Synthesis and characterization of intramolecularly coordinated alanes with new sterically demanding trisyl-based ligands

2007 ◽  
Vol 85 (7-8) ◽  
pp. 483-490 ◽  
Author(s):  
Clinton L Lund ◽  
Olimpiu Stanga ◽  
J Wilson Quail ◽  
Jens Müller
Keyword(s):  
Solid State ◽  
Molecular Structures ◽  
Synthesis And Characterization ◽  
Ortho Position ◽  
Donor Group ◽  
Pyridyl Group ◽  
X Ray ◽  
Sterically Demanding ◽  
Derivatives Of

Five new intramolecularly coordinated aluminum species, whose molecular structures have been elucidated in solution by NMR spectroscopy and in the solid state by single crystal X-ray analysis, are described. All species are equipped with a trisyl-based ligand with a pyridyl donor group [Pytsi stands for -C(SiMe3)2SiMe2(2-C5H4N)]. While the compound (Pytsi)AlMeCl was accessible either from Li(THF)(Pytsi) and MeAlCl2 or from (Pytsi)AlCl2 and LiMe, the tert-butyl derivative (Pytsi)AltBuCl could only be obtained from Li(THF)(Pytsi) and tBuAlCl2. Attempted synthesis of (Pytsi)AltBuCl from (Pytsi)AlCl2 and LitBu or from (Pytsi)AlCl2 and tBuMgCl failed. Three other compounds (3-5) were synthesized and can be described as derivatives of (Pytsi)AlMe2 with additional groups in the ortho position of the pyridyl group. Compound 3 carried a Me group in the ortho position, while compounds 4 and 5 were equipped with Ph and 2,6-diisopropylphenyl moieties, respectively.Key words: aluminum, trisyl ligands, methyl alanes.

Synthesis and characterization of the binuclear diamido titanium chalcogenides [(Ar)NCH2CH2CH2N(Ar)]2Ti(µ-E)2 (E = Se, Te)

2002 ◽  
Vol 80 (11) ◽  
pp. 1524-1529 ◽  
Author(s):  
Tianle Zhang ◽  
Warren E Piers ◽  
Masood Parvez
Keyword(s):  
Solid State ◽  
Key Words ◽  
Synthesis And Characterization ◽  
Catalyst Precursor ◽  
Tellurium Atom ◽  
Titanium Complex ◽  
X Ray ◽  
X Ray Crystallography ◽  
Atom Source

Reaction of McConville's chelating amido titanium complex [(Ar)NCH2CH2CH2N(Ar)]Ti(CH3)2 (Ar = 2,6-i-Pr2C6H3) with either elemental Se or the tellurium atom source Te=PBu3 resulted in the formation of bis-µ-chalcogenido dimers [(Ar)NCH2CH2CH2N(Ar)]2Ti(µ-E)2 (E = Se, 2; Te, 3) with concommitant loss of EMe2. The dimers 2 and 3 were characterized spectroscopically and via X-ray crystallography. The two compounds are isostructural in the solid state. The tellurido dimer 3 may also be synthesized by reduction of the diamido dichloride [(Ar)NCH2CH2CH2N(Ar)]2TiCl2 with Na–Hg amalgam followed by treatment with Te=PBu3. This dimer is unreactive toward further Te=PBu3 or stannanes such as HSnBu3. Unlike decamethyltitanocene derivatives, the diamido complex is not an effective catalyst precursor for the heterohydrodecoupling of Te=PBu3 and HSnBu3.Key words: diamido titanium complexes, selenides, tellurides.

1,2-Dicyanoferrocene: synthesis and characterization

2016 ◽  
Vol 94 (6) ◽  
pp. 547-551 ◽  
Author(s):  
Mohammad A. Abdulmalic ◽  
Steve W. Lehrich ◽  
Heinrich Lang ◽  
Tobias Rüffer
Keyword(s):  
Cyclic Voltammetry ◽  
Solid State ◽  
Single Crystal ◽  
Square Wave Voltammetry ◽  
Molecular Structures ◽  
Synthesis And Characterization ◽  
X Ray ◽  
Square Wave ◽  
Wave Voltammetry ◽  
Convenient Synthesis

A convenient synthesis of 1,2-dicyanoferrocene (3) was developed by using 2,4-dinitrofluorobenzene as a dehydrating agent for the treatment of 1,2-ferrocenedicarbaldehyde dioxime (2) to give 3 in yields exceeding 80%. Compounds 2 and 3 have been characterized by IR and NMR (1H, 13C{1H}) spectroscopy and by electrochemistry (cyclic voltammetry and square-wave voltammetry). Furthermore, the molecular structures of 2 and 3 in the solid state have been determined by single-crystal X-ray crystallographic studies.

Solid State Synthesis and Characterization of Spintronics Material Cd0.55 Hg0.45 Te

2010 ◽  
Vol 44-47 ◽  
pp. 2299-2306
Author(s):  
H.M.Noor Ul Huda Khan Asghar ◽  
M. Asghar ◽  
M.S. Awan
Keyword(s):  
Solid State ◽  
Synthesis And Characterization ◽  
Chemical Analyses ◽  
X Ray Diffraction ◽  
Conventional Solid State Reaction ◽  
Cubic Crystal ◽  
X Ray ◽  
Edx Analyses ◽  
Scanning Electron

Polycrystalline spintronic material (Cd0.55Hg0.45Te) was synthesized by conventional solid state reaction. The samples ( = 5 mm and T = 1.5 mm) were prepared by uni-axial pressing. Samples were melted at 800°C for 3-2 hours. For chemical analyses, surface morphology and structural analyses, scanning electron microscopy (SEM) equipped with EDX system and X-ray diffraction studies were performed. XRD confirmed the cubic crystal structure. The Lattice constant of (Cd0.55Hg0.45Te) as determined by XRD was 0.6464 nm. The Miller indices (hkl) have been found by using crystallography method. The observed planes were (200), (210) and (331). The EDX analyses showed the typically compositions: Te 24.8% Cd 14.8% Al 5% and O2 46.4 % & C 9% (3 hours treatment) and Te 28.1% Cd 16% Al 4.1% and O2 39.3 %, Si 0.360% & C 12.1% (2 hours treatment) however we could not find any representative peak for Hg in all of the EDX analyses.

scholarly journals Synthesis and Characterization of Sr2CeO4 Phosphor Doped with Erbium

2010 ◽  
Vol 13 (1-2) ◽  
pp. 17
Author(s):  
K.V.R. Murthy ◽  
K. Suresh ◽  
B. Nageswara Rao ◽  
B. Walter Ratna Kumar ◽  
Ch. Atchyutha Rao ◽  
...  
Keyword(s):  
Rare Earth ◽  
Solid State ◽  
Sem Analysis ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Rare Earth Ion ◽  
Solid State Reaction Technique ◽  
X Ray ◽  
Pl Emission

<p>The present paper reports the Photoluminescence (PL) of the Sr<sub>2</sub>CeO<sub>4</sub> phosphor, singly doped with Erbium rare-earth ion with different concentrations (0.01, 0.1, 0.2, 0.5 and 1%).The phosphor samples were synthesized using the standard solid state reaction technique. The effect of Er dopant on the structural, morphological, and Photoluminescent properties of the samples are studied with X-ray diffraction (XRD), PL and SEM analysis. The PL emission of undoped Sr<sub>2</sub>CeO<sub>4</sub> phosphor was observed at 470 nm with high intensity followed by the primary Er emissions with good intensity at 525, 530, 549, 557 and 565 nm.</p>

scholarly journals Synthesis and Characterization of Bidentate Isonitrile Iron Complexes

2021 ◽  
Author(s):  
Marion Till ◽  
John A. Kelly ◽  
Christoph G. P. Ziegler ◽  
Robert Wolf ◽  
Tianao Guo ◽  
...  
Keyword(s):  
New Species ◽  
Ir Spectroscopy ◽  
Iron Complexes ◽  
Molecular Structures ◽  
Synthesis And Characterization ◽  
Carbonyl Complexes ◽  
Subsequent Reduction ◽  
X Ray ◽  
X Ray Crystallography

Divalent iron complexes trans-[FeBr2(BINC)2], [Cp*FeCl(BINC)] (Cp* = Me5C5) and [FeBr2(CNAr3NC)2] with chelat-ing bis(isonitrile) ligands BINC (bis(2-isocyanophenyl)phenylphosphonate) and CNAr3NC (2,2’’-diisocyano-3,5,3’’,5’’tetramethyl-1,1’:3’,1’’-terphenyl) have been prepared and characterized. Their subsequent reduction yields di- and trinuclear compounds [Fe3(BINC)6], [Cp*Fe(BINC)]2, [Fe(CNAr3NC)2]2 and [K(Et2O)]2[Fe(CNAr3NC)2]2. The molecular structures of all new species were determined by X-ray crystallography. The molecular structures are compared to related iron carbonyl complexes. The complexes were further characterized by NMR and IR spectroscopy, and the electrochemical properties of selected compounds were analyzed by UV-Vis-NIR spectroelectrochemistry. <br>

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