Literature DB >> 21522542

Poly[μ(3)-hydroxido-μ-(pyridine-2,4,6-tricarboxyl-ato)-dilead(II)].

Ying-Hua Zhou1, Jian Chen, Yong Cheng, Nian-Rong Zhang.   

Abstract

The asymmetric unit of the title coordination polymer, [Pb(2)(C(8)H(2)NO(6))(OH)](n), contains two crystallographically independent Pb(II) ions, one pyridine-2,4,6-tricarboxyl-ate (ptc) trianion and one hydroxide anion. One of the Pb(II) atoms is coordinated by one pyridine N and four carboxyl-ate O atoms from the ptc trianion and a hydroxide O atom in a distorted octa-hedral geometry. The other Pb(II) atom is five-coordinated by three carboxyl-ate O atoms and two hydroxide O atoms in a distorted tetra-gonal-pyramidal geometry. Four neighbouring Pb(II) atoms are bridged through two μ(3)-hydroxide ligands, forming the centrosymmetric Pb(4)(OH)(2) core. The three-dimensional structure is further achieved through bridging carboxyl-ate groups. There are also O-H⋯O hydrogen bonds between the hydroxide ligand and the carboxyl-ate group.

Entities:  

Year:  2010        PMID： 21522542      PMCID： PMC3050173          DOI： 10.1107/S1600536810049275

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


Related literature

For general background to pyridine-2,4,6-tricarb­oxy­lic acid complexes and their derivatives, see: Das et al. (2009 ▶); Ding et al. (2009 ▶); Ghosh et al. (2006 ▶); O’Keeffe et al. (2008 ▶); Shi et al. (2010 ▶); Xu et al. (2010 ▶); Yigit et al. (2005 ▶); Zhang et al. (2009 ▶); Zhao et al. (2009 ▶). For our previous work on metal complexes, see: Zhou et al. (2007 ▶); Wu et al. (2007 ▶).

Experimental

Crystal data

[Pb2(C8H2NO6)(OH)] M = 639.49 Monoclinic, a = 7.5391 (9) Å b = 14.1845 (17) Å c = 10.3084 (12) Å β = 100.468 (1)° V = 1084.0 (2) Å3 Z = 4 Mo Kα radiation μ = 31.05 mm−1 T = 291 K 0.38 × 0.26 × 0.25 mm

Data collection

Bruker SMART APEX CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.030, T max = 0.047 7870 measured reflections 2014 independent reflections 1903 reflections with I > 2σ(I) R int = 0.036

Refinement

R[F 2 > 2σ(F 2)] = 0.028 wR(F 2) = 0.069 S = 1.08 2014 reflections 157 parameters H-atom parameters constrained Δρmax = 1.64 e Å−3 Δρmin = −2.07 e Å−3 Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810049275/is2628sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810049275/is2628Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Pb2(C8H2NO6)(OH)]F(000) = 1112
Mr = 639.49Dx = 3.918 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 5542 reflections
a = 7.5391 (9) Åθ = 2.5–28.2°
b = 14.1845 (17) ŵ = 31.05 mm−1
c = 10.3084 (12) ÅT = 291 K
β = 100.468 (1)°Block, white
V = 1084.0 (2) Å30.38 × 0.26 × 0.25 mm
Z = 4
Bruker SMART APEX CCD area-detector diffractometer2014 independent reflections
Radiation source: fine-focus sealed tube1903 reflections with I > 2σ(I)
graphiteRint = 0.036
φ and ω scansθmax = 25.5°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −9→9
Tmin = 0.030, Tmax = 0.047k = −17→17
7870 measured reflectionsl = −12→12
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.069H-atom parameters constrained
S = 1.08w = 1/[σ2(Fo2) + (0.0382P)2 + 7.726P] where P = (Fo2 + 2Fc2)/3
2014 reflections(Δ/σ)max = 0.001
157 parametersΔρmax = 1.64 e Å−3
0 restraintsΔρmin = −2.07 e Å−3
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)are estimated using the full covariance matrix. The cell e.s.d.'s are takeninto account individually in the estimation of e.s.d.'s in distances, anglesand torsion angles; correlations between e.s.d.'s in cell parameters are onlyused when they are defined by crystal symmetry. An approximate (isotropic)treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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.
xyzUiso*/Ueq
Pb10.06507 (4)0.84421 (2)0.28447 (3)0.01366 (11)
Pb20.18306 (4)0.93099 (2)−0.06649 (3)0.01411 (11)
O10.2977 (9)0.9297 (5)0.1872 (6)0.0289 (11)
O20.5925 (8)0.9461 (5)0.1816 (6)0.0289 (11)
O30.9877 (8)0.9721 (4)0.6667 (6)0.0225 (13)
O40.9167 (8)0.8519 (4)0.7875 (6)0.0250 (14)
O50.2690 (8)0.7768 (4)0.7342 (6)0.0213 (12)
O60.1106 (8)0.7676 (4)0.5298 (5)0.0229 (13)
O70.0597 (7)1.0796 (4)−0.0536 (5)0.0152 (11)
H70.11171.1285−0.02320.023*
N10.3717 (8)0.8650 (4)0.4344 (6)0.0105 (12)
C10.5100 (10)0.9033 (5)0.3862 (7)0.0112 (14)
C20.6798 (11)0.9170 (5)0.4616 (8)0.0162 (16)
H20.77200.94380.42490.019*
C30.7094 (10)0.8896 (5)0.5943 (8)0.0140 (15)
C40.5682 (11)0.8484 (5)0.6457 (8)0.0175 (17)
H40.58470.82880.73310.021*
C50.4032 (10)0.8379 (5)0.5626 (8)0.0116 (15)
C60.4651 (11)0.9281 (5)0.2410 (8)0.0150 (16)
C70.8872 (11)0.9068 (6)0.6901 (8)0.0163 (16)
C80.2459 (11)0.7909 (5)0.6105 (7)0.0147 (16)
U11U22U33U12U13U23
Pb10.01119 (17)0.01504 (17)0.01652 (18)−0.00022 (11)0.00723 (12)0.00207 (10)
Pb20.01304 (18)0.01647 (18)0.01407 (17)0.00281 (11)0.00580 (12)0.00070 (10)
O10.018 (2)0.048 (3)0.021 (2)−0.010 (2)0.0067 (19)0.010 (2)
O20.018 (2)0.048 (3)0.021 (2)−0.010 (2)0.0067 (19)0.010 (2)
O30.013 (3)0.022 (3)0.032 (3)−0.007 (3)0.004 (3)−0.010 (3)
O40.019 (3)0.037 (4)0.019 (3)0.003 (3)0.002 (2)0.002 (3)
O50.023 (3)0.025 (3)0.018 (3)−0.003 (3)0.010 (2)0.003 (2)
O60.021 (3)0.030 (3)0.019 (3)−0.017 (3)0.006 (3)−0.002 (2)
O70.014 (3)0.013 (3)0.021 (3)−0.002 (2)0.008 (2)−0.001 (2)
N10.010 (3)0.008 (3)0.016 (3)−0.002 (2)0.006 (3)0.001 (2)
C10.012 (4)0.009 (3)0.014 (4)−0.001 (3)0.008 (3)0.001 (3)
C20.016 (4)0.012 (4)0.023 (4)0.001 (3)0.008 (3)−0.002 (3)
C30.011 (4)0.008 (3)0.024 (4)−0.003 (3)0.005 (3)−0.004 (3)
C40.017 (4)0.019 (4)0.016 (4)−0.002 (3)0.002 (3)0.001 (3)
C50.011 (4)0.009 (4)0.016 (4)0.000 (3)0.003 (3)−0.003 (3)
C60.012 (4)0.019 (4)0.015 (4)−0.005 (3)0.005 (3)0.003 (3)
C70.017 (4)0.017 (4)0.016 (4)0.009 (3)0.005 (3)−0.002 (3)
C80.023 (4)0.008 (3)0.015 (4)0.000 (3)0.009 (3)−0.001 (3)
Pb1—O5i2.422 (6)O5—C81.272 (9)
Pb1—O12.489 (6)O5—Pb1vii2.422 (6)
Pb1—N12.554 (6)O6—C81.238 (10)
Pb1—O7ii2.627 (5)O7—Pb2ii2.393 (5)
Pb1—O3iii2.697 (6)O7—Pb1ii2.627 (5)
Pb1—O62.716 (6)O7—H70.8286
Pb2—O12.600 (6)N1—C11.348 (10)
Pb2—O2iv2.836 (7)N1—C51.355 (10)
Pb2—O4v2.541 (6)C1—C21.385 (11)
Pb2—O72.318 (5)C1—C61.515 (10)
Pb2—O7ii2.393 (5)C2—C31.401 (11)
O1—C61.283 (10)C2—H20.9300
O2—C61.256 (10)C3—C41.400 (12)
O3—C71.247 (11)C3—C71.533 (11)
O3—Pb1iii2.698 (6)C4—C51.384 (11)
O4—C71.258 (10)C4—H40.9300
O4—Pb2vi2.541 (6)C5—C81.519 (11)
O5i—Pb1—O174.8 (2)Pb2—O7—H7127.9
O5i—Pb1—N170.8 (2)Pb2ii—O7—H7102.2
O1—Pb1—N164.0 (2)Pb1ii—O7—H793.8
O5i—Pb1—O7ii103.54 (18)C1—N1—C5117.6 (6)
O1—Pb1—O7ii66.24 (19)C1—N1—Pb1119.9 (5)
N1—Pb1—O7ii129.54 (18)C5—N1—Pb1122.5 (5)
O5i—Pb1—O3iii147.70 (19)N1—C1—C2123.2 (7)
O1—Pb1—O3iii75.1 (2)N1—C1—C6114.1 (6)
N1—Pb1—O3iii85.62 (18)C2—C1—C6122.6 (7)
O7ii—Pb1—O3iii74.41 (17)C1—C2—C3118.4 (7)
O5i—Pb1—O686.45 (19)C1—C2—H2120.8
O1—Pb1—O6126.23 (19)C3—C2—H2120.8
N1—Pb1—O662.30 (18)C4—C3—C2119.2 (7)
O7ii—Pb1—O6166.35 (17)C4—C3—C7117.3 (7)
O3iii—Pb1—O6102.15 (18)C2—C3—C7123.4 (7)
O7—Pb2—O7ii71.0 (2)C5—C4—C3118.1 (7)
O7—Pb2—O4v98.8 (2)C5—C4—H4121.0
O7ii—Pb2—O4v71.47 (19)C3—C4—H4121.0
O7—Pb2—O190.7 (2)N1—C5—C4123.5 (7)
O7ii—Pb2—O167.99 (19)N1—C5—C8115.6 (7)
O4v—Pb2—O1132.45 (19)C4—C5—C8120.9 (7)
C6—O1—Pb1121.8 (5)O2—C6—O1124.4 (7)
C6—O1—Pb2123.8 (5)O2—C6—C1118.4 (7)
Pb1—O1—Pb2106.2 (2)O1—C6—C1117.2 (7)
C7—O3—Pb1iii124.4 (5)O3—C7—O4126.0 (8)
C7—O4—Pb2vi101.9 (5)O3—C7—C3119.0 (7)
C8—O5—Pb1vii110.5 (5)O4—C7—C3115.0 (7)
C8—O6—Pb1117.9 (5)O6—C8—O5125.3 (7)
Pb2—O7—Pb2ii108.9 (2)O6—C8—C5119.7 (7)
Pb2—O7—Pb1ii113.8 (2)O5—C8—C5115.0 (7)
Pb2ii—O7—Pb1ii108.2 (2)
O5i—Pb1—O1—C6−61.3 (6)C5—N1—C1—C6177.8 (6)
N1—Pb1—O1—C614.5 (6)Pb1—N1—C1—C6−1.6 (8)
O7ii—Pb1—O1—C6−173.9 (7)N1—C1—C2—C30.1 (11)
O3iii—Pb1—O1—C6106.9 (6)C6—C1—C2—C3−178.4 (7)
O6—Pb1—O1—C612.5 (7)C1—C2—C3—C40.8 (11)
O5i—Pb1—O1—Pb288.2 (3)C1—C2—C3—C7−175.9 (7)
N1—Pb1—O1—Pb2163.9 (3)C2—C3—C4—C5−0.9 (11)
O7ii—Pb1—O1—Pb2−24.43 (19)C7—C3—C4—C5175.9 (7)
O3iii—Pb1—O1—Pb2−103.7 (3)C1—N1—C5—C40.6 (11)
O6—Pb1—O1—Pb2162.02 (19)Pb1—N1—C5—C4180.0 (6)
O7—Pb2—O1—C6−115.5 (6)C1—N1—C5—C8−177.3 (6)
O7ii—Pb2—O1—C6175.3 (7)Pb1—N1—C5—C82.1 (8)
O4v—Pb2—O1—C6141.8 (6)C3—C4—C5—N10.2 (11)
O7—Pb2—O1—Pb195.8 (3)C3—C4—C5—C8178.0 (7)
O7ii—Pb2—O1—Pb126.6 (2)Pb1—O1—C6—O2159.2 (7)
O4v—Pb2—O1—Pb1−6.8 (4)Pb2—O1—C6—O215.2 (11)
O5i—Pb1—O6—C882.5 (6)Pb1—O1—C6—C1−21.2 (9)
O1—Pb1—O6—C814.3 (7)Pb2—O1—C6—C1−165.2 (5)
N1—Pb1—O6—C812.3 (5)N1—C1—C6—O2−165.9 (7)
O7ii—Pb1—O6—C8−139.9 (7)C2—C1—C6—O212.7 (12)
O3iii—Pb1—O6—C8−66.1 (6)N1—C1—C6—O114.5 (10)
O7ii—Pb2—O7—Pb2ii0.001 (1)C2—C1—C6—O1−167.0 (7)
O4v—Pb2—O7—Pb2ii66.8 (2)Pb1iii—O3—C7—O4−100.9 (9)
O1—Pb2—O7—Pb2ii−66.4 (2)Pb1iii—O3—C7—C378.7 (8)
O7ii—Pb2—O7—Pb1ii−120.9 (3)Pb2vi—O4—C7—O311.2 (9)
O4v—Pb2—O7—Pb1ii−54.0 (2)Pb2vi—O4—C7—C3−168.5 (5)
O1—Pb2—O7—Pb1ii172.7 (2)C4—C3—C7—O3−152.7 (7)
O5i—Pb1—N1—C176.4 (5)C2—C3—C7—O324.0 (11)
O1—Pb1—N1—C1−5.6 (5)C4—C3—C7—O427.0 (10)
O7ii—Pb1—N1—C1−15.5 (6)C2—C3—C7—O4−156.3 (7)
O3iii—Pb1—N1—C1−81.2 (5)Pb1—O6—C8—O5165.4 (6)
O6—Pb1—N1—C1172.7 (6)Pb1—O6—C8—C5−16.6 (9)
O5i—Pb1—N1—C5−103.0 (5)Pb1vii—O5—C8—O618.5 (10)
O1—Pb1—N1—C5175.0 (6)Pb1vii—O5—C8—C5−159.6 (5)
O7ii—Pb1—N1—C5165.1 (5)N1—C5—C8—O610.3 (10)
O3iii—Pb1—N1—C599.5 (5)C4—C5—C8—O6−167.6 (7)
O6—Pb1—N1—C5−6.7 (5)N1—C5—C8—O5−171.5 (6)
C5—N1—C1—C2−0.7 (11)C4—C5—C8—O510.6 (11)
Pb1—N1—C1—C2179.8 (6)
D—H···AD—HH···AD···AD—H···A
O7—H7···O6viii0.832.582.989 (8)112.
O7—H7···O4iii0.832.492.884 (8)110.
Table 1

Selected bond lengths (Å)

Pb1—O5i2.422 (6)
Pb1—O12.489 (6)
Pb1—N12.554 (6)
Pb1—O7ii2.627 (5)
Pb1—O3iii2.697 (6)
Pb1—O62.716 (6)
Pb2—O12.600 (6)
Pb2—O2iv2.836 (7)
Pb2—O4v2.541 (6)
Pb2—O72.318 (5)
Pb2—O7ii2.393 (5)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O7—H7⋯O6vi0.832.582.989 (8)112
O7—H7⋯O4iii0.832.492.884 (8)110

Symmetry codes: (iii) ; (vi) .

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