—C4—O3	122.8 (3)
O5—Pb1—O1ⁱ	72.23 (7)	O4—C4—C3	119.8 (4)
O1—Pb1—O1ⁱ	160.68 (10)	O3—C4—C3	117.3 (3)
N1—Pb1—O4ⁱⁱ	153.57 (9)	N1—C5—N2	110.3 (3)
N1ⁱ—Pb1—O4ⁱⁱ	107.45 (9)	N1—C5—C6	127.6 (3)
O5ⁱ—Pb1—O4ⁱⁱ	69.71 (9)	N2—C5—C6	122.1 (3)
O5—Pb1—O4ⁱⁱ	123.10 (9)	C5—C6—C7	113.2 (3)
O1—Pb1—O4ⁱⁱ	92.16 (8)	C5—C6—H6A	108.9
O1ⁱ—Pb1—O4ⁱⁱ	71.71 (8)	C7—C6—H6A	108.9
N1—Pb1—O4ⁱⁱⁱ	107.46 (9)	C5—C6—H6B	108.9
N1ⁱ—Pb1—O4ⁱⁱⁱ	153.56 (9)	C7—C6—H6B	108.9
O5ⁱ—Pb1—O4ⁱⁱⁱ	123.10 (9)	H6A—C6—H6B	107.8
O5—Pb1—O4ⁱⁱⁱ	69.70 (9)	C8—C7—C6	112.3 (3)
O1—Pb1—O4ⁱⁱⁱ	71.72 (8)	C8—C7—H7A	109.1
O1ⁱ—Pb1—O4ⁱⁱⁱ	92.16 (8)	C6—C7—H7A	109.1
O4ⁱⁱ—Pb1—O4ⁱⁱⁱ	69.29 (14)	C8—C7—H7B	109.1
C5—N1—C2	106.2 (3)	C6—C7—H7B	109.1
C5—N1—Pb1	136.9 (2)	H7A—C7—H7B	107.9
C2—N1—Pb1	116.79 (19)	C7—C8—H8A	109.5
C5—N2—C3	108.3 (3)	C7—C8—H8B	109.5
C5—N2—H2	125.9	H8A—C8—H8B	109.5
C3—N2—H2	125.9	C7—C8—H8C	109.5
C1—O1—Pb1	119.8 (2)	H8A—C8—H8C	109.5
C4—O3—H3	109.5	H8B—C8—H8C	109.5
C4—O4—Pb1^iv	163.7 (3)

N1ⁱ—Pb1—N1—C5	39.1 (3)	Pb1—N1—C2—C1	−7.6 (3)
O5ⁱ—Pb1—N1—C5	115.6 (3)	O1—C1—C2—C3	174.0 (3)
O5—Pb1—N1—C5	−54.8 (3)	O2—C1—C2—C3	−4.4 (5)
O1—Pb1—N1—C5	−176.2 (3)	O1—C1—C2—N1	−0.5 (4)
O1ⁱ—Pb1—N1—C5	−6.9 (3)	O2—C1—C2—N1	−178.9 (3)
O4ⁱⁱ—Pb1—N1—C5	163.3 (3)	C5—N2—C3—C2	0.4 (4)
O4ⁱⁱⁱ—Pb1—N1—C5	−118.2 (3)	C5—N2—C3—C4	176.8 (3)
N1ⁱ—Pb1—N1—C2	−137.1 (2)	N1—C2—C3—N2	0.0 (3)
O5ⁱ—Pb1—N1—C2	−60.6 (2)	C1—C2—C3—N2	−175.0 (3)
O5—Pb1—N1—C2	129.0 (2)	N1—C2—C3—C4	−175.8 (3)
O1—Pb1—N1—C2	7.63 (19)	C1—C2—C3—C4	9.3 (6)
O1ⁱ—Pb1—N1—C2	176.89 (18)	Pb1^iv—O4—C4—O3	−108.0 (9)
O4ⁱⁱ—Pb1—N1—C2	−12.9 (3)	Pb1^iv—O4—C4—C3	74.0 (10)
O4ⁱⁱⁱ—Pb1—N1—C2	65.6 (2)	N2—C3—C4—O4	−4.3 (5)
N1—Pb1—O1—C1	−8.6 (2)	C2—C3—C4—O4	171.0 (4)
N1ⁱ—Pb1—O1—C1	45.2 (3)	N2—C3—C4—O3	177.7 (3)
O5ⁱ—Pb1—O1—C1	94.6 (2)	C2—C3—C4—O3	−7.1 (6)
O5—Pb1—O1—C1	−70.9 (2)	C2—N1—C5—N2	0.7 (3)
O1ⁱ—Pb1—O1—C1	−164.9 (2)	Pb1—N1—C5—N2	−175.8 (2)
O4ⁱⁱ—Pb1—O1—C1	162.5 (2)	C2—N1—C5—C6	−176.9 (3)
O4ⁱⁱⁱ—Pb1—O1—C1	−130.2 (2)	Pb1—N1—C5—C6	6.7 (5)
Pb1—O1—C1—O2	−173.4 (2)	C3—N2—C5—N1	−0.7 (4)
Pb1—O1—C1—C2	8.3 (4)	C3—N2—C5—C6	177.0 (3)
C5—N1—C2—C3	−0.4 (3)	N1—C5—C6—C7	105.0 (4)
Pb1—N1—C2—C3	176.90 (19)	N2—C5—C6—C7	−72.3 (4)
C5—N1—C2—C1	175.1 (3)	C5—C6—C7—C8	173.3 (3)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5D···O4^v	0.85	2.58	3.182 (4)	129
O5—H5D···O3^v	0.85	2.16	3.004 (3)	176
O5—H5C···O1^vi	0.85	2.19	3.035 (3)	176
O3—H3···O2	0.82	1.64	2.459 (3)	178
N2—H2···O1^vii	0.86	2.05	2.909 (4)	172

Symmetry codes: (v) x+1/2, −y+3/2, z−1/2; (vi) x, −y+1, z−1/2; (vii) −x+1/2, y+1/2, −z+3/2.

Experimental details

Crystal data
Chemical formula	[Pb(C₈H₉N₂O₄)₂(H₂O)₂]
M_r	637.57
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	293
a, b, c (Å)	13.1201 (15), 13.2929 (16), 11.5910 (13)
β (°)	98.531 (2)
V (Å³)	1999.2 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	8.50
Crystal size (mm)	0.45 × 0.17 × 0.13

Data collection
Diffractometer	Bruker SMART 1000 CCD area-detector
Absorption correction	Multi-scan (SADABS; Bruker, 2007)
T_min, T_max	0.114, 0.404
No. of measured, independent and observed [I > 2σ(I)] reflections	4884, 1751, 1640
R_int	0.048
(sin θ/λ)_max (Å⁻¹)	0.594

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.019, 0.039, 1.02
No. of reflections	1751
No. of parameters	143
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.82, −0.69

Computer programs: SMART (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5D···O4ⁱ	0.85	2.58	3.182 (4)	129.1
O5—H5D···O3ⁱ	0.85	2.16	3.004 (3)	175.7
O5—H5C···O1ⁱⁱ	0.85	2.19	3.035 (3)	175.8
O3—H3···O2	0.82	1.64	2.459 (3)	178.1
N2—H2···O1ⁱⁱⁱ	0.86	2.05	2.909 (4)	172.0

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

Acknowledgements

The authors acknowledge Henan University of Urban Construction for supporting this work.

References

Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Bruker (2007). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
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