Search results for "Spectroscopy"
showing 10 items of 10293 documents
Crystal structure and mössbauer spectroscopy studies of the ferrimagnetic complex bimetallic salt hexaamminechromium (III) hexachloroferrate (III), […
1992
The crystal and molecular structures of the ferrimagnetic bimetallic complex salt hexaamminechromium(III) hexachloroferrate(III), [Cr(NH3)6][FeCl6], have been determined from single-crystal, three-dimensional x-ray diffraction counter data. The compound crystallizes as orange coloured crystals in the space groupC2/c of the monoclinic system with Z=4 and has cell dimensionsa=11.325(1) A,b=11.387(1) A,c=11.233(1) A, and β=90.83(1)A. The structure was refined by using segmented block diagonal least-squares techniques to discrepancy indices R and Rw of 0.0233 and 0.0285, respectively. The metal ions occupy sites with symmetry $$\bar 1$$ and are nearly octahedrally coordinated. In the [FeCl6]3− …
Protonation of 3-aminopyrroles
1987
Abstract The protonation of 3-aminopyrroles has been investigated using H and 13C n.m.r. spectroscopy. The spectral data are compatible with predominant protonation of the amino group with no evidence for protonation of the pyrrole ring.
An experimental and theoretical study of the isomerization of mononuclear bis(arylselenolato)bis(triphenylphosphine)platinum complexes [Pt(SeR)2(PPh3…
2003
Abstract Mononuclear bis(thienylselenolato)bis(triphenylphosphine)platinum [Pt(SeTh)2(PPh3)2] (Th=2-thienyl, C4H3S) has been prepared by the treatment of cis-[PtCl2(PPh3)2] with NaSeTh. The 31P-NMR spectroscopic information indicates that cis-[Pt(SeTh)2(PPh3)2] is initially formed in the reaction. Upon prolonged standing in solution it isomerizes to trans-[Pt(SeTh)2(PPh3)2]. The reaction of cis-[PtCl2(PPh3)2] with LiSeFu (Fu=2-furyl, C4H3O) affords immediately a mixture of cis- and trans-isomers of [Pt(SeFu)2(PPh3)2] with the relative amount of the trans-isomer increasing with time. The recrystallization of the two reaction mixtures yielded cis,anti- and trans,syn-isomers of [Pt(SeTh)2(PPh3…
Reaction of complex ligands: Part 95. Chromium tricarbonyl complexes of polysubstituted naphthohydroquinones: regioselective synthesis via [3+2+1]-be…
2003
Abstract A series of polysubstituted naphthohydroquinoid tricarbonyl chromium complexes were prepared by chromium mediated [3+2+1]-benzannulation of Fischer-type carbene complexes with alkynes. The kinetics and the thermodynamic data of the η6-η6-haptotropic rearrangements were investigated by in-situ NMR spectroscopy. The free activation energies ΔG# range from 23 to 26 kcal mol−1 and only slightly depend on the bulk and the donor/acceptor properties of the substituents. Equilibrium of metal migration was observed for naphthohydroquinone complexes bearing methoxy substituents at the non-hyroquinoid ring (ring A). In complexes bearing methyl groups or only hydrogen substituents at ring A th…
Über polygermane
1986
Abstract The synthesis of GePh4 and Ge2Ph6 by Grignard reaction in THF or ether/toluene leads to the by-products Ge3Ph8 (up to 11%) and Ge4Ph10 (up to 18%) which is dependant on using an excess of Mg. A quantitative analysis of the resulting products by HPLC and a semipreparative separation by column, flash, and HPL chromatography is described. The crystal structures of Ge3Ph8 (R = 0.075) and Ge4Ph10 · 2C6H6 (R = 0.054) have been determined. Ge4Ph10 has Ci symmetry and both chain conformations are well staggered (49–70° for Ge3Ph8, 53–66° for Ge4Ph10). The GeGe distances and GeGeGe angles are 244 pm and 121° (Ge3Ph8), and 246 pm and 118° (Ge4Ph10).
Synthesis and low-frequency vibrational spectra of some halo- and pseudohalo-diphenylantimonates(V)
1976
Abstract The syntheses of diphenylantimonates(V) of the type M(I) [PH 2 XbX 4 ] (M(I) = PH 4 As; X = F, Cl, Br, N 3 , NCS; X 4 = Cl 3 Br, Cl 3 N 3 ) are described. Far-Ir spectra of these compounds and of previously synthesized M(I) [Ph 2 SbCl 3 X] species (M(I) = Me 4 N; X = Cl, Br, N 3 ; M(I) = Ph 4 As; X = NCS) are reported. Raman spectra of tetrafluoro and tetrachloro salts are also given. Vibrational data are interpreted in terms of the presence of solid of trans -Ph 2 SbX 4 - species and assignments of skeletal modes are suggested.
Interaction of methylmercury(II) with the bifunctional ligand o-diphenylphosphinobenzoate, dpb. Synthesis and characterization of [(dpb)HgMe] and [(d…
1998
Abstract The complex [(dpb)HgMe] (1) is obtained by reaction of MeHg(OH) with o-diphenylphosphinobenzoic acid (Hdpb); alternatively the solvate [(dpb)HgMe] · 0.5H2O · 0.5C5H5N (1bis) can be prepared by reacting MeHgCl with Hdpb and pyridine. The derivative [(dpbo)HgMe] (2), where dpbo is o-diphenylphosphinoxidebenzoate, is formed by reaction of 1 or 1bis solutions with atmospheric oxygen. Crystal data for 1bis: monoclinic, space group P2/n, a=10.413(4), b=9.831(3), c=20.674(3) A, β=102.51(3)°, Z=2. Crystal data for 2: triclinic, space group P1, a=11.535(2), b=12.897(5), c=13.275(7) A, α=88.31(4), β=73.65(4), γ=85.27(4)°, Z=2. In 1bis the mercury atom displays a distorted linear fashion, bei…
Metal ion complexation by tetraester derivatives of bridged calix [4] arenes
1992
A series of bridged calix [4] arenes (5–10 methylene groups in the bridge) were synthesized and transformed into their tetraester derivatives by reaction with ethyl bromoacetate. The stability constants for complexes of the tetraester derivatives with sodium, potassium and silver cations, determined in methanol by spectroscopic or potentiometric techniques, show a drastic decrease (more than 105 for Na +) for the shorter methylene chains. 1H NMR studies demonstrate a conformational rearrangement of the calixarene part to fourfold symmetry to be necessary for the complexation of a cation, which is prevented by the shorter chains. This is further confirmed by the X-ray structure of a tetraest…
Two-step radiosynthesis of [18F]FE-β-CIT and [18F]PR04.MZ
2013
The cocaine-derived dopamine reuptake inhibitors FE-β-CIT (8-(2-fluoroethyl)-3-(4-iodophenyl)-8-azabicyclo[3.2.1]octane-2-carboxylic acid methyl ester) (1) and PR04.MZ(8-(4-fluorobut-2-ynyl)-3-p-tolyl-8-azabicyclo[3.2.1]octane-2-carboxylic acid methyl ester) (2) were labelled with (18)F-fluorine using a two-step route. 2-[(18)F]Fluoroethyltosylate and 4-[(18)F]fluorobut-2-yne-1-yl tosylate were used as labelling reagents, respectively. Radiochemically pure (>98%) [(18)F]FE-β-CIT and [(18)F]PRD04.MZ (32-86 GBq/µmol) were obtained after a synthesis time of 100 min in about 25% non-decay-corrected overall yield.
Structural study of ethyl 3-arylcarbamoyl-2,3-diazabicyclo[2.2.1]hept-5-ene-2-carboxylates: conformation and transmission of substituent effects acro…
2001
Nine new ethyl 3-arylcarbamoyl-2,3-diazabicyclo[2.2.1]hept-5-ene-2-carboxylates were prepared by a [4 + 2] cycloaddition and their FTIR, 1H, 13C and 15N NMR spectra were measured and assigned. Single crystals were grown for five compounds and their X-ray data were obtained. The electronic structure and the conformations were calculated by the semi-empirical AM1 method. Using correlations between the spectral, empirical and theoretical structural data, the transmission of substituent effects and the preferential conformation connected with the consecutive double nitrogen inversion and regarding the mutual orientation of NH and CO bonds were investigated. The results are compared with those f…