Poly[aqua­(μ-pyrazine-2-carboxyl­ato-κ3N,O:O)(μ-pyrazine-2-carboxyl­ato-κ3N,O:O′)lead(II)]

Starosta, W.; Leciejewicz, J.

doi:10.1107/S1600536810013188

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 5| May 2010| Pages m525-m526

https://doi.org/10.1107/S1600536810013188

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Poly[aqua(μ-pyrazine-2-carboxylato-κ³N,O:O)(μ-pyrazine-2-carboxylato-κ³N,O:O′)lead(II)]

Wojciech Starosta ^a and Janusz Leciejewicz ^a ^*

^aInstitute of Nuclear Chemistry and Technology, ul. Dorodna 16, 03-195 Warszawa, Poland
^*Correspondence e-mail: j.leciejewicz@ichtj.waw.pl

(Received 30 March 2010; accepted 9 April 2010; online 17 April 2010)

The polymeric structure of the title compound, [Pb(C₅H₃N₂O₂)₂(H₂O)]_n, is built up from centrosymmetric [Pb(C₅H₃N₂O₂)₂(H₂O)]₂ dimers, which are bridged by ligand carboxylate O atoms. The Pb^II ion adopts an irregular PbN₂O₅ coordination polyhedron; it is chelated by one N,O-bidentate ligand and also bonds to a water O atom. A second N,O-bidentate ligand forms the dimer bridge and another bridging O atom from a nearby dimer also bonds to the Pb^II ion, leading to layers propagating in (100). A network of O—H⋯O hydrogen bonds operates between water O atoms (donors) and carboxylate O atoms (acceptors).

Related literature

For the crystal structures of divalent metal ions with pyrazine-2-carboxylate and water ligands, see, for example: Alcock et al. (1996 ); Ptasiewicz-Bąk et al. (1995 , 1998 ). The structures of lead(II) complexes with pyrazine-4-carboxylate (Starosta & Leciejewicz, 2009 ) and pyrazine-3-carboxylate ligands (Starosta & Leciejewicz, 2010 ) have also been reported.

Experimental

Crystal data

[Pb(C₅H₃N₂O₂)₂(H₂O)]
M_r = 471.39
Monoclinic, P 2₁ /c
a = 11.098 (2) Å
b = 10.382 (2) Å
c = 11.678 (2) Å
β = 114.13 (3)°
V = 1228.0 (4) Å³
Z = 4
Mo Kα radiation
μ = 13.77 mm⁻¹
T = 293 K
0.29 × 0.16 × 0.12 mm

Data collection

Kuma KM-4 four-circle diffractometer
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008 $[Oxford Diffraction (2008). CrysAlis RED. Oxford Diffraction Ltd, Yarnton, Oxfordshire, England.]$ ) T_min = 0.135, T_max = 0.251
3579 measured reflections
3411 independent reflections
2230 reflections with I > 2σ(I)
R_int = 0.051
3 standard reflections every 200 reflections intensity decay: 20.2%

Refinement

R[F² > 2σ(F²)] = 0.058
wR(F²) = 0.163
S = 1.02
3411 reflections
188 parameters
5 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 6.45 e Å⁻³
Δρ_min = −5.86 e Å⁻³

Table 1
Selected bond lengths (Å)

Pb1—O21	2.341 (7)
Pb1—O11ⁱ	2.508 (7)
Pb1—O1	2.573 (9)
Pb1—O11	2.572 (8)
Pb1—N21	2.577 (9)
Pb1—N11	2.807 (9)
Pb1—O22ⁱⁱ	2.856 (8)
Symmetry codes: (i) -x+1, -y, -z+1; (ii) $[x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ .

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H2⋯O21ⁱⁱ	0.84 (2)	2.17 (5)	2.837 (13)	136 (7)
O1—H1⋯O22ⁱⁱⁱ	0.84 (2)	2.29 (5)	2.969 (15)	139 (7)
O1—H1⋯O12ⁱⁱ	0.84 (2)	2.49 (7)	3.056 (13)	126 (7)
Symmetry codes: (ii) $[x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (iii) -x+1, -y+1, -z+1.

Data collection: KM-4 Software (Kuma, 1996 $[Kuma (1996). KM-4 Software. Kuma Diffraction Ltd, Wrocław, Poland.]$ ); cell refinement: KM-4 Software; data reduction: DATAPROC (Kuma, 2001 $[Kuma (2001). DATAPROC. Kuma Diffraction Ltd, Wrocław, Poland.]$ ); program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810013188/hb5383sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810013188/hb5383Isup2.hkl

checkCIF report

Comment top

Divalent UO₂(II) ion (Alcock et al.,1996), 3-d metal M(II) ions (Ptasiewicz-Bąk et al.,(1995), Ca(II) and Sr(II) ions (Ptasiewicz-Bąk et al.,1998) form with pyrazine-2-carboxylate and water ligands monomeric molecules with coordination modes characteristic for particular ions. On the other hand, the structure of a Pb(II) complex with pyridazine-4-carboxylate and water ligands is composed of dimeric molecules (Starosta & Leciejewicz, 2009), while the structure of a Pb(II) complex with pyridazine-3-carboxylate and water ligands is polymeric (Starosta & Leciejewicz, 2010). The structure of title compound (I) is composed of centrosymmetric dimeric molecules in which each of the two Pb(II) ions is cheletated by two symmetry independent ligands via their N,O bonding groups. Their planes make at the metal ion an angle of 85.1 (2)^o each to the other. Pb(II) ions are bridged by O11 and O11⁽ⁱ⁾ atoms donated by symmetry related ligands L1. The O12 and O12⁽ⁱ⁾ atoms do not take part in coordination. A water O atom is chelated to each metal ion. The second pair of ligand molecules L2 also coordinates the Pb(II) ions by their N,O bonding groups while the O22 and O22⁽ⁱ⁾ atoms act as bridges to Pb(II) ions in adjacent dimers. A polymeric structure is formed in this way. The coordination geometry of a Pb(II) ion is represented by a pyramid in which N11, O11, O11^(I) and O1 atoms form an equatorial plane [ r.m.s. 0.0083 (1) Å] with a Pb(II) ion shifted from it by 0.3079 (2) Å; N21 and O21 atoms make two apices of the pyramid while the bridging O22^(II) atom forms a single apex on the other side of the equatorial plane. Bond angles reveal an empty space around the metal ion between Pb—O11^(I)and Pb—O1 bonds It may indicate the stereochemical activity of the lone 6 s² electron pair of the Pb(II) ion. Pyrazine rings of both ligands are planar: r.m.s. 0.0089 (2)Å in L1 and 0.0046 (1)Å in L2. The C17/O11/O12 carboxylic group makes an angle of 6.7 (1)° with pyrazine ring L1, the carboxylic group C27/O21/O22 - an angle of 9.1 (1)° with L2. Weak hydrogen bonds operate between the coordinated water O atoms (donors) and carboxylate O21 and O22 atoms (acceptors) in adjacent dimers.

Related literature top

For the crystal structures of divalent metal ions with pyrazine-2-carboxylate and water ligands, see, for example: Alcock et al. (1996); Ptasiewicz-Bąk et al. (1995, 1998). The structures of lead(II) complexes with pyrazine-4-carboxylate (Starosta & Leciejewicz, 2009) and pyrazine-3-carboxylate ligands (Starosta & Leciejewicz, 2010) have also been reported.

Experimental top

The title compound was synthetized by reacting boiling aqueous solution of pyrazine-2-carboxylic acid dihydrate (Aldrich) with some excess of lead(II) hydroxide. The mixture was boiled under reflux for three hours and after cooling to room temperature, filtered and left for crystallization. Few days later, colourless blocks of (I) were found after evaporation to dryness. They were extracted, washed with cold ethanol and dried in the air.

Structure description top

# Used for convenience to store draft or replaced versions # of the abstract, comment etc. # Its contents will not be output

#==============================================================================

Computing details top

Data collection: KM-4 Software (Kuma, 1996); cell refinement: KM-4 Software (Kuma, 1996); data reduction: DATAPROC (Kuma, 2001); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. A structural unit of (1) with 50% probability displacement ellipsoids. Symmetry codes: (i) -x+1,-y,-z+1; (ii) x,-y+1/2,z-1/2.
	Fig. 2. Packing diagram of the structure of (I).

Poly[aqua(µ-pyrazine-2-carboxylato-κ³N,O:O)(µ- pyrazine-2-carboxylato-κ³N,O:O')lead(II)] top

Crystal data top

[Pb(C₅H₃N₂O₂)₂(H₂O)]	F(000) = 872
M_r = 471.39	D_x = 2.550 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 25 reflections
a = 11.098 (2) Å	θ = 6–15°
b = 10.382 (2) Å	µ = 13.77 mm⁻¹
c = 11.678 (2) Å	T = 293 K
β = 114.13 (3)°	Blocks, colourless
V = 1228.0 (4) Å³	0.29 × 0.16 × 0.12 mm
Z = 4

Data collection top

Kuma KM-4 four-circle diffractometer	2230 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.051
Graphite monochromator	θ_max = 30.1°, θ_min = 2.0°
profile data from ω/2θ scans	h = 0→14
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008)	k = −14→0
T_min = 0.135, T_max = 0.251	l = −15→14
3579 measured reflections	3 standard reflections every 200 reflections
3411 independent reflections	intensity decay: 20.2%

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)] = 0.058	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.163	w = 1/[σ²(F_o²) + (0.1217P)²] where P = (F_o² + 2F_c²)/3
S = 1.02	(Δ/σ)_max < 0.001
3411 reflections	Δρ_max = 6.45 e Å⁻³
188 parameters	Δρ_min = −5.86 e Å⁻³
5 restraints	Extinction correction: SHELXTL (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0154 (12)

Crystal data top

[Pb(C₅H₃N₂O₂)₂(H₂O)]	V = 1228.0 (4) Å³
M_r = 471.39	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 11.098 (2) Å	µ = 13.77 mm⁻¹
b = 10.382 (2) Å	T = 293 K
c = 11.678 (2) Å	0.29 × 0.16 × 0.12 mm
β = 114.13 (3)°

Data collection top

Kuma KM-4 four-circle diffractometer	2230 reflections with I > 2σ(I)
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008)	R_int = 0.051
T_min = 0.135, T_max = 0.251	3 standard reflections every 200 reflections
3579 measured reflections	intensity decay: 20.2%
3411 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.058	5 restraints
wR(F²) = 0.163	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	Δρ_max = 6.45 e Å⁻³
3411 reflections	Δρ_min = −5.86 e Å⁻³
188 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	0.47863 (3)	0.12876 (4)	0.35712 (3)	0.02848 (19)
O11	0.3570 (7)	−0.0031 (8)	0.4636 (8)	0.0413 (18)
C22	0.6620 (9)	0.3784 (10)	0.5171 (10)	0.034 (2)
O21	0.4811 (9)	0.2586 (8)	0.5220 (8)	0.0399 (18)
N21	0.6655 (8)	0.2972 (9)	0.4344 (8)	0.0327 (18)
C12	0.1581 (9)	0.1152 (9)	0.3625 (10)	0.0299 (19)
C13	0.0296 (11)	0.1383 (11)	0.3473 (11)	0.039 (2)
H13	−0.0039	0.0957	0.3980	0.047*
C27	0.5599 (12)	0.3532 (11)	0.5717 (12)	0.040 (2)
N22	0.8312 (12)	0.5089 (11)	0.5106 (13)	0.059 (3)
C26	0.7546 (11)	0.3203 (12)	0.3893 (12)	0.039 (2)
H26	0.7616	0.2642	0.3303	0.047*
N11	0.2083 (9)	0.1695 (10)	0.2906 (9)	0.0362 (19)
C16	0.1307 (12)	0.2491 (12)	0.2013 (12)	0.045 (3)
H16	0.1628	0.2889	0.1481	0.054*
C23	0.7440 (13)	0.4853 (12)	0.5559 (14)	0.050 (3)
H23	0.7365	0.5409	0.6151	0.060*
O1	0.4080 (11)	0.3287 (10)	0.2149 (9)	0.056 (2)
H1	0.378 (11)	0.402 (7)	0.218 (10)	0.084*
H2	0.385 (8)	0.312 (13)	0.138 (3)	0.084*
O12	0.2045 (8)	−0.0170 (9)	0.5394 (8)	0.0445 (19)
C17	0.2455 (9)	0.0251 (9)	0.4646 (9)	0.0275 (18)
N12	−0.0479 (10)	0.2225 (11)	0.2591 (11)	0.050 (3)
C15	0.0023 (12)	0.2730 (13)	0.1871 (12)	0.047 (3)
H15	−0.0500	0.3278	0.1230	0.056*
C25	0.8376 (14)	0.4253 (14)	0.4272 (15)	0.055 (3)
H25	0.8995	0.4379	0.3935	0.066*
O22	0.5643 (12)	0.4168 (10)	0.6610 (9)	0.054 (2)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.0271 (2)	0.0296 (2)	0.0327 (3)	0.00255 (14)	0.01621 (15)	0.00445 (14)
O11	0.024 (3)	0.044 (4)	0.060 (5)	0.005 (3)	0.020 (3)	0.021 (4)
C22	0.019 (4)	0.039 (5)	0.041 (5)	−0.002 (4)	0.010 (4)	0.008 (4)
O21	0.045 (4)	0.035 (4)	0.058 (5)	−0.011 (3)	0.040 (4)	−0.012 (3)
N21	0.024 (4)	0.044 (5)	0.038 (5)	−0.005 (4)	0.021 (3)	−0.002 (4)
C12	0.018 (4)	0.035 (5)	0.038 (5)	−0.002 (3)	0.012 (3)	−0.003 (4)
C13	0.031 (5)	0.048 (7)	0.041 (6)	0.009 (4)	0.019 (4)	−0.001 (4)
C27	0.038 (6)	0.039 (6)	0.047 (6)	−0.005 (4)	0.020 (5)	−0.001 (4)
N22	0.048 (6)	0.050 (6)	0.091 (9)	−0.021 (5)	0.042 (6)	−0.007 (6)
C26	0.034 (5)	0.050 (6)	0.050 (6)	−0.004 (5)	0.032 (5)	−0.003 (5)
N11	0.027 (4)	0.043 (5)	0.040 (5)	0.001 (4)	0.016 (4)	0.009 (4)
C16	0.039 (7)	0.046 (6)	0.051 (7)	0.008 (5)	0.018 (6)	0.021 (5)
C23	0.042 (6)	0.040 (6)	0.077 (9)	−0.017 (5)	0.032 (6)	−0.012 (6)
O1	0.072 (7)	0.052 (5)	0.042 (5)	0.009 (5)	0.022 (5)	0.013 (4)
O12	0.040 (4)	0.056 (5)	0.044 (4)	0.002 (4)	0.024 (3)	0.011 (4)
C17	0.022 (4)	0.027 (4)	0.033 (5)	−0.007 (3)	0.011 (3)	−0.003 (3)
N12	0.031 (5)	0.064 (7)	0.054 (6)	0.018 (5)	0.016 (5)	−0.003 (5)
C15	0.030 (6)	0.057 (8)	0.045 (7)	0.011 (5)	0.008 (5)	0.012 (5)
C25	0.044 (7)	0.055 (8)	0.081 (10)	−0.015 (6)	0.041 (7)	0.003 (7)
O22	0.077 (6)	0.062 (6)	0.042 (5)	−0.030 (5)	0.043 (4)	−0.017 (4)

Geometric parameters (Å, º) top

Pb1—O21	2.341 (7)	C13—N12	1.357 (15)
Pb1—O11ⁱ	2.508 (7)	C13—H13	0.9300
Pb1—O1	2.573 (9)	C27—O22	1.217 (15)
Pb1—O11	2.572 (8)	N22—C23	1.302 (17)
Pb1—N21	2.577 (9)	N22—C25	1.328 (19)
Pb1—N11	2.807 (9)	C26—C25	1.378 (18)
Pb1—O22ⁱⁱ	2.856 (8)	C26—H26	0.9300
O11—C17	1.277 (12)	N11—C16	1.334 (14)
O11—Pb1ⁱ	2.508 (7)	C16—C15	1.388 (17)
C22—N21	1.295 (14)	C16—H16	0.9300
C22—C23	1.389 (15)	C23—H23	0.9300
C22—C27	1.532 (16)	O1—H1	0.84 (2)
O21—C27	1.285 (14)	O1—H2	0.84 (2)
N21—C26	1.318 (12)	O12—C17	1.219 (12)
C12—N11	1.310 (13)	N12—C15	1.295 (17)
C12—C13	1.385 (13)	C15—H15	0.9300
C12—C17	1.513 (13)	C25—H25	0.9300

O21—Pb1—O11ⁱ	81.6 (3)	C13—C12—C17	120.2 (9)
O21—Pb1—O1	88.0 (3)	N12—C13—C12	120.6 (11)
O11ⁱ—Pb1—O1	152.2 (3)	N12—C13—H13	119.7
O21—Pb1—O11	75.0 (3)	C12—C13—H13	119.7
O11ⁱ—Pb1—O11	70.5 (3)	O22—C27—O21	125.7 (12)
O1—Pb1—O11	131.3 (3)	O22—C27—C22	119.1 (10)
O21—Pb1—N21	65.4 (3)	O21—C27—C22	115.1 (10)
O11ⁱ—Pb1—N21	81.6 (3)	C23—N22—C25	116.5 (11)
O1—Pb1—N21	70.6 (3)	N21—C26—C25	121.9 (11)
O11—Pb1—N21	134.3 (3)	N21—C26—H26	119.0
O21—Pb1—N11	78.0 (3)	C25—C26—H26	119.0
O11ⁱ—Pb1—N11	129.8 (3)	C12—N11—C16	117.4 (10)
O1—Pb1—N11	72.0 (3)	C12—N11—Pb1	116.4 (6)
O11—Pb1—N11	60.1 (3)	C16—N11—Pb1	125.8 (8)
N21—Pb1—N11	127.6 (3)	N11—C16—C15	120.5 (11)
O21—Pb1—O22ⁱⁱ	149.2 (3)	N11—C16—H16	119.8
O11ⁱ—Pb1—O22ⁱⁱ	102.5 (3)	C15—C16—H16	119.8
O1—Pb1—O22ⁱⁱ	74.3 (3)	N22—C23—C22	121.0 (13)
O11—Pb1—O22ⁱⁱ	135.4 (3)	N22—C23—H23	119.5
N21—Pb1—O22ⁱⁱ	84.8 (3)	C22—C23—H23	119.5
N11—Pb1—O22ⁱⁱ	118.2 (3)	Pb1—O1—H1	137 (10)
C17—O11—Pb1ⁱ	119.3 (6)	Pb1—O1—H2	113 (9)
C17—O11—Pb1	125.8 (6)	H1—O1—H2	106 (3)
Pb1ⁱ—O11—Pb1	109.5 (3)	O12—C17—O11	124.8 (9)
N21—C22—C23	123.2 (11)	O12—C17—C12	118.7 (9)
N21—C22—C27	116.9 (9)	O11—C17—C12	116.5 (8)
C23—C22—C27	119.9 (11)	C15—N12—C13	116.5 (10)
C27—O21—Pb1	126.1 (7)	N12—C15—C16	122.9 (11)
C22—N21—C26	115.8 (10)	N12—C15—H15	118.5
C22—N21—Pb1	116.0 (6)	C16—C15—H15	118.5
C26—N21—Pb1	127.7 (8)	N22—C25—C26	121.5 (11)
N11—C12—C13	121.9 (10)	N22—C25—H25	119.2
N11—C12—C17	117.9 (8)	C26—C25—H25	119.2

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H2···O21ⁱⁱ	0.84 (2)	2.17 (5)	2.837 (13)	136 (7)
O1—H1···O22ⁱⁱⁱ	0.84 (2)	2.29 (5)	2.969 (15)	139 (7)
O1—H1···O12ⁱⁱ	0.84 (2)	2.49 (7)	3.056 (13)	126 (7)

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

Experimental details

Crystal data
Chemical formula	[Pb(C₅H₃N₂O₂)₂(H₂O)]
M_r	471.39
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	11.098 (2), 10.382 (2), 11.678 (2)
β (°)	114.13 (3)
V (Å³)	1228.0 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	13.77
Crystal size (mm)	0.29 × 0.16 × 0.12

Data collection
Diffractometer	Kuma KM-4 four-circle diffractometer
Absorption correction	Analytical (CrysAlis RED; Oxford Diffraction, 2008)
T_min, T_max	0.135, 0.251
No. of measured, independent and observed [I > 2σ(I)] reflections	3579, 3411, 2230
R_int	0.051
(sin θ/λ)_max (Å⁻¹)	0.706

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.058, 0.163, 1.02
No. of reflections	3411
No. of parameters	188
No. of restraints	5
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	6.45, −5.86

Computer programs: KM-4 Software (Kuma, 1996), DATAPROC (Kuma, 2001), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Pb1—O21	2.341 (7)	Pb1—N21	2.577 (9)
Pb1—O11ⁱ	2.508 (7)	Pb1—N11	2.807 (9)
Pb1—O1	2.573 (9)	Pb1—O22ⁱⁱ	2.856 (8)
Pb1—O11	2.572 (8)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H2···O21ⁱⁱ	0.84 (2)	2.17 (5)	2.837 (13)	136 (7)
O1—H1···O22ⁱⁱⁱ	0.84 (2)	2.29 (5)	2.969 (15)	139 (7)
O1—H1···O12ⁱⁱ	0.84 (2)	2.49 (7)	3.056 (13)	126 (7)

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

References

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Volume 66| Part 5| May 2010| Pages m525-m526

https://doi.org/10.1107/S1600536810013188

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