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.

Synthesis, characterization, and reactivity of the first hafnium alkyl complex stabilized by amidate ligands

2005 ◽  
Vol 83 (6-7) ◽  
pp. 1037-1042 ◽  
Author(s):  
Robert K Thomson ◽  
Brian O Patrick ◽  
Laurel L Schafer
Keyword(s):  
Coordination Chemistry ◽  
Solid State ◽  
Key Words ◽  
Low Temperatures ◽  
Variable Temperature ◽  
X Ray ◽  
X Ray Crystallography ◽  
Exchange Processes ◽  
Hydrolysis Of

A photo and thermally stable bis(amidate)–dibenzyl complex of Hf ([DMP(NO)Ph]2Hf(CH2Ph)2(THF) (2a) was formed as a monosolvated THF adduct in near quantitative yield from Hf(CH2Ph)4 and N-2,6-dimethylphenyl(phenyl)amide (1). Isomerization between the THF-bound product and the THF-free product can be observed visually by the conversion from a red-orange product at low temperatures to a pale yellow product at high temperatures. Solid-state crystallographic characterization of the orange product confirmed its constitution as a monosolvated species. Kinetic parameters for the exchange of the THF moiety were determined from variable-temperature NMR experiments. The product of the hydrolysis of the Hf dibenzyl species by water was characterized by X-ray crystallography, and was found to be a rare tetrametallic Hf oxo cluster species (3).Key words: hafnium, protonolysis, amidate, coordination chemistry, organometallic chemistry, exchange processes.

Synthesis and structural characterization of a magnesium phthalocyanine(3–) anion

2012 ◽  
Vol 16 (01) ◽  
pp. 154-162 ◽  
Author(s):  
Edwin W.Y. Wong ◽  
Daniel B. Leznoff
Keyword(s):  
Absorption Spectrum ◽  
Solid State ◽  
Single Crystal ◽  
Structural Characterization ◽  
Heterometallic Complex ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography

The reduction of magnesium phthalocyanine (MgPc) with 2.2 equivalents of potassium graphite in 1,2-dimethoxyethane (DME) gives [K2(DME)4]PcMg(OH)(1) in 67% yield. Compound 1 was structurally characterized using single crystal X-ray crystallography and was found to be a monomeric, heterometallic complex consisting of a μ3-OH ligand that bridges a [MgIIPc3-]- anion to two potassium cations solvated by four DME molecules. An absorption spectrum of 1 confirms the Pc ligand is singly reduced and has a 3–charge. The solid-state structure of 1 does not indicate breaking of the aromaticity of the Pc ligand. Compound 1 is only the second Pc3- complex and the first reduced MgPc to be isolated and structurally characterized.

Preparation and characterization of a new series of Cr(II) hydroborates

1995 ◽  
Vol 73 (7) ◽  
pp. 1126-1134 ◽  
Author(s):  
Michel Dionne ◽  
Shoukang Hao ◽  
Sandro Gambarotta
Keyword(s):  
Trinuclear Complex ◽  
Synthesis And Characterization ◽  
Crystal Data ◽  
X Ray ◽  
X Ray Crystallography ◽  
Quadruple Bond ◽  
Quadruple Bonds ◽  
Reaction Proceeds

The synthesis and characterization of a new series of mono-, di-, and trinuclear Cr(II) borohydride compounds is described. The reaction of CrCl2(TMEDA) with two equivalents of NaBH4 afforded the thermally unstable (TMEDA)Cr(BH4)2 (1), which was converted by treatment with pyridine into the octahedral monomeric (Py)4Cr(BH4)2 (2). The reaction proceeds via formation of an intermediate trinuclear complex {[(TMEDA)(Py)Cr(η2-BH4)]2[(Py)2Cr(η2-BH4)2]}(µ,η1-BH4)2 (3), which was isolated and characterized by X-ray crystallography. Reaction of 1 and 2 with both CO2 and RN=C=NR (R = Cy, iPr) afforded hydride insertion and formation of the corresponding diamagnetic lantern-type Cr(II) formate (HCO2)4Cr2Py2 (4) and formamidinate compounds [RNC(H)NR]2Cr2(µ-BH)4 (R = Cy (5a), iPr (5b)), respectively, with supershort Cr—Cr quadruple bonds. The structures of 1, 2, 3, and 5b were elucidated by X-ray analysis. Crystal data are as follows. 1: C6H24N2B2Cr, monoclinic, Cc, a = 8.517(2) Å, b = 15.921(5) Å, c = 9.624(2) Å, β = 115.59(1)°, Z = 4, R = 0.022, Rw = 0.029; 2: C28H44N4B2O2Cr, monoclinic, P21/n, a = 12.021(1) Å, b = 15.555(1) Å, c = 15.723(1) Å, β = 90.13(2)°, Z = 4, R = 0.074, Rw = 0.086; 3: C32H76N8B6Cr3, monoclinic, P21/n, a = 8.515(1) Å, b = 14.525(1) Å, c = 18.286(2) Å, β = 91.38(1)°, Z = 2, R = 0.051, Rw = 0.060; 5b: C21H49N6BCr2, monoclinic, C2/c, a = 17.000(1) Å, b = 9.033(1) Å, c = 19.160(1) Å, β = 105.579(9)°, Z = 4, R = 0.069, Rw = 0.078. Keywords: divalent chromium, borohydride, Cr—Cr quadruple bond.

scholarly journals CAAC Boranes. Synthesis and characterization of cyclic (alkyl) (amino) carbene borane complexes from BF3 and BH3

2010 ◽  
Vol 6 ◽  
pp. 709-712 ◽  
Author(s):  
Julien Monot ◽  
Louis Fensterbank ◽  
Max Malacria ◽  
Emmanuel Lacôte ◽  
Steven J Geib ◽  
...  
Keyword(s):  
Silica Gel ◽  
Synthesis And Characterization ◽  
Gel Chromatography ◽  
Nmr Analysis ◽  
X Ray ◽  
X Ray Crystallography ◽  
In Situ Formation ◽  
Silica Gel Chromatography

In situ formation of two cyclic (alkyl) (amino) carbenes (CAACs) followed by addition of BF3•Et2O provided the first two examples of CAAC–BF3 complexes: 1-(2,6-diisopropylphenyl)-3,5,5-trimethyl-3-phenylpyrrolidin-2-ylidene trifluoroborane, and 2-(2,6-diisopropylphenyl)-3,3-dimethyl-2-azaspiro[4.5]decan-1-ylidene trifluoroborane. These CAAC–BF3 complexes are robust compounds that are stable to ambient laboratory conditions and silica gel chromatography. They were characterized by spectroscopy and X-ray crystallography. In contrast, a CAAC complex with borane (BH3) was readily formed in situ according to 1H and 11B NMR analysis, but did not survive the workup conditions. These results set the stage for further studies of the chemistry of CAAC boranes.

scholarly journals Synthesis and characterization of novel bioactive 1,2,4-oxadiazole natural product analogs bearing the N-phenylmaleimide and N-phenylsuccinimide moieties

2013 ◽  
Vol 9 ◽  
pp. 2202-2215 ◽  
Author(s):  
Catalin V Maftei ◽  
Elena Fodor ◽  
Peter G Jones ◽  
M Heiko Franz ◽  
Gerhard Kelter ◽  
...  
Keyword(s):  
Natural Product ◽  
Synthesis And Characterization ◽  
Aminobenzoic Acid ◽  
One Pot ◽  
X Ray ◽  
X Ray Crystallography ◽  
Quisqualic Acid ◽  
Oxobutanoic Acid

Taking into consideration the biological activity of the only natural products containing a 1,2,4-oxadiazole ring in their structure (quisqualic acid and phidianidines A and B), the natural product analogs 1-(4-(3-tert-butyl-1,2,4-oxadiazol-5-yl)phenyl)pyrrolidine-2,5-dione (4) and 1-(4-(3-tert-butyl-1,2,4-oxadiazol-5-yl)phenyl)-1H-pyrrole-2,5-dione (7) were synthesized starting from 4-(3-tert-butyl-1,2,4-oxadiazol-5-yl)aniline (1) in two steps by isolating the intermediates 4-(4-(3-tert-butyl-1,2,4-oxadiazol-5-yl)phenylamino)-4-oxobutanoic acid (3) and (Z)-4-(4-(3-tert-butyl-1,2,4-oxadiazol-5-yl)phenylamino)-4-oxobut-2-enoic acid (6). The two natural product analogs 4 and 7 were then tested for antitumor activity toward a panel of 11 cell lines in vitro by using a monolayer cell-survival and proliferation assay. Compound 7 was the most potent and exhibited a mean IC50 value of approximately 9.4 µM. Aniline 1 was synthesized by two routes in one-pot reactions starting from tert-butylamidoxime and 4-aminobenzoic acid or 4-nitrobenzonitrile. The structures of compounds 1, 2, 4, 5 and 6 were confirmed by X-ray crystallography.

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.

Synthesis and characterization of 5,12-dimethyl-7,14-diphenyl-1,4,8,11- tetraazacyclotetradecane-4,11-diacetic acid and its transition metal complexes; crystal structure of the copper(II) complex of the macrocycle

1993 ◽  
Vol 71 (11) ◽  
pp. 1805-1809 ◽  
Author(s):  
Liqin Chen ◽  
Laurence K. Thompson ◽  
John N. Bridson ◽  
Jide Xu ◽  
Shisheng Ni ◽  
...  
Keyword(s):  
Transition Metal Complexes ◽  
Esr Spectra ◽  
Synthesis And Characterization ◽  
Diacetic Acid ◽  
X Ray ◽  
X Ray Crystallography ◽  
Carboxylate Oxygen ◽  
Spin Resonance ◽  
Oxygen Donors

The synthesis and characterization of a new 14-membered tetraazamacrocyclic ligand 5,12-dimethyl-7,14-diphenyl-1,4,8,11-tetraazacyclotetradecane-4,11-diacetic acid (H2L1) is reported. Cobalt(III), nickel(II), and copper(II) complexes with this ligand were prepared and characterized by infrared, electronic, and electron spin resonance (esr) spectra and in one case by X-ray crystallography. The complex CuL1•2CH3CH2OH (3) crystallized in the triclinic system, space group[Formula: see text], with a = 8.440(2), b = 13.445(2), c = 7.523(1) Å, α = 99.30(1), β = 106.57(1), γ = 87.00(1)° and Z = 2 (R = 0.027, Rw = 0.028 for 2618 reflections). The complex shows a distorted trans-octahedral geometry with four amino nitrogens in a plane and two apical carboxylate oxygen donors.

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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