Synthesis and spectroscopic characterization of bis(trifluorophosphinyl)-gold(I) undecafluorodiantimonate(V) [Au(PF3)2][Sb2F11]

1996 ◽  
Vol 74 (11) ◽  
pp. 2392-2394 ◽  
Author(s):  
B. Bley ◽  
M. Bodenbinder ◽  
G. Balzer ◽  
H. Willner ◽  
G. Hägele ◽  
...  

The synthesis of [Au(PF3)2][Sb2F11], the first example of a linear, thermally stable metal bis(trifluorophosphine) complex is achieved by CO substitution of [Au(CO)2][Sb2F11] by PF3. The [Au(PF3)2]+ cation can also be generated by reductive phosphorylation by an excess of PF3 in fluorosulfuric acid. Spectroscopic characterization involves 19F and 31P NMR in HSO3F and SO2 solution including spectral simulation by the WIN-DAISY method and FT-IR and Raman spectra. Spectroscopic evidence suggests that the metal–ligand bond involves predominantly σ-bonding with drastically reduced π-back-donation. Key words: gold(I) complex, linear; gold(I) PF3 complex; 31P NMR; 19F NMR; vibrational spectra.

2001 ◽  
Vol 55 (9) ◽  
pp. 1155-1160 ◽  
Author(s):  
Jonathan J. Wylde ◽  
Geoffrey C. Allen ◽  
Ian R. Collins

2018 ◽  
Vol 91 (3) ◽  
pp. 389-396 ◽  
Author(s):  
Yanshan Yin ◽  
Jie Yin ◽  
Wei Zhang ◽  
Hong Tian ◽  
Zhangmao Hu ◽  
...  

2020 ◽  
Vol 45 (5) ◽  
Author(s):  
V.O. Uduah ◽  
J.J. Gongden ◽  
M.L. Kagoro ◽  
K.K. Gurumyen ◽  
Y.N. Lohdip ◽  
...  

This work presents a dry synthesis of Iron (III) complex with urea isolated from human urine and Fe (III) obtained from iron rust particles. Iron (III), PI (Purified iron rust), was isolated from iron rust in 10% hydrochloric acid, HCl and distilled water respectively. The complex was synthesized via dry-synthesis method using the melted urea as reaction medium. The isolated Fe (III) was characterized by elemental analysis which was done using XRF Cu-Zn method. The complex was prepared in a 1:4 metal to ligand (M-L) ratio. The stoichiometry of reaction indicate a 1:3 ratio of M-L (Fe-U). The complex was characterized by FT-IR, UV-vis, XRF and XRD spectroscopic techniques. The Fe (III) isolate and Fe-U complex shows percentage yields of 35.7% and ~92% respectively. The elemental and oxide composition of Fe and Fe2O3 (i.e., PI) were 40.387% and 57.753% respectively. The results obtained from the characterization of the iron-urea complex, IUC, indicate FT-IR result as symmetric and asymmetric frequencies with peaks of a combination band of Vs (NH) and Vas (NH), C=O and V (C-N) all stretched, XRD showed the crystal to be amorphous. The elemental and oxide composition of the Fe and Fe2O3 in IUC were 40.007 and 44.201 respectively. The results obtained revealed that useful complexes can be synthesized easily from waste materials, such as urine and iron rust particles, which complement Green chemistry.


Polymers ◽  
2019 ◽  
Vol 11 (9) ◽  
pp. 1498 ◽  
Author(s):  
Abdul Hafeez ◽  
Zareen Akhter ◽  
John F. Gallagher ◽  
Nawazish Ali Khan ◽  
Asghari Gul ◽  
...  

Bis-aldehyde monomers 4-(4′-formyl-phenoxy)benzaldehyde (3a), 3-methoxy-4-(4′-formyl-phenoxy)benzaldehyde (3b), and 3-ethoxy-4-(4′-formyl-phenoxy)benzaldehyde (3c) were synthesized by etherification of 4-fluorobenzaldehyde (1) with 4-hydroxybenzaldehyde (2a), 3-methoxy-4-hydroxybenzaldehyde (2b), and 3-ethoxy-4-hydroxybenzaldehyde (2c), respectively. Each monomer was polymerized with p-phenylenediamine and 4,4′-diaminodiphenyl ether to yield six poly(azomethine)s. Single crystal X-ray diffraction structures of 3b and 3c were determined. The structural characterization of the monomers and poly(azomethine)s was performed by FT-IR and NMR spectroscopic techniques and elemental analysis. Physicochemical properties of polymers were investigated by powder X-ray diffraction, thermogravimetric analysis (TGA), viscometry, UV–vis, spectroscopy and photoluminescence. These polymers were subjected to electrical conductivity measurements by the four-probe method, and their conductivities were found to be in the range 4.0 × 10−5 to 6.4 × 10−5 Scm−1, which was significantly higher than the values reported so far.


1988 ◽  
Vol 43 (4) ◽  
pp. 371-381 ◽  
Author(s):  
K. Bütje ◽  
W. Preetz

AbstractWell-resolved IR and Raman spectra of the two sets of all 10 isomeric complexes [Os(NCS)n(SCN)6-n]3-/2-, n = 0-6, have been recorded. For both series, νCS(N) > νCS(S) and δNCS > δSCN; for the Os(III) complexes, vCN(N) ~ vCN(S) and vOsN ≥ vOsS while for the Os(IV) compounds, vCN(N) < vCN(S) and vOsN ~ vOsS. The vibrational spectra of the n = 0 and n = 6 members of both sets are assigned according to D3d and Oh point symmetry, respectively. For the mixed linkage isomers the band pattern is strongly influenced by pseudo-octahedral coupling wherever frequencies of N- and S-bonded groups coincide. The metal-ligand stretching region is therefore assigned according rather to pseudo-Oh, pseudo-D3d and pseudo-D4h symmetry than to D4h, C4v, C3v and C2v microsymmetry. The charge-transfer spectra of both series are similar, showing a parallel hypsochromic shift with increasing n value. Upon oxidation, a bathochromic shift of the CT bands by an average of 5400 cm-1 is observed, and the intensity increases by a factor 2-2.5. Weak absorptions in the near infrared region are assigned to intraconfigurational transitions.


2019 ◽  
Vol 21 (8) ◽  
pp. 4421-4434 ◽  
Author(s):  
Ashour A. Ahmed ◽  
Stella Gypser ◽  
Peter Leinweber ◽  
Dirk Freese ◽  
Oliver Kühn

The molecular binding mechanisms for the adsorbed phosphate at the goethite–water interface have been explored via a joint experimental/theoretical study. This study involved performing sorption experiments, characterization by FT-IR spectroscopy, and performing periodic DFT calculations.


1989 ◽  
Vol 44 (6) ◽  
pp. 641-646 ◽  
Author(s):  
Hidenari Inoue ◽  
Takeshi Kuroiwa ◽  
Tsuneo Shirai ◽  
Ekkehard Fluck

The 57Fe Mößbauer spectra of mixed ligand complexes of the type trans-Fe(CO)3L1L2 (L1 = triphenylphosphine or triphenylphosphite and L2 = phosphine or phosphite) show a quadrupolesplitting doublet typical of the disubstituted iron carbonyls in trigonal bipyramidal symmetry. The inverse linear dependence of the isomer shifts on the CO stretching frequencies is interpreted on the basis of the strengthening triple-bond nature of the carbonyl ligands with increasing iron-to-phosphorus π-back donation. A linear correlation, with a positive slope, between the isomer shifts and the quadrupole splittings has revealed that the phosphorus-to-iron σ-donation is offset by the iron-to-phosphorus π-back donation. A correlation between the coordination shifts and the isomer shifts demonstrates that the iron-to-phosphorus π-back donation plays an important role in the Fe-P bond. The relatively large coupling constant of 2J(P,P) reflects a strong interaction between trans-phosphorus ligands through the P-Fe-P bond


Materials ◽  
2020 ◽  
Vol 13 (2) ◽  
pp. 274 ◽  
Author(s):  
Andreea Madalina Pandele ◽  
Andreea Constantinescu ◽  
Ionut Cristian Radu ◽  
Florin Miculescu ◽  
Stefan Ioan Voicu ◽  
...  

This article presents a facile synthesis method used to obtain new composite films based on polylactic acid and micro-structured hydroxyapatite particles. The composite films were synthesized starting from a polymeric solution in chloroform (12 wt.%) in which various concentrations of hydroxyapatite (1, 2, and 4 wt.% related to polymer) were homogenously dispersed using ultrasonication followed by solvent evaporation. The synthesized composite films were morphologically (through SEM and atomic force microscopy (AFM)) and structurally (through FT-IR and Raman spectroscopy) characterized. The thermal behavior of the composite films was also determined. The SEM and AFM analyses showed the presence of micro-structured hydroxyapatite particles in the film’s structure, as well as changes in the surface morphology. There was a significant decrease in the crystallinity of the composite films compared to the pure polymer, this being explained by a decrease in the arrangement of the polymer chains and a concurrent increase in the degree of their clutter. The presence of hydroxyapatite crystals did not have a significant influence on the degradation temperature of the composite film.


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