Synthesis and Crystal Structure of a Novel Neutral Polymeric Lead(II)-thiosemicarbazonato Complex

Abstract

The reaction between lead(II) acetate and 2-acetylpyridine 4N-methylthiosemicarbazone (H4ML) produced a complex of the formula [Pb(4ML)(OOCMe)] with an unusual polymeric structure in which the lead atom is hepta-coordinate, the deprotonated thiosemicarbazone is a tetradentate bridge, and the acetate group both chelates and bridges. The complex crystallizes in the triclinic space group P1̄ with a = 8.860(2), b = 9.394(2), c = 9.783(3) A, α = 108.93(4), β = 98.67(3), γ = 107.87(5)°, V = 704.1(3) Å3 , Z = 2.

Bonding and structure trends of thiosemicarbazone derivatives of metals—An overview

“…Tin(IV) complexes were prepared using SnMe 2 O, SnMe 2 Cl 2, or Ph 2 SnO [130][131][132][133]. For lead complexes, PbPh 2 Cl 2 has been used as a precursor [134,135], however, electrochemical methods are also reported [136]. In case of bismuth, BiCl 3 , or Bi(NO 3 ) 3 were reacted with a thiosemicarbazone used in acetone [137,138].…”

“…Compounds in the tetravalent state are only with organolead(IV) substrates. Lead(II) forms a tetrahedral complex, [Pb(L)(OAc)] 555[136], and an octahedral complex, [PbL 2 ] 556[339] (Chart 76), with uninegative tridentate N 4 , N 3 , S-donor ligands in the former, and O, N 3 , S-donors in the latter complex.…”

UTILIZACIÓN DE LA QUÍMICA COMPUTACIONAL: MÉTODO SEMIEMPÍRICO PM3, PARA ELUCIDAR LA ESTRUCTURA DEL COMPLEJO BIS (1,5- DIFENIL-1,2, 4-TRIAZOL-3-TIONATO) PLOMO (II) (Pb(DTT) ).

“…Los datos experimentales muestran por medio de los espectros IR, C (H )-APT y H -RMN que el ligando está totalmente desprotonado en el complejo, además de que sus puntos de coordinación son por medio del átomo de azufre y del nitrógeno hidrazínico (figura 1c). En estudios estructurales con difracción de rayos X de complejos de plomo (II) 18 tetracoordinados con tiosemicarbazona muestran la formación de enlace Pb-S (2.730A) y Pb- 19 N (2.482 Å), también los complejos de Pb (II) con 3-hexametileneiminiltiosemicarbazona exhiben puntos de coordinación en los átomos de azufre Pb-S (2.7064 Å) y nitrógeno hidrazínico (2.628 Å). Esto verificaría que la estructura (1c) es la que probablemente se formaría, ya que posee los mismos puntos de coordinación antes mencionados, además, los cálculos obtenidos muestran que dicha estructura posee mayor estabilidad y alta dureza global.…”

Lead(II)-induced formation and coordination of 3,4-dihydro-3-thioxo-1,2,4-triazin-5(2H)-one

“…Whether or not the thiosemicarbazone ligands had undergone cyclization upon coordination was easily detected by examination of the main IR bands of the complexes [6,7], since the spectra of triazines differ clearly from those of thiosemicarbazones. The spectra of the complexes [Pb(BuTSC where HL is 2-acetylpyridine 4 N-methylthiosemicarbazone [14].…”