Literature DB >> 21588176

Bis(quinoline-2-carboxyl-ato-κN,O)lead(II).

Gholamhossein Mohammadnezhad, Ali Reza Ghanbarpour, Mostafa M Amini, Seik Weng Ng.   

Abstract

The Pb(II) atom in the title compound, [Pb(C(10)H(6)NO(2))(2)], is N,O-chelated by two quinoline-2-carboxyl-ate anions in a distorted Ψ-trigonal-bipyramidal environment; four atoms are connected to the Pb(II) atom by regular coordination bonds. The structure also features two somewhat long Pb⋯O inter-actions [2.952 (3) and 3.014 (3) Å]. These long inter-actions give rise to a layer coordination polymer having the lead atom in a distorted Ψ-monocapped octa-hedral geometry.

Entities:  

Year:  2010        PMID: 21588176      PMCID: PMC3007439          DOI: 10.1107/S1600536810027509

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For a related structure, see: Zhang et al. (2007 ▶).

Experimental

Crystal data

[Pb(C10H6NO2)2] M = 551.51 Monoclinic, a = 16.4510 (15) Å b = 7.2895 (7) Å c = 14.1877 (13) Å β = 108.981 (1)° V = 1608.9 (3) Å3 Z = 4 Mo Kα radiation μ = 10.52 mm−1 T = 100 K 0.15 × 0.10 × 0.05 mm

Data collection

Bruker SMART APEX diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.301, T max = 0.621 9758 measured reflections 3669 independent reflections 3119 reflections with I > 2σ(I) R int = 0.033

Refinement

R[F 2 > 2σ(F 2)] = 0.026 wR(F 2) = 0.058 S = 1.03 3669 reflections 244 parameters 6 restraints H-atom parameters constrained Δρmax = 1.64 e Å−3 Δρmin = −0.93 e Å−3 Data collection: APEX2 (Bruker, 2009 ▶); cell refinement: SAINT (Bruker, 2009 ▶); data reduction: SAINT; 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 ▶). Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810027509/xu2797sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810027509/xu2797Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Pb(C10H6NO2)2]F(000) = 1040
Mr = 551.51Dx = 2.277 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3819 reflections
a = 16.4510 (15) Åθ = 2.6–28.3°
b = 7.2895 (7) ŵ = 10.52 mm1
c = 14.1877 (13) ÅT = 100 K
β = 108.981 (1)°Prism, colorless
V = 1608.9 (3) Å30.15 × 0.10 × 0.05 mm
Z = 4
Bruker SMART APEX diffractometer3669 independent reflections
Radiation source: fine-focus sealed tube3119 reflections with I > 2σ(I)
graphiteRint = 0.033
ω scansθmax = 27.5°, θmin = 1.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −12→21
Tmin = 0.301, Tmax = 0.621k = −8→9
9758 measured reflectionsl = −18→18
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.026Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.058H-atom parameters constrained
S = 1.02w = 1/[σ2(Fo2) + (0.0278P)2 + 0.2749P] where P = (Fo2 + 2Fc2)/3
3669 reflections(Δ/σ)max = 0.002
244 parametersΔρmax = 1.64 e Å3
6 restraintsΔρmin = −0.92 e Å3
xyzUiso*/Ueq
Pb10.747914 (11)0.70412 (2)0.535665 (12)0.00980 (6)
O10.7953 (2)0.6837 (4)0.4000 (2)0.0147 (7)
O20.7691 (2)0.6491 (5)0.2362 (2)0.0184 (7)
O30.7075 (2)1.0028 (4)0.4949 (2)0.0144 (7)
O40.7419 (2)1.2990 (4)0.4913 (3)0.0196 (7)
N10.6232 (2)0.6704 (5)0.3714 (3)0.0107 (8)
N20.8766 (2)0.9163 (5)0.5793 (3)0.0114 (8)
C10.7447 (3)0.6590 (6)0.3111 (3)0.0126 (10)
C20.6487 (3)0.6425 (6)0.2937 (3)0.0103 (9)
C30.5919 (3)0.6023 (6)0.1978 (3)0.0131 (9)
H30.61310.58080.14390.016*
C40.5058 (3)0.5948 (6)0.1835 (3)0.0138 (9)
H40.46630.57010.11910.017*
C50.4753 (3)0.6238 (6)0.2649 (3)0.0136 (9)
C60.3874 (3)0.6160 (6)0.2565 (3)0.0155 (10)
H60.34560.59140.19360.019*
C70.3621 (3)0.6437 (6)0.3383 (4)0.0176 (10)
H70.30290.63580.33200.021*
C80.4233 (3)0.6839 (6)0.4319 (4)0.0159 (10)
H80.40490.70410.48800.019*
C90.5090 (3)0.6940 (6)0.4427 (3)0.0152 (10)
H90.54960.72280.50580.018*
C100.5372 (3)0.6615 (6)0.3599 (3)0.0087 (9)
C110.7614 (3)1.1369 (6)0.5093 (3)0.0134 (10)
C120.8565 (3)1.0885 (6)0.5515 (3)0.0104 (9)
C130.9195 (3)1.2240 (6)0.5577 (3)0.0138 (10)
H130.90311.34560.53560.017*
C141.0048 (3)1.1769 (6)0.5963 (3)0.0146 (10)
H141.04801.26570.60020.018*
C151.0278 (3)0.9972 (6)0.6300 (3)0.0126 (9)
C161.1143 (3)0.9387 (6)0.6713 (3)0.0155 (10)
H161.15971.02430.68050.019*
C171.1325 (3)0.7599 (7)0.6981 (3)0.0169 (10)
H171.19070.72130.72330.020*
C181.0664 (3)0.6316 (7)0.6888 (3)0.0141 (10)
H181.08030.50820.70930.017*
C190.9823 (3)0.6841 (6)0.6505 (3)0.0136 (10)
H190.93790.59730.64460.016*
C200.9612 (3)0.8672 (6)0.6195 (3)0.0093 (9)
U11U22U33U12U13U23
Pb10.00792 (9)0.01030 (9)0.01183 (8)−0.00087 (7)0.00412 (6)0.00058 (7)
O10.0075 (17)0.0208 (19)0.0172 (16)−0.0020 (14)0.0061 (13)−0.0022 (13)
O20.0192 (19)0.0226 (18)0.0175 (16)0.0033 (15)0.0117 (14)−0.0028 (14)
O30.0095 (17)0.0113 (17)0.0208 (16)−0.0028 (14)0.0028 (14)−0.0009 (13)
O40.020 (2)0.0117 (17)0.0315 (19)0.0039 (15)0.0149 (15)0.0054 (15)
N10.012 (2)0.0061 (18)0.0169 (18)−0.0005 (15)0.0080 (16)0.0009 (14)
N20.014 (2)0.0097 (19)0.0115 (17)−0.0021 (16)0.0052 (15)−0.0014 (14)
C10.013 (3)0.008 (2)0.020 (2)0.0001 (18)0.009 (2)0.0037 (17)
C20.007 (2)0.006 (2)0.017 (2)0.0002 (17)0.0025 (18)0.0001 (16)
C30.014 (2)0.013 (2)0.013 (2)−0.0032 (19)0.0045 (18)−0.0013 (18)
C40.015 (3)0.007 (2)0.015 (2)−0.0004 (19)−0.0009 (18)0.0007 (17)
C50.014 (3)0.010 (2)0.016 (2)0.000 (2)0.0039 (19)0.0010 (18)
C60.012 (3)0.013 (2)0.019 (2)0.001 (2)0.0007 (19)0.0007 (19)
C70.010 (3)0.015 (2)0.026 (3)0.000 (2)0.004 (2)0.0054 (19)
C80.013 (3)0.012 (2)0.023 (2)0.001 (2)0.007 (2)0.0040 (19)
C90.014 (3)0.013 (2)0.016 (2)0.001 (2)0.0012 (19)0.0003 (18)
C100.005 (2)0.005 (2)0.014 (2)−0.0006 (16)0.0015 (17)0.0007 (15)
C110.017 (3)0.013 (2)0.012 (2)0.005 (2)0.0062 (19)0.0029 (17)
C120.013 (2)0.012 (2)0.0087 (19)0.0034 (18)0.0066 (17)−0.0013 (16)
C130.019 (3)0.008 (2)0.014 (2)0.001 (2)0.0065 (19)0.0034 (17)
C140.015 (3)0.013 (2)0.017 (2)−0.0075 (19)0.0074 (19)−0.0052 (18)
C150.014 (2)0.013 (2)0.013 (2)−0.0028 (19)0.0073 (18)−0.0023 (17)
C160.010 (2)0.017 (2)0.020 (2)−0.0033 (19)0.0052 (19)−0.0039 (19)
C170.012 (3)0.021 (3)0.016 (2)0.004 (2)0.0020 (19)−0.0007 (18)
C180.012 (3)0.015 (2)0.015 (2)0.001 (2)0.0041 (19)0.0008 (18)
C190.013 (2)0.014 (2)0.013 (2)−0.003 (2)0.0024 (18)−0.0011 (18)
C200.007 (2)0.013 (2)0.0096 (19)−0.0013 (18)0.0049 (17)−0.0030 (17)
Pb1—O12.304 (3)C6—H60.9500
Pb1—O2i2.952 (3)C7—C81.412 (7)
Pb1—O32.295 (3)C7—H70.9500
Pb1—O4ii3.014 (3)C8—C91.370 (7)
Pb1—N12.567 (4)C8—H80.9500
Pb1—N22.531 (4)C9—C101.417 (6)
O1—C11.279 (6)C9—H90.9500
O2—C11.255 (5)C11—C121.525 (6)
O3—C111.290 (6)C12—C131.413 (6)
O4—C111.229 (5)C13—C141.373 (7)
N1—C21.318 (6)C13—H130.9500
N1—C101.370 (6)C14—C151.404 (6)
N2—C121.325 (5)C14—H140.9500
N2—C201.368 (6)C15—C161.417 (6)
C1—C21.521 (6)C15—C201.419 (6)
C2—C31.408 (6)C16—C171.363 (6)
C3—C41.366 (6)C16—H160.9500
C3—H30.9500C17—C181.408 (7)
C4—C51.416 (6)C17—H170.9500
C4—H40.9500C18—C191.366 (6)
C5—C61.413 (6)C18—H180.9500
C5—C101.427 (6)C19—C201.413 (6)
C6—C71.370 (6)C19—H190.9500
O3—Pb1—O189.98 (11)C6—C7—H7119.8
O3—Pb1—N268.45 (11)C8—C7—H7119.8
O1—Pb1—N276.13 (11)C9—C8—C7120.6 (5)
O3—Pb1—N177.38 (11)C9—C8—H8119.7
O1—Pb1—N167.90 (11)C7—C8—H8119.7
N2—Pb1—N1129.71 (11)C8—C9—C10120.1 (4)
O3—Pb1—O2i80.37 (10)C8—C9—H9120.0
O1—Pb1—O2i149.57 (10)C10—C9—H9120.0
N2—Pb1—O2i73.48 (10)N1—C10—C9119.8 (4)
N1—Pb1—O2i135.90 (11)N1—C10—C5120.9 (4)
O3—Pb1—O4ii152.83 (10)C9—C10—C5119.3 (4)
O1—Pb1—O4ii76.09 (10)O4—C11—O3125.2 (4)
N2—Pb1—O4ii128.16 (11)O4—C11—C12118.0 (4)
N1—Pb1—O4ii75.78 (10)O3—C11—C12116.8 (4)
O2i—Pb1—O4ii122.81 (9)N2—C12—C13122.4 (4)
C1—O1—Pb1122.9 (3)N2—C12—C11117.5 (4)
C11—O3—Pb1123.4 (3)C13—C12—C11120.1 (4)
C2—N1—C10119.3 (4)C14—C13—C12118.9 (4)
C2—N1—Pb1113.3 (3)C14—C13—H13120.5
C10—N1—Pb1127.0 (3)C12—C13—H13120.5
C12—N2—C20119.6 (4)C13—C14—C15119.8 (4)
C12—N2—Pb1113.4 (3)C13—C14—H14120.1
C20—N2—Pb1126.7 (3)C15—C14—H14120.1
O2—C1—O1123.9 (4)C14—C15—C16123.0 (4)
O2—C1—C2117.3 (4)C14—C15—C20118.3 (4)
O1—C1—C2118.8 (4)C16—C15—C20118.6 (4)
N1—C2—C3123.3 (4)C17—C16—C15120.2 (4)
N1—C2—C1116.6 (4)C17—C16—H16119.9
C3—C2—C1120.1 (4)C15—C16—H16119.9
C4—C3—C2118.8 (4)C16—C17—C18121.1 (5)
C4—C3—H3120.6C16—C17—H17119.5
C2—C3—H3120.6C18—C17—H17119.5
C3—C4—C5119.9 (4)C19—C18—C17120.1 (5)
C3—C4—H4120.0C19—C18—H18119.9
C5—C4—H4120.0C17—C18—H18119.9
C6—C5—C4123.3 (4)C18—C19—C20120.2 (4)
C6—C5—C10119.0 (4)C18—C19—H19119.9
C4—C5—C10117.8 (4)C20—C19—H19119.9
C7—C6—C5120.5 (4)N2—C20—C19119.4 (4)
C7—C6—H6119.7N2—C20—C15121.0 (4)
C5—C6—H6119.7C19—C20—C15119.6 (4)
C6—C7—C8120.5 (5)
O3—Pb1—O1—C1−79.2 (3)C4—C5—C6—C7179.4 (5)
N2—Pb1—O1—C1−147.0 (3)C10—C5—C6—C7−0.2 (7)
N1—Pb1—O1—C1−2.8 (3)C5—C6—C7—C81.2 (7)
O2i—Pb1—O1—C1−149.9 (3)C6—C7—C8—C9−0.7 (7)
O4ii—Pb1—O1—C177.2 (3)C7—C8—C9—C10−0.9 (7)
O1—Pb1—O3—C11−74.7 (3)C2—N1—C10—C9−179.1 (4)
N2—Pb1—O3—C110.4 (3)Pb1—N1—C10—C97.8 (5)
N1—Pb1—O3—C11−142.0 (3)C2—N1—C10—C5−0.4 (6)
O2i—Pb1—O3—C1176.3 (3)Pb1—N1—C10—C5−173.5 (3)
O4ii—Pb1—O3—C11−132.9 (3)C8—C9—C10—N1−179.5 (4)
O3—Pb1—N1—C2100.8 (3)C8—C9—C10—C51.9 (6)
O1—Pb1—N1—C25.6 (3)C6—C5—C10—N1−180.0 (4)
N2—Pb1—N1—C253.2 (3)C4—C5—C10—N10.4 (6)
O2i—Pb1—N1—C2162.2 (3)C6—C5—C10—C9−1.3 (6)
O4ii—Pb1—N1—C2−75.0 (3)C4—C5—C10—C9179.1 (4)
O3—Pb1—N1—C10−85.8 (3)Pb1—O3—C11—O4−177.6 (3)
O1—Pb1—N1—C10179.0 (4)Pb1—O3—C11—C122.8 (5)
N2—Pb1—N1—C10−133.3 (3)C20—N2—C12—C132.8 (6)
O2i—Pb1—N1—C10−24.3 (4)Pb1—N2—C12—C13−172.1 (3)
O4ii—Pb1—N1—C1098.5 (3)C20—N2—C12—C11−178.7 (3)
O3—Pb1—N2—C12−3.8 (3)Pb1—N2—C12—C116.5 (4)
O1—Pb1—N2—C1291.8 (3)O4—C11—C12—N2173.9 (4)
N1—Pb1—N2—C1246.9 (3)O3—C11—C12—N2−6.5 (6)
O2i—Pb1—N2—C12−89.8 (3)O4—C11—C12—C13−7.6 (6)
O4ii—Pb1—N2—C12151.2 (2)O3—C11—C12—C13172.1 (4)
O3—Pb1—N2—C20−178.2 (3)N2—C12—C13—C14−1.7 (6)
O1—Pb1—N2—C20−82.6 (3)C11—C12—C13—C14179.8 (4)
N1—Pb1—N2—C20−127.5 (3)C12—C13—C14—C15−0.9 (7)
O2i—Pb1—N2—C2095.9 (3)C13—C14—C15—C16−179.5 (4)
O4ii—Pb1—N2—C20−23.2 (4)C13—C14—C15—C202.3 (6)
Pb1—O1—C1—O2179.4 (3)C14—C15—C16—C17−176.7 (4)
Pb1—O1—C1—C20.1 (5)C20—C15—C16—C171.5 (6)
C10—N1—C2—C3−0.4 (6)C15—C16—C17—C18−2.4 (7)
Pb1—N1—C2—C3173.6 (3)C16—C17—C18—C191.5 (7)
C10—N1—C2—C1178.5 (4)C17—C18—C19—C200.3 (7)
Pb1—N1—C2—C1−7.5 (5)C12—N2—C20—C19179.0 (4)
O2—C1—C2—N1−173.8 (4)Pb1—N2—C20—C19−6.9 (5)
O1—C1—C2—N15.5 (6)C12—N2—C20—C15−1.3 (6)
O2—C1—C2—C35.2 (6)Pb1—N2—C20—C15172.8 (3)
O1—C1—C2—C3−175.5 (4)C18—C19—C20—N2178.6 (4)
N1—C2—C3—C41.2 (7)C18—C19—C20—C15−1.1 (6)
C1—C2—C3—C4−177.7 (4)C14—C15—C20—N2−1.3 (6)
C2—C3—C4—C5−1.1 (7)C16—C15—C20—N2−179.5 (4)
C3—C4—C5—C6−179.2 (4)C14—C15—C20—C19178.5 (4)
C3—C4—C5—C100.4 (7)C16—C15—C20—C190.2 (6)
Table 1

Selected bond lengths (Å)

Pb1—O12.304 (3)
Pb1—O2i2.952 (3)
Pb1—O32.295 (3)
Pb1—O4ii3.014 (3)
Pb1—N12.567 (4)
Pb1—N22.531 (4)

Symmetry codes: (i) ; (ii) .

  1 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

  1 in total
  1 in total

1.  Bis(μ-quinoline-2-carboxyl-ato)-κN,O:O;κO:N,O-bis-[(acetato-κO,O')(methanol-κO)lead(II)].

Authors:  Gholamhossein Mohammadnezhad; Ali Reza Ghanbarpour; Mostafa M Amini; Seik Weng Ng
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-07-17
  1 in total

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