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Bis(μ-2-methyl­quinolin-8-olato)-κ3N,O:O;κ3O:N,O-bis­­[(acetato-κ2O,O′)lead(II)]

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 27 January 2009; accepted 29 January 2009; online 11 February 2009)

Both independent PbII atoms in the title compound, [Pb2(C10H8NO)2(C2H3O2)2], are chelated by acetate and substituted quinolin-8-olate anions; the O atoms of the quinolin-8-olates also bridge to confer a five-coordinate status to each metal center. The geometry approximates a distorted Ψ-fac octa­hedron in which one of the sites is occupied by a stereochemically active lone pair.

Related literature

The structural chemistry of lead(II) 8-hydroxy­quinolinates has been reviewed, including bis­(μ-acetato)diacetatotetra­kis(μ-quinolin-8-olato)tetra­lead dihydrate (Shahverdizadeh et al., 2008[Shahverdizadeh, G. H., Soudi, A. A., Morsali, A. & Retailleau, P. (2008). Inorg. Chim. Acta, 361, 1875-1884.]).

[Scheme 1]

Experimental

Crystal data
  • [Pb2(C10H8NO)2(C2H3O2)2]

  • Mr = 848.82

  • Orthorhombic, P b c a

  • a = 13.7421 (2) Å

  • b = 18.0682 (3) Å

  • c = 18.6113 (4) Å

  • V = 4621.1 (1) Å3

  • Z = 8

  • Mo Kα radiation

  • μ = 14.60 mm−1

  • T = 100 (2) K

  • 0.20 × 0.10 × 0.08 mm

Data collection
  • Bruker SMART APEX diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.158, Tmax = 0.388 (expected range = 0.127–0.311)

  • 33016 measured reflections

  • 4063 independent reflections

  • 3133 reflections with I > 2σ(I)

  • Rint = 0.090

Refinement
  • R[F2 > 2σ(F2)] = 0.046

  • wR(F2) = 0.115

  • S = 1.45

  • 4063 reflections

  • 264 parameters

  • 192 restraints

  • H-atom parameters constrained

  • Δρmax = 4.37 e Å−3

  • Δρmin = −2.70 e Å−3

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). 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, 2009[Westrip, S. P. (2009). publCIF. In preparation.]).

Supporting information


Related literature top

The structural chemistry of lead(II) 8-hydroxyquinolinates has been reviewed; for bis(µ-acetato)diacetatotetrakis(µ-quinolin-8-olato)tetralead dihydrate in particular, see: Shahverdizadeh et al. (2008).

Experimental top

Lead acetate (0.38 g, 1 mmol) and 2-methyl-8-hydroxyquinoline (0.32 g, 2 mmol) were loaded into a convection tube; the tube was filled with dry methanol and kept at 333 K. Crystals were collected from the side arm after 1 day.

Refinement top

Carbon-bound H-atoms were placed in calculated positions (C—H 0.93 to 0.98 Å) and were included in the refinement in the riding model approximation, with U(H) set to 1.2 to 1.5U(C).

The quinolinyl ring was refined as a rigid group with C-C = 1.39 Å. The crystal diffracted strongly owing to two extremely heavy metal atoms. However, their presence introduced severe absorption problems that could not be corrected analytically as the crystal did not have regular faces. Although a sphere of reflections was measured, multi-scan treatment only marginally improved the quality. The final difference Fourier map had large peaks/deep holes near the lead atoms. The anisotropic displacement factors of the carbon, nitrogen and oxygen atoms had to be restrained to be nearly isotropic.

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 2008); 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, 2009).

Figures top
[Figure 1] Fig. 1. Thermal ellipsoid plot (Barbour, 2001) of Pb2(C2H3O2)2(C10H8NO)2 at the 70% probability level. Hydrogen atoms are drawn as spheres of arbitrary radius.
Bis(µ-2-methylquinolin-8-οlato)- κ3N,O:O;κ3O:N,O- bis[(acetato-κ2O,O')lead(II)] top
Crystal data top
[Pb2(C10H8NO)2(C2H3O2)2]F(000) = 3136
Mr = 848.82Dx = 2.440 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 6225 reflections
a = 13.7421 (2) Åθ = 2.2–28.3°
b = 18.0682 (3) ŵ = 14.60 mm1
c = 18.6113 (4) ÅT = 100 K
V = 4621.1 (1) Å3Block, yellow
Z = 80.20 × 0.10 × 0.08 mm
Data collection top
Bruker SMART APEX
diffractometer
4063 independent reflections
Radiation source: fine-focus sealed tube3133 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.090
ω scansθmax = 25.0°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1616
Tmin = 0.158, Tmax = 0.388k = 2121
33016 measured reflectionsl = 2221
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)] = 0.046Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.115H-atom parameters constrained
S = 1.45 w = 1/[σ2(Fo2) + (0.0388P)2 + 1P]
where P = (Fo2 + 2Fc2)/3
4063 reflections(Δ/σ)max = 0.001
264 parametersΔρmax = 4.37 e Å3
192 restraintsΔρmin = 2.70 e Å3
Crystal data top
[Pb2(C10H8NO)2(C2H3O2)2]V = 4621.1 (1) Å3
Mr = 848.82Z = 8
Orthorhombic, PbcaMo Kα radiation
a = 13.7421 (2) ŵ = 14.60 mm1
b = 18.0682 (3) ÅT = 100 K
c = 18.6113 (4) Å0.20 × 0.10 × 0.08 mm
Data collection top
Bruker SMART APEX
diffractometer
4063 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
3133 reflections with I > 2σ(I)
Tmin = 0.158, Tmax = 0.388Rint = 0.090
33016 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.046192 restraints
wR(F2) = 0.115H-atom parameters constrained
S = 1.45Δρmax = 4.37 e Å3
4063 reflectionsΔρmin = 2.70 e Å3
264 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb10.28159 (3)0.37522 (2)0.52835 (2)0.01649 (15)
Pb20.56385 (3)0.38486 (2)0.48211 (2)0.01580 (14)
O10.3933 (6)0.4289 (4)0.4554 (4)0.0190 (18)
O20.4542 (5)0.3401 (4)0.5634 (4)0.0193 (17)
O30.3217 (6)0.4747 (4)0.6014 (5)0.029 (2)
O40.1631 (6)0.4725 (4)0.5938 (5)0.027 (2)
O50.5071 (6)0.2851 (4)0.4186 (4)0.027 (2)
O60.6648 (6)0.2738 (4)0.3994 (5)0.030 (2)
C10.3673 (3)0.4758 (3)0.4007 (3)0.017 (2)
C20.4354 (3)0.5134 (3)0.3593 (3)0.021 (3)
H20.50290.50760.36890.026*
C30.4048 (3)0.5595 (3)0.3040 (3)0.020 (3)
H30.45140.58520.27570.024*
C40.3061 (4)0.5680 (3)0.2900 (3)0.019 (3)
H40.28520.59960.25220.023*
C50.2380 (3)0.53044 (19)0.3314 (2)0.021 (3)
C60.2686 (3)0.48434 (18)0.3868 (2)0.015 (2)
N10.2004 (3)0.4467 (2)0.4282 (2)0.016 (2)
C90.1017 (3)0.4552 (3)0.4142 (3)0.017 (2)
C80.0711 (3)0.5013 (3)0.3589 (3)0.022 (3)
H80.00360.50720.34940.026*
C70.1392 (3)0.5389 (3)0.3175 (3)0.019 (3)
H70.11830.57050.27970.023*
C100.0363 (9)0.4109 (6)0.4591 (7)0.025 (3)
H10A0.05350.35850.45470.038*
H10B0.03100.41830.44320.038*
H10C0.04270.42640.50930.038*
C110.4812 (3)0.2885 (3)0.6133 (3)0.017 (2)
C120.4148 (3)0.2545 (3)0.6589 (3)0.024 (3)
H120.34750.26590.65540.028*
C130.4469 (3)0.2036 (3)0.7097 (3)0.018 (3)
H130.40160.18030.74090.022*
C140.5454 (4)0.1868 (3)0.7148 (3)0.022 (3)
H140.56730.15210.74960.026*
C150.6118 (3)0.22089 (19)0.6692 (2)0.018 (3)
C160.5797 (3)0.27173 (19)0.6184 (2)0.013 (2)
N20.6460 (3)0.3058 (2)0.5728 (2)0.015 (2)
C190.7445 (3)0.2890 (3)0.5779 (3)0.017 (3)
C180.7766 (3)0.2382 (3)0.6287 (3)0.021 (3)
H180.84390.22670.63220.026*
C170.7102 (3)0.2041 (3)0.6743 (3)0.017 (2)
H170.73220.16940.70900.021*
C200.8077 (9)0.3291 (6)0.5282 (7)0.024 (3)
H20A0.80220.38240.53720.036*
H20B0.78800.31840.47870.036*
H20C0.87520.31340.53550.036*
C210.2377 (9)0.5005 (6)0.6175 (6)0.019 (3)
C220.2349 (10)0.5681 (6)0.6657 (7)0.031 (3)
H22A0.25600.61160.63850.047*
H22B0.27850.56050.70670.047*
H22C0.16830.57570.68310.047*
C230.5803 (8)0.2518 (6)0.3911 (6)0.017 (3)
C240.5582 (9)0.1846 (6)0.3472 (6)0.023 (3)
H24A0.57220.19480.29650.035*
H24B0.48940.17170.35260.035*
H24C0.59870.14320.36370.035*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.0121 (3)0.0160 (2)0.0214 (3)0.00051 (15)0.00086 (17)0.00142 (16)
Pb20.0108 (2)0.0164 (2)0.0201 (3)0.00012 (15)0.00039 (17)0.00064 (17)
O10.011 (4)0.024 (4)0.023 (4)0.004 (3)0.002 (3)0.008 (3)
O20.013 (4)0.021 (4)0.023 (4)0.003 (3)0.002 (3)0.004 (3)
O30.013 (5)0.027 (4)0.047 (5)0.002 (3)0.000 (4)0.013 (4)
O40.018 (5)0.031 (4)0.033 (5)0.003 (3)0.001 (4)0.008 (3)
O50.018 (4)0.027 (4)0.034 (5)0.005 (3)0.001 (4)0.012 (3)
O60.020 (5)0.034 (4)0.036 (5)0.001 (4)0.000 (4)0.004 (4)
C10.013 (6)0.018 (5)0.019 (6)0.004 (4)0.004 (4)0.001 (4)
C20.018 (6)0.018 (5)0.028 (6)0.003 (4)0.001 (5)0.002 (4)
C30.018 (6)0.022 (5)0.020 (6)0.005 (4)0.002 (5)0.001 (4)
C40.020 (6)0.018 (5)0.020 (6)0.002 (4)0.006 (5)0.001 (4)
C50.022 (6)0.014 (5)0.025 (6)0.003 (4)0.000 (5)0.002 (4)
C60.006 (5)0.018 (5)0.020 (6)0.003 (4)0.005 (4)0.002 (4)
N10.018 (5)0.012 (4)0.018 (5)0.010 (3)0.003 (4)0.002 (3)
C90.011 (5)0.017 (5)0.024 (6)0.001 (4)0.001 (4)0.007 (4)
C80.014 (6)0.024 (5)0.027 (6)0.003 (4)0.005 (5)0.001 (4)
C70.016 (6)0.018 (5)0.023 (6)0.001 (4)0.004 (5)0.004 (4)
C100.020 (6)0.027 (5)0.029 (6)0.002 (5)0.000 (5)0.002 (5)
C110.014 (6)0.024 (5)0.014 (5)0.003 (4)0.001 (4)0.000 (4)
C120.020 (6)0.027 (5)0.025 (6)0.001 (4)0.002 (5)0.002 (5)
C130.016 (6)0.019 (5)0.020 (6)0.007 (4)0.003 (5)0.000 (4)
C140.026 (6)0.023 (5)0.016 (6)0.004 (5)0.002 (5)0.001 (4)
C150.020 (6)0.014 (5)0.021 (6)0.002 (4)0.001 (5)0.005 (4)
C160.012 (6)0.016 (5)0.012 (5)0.003 (4)0.001 (4)0.005 (4)
N20.020 (5)0.013 (4)0.013 (5)0.005 (4)0.001 (4)0.001 (3)
C190.013 (6)0.019 (5)0.018 (6)0.001 (4)0.002 (4)0.000 (4)
C180.016 (6)0.025 (5)0.023 (6)0.005 (4)0.002 (5)0.000 (4)
C170.017 (6)0.016 (5)0.019 (6)0.003 (4)0.002 (5)0.004 (4)
C200.020 (6)0.021 (5)0.031 (6)0.002 (4)0.003 (5)0.001 (4)
C210.017 (6)0.017 (5)0.022 (6)0.002 (4)0.001 (5)0.006 (4)
C220.036 (7)0.022 (5)0.036 (7)0.002 (5)0.005 (6)0.003 (5)
C230.015 (6)0.018 (5)0.019 (5)0.003 (4)0.000 (5)0.003 (4)
C240.023 (6)0.023 (5)0.023 (6)0.001 (5)0.001 (5)0.000 (4)
Geometric parameters (Å, º) top
Pb1—O12.267 (8)C7—H70.9500
Pb1—O32.321 (8)C10—H10A0.9800
Pb1—N12.527 (4)C10—H10B0.9800
Pb1—O22.541 (7)C10—H10C0.9800
Pb1—O42.688 (8)C11—C121.3900
Pb2—O22.283 (7)C11—C161.3900
Pb2—O52.292 (7)C12—C131.3900
Pb2—N22.482 (4)C12—H120.9500
Pb2—O12.525 (7)C13—C141.3900
Pb2—O46.095 (8)C13—H130.9500
O1—C11.372 (8)C14—C151.3900
O2—C111.366 (8)C14—H140.9500
O3—C211.280 (14)C15—C161.3900
O4—C211.226 (14)C15—C171.3900
O5—C231.279 (13)C16—N21.3900
O6—C231.237 (13)N2—C191.3900
C1—C21.3900C19—C181.3900
C1—C61.3900C19—C201.460 (12)
C2—C31.3900C18—C171.3900
C2—H20.9500C18—H180.9500
C3—C41.3900C17—H170.9500
C3—H30.9500C20—H20A0.9800
C4—C51.3900C20—H20B0.9800
C4—H40.9500C20—H20C0.9800
C5—C61.3900C21—C221.515 (16)
C5—C71.3900C22—H22A0.9800
C6—N11.3900C22—H22B0.9800
N1—C91.3900C22—H22C0.9800
C9—C81.3900C23—C241.494 (15)
C9—C101.465 (12)C24—H24A0.9800
C8—C71.3900C24—H24B0.9800
C8—H80.9500C24—H24C0.9800
O1—Pb1—O381.9 (3)C9—C10—H10A109.5
O1—Pb1—N168.8 (2)C9—C10—H10B109.5
O3—Pb1—N198.1 (2)H10A—C10—H10B109.5
O1—Pb1—O268.2 (2)C9—C10—H10C109.5
O3—Pb1—O279.7 (3)H10A—C10—H10C109.5
N1—Pb1—O2136.80 (19)H10B—C10—H10C109.5
O1—Pb1—O4113.7 (2)O2—C11—C12122.6 (4)
O3—Pb1—O451.1 (3)O2—C11—C16117.4 (4)
N1—Pb1—O474.5 (2)C12—C11—C16120.0
O2—Pb1—O4127.8 (2)C11—C12—C13120.0
O2—Pb2—O580.7 (3)C11—C12—H12120.0
O2—Pb2—N269.3 (2)C13—C12—H12120.0
O5—Pb2—N293.0 (2)C14—C13—C12120.0
O2—Pb2—O168.3 (2)C14—C13—H13120.0
O5—Pb2—O180.3 (3)C12—C13—H13120.0
N2—Pb2—O1137.5 (2)C13—C14—C15120.0
O2—Pb2—O443.12 (19)C13—C14—H14120.0
O5—Pb2—O494.2 (2)C15—C14—H14120.0
N2—Pb2—O4109.19 (13)C14—C15—C16120.0
O1—Pb2—O431.4 (2)C14—C15—C17120.0
C1—O1—Pb1122.2 (5)C16—C15—C17120.0
C1—O1—Pb2125.6 (5)N2—C16—C15120.0
Pb1—O1—Pb2112.1 (3)N2—C16—C11120.0
C11—O2—Pb2120.9 (5)C15—C16—C11120.0
C11—O2—Pb1126.7 (5)C16—N2—C19120.0
Pb2—O2—Pb1111.0 (3)C16—N2—Pb2111.83 (17)
C21—O3—Pb1101.8 (7)C19—N2—Pb2127.96 (17)
C21—O4—Pb185.8 (7)N2—C19—C18120.0
C21—O4—Pb258.3 (7)N2—C19—C20115.3 (6)
C23—O5—Pb2108.0 (7)C18—C19—C20124.7 (6)
O1—C1—C2122.5 (4)C17—C18—C19120.0
O1—C1—C6117.5 (4)C17—C18—H18120.0
C2—C1—C6120.0C19—C18—H18120.0
C3—C2—C1120.0C18—C17—C15120.0
C3—C2—H2120.0C18—C17—H17120.0
C1—C2—H2120.0C15—C17—H17120.0
C2—C3—C4120.0C19—C20—H20A109.5
C2—C3—H3120.0C19—C20—H20B109.5
C4—C3—H3120.0H20A—C20—H20B109.5
C5—C4—C3120.0C19—C20—H20C109.5
C5—C4—H4120.0H20A—C20—H20C109.5
C3—C4—H4120.0H20B—C20—H20C109.5
C6—C5—C4120.0O4—C21—O3121.3 (10)
C6—C5—C7120.0O4—C21—C22121.6 (11)
C4—C5—C7120.0O3—C21—C22117.1 (11)
N1—C6—C5120.0C21—C22—H22A109.5
N1—C6—C1120.0C21—C22—H22B109.5
C5—C6—C1120.0H22A—C22—H22B109.5
C6—N1—C9120.0C21—C22—H22C109.5
C6—N1—Pb1111.19 (17)H22A—C22—H22C109.5
C9—N1—Pb1128.68 (17)H22B—C22—H22C109.5
C8—C9—N1120.0O6—C23—O5122.4 (10)
C8—C9—C10124.4 (6)O6—C23—C24121.3 (11)
N1—C9—C10115.6 (6)O5—C23—C24116.2 (10)
C9—C8—C7120.0C23—C24—H24A109.5
C9—C8—H8120.0C23—C24—H24B109.5
C7—C8—H8120.0H24A—C24—H24B109.5
C8—C7—C5120.0C23—C24—H24C109.5
C8—C7—H7120.0H24A—C24—H24C109.5
C5—C7—H7120.0H24B—C24—H24C109.5
O3—Pb1—O1—C196.4 (6)C2—C1—C6—N1180.0
N1—Pb1—O1—C15.6 (5)O1—C1—C6—C5179.2 (6)
O2—Pb1—O1—C1178.6 (7)C2—C1—C6—C50.0
O4—Pb1—O1—C155.5 (7)C5—C6—N1—C90.0
O3—Pb1—O1—Pb287.6 (3)C1—C6—N1—C9180.0
N1—Pb1—O1—Pb2170.4 (4)C5—C6—N1—Pb1176.3 (3)
O2—Pb1—O1—Pb25.5 (3)C1—C6—N1—Pb13.7 (3)
O4—Pb1—O1—Pb2128.5 (3)O1—Pb1—N1—C64.6 (2)
O2—Pb2—O1—C1178.1 (7)O3—Pb1—N1—C673.3 (3)
O5—Pb2—O1—C198.1 (6)O2—Pb1—N1—C610.3 (4)
N2—Pb2—O1—C1178.1 (5)O4—Pb1—N1—C6119.1 (3)
O4—Pb2—O1—C1146.9 (8)O1—Pb1—N1—C9179.5 (3)
O2—Pb2—O1—Pb16.1 (3)O3—Pb1—N1—C9102.5 (3)
O5—Pb2—O1—Pb177.7 (3)O2—Pb1—N1—C9173.9 (3)
N2—Pb2—O1—Pb16.1 (5)O4—Pb1—N1—C956.8 (3)
O4—Pb2—O1—Pb137.3 (2)C6—N1—C9—C80.0
O5—Pb2—O2—C1189.3 (6)Pb1—N1—C9—C8175.5 (3)
N2—Pb2—O2—C117.5 (5)C6—N1—C9—C10177.7 (6)
O1—Pb2—O2—C11172.5 (6)Pb1—N1—C9—C106.8 (6)
O4—Pb2—O2—C11164.3 (7)N1—C9—C8—C70.0
O5—Pb2—O2—Pb177.7 (3)C10—C9—C8—C7177.4 (7)
N2—Pb2—O2—Pb1174.6 (3)C9—C8—C7—C50.0
O1—Pb2—O2—Pb15.4 (2)C6—C5—C7—C80.0
O4—Pb2—O2—Pb128.68 (16)C4—C5—C7—C8180.0
O1—Pb1—O2—C11172.1 (7)Pb2—O2—C11—C12173.4 (2)
O3—Pb1—O2—C11102.6 (6)Pb1—O2—C11—C128.6 (7)
N1—Pb1—O2—C11166.5 (5)Pb2—O2—C11—C168.0 (7)
O4—Pb1—O2—C1184.2 (6)Pb1—O2—C11—C16172.8 (3)
O1—Pb1—O2—Pb26.0 (3)O2—C11—C12—C13178.6 (6)
O3—Pb1—O2—Pb291.3 (3)C16—C11—C12—C130.0
N1—Pb1—O2—Pb20.4 (5)C11—C12—C13—C140.0
O4—Pb1—O2—Pb2109.7 (3)C12—C13—C14—C150.0
O1—Pb1—O3—C21130.1 (7)C13—C14—C15—C160.0
N1—Pb1—O3—C2163.0 (7)C13—C14—C15—C17180.0
O2—Pb1—O3—C21160.8 (7)C14—C15—C16—N2180.0
O4—Pb1—O3—C210.5 (6)C17—C15—C16—N20.0
O1—Pb1—O4—C2157.0 (7)C14—C15—C16—C110.0
O3—Pb1—O4—C210.5 (7)C17—C15—C16—C11180.0
N1—Pb1—O4—C21114.9 (7)O2—C11—C16—N21.4 (6)
O2—Pb1—O4—C2123.0 (8)C12—C11—C16—N2180.0
O1—Pb1—O4—Pb237.8 (2)O2—C11—C16—C15178.6 (6)
O3—Pb1—O4—Pb218.6 (4)C12—C11—C16—C150.0
N1—Pb1—O4—Pb295.7 (2)C15—C16—N2—C190.0
O2—Pb1—O4—Pb242.2 (2)C11—C16—N2—C19180.0
O2—Pb2—O4—C2197.5 (8)C15—C16—N2—Pb2175.1 (3)
O5—Pb2—O4—C21169.2 (8)C11—C16—N2—Pb24.9 (3)
N2—Pb2—O4—C2174.5 (8)O2—Pb2—N2—C166.2 (2)
O1—Pb2—O4—C21127.3 (8)O5—Pb2—N2—C1672.7 (3)
O2—Pb2—O4—Pb159.9 (3)O1—Pb2—N2—C166.2 (4)
O5—Pb2—O4—Pb111.8 (3)O4—Pb2—N2—C1622.8 (2)
N2—Pb2—O4—Pb182.9 (3)O2—Pb2—N2—C19179.2 (3)
O1—Pb2—O4—Pb175.4 (4)O5—Pb2—N2—C19101.9 (3)
O2—Pb2—O5—C23135.3 (7)O1—Pb2—N2—C19179.2 (3)
N2—Pb2—O5—C2366.8 (7)O4—Pb2—N2—C19162.6 (2)
O1—Pb2—O5—C23155.4 (7)C16—N2—C19—C180.0
O4—Pb2—O5—C23176.4 (7)Pb2—N2—C19—C18174.2 (3)
Pb1—O1—C1—C2174.9 (3)C16—N2—C19—C20178.9 (6)
Pb2—O1—C1—C29.7 (7)Pb2—N2—C19—C206.9 (6)
Pb1—O1—C1—C65.9 (7)N2—C19—C18—C170.0
Pb2—O1—C1—C6169.5 (3)C20—C19—C18—C17178.8 (7)
O1—C1—C2—C3179.2 (6)C19—C18—C17—C150.0
C6—C1—C2—C30.0C14—C15—C17—C18180.0
C1—C2—C3—C40.0C16—C15—C17—C180.0
C2—C3—C4—C50.0Pb1—O4—C21—O30.9 (11)
C3—C4—C5—C60.0Pb2—O4—C21—O310.0 (8)
C3—C4—C5—C7180.0Pb1—O4—C21—C22179.5 (10)
C4—C5—C6—N1180.0Pb2—O4—C21—C22168.6 (13)
C7—C5—C6—N10.0Pb1—O3—C21—O41.0 (13)
C4—C5—C6—C10.0Pb1—O3—C21—C22179.7 (8)
C7—C5—C6—C1180.0Pb2—O5—C23—O60.7 (13)
O1—C1—C6—N10.8 (5)Pb2—O5—C23—C24180.0 (7)

Experimental details

Crystal data
Chemical formula[Pb2(C10H8NO)2(C2H3O2)2]
Mr848.82
Crystal system, space groupOrthorhombic, Pbca
Temperature (K)100
a, b, c (Å)13.7421 (2), 18.0682 (3), 18.6113 (4)
V3)4621.1 (1)
Z8
Radiation typeMo Kα
µ (mm1)14.60
Crystal size (mm)0.20 × 0.10 × 0.08
Data collection
DiffractometerBruker SMART APEX
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.158, 0.388
No. of measured, independent and
observed [I > 2σ(I)] reflections
33016, 4063, 3133
Rint0.090
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.046, 0.115, 1.45
No. of reflections4063
No. of parameters264
No. of restraints192
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)4.37, 2.70

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

 

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 (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationShahverdizadeh, G. H., Soudi, A. A., Morsali, A. & Retailleau, P. (2008). Inorg. Chim. Acta, 361, 1875–1884.  Web of Science CSD CrossRef CAS 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. (2009). publCIF. In preparation.  Google Scholar

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