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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 8| August 2010| Page m963
https://doi.org/10.1107/S1600536810027777

Bis(μ-quinoline-2-carboxyl­ato)-κ3N,O:O;κ3O:N,O-bis­­[(acetato-κ2O,O′)(methanol-κO)lead(II)]

Gholamhossein Mohammadnezhad,a Ali Reza Ghanbarpour,a Mostafa M. Aminia and Seik Weng Ngb*

aDepartment of Chemistry, General Campus, Shahid Beheshti University, Tehran 1983963113, Iran, and bDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
*Correspondence e-mail: seikweng@um.edu.my

(Received 11 July 2010; accepted 13 July 2010; online 17 July 2010)

The dinuclear title compound, [Pb2(C10H6NO2)2(CH3COO)2(CH3OH)2], lies across an inversion center. The methanol-coordinated PbII atom is chelated by the acetate anion as well as by the quinoline-2-carboxyl­ate anion. One O atom of the quinoline-2-carboxyl­ate anion bridges two symmetry-related PbII atoms, forming the dinuclear compound. Aside from the six atoms connected to the PbII atom by regular coordination bonds, the structure features a long Pb⋯O inter­action [3.145 (3) Å] that gives rise to a distorted Ψ-square-anti­prismatic geometry at the metal center. The H atom of the methanol is hydrogen bonded to an O atom of the acetate.

Related literature

For a related structure, see: Mohammadnezhad et al. (2010[Mohammadnezhad, G., Ghanbarpour, A. R., Amini, M. M. & Ng, S. W. (2010). Acta Cryst. E66, m946.]).

[Scheme 1]

Experimental

Crystal data

  • [Pb2(C10H6NO2)2(C2H3O2)2(CH4O)2]

  • Mr = 940.87

  • Monoclinic, P 21 /c

  • a = 7.3197 (3) Å

  • b = 8.3065 (4) Å

  • c = 23.3247 (10) Å

  • β = 90.397 (1)°

  • V = 1418.13 (11) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 11.91 mm−1

  • T = 100 K

  • 0.25 × 0.15 × 0.10 mm
Data collection

  • Bruker SMART APEX diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.155, Tmax = 0.382

  • 13298 measured reflections

  • 3267 independent reflections

  • 3055 reflections with I > 2σ(I)

  • Rint = 0.025
Refinement

  • R[F2 > 2σ(F2)] = 0.019

  • wR(F2) = 0.049

  • S = 1.06

  • 3267 reflections

  • 186 parameters

  • 1 restraint

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 1.65 e Å−3

  • Δρmin = −1.43 e Å−3

Table 1
Selected bond lengths (Å)

Pb1—O1 2.377 (3)
Pb1—O1i 2.490 (2)
Pb1—O2ii 3.145 (3)
Pb1—O3 2.382 (3)
Pb1—O4 2.761 (3)
Pb1—O5 2.696 (3)
Pb1—N1 2.643 (3)
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) x-1, y, z.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O5—H5⋯O3i 0.84 (4) 1.89 (4) 2.685 (4) 158 (5)
Symmetry code: (i) -x+1, -y+1, -z+1.

Data collection: APEX2 (Bruker, 2009[Bruker (2009). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2009[Bruker (2009). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: X-SEED (Barbour, 2001[Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536810027777/xu2798sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810027777/xu2798Isup2.hkl

checkCIF report


Comment top

The lead(II) atom in Pb(C10H6NO2)2 is N,O-chelated by the carboxylate anions in a Ψ-trigonal bipyramidal environment; four atoms are connected to the lead atom by regular coordination bonds (Mohammadnezhad et al., 2010). This compound was synthesized by the reaction of lead acetate and quinoline-2-carboxylic acid in the presence of potassium nitrite. With potassium nitrate in place of potassium nitrite, the synthesized yielded instead dinuclear [Pb(CH4O)2(C2H3O2)2(C10H6NO2)2]2 (Scheme I, Fig. 1) in which only one of the acetate groups is replaced by the quinoline-2-carboxylate group. The methanol-coordinated lead(II) atom is chelated by the acetate anion as well as by the quinoline-2-carboxylate anion; the oxygen atom involved in chelation is also datively coordinated to the symmetry-related lead atom. When a long Pb···O2ii (ii = x - 1, y, z) interaction of 3.145 (3) Å is considered to be a bond, the geometry is a Ψ-antiprism (Fig. 2).

Related literature top

For a related structure, see: Mohammadnezhad et al. (2010).

Experimental top

Lead(II) acetate (1 mmol, 0.38 g), quinoline-2-carboxylic acid (1 mmol, 0.17 g) and potassium nitrate (1 mmol, 0.10 g) were loaded into one arm of a convection tube and both of the arms were filled slowly by methanol. The chemical-bearing arm was immersed in an oil bath kept at 333 K. Crystals were formed on the inside surface of the arm kept at ambient temperature after a weekfew days.

Refinement top

Hydrogen atoms were placed in calculated positions (C–H 0.95–0.98 Å) and included in the refinement in the riding model approximation, with U(H) set to 1.2–1.5Ueq(C).

The hydroxy H-atom was located in a difference Fourier map, and was refined with a distance restraint of O–H 0.84±0.01 Å; its temperature factor was refined.

The final difference Fourier map had a peak/hole in the vicinity of Pb1.

Structure description top

The lead(II) atom in Pb(C10H6NO2)2 is N,O-chelated by the carboxylate anions in a Ψ-trigonal bipyramidal environment; four atoms are connected to the lead atom by regular coordination bonds (Mohammadnezhad et al., 2010). This compound was synthesized by the reaction of lead acetate and quinoline-2-carboxylic acid in the presence of potassium nitrite. With potassium nitrate in place of potassium nitrite, the synthesized yielded instead dinuclear [Pb(CH4O)2(C2H3O2)2(C10H6NO2)2]2 (Scheme I, Fig. 1) in which only one of the acetate groups is replaced by the quinoline-2-carboxylate group. The methanol-coordinated lead(II) atom is chelated by the acetate anion as well as by the quinoline-2-carboxylate anion; the oxygen atom involved in chelation is also datively coordinated to the symmetry-related lead atom. When a long Pb···O2ii (ii = x - 1, y, z) interaction of 3.145 (3) Å is considered to be a bond, the geometry is a Ψ-antiprism (Fig. 2).

For a related structure, see: Mohammadnezhad et al. (2010).

Computing details top

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. Thermal ellipsoid plot (Barbour, 2001) of [Pb(CH4O)2(C2H3O2)2(C10H6NO2)2]2 at the 70% probability level. Hydrogen atoms are drawn as spheres of arbitrary radius. The dinuclear molecule lies on a center-of-inversion.
[Figure 2] Fig. 2. Ψ-Square antiprismatic geometry of lead. Symmetry codes are given in Table 1.
Bis(µ-quinoline-2-carboxylato)- κ3N,O:O;κ3O:N,O-bis[(acetato- κ2O,O')(methanol-κO)lead(II)] top
Crystal data top
[Pb2(C10H6NO2)2(C2H3O2)2(CH4O)2]F(000) = 880
Mr = 940.87Dx = 2.203 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 8885 reflections
a = 7.3197 (3) Åθ = 2.6–28.3°
b = 8.3065 (4) ŵ = 11.91 mm−1
c = 23.3247 (10) ÅT = 100 K
β = 90.397 (1)°Block, colorless
V = 1418.13 (11) Å30.25 × 0.15 × 0.10 mm
Z = 2
Data collection top
Bruker SMART APEX
diffractometer		3267 independent reflections
Radiation source: fine-focus sealed tube3055 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
ω scansθmax = 27.5°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −9→9
Tmin = 0.155, Tmax = 0.382k = −10→10
13298 measured reflectionsl = −30→29
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.019Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.049H atoms treated by a mixture of independent and constrained refinement
S = 1.06 w = 1/[σ2(Fo2) + (0.0252P)2 + 2.8416P]
where P = (Fo2 + 2Fc2)/3
3267 reflections(Δ/σ)max = 0.001
186 parametersΔρmax = 1.65 e Å−3
1 restraintΔρmin = −1.43 e Å−3
Crystal data top
[Pb2(C10H6NO2)2(C2H3O2)2(CH4O)2]V = 1418.13 (11) Å3
Mr = 940.87Z = 2
Monoclinic, P21/cMo Kα radiation
a = 7.3197 (3) ŵ = 11.91 mm−1
b = 8.3065 (4) ÅT = 100 K
c = 23.3247 (10) Å0.25 × 0.15 × 0.10 mm
β = 90.397 (1)°
Data collection top
Bruker SMART APEX
diffractometer		3267 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		3055 reflections with I > 2σ(I)
Tmin = 0.155, Tmax = 0.382Rint = 0.025
13298 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0191 restraint
wR(F2) = 0.049H atoms treated by a mixture of independent and constrained refinement
S = 1.06Δρmax = 1.65 e Å−3
3267 reflectionsΔρmin = −1.43 e Å−3
186 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb10.271223 (16)0.534286 (15)0.449130 (5)0.01353 (5)
O10.5946 (3)0.5505 (3)0.45723 (11)0.0199 (5)
O20.8654 (3)0.6518 (3)0.43362 (11)0.0240 (6)
O30.3648 (4)0.2628 (4)0.43453 (12)0.0313 (7)
O40.1736 (4)0.3174 (3)0.36464 (12)0.0294 (6)
O50.3561 (4)0.8211 (4)0.49639 (12)0.0284 (6)
H50.454 (4)0.818 (7)0.515 (2)0.043*
N10.4435 (4)0.6512 (3)0.35907 (12)0.0142 (5)
C10.7022 (4)0.6278 (4)0.42410 (14)0.0158 (7)
C20.6171 (4)0.6881 (4)0.36843 (14)0.0154 (6)
C30.7256 (5)0.7731 (5)0.32939 (16)0.0212 (7)
H30.84770.80200.33890.025*
C40.6514 (5)0.8138 (5)0.27705 (17)0.0247 (8)
H40.72300.86890.24950.030*
C50.4697 (5)0.7735 (4)0.26467 (15)0.0185 (7)
C60.3834 (5)0.8108 (5)0.21153 (16)0.0252 (8)
H60.45120.86280.18230.030*
C70.2051 (6)0.7731 (5)0.20205 (15)0.0251 (8)
H70.14890.80010.16650.030*
C80.1033 (5)0.6945 (5)0.24449 (15)0.0238 (8)
H8−0.02070.66720.23710.029*
C90.1807 (5)0.6563 (5)0.29670 (15)0.0200 (7)
H90.10990.60460.32530.024*
C100.3661 (5)0.6944 (4)0.30758 (14)0.0152 (6)
C110.2681 (5)0.2208 (5)0.39130 (15)0.0213 (7)
C120.2797 (8)0.0481 (5)0.3721 (2)0.0366 (11)
H12A0.17870.02460.34560.055*
H12B0.2717−0.02290.40560.055*
H12C0.39620.03020.35270.055*
C130.2189 (7)0.8980 (7)0.5289 (2)0.0478 (13)
H13A0.09840.86080.51600.072*
H13B0.22761.01480.52370.072*
H13C0.23560.87170.56960.072*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.00951 (7)0.01915 (8)0.01191 (7)0.00240 (5)−0.00103 (4)0.00037 (5)
O10.0138 (12)0.0310 (15)0.0148 (12)0.0017 (10)−0.0010 (9)0.0060 (10)
O20.0141 (12)0.0336 (15)0.0244 (13)−0.0003 (11)−0.0035 (10)0.0041 (11)
O30.0334 (16)0.0291 (15)0.0313 (15)0.0141 (13)−0.0169 (12)−0.0117 (12)
O40.0368 (16)0.0248 (14)0.0264 (14)0.0051 (13)−0.0145 (12)−0.0018 (12)
O50.0276 (15)0.0275 (14)0.0300 (15)0.0107 (12)−0.0137 (12)−0.0051 (12)
N10.0136 (13)0.0167 (14)0.0123 (13)0.0012 (11)−0.0002 (10)0.0004 (11)
C10.0140 (15)0.0187 (17)0.0147 (15)0.0024 (13)−0.0004 (12)−0.0010 (13)
C20.0140 (15)0.0158 (16)0.0164 (16)0.0025 (13)0.0001 (12)−0.0024 (13)
C30.0126 (16)0.0240 (18)0.0270 (19)−0.0014 (14)0.0025 (14)0.0049 (15)
C40.0204 (18)0.0270 (19)0.0269 (19)0.0012 (16)0.0050 (15)0.0112 (16)
C50.0208 (17)0.0197 (17)0.0151 (16)0.0040 (14)0.0011 (13)0.0045 (13)
C60.029 (2)0.030 (2)0.0169 (17)0.0070 (17)0.0022 (15)0.0094 (15)
C70.028 (2)0.034 (2)0.0130 (17)0.0087 (17)−0.0044 (14)0.0041 (15)
C80.0205 (18)0.033 (2)0.0176 (17)0.0043 (16)−0.0045 (14)−0.0012 (15)
C90.0181 (17)0.0249 (18)0.0171 (16)0.0017 (14)−0.0004 (13)0.0005 (14)
C100.0163 (16)0.0159 (16)0.0135 (15)0.0049 (13)0.0007 (12)−0.0016 (12)
C110.0220 (18)0.0237 (19)0.0182 (17)0.0009 (15)−0.0047 (14)0.0001 (14)
C120.055 (3)0.023 (2)0.032 (2)0.0088 (19)−0.012 (2)−0.0055 (17)
C130.047 (3)0.047 (3)0.049 (3)0.022 (3)−0.006 (2)−0.013 (3)
Geometric parameters (Å, º) top
Pb1—O12.377 (3)C4—C51.400 (5)
Pb1—O1i2.490 (2)C4—H40.9500
Pb1—O2ii3.145 (3)C5—C101.421 (5)
Pb1—O32.382 (3)C5—C61.422 (5)
Pb1—O42.761 (3)C6—C71.359 (6)
Pb1—O52.696 (3)C6—H60.9500
Pb1—N12.643 (3)C7—C81.404 (5)
O1—C11.280 (4)C7—H70.9500
O2—C11.230 (4)C8—C91.376 (5)
O3—C111.276 (4)C8—H80.9500
O4—C111.226 (4)C9—C101.415 (5)
O5—C131.416 (6)C9—H90.9500
O5—H50.84 (4)C11—C121.505 (5)
N1—C21.324 (4)C12—H12A0.9800
N1—C101.372 (4)C12—H12B0.9800
C1—C21.521 (5)C12—H12C0.9800
C2—C31.403 (5)C13—H13A0.9800
C3—C41.375 (5)C13—H13B0.9800
C3—H30.9500C13—H13C0.9800
O1—Pb1—O377.17 (10)C4—C3—H3120.7
O1—Pb1—O1i63.88 (10)C2—C3—H3120.7
O3—Pb1—O1i75.27 (9)C3—C4—C5119.6 (3)
O1—Pb1—N164.02 (8)C3—C4—H4120.2
O3—Pb1—N195.46 (10)C5—C4—H4120.2
O1i—Pb1—N1127.85 (8)C4—C5—C10118.4 (3)
O1—Pb1—O571.99 (9)C4—C5—C6122.9 (3)
O3—Pb1—O5146.04 (8)C10—C5—C6118.6 (3)
O1i—Pb1—O578.63 (8)C7—C6—C5120.8 (4)
N1—Pb1—O583.70 (9)C7—C6—H6119.6
O1—Pb1—O4110.27 (9)C5—C6—H6119.6
O3—Pb1—O449.71 (8)C6—C7—C8120.4 (3)
O1i—Pb1—O4122.70 (8)C6—C7—H7119.8
N1—Pb1—O478.17 (9)C8—C7—H7119.8
O5—Pb1—O4157.89 (8)C9—C8—C7120.9 (4)
O1—Pb1—O2i105.53 (7)C9—C8—H8119.5
O3—Pb1—O2i76.37 (9)C7—C8—H8119.5
O1i—Pb1—O2i42.37 (7)C8—C9—C10119.7 (3)
N1—Pb1—O2i168.31 (8)C8—C9—H9120.2
O5—Pb1—O2i98.35 (8)C10—C9—H9120.2
O4—Pb1—O2i101.97 (8)N1—C10—C9119.2 (3)
C1—O1—Pb1126.7 (2)N1—C10—C5121.2 (3)
C1—O1—Pb1i115.5 (2)C9—C10—C5119.5 (3)
Pb1—O1—Pb1i116.12 (10)O4—C11—O3122.0 (4)
C11—O3—Pb1102.3 (2)O4—C11—C12120.4 (3)
C11—O4—Pb185.6 (2)O3—C11—C12117.6 (3)
C13—O5—Pb1117.1 (3)C11—C12—H12A109.5
C13—O5—H5110 (4)C11—C12—H12B109.5
Pb1—O5—H5112 (4)H12A—C12—H12B109.5
C2—N1—C10118.3 (3)C11—C12—H12C109.5
C2—N1—Pb1114.6 (2)H12A—C12—H12C109.5
C10—N1—Pb1126.5 (2)H12B—C12—H12C109.5
O2—C1—O1125.0 (3)O5—C13—H13A109.5
O2—C1—C2119.5 (3)O5—C13—H13B109.5
O1—C1—C2115.5 (3)H13A—C13—H13B109.5
N1—C2—C3123.8 (3)O5—C13—H13C109.5
N1—C2—C1116.9 (3)H13A—C13—H13C109.5
C3—C2—C1119.3 (3)H13B—C13—H13C109.5
C4—C3—C2118.6 (3)
O3—Pb1—O1—C1116.0 (3)O5—Pb1—N1—C10−110.9 (3)
O1i—Pb1—O1—C1−164.3 (3)O4—Pb1—N1—C1056.4 (3)
N1—Pb1—O1—C113.3 (3)O2i—Pb1—N1—C10148.3 (3)
O5—Pb1—O1—C1−78.4 (3)Pb1—O1—C1—O2169.7 (3)
O4—Pb1—O1—C178.3 (3)Pb1i—O1—C1—O25.3 (4)
O2i—Pb1—O1—C1−172.3 (3)Pb1—O1—C1—C2−12.1 (4)
O3—Pb1—O1—Pb1i−79.70 (12)Pb1i—O1—C1—C2−176.6 (2)
O1i—Pb1—O1—Pb1i0.0C10—N1—C2—C32.0 (5)
N1—Pb1—O1—Pb1i177.62 (15)Pb1—N1—C2—C3−170.2 (3)
O5—Pb1—O1—Pb1i85.90 (12)C10—N1—C2—C1−175.7 (3)
O4—Pb1—O1—Pb1i−117.41 (11)Pb1—N1—C2—C112.1 (4)
O2i—Pb1—O1—Pb1i−8.01 (13)O2—C1—C2—N1176.4 (3)
O1—Pb1—O3—C11−134.9 (3)O1—C1—C2—N1−1.8 (5)
O1i—Pb1—O3—C11159.2 (3)O2—C1—C2—C3−1.3 (5)
N1—Pb1—O3—C11−73.1 (3)O1—C1—C2—C3−179.6 (3)
O5—Pb1—O3—C11−159.9 (2)N1—C2—C3—C4−3.5 (6)
O4—Pb1—O3—C11−3.6 (2)C1—C2—C3—C4174.1 (3)
O2i—Pb1—O3—C11115.4 (3)C2—C3—C4—C51.7 (6)
O1—Pb1—O4—C1155.1 (2)C3—C4—C5—C101.4 (6)
O3—Pb1—O4—C113.7 (2)C3—C4—C5—C6−179.8 (4)
O1i—Pb1—O4—C11−16.2 (3)C4—C5—C6—C7−178.2 (4)
N1—Pb1—O4—C11111.5 (2)C10—C5—C6—C70.6 (6)
O5—Pb1—O4—C11147.1 (3)C5—C6—C7—C8−0.8 (6)
O2i—Pb1—O4—C11−56.6 (2)C6—C7—C8—C91.0 (6)
O1—Pb1—O5—C13−157.6 (3)C7—C8—C9—C10−1.0 (6)
O3—Pb1—O5—C13−131.9 (3)C2—N1—C10—C9−180.0 (3)
O1i—Pb1—O5—C13−91.6 (3)Pb1—N1—C10—C9−8.8 (4)
N1—Pb1—O5—C13137.7 (3)C2—N1—C10—C51.4 (5)
O4—Pb1—O5—C13102.7 (4)Pb1—N1—C10—C5172.5 (2)
O2i—Pb1—O5—C13−53.9 (3)C8—C9—C10—N1−177.9 (3)
O1—Pb1—N1—C2−12.5 (2)C8—C9—C10—C50.8 (5)
O3—Pb1—N1—C2−85.3 (2)C4—C5—C10—N1−3.0 (5)
O1i—Pb1—N1—C2−9.8 (3)C6—C5—C10—N1178.1 (3)
O5—Pb1—N1—C260.5 (2)C4—C5—C10—C9178.3 (3)
O4—Pb1—N1—C2−132.2 (2)C6—C5—C10—C9−0.6 (5)
O2i—Pb1—N1—C2−40.3 (5)Pb1—O4—C11—O3−6.2 (4)
O1—Pb1—N1—C10176.1 (3)Pb1—O4—C11—C12176.4 (4)
O3—Pb1—N1—C10103.2 (3)Pb1—O3—C11—O47.4 (5)
O1i—Pb1—N1—C10178.8 (2)Pb1—O3—C11—C12−175.2 (3)
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x−1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5···O3i0.84 (4)1.89 (4)2.685 (4)158 (5)
Symmetry code: (i) −x+1, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula[Pb2(C10H6NO2)2(C2H3O2)2(CH4O)2]
Mr940.87
Crystal system, space groupMonoclinic, P21/c
Temperature (K)100
a, b, c (Å)7.3197 (3), 8.3065 (4), 23.3247 (10)
β (°) 90.397 (1)
V (Å3)1418.13 (11)
Z2
Radiation typeMo Kα
µ (mm−1)11.91
Crystal size (mm)0.25 × 0.15 × 0.10
Data collection
DiffractometerBruker SMART APEX
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.155, 0.382
No. of measured, independent and
observed [I > 2σ(I)] reflections		13298, 3267, 3055
Rint0.025
(sin θ/λ)max (Å−1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.019, 0.049, 1.06
No. of reflections3267
No. of parameters186
No. of restraints1
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)1.65, −1.43

Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2010).

Selected bond lengths (Å) top
Pb1—O12.377 (3)Pb1—O42.761 (3)
Pb1—O1i2.490 (2)Pb1—O52.696 (3)
Pb1—O2ii3.145 (3)Pb1—N12.643 (3)
Pb1—O32.382 (3)
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x−1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5···O3i0.84 (4)1.89 (4)2.685 (4)158 (5)
Symmetry code: (i) −x+1, −y+1, −z+1.
 

Acknowledgements

We thank Shahid Beheshti University and the University of Malaya for supporting this study.

References

First citationBarbour, L. J. (2001). J. Supramol. Chem. 1, 189–191.  CrossRef CAS Google Scholar
 First citationBruker (2009). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
 First citationMohammadnezhad, G., Ghanbarpour, A. R., Amini, M. M. & Ng, S. W. (2010). Acta Cryst. E66, m946.  Web of Science CSD CrossRef IUCr Journals Google Scholar
 First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.  Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
 First citationWestrip, S. P. (2010). J. Appl. Cryst. 43, 920–925.  Web of Science CrossRef CAS IUCr Journals Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

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ISSN: 2056-9890
Volume 66| Part 8| August 2010| Page m963
https://doi.org/10.1107/S1600536810027777
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