Literature DB >> 21588188

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

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

Abstract

The dinuclear title compound, [Pb(2)(C(10)H(6)NO(2))(2)(CH(3)COO)(2)(CH(3)OH)(2)], lies across an inversion center. The methanol-coordinated Pb(II) atom is chelated by the acetate anion as well as by the quinoline-2-carboxyl-ate anion. One O atom of the quinoline-2-carboxyl-ate anion bridges two symmetry-related Pb(II) atoms, forming the dinuclear compound. Aside from the six atoms connected to the Pb(II) atom by regular coordination bonds, the structure features a long Pb⋯O inter-action [3.145 (3) Å] that gives rise to a distorted Ψ-square-anti-prismatic geometry at the metal center. The H atom of the methanol is hydrogen bonded to an O atom of the acetate.

Entities:  

Year:  2010        PMID: 21588188      PMCID: PMC3007209          DOI: 10.1107/S1600536810027777

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


Related literature

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

Experimental

Crystal data

[Pb2(C10H6NO2)2(C2H3O2)2(CH4O)2] M = 940.87 Monoclinic, 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 ▶) T min = 0.155, T max = 0.382 13298 measured reflections 3267 independent reflections 3055 reflections with I > 2σ(I) R int = 0.025

Refinement

R[F 2 > 2σ(F 2)] = 0.019 wR(F 2) = 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 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/S1600536810027777/xu2798sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810027777/xu2798Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Pb2(C10H6NO2)2(C2H3O2)2(CH4O)2]F(000) = 880
Mr = 940.87Dx = 2.203 Mg m3
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 mm1
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
Bruker SMART APEX diffractometer3267 independent reflections
Radiation source: fine-focus sealed tube3055 reflections with I > 2σ(I)
graphiteRint = 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 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 = 1.06w = 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 Å3
1 restraintΔρmin = −1.43 e Å3
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*
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)
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)
D—H···AD—HH···AD···AD—H···A
O5—H5···O3i0.84 (4)1.89 (4)2.685 (4)158 (5)
Table 1

Selected bond lengths (Å)

Pb1—O12.377 (3)
Pb1—O1i2.490 (2)
Pb1—O2ii3.145 (3)
Pb1—O32.382 (3)
Pb1—O42.761 (3)
Pb1—O52.696 (3)
Pb1—N12.643 (3)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
O5—H5⋯O3i0.84 (4)1.89 (4)2.685 (4)158 (5)

Symmetry code: (i) .

  2 in total

1.  A short history of SHELX.

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

2.  Bis(quinoline-2-carboxyl-ato-κN,O)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
  2 in total
  2 in total

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

Authors:  Ezzatollah Najafi; Mostafa M Amini; Seik Weng Ng
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-01-29

2.  Crystal structures of three lead(II) acetate-bridged di-amino-benzene coordination polymers.

Authors:  David K Geiger; Dylan E Parsons; Patricia L Zick
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2014-11-21
  2 in total

北京卡尤迪生物科技股份有限公司 © 2022-2023.