Synthesis and characterization of tantalum(V) metallaheterocycle (Me2N)3 and chloro-mixed-amide (Me2N)3Ta(Cl)[N(SiMe3)2]

2003 ◽  
Vol 81 (11) ◽  
pp. 1398-1405 ◽  
Author(s):  
Hu Cai ◽  
Xianghua Yu ◽  
Tianniu Chen ◽  
Xue-Tai Chen ◽  
Xiao-Zeng You ◽  
...  
Keyword(s):  
Solid State ◽  
Hydrogen Abstraction ◽  
Synthesis And Characterization ◽  
Amido Complexes ◽  
X Ray ◽  
Trigonal Bipyramidal Geometry ◽  
Trigonal Bipyramidal ◽  
State 1 ◽  
Distorted Trigonal Bipyramidal

A new mixed-amido complex (Me2N)3Ta(Cl)[N(SiMe3)2] (1) was prepared from the reaction of (Me2N)3TaCl2 with 1 equiv. of LiN(SiMe3)2. The reactions of 1 with 1 equiv. of LiN(SiMe3)2 or (Me2N)3TaCl2 with 2 equiv. of LiN(SiMe3)2 gave (Me2N)3[Formula: see text] (2) with a four-membered metallaheterocyclic ring through γ-hydrogen abstraction. In the solid state, 1 adopts a distorted trigonal bipyramidal geometry with the -N(SiMe3)2 and -Cl ligands in the equatorial and axial positions, respectively. The X-ray structure of 2 reveals that it is in a distorted trigonal bipyramidal geometry with a planar metallaheterocyclic ring.Key words: tantalum, γ-hydrogen abstraction, C-H activation, amido complexes, metallacycle.

scholarly journals Synthesis and characterization of novel coumarin-based terpyridine ligands and their Zn(II) complexes

2020 ◽  
Vol 44 (11-12) ◽  
pp. 721-726
Author(s):  
Xiaolong Wang ◽  
Xian Yue ◽  
Long Deng
Keyword(s):  
Solvothermal Method ◽  
Emission Spectra ◽  
Synthesis And Characterization ◽  
Spectroscopic Methods ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Terpyridine Ligands ◽  
Distorted Trigonal Bipyramidal

Two novel mononuclear Zn(II) complexes, [ZnL1Cl2] (1) (L1=( E)-3-(4-(2,2′:6′,2″-tripyridyl)-4′-styryl)-7-diethylaminocoumarin) and [ZnL2Cl2] (2) (L2=3-(4-(2,2′:6′,2″-tripyridyl)-4′-phenylimine)-7-diethylaminocoumarin), were obtained by the solvothermal method from ZnCl2 and coumarin-based terpyridine ligands. The complexes were characterized by spectroscopic methods and single-crystal X-ray diffraction. The Zn2+ in the complexes is coordinated by three nitrogen atoms of the terpyridine ligand and two chloride anions, forming a distorted trigonal bipyramidal environment. Moreover, the UV–Vis absorption and emission spectra of the ligands and complexes in diluted dichloromethane solutions were measured.

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.

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>

Synthesis and characterization of octahedral and trigonal bipyramidal transition metal complexes incorporating chelating gallate ligands: crystal and molecular structure of [Me2Ga(N2C5H7)(OCH2CH2NMe2)]Ni[(N2C5H7)2GaMe2]

1980 ◽  
Vol 58 (11) ◽  
pp. 1091-1100 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Transition Metal Complexes ◽  
Crystal And Molecular Structure ◽  
Synthesis And Characterization ◽  
Chelating Ligands ◽  
Full Matrix ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

The preparation and physical properties of octahedral and trigonal bipyramidal complexes incorporating the tris-chelating ligands [Me2Ga(N2C5H7)(OCH2CH2NR′2)]− (R′ = H or Me) are described. Crystals of [dimethylbis(3,5-dimethyl-1-pyrazolyl)gallato (N(2),N′(2))][dimethyl (3,5 - dimethyl-1-pyrazolyl) (N,N-dimethylethanolamino(gallato (N(2), O, N(3))]nickel(II) are triclinic, a = 20.8562(11), b = 9.1536(4), c = 8.2798(4) Å, α = 100.204(3), β = 85.513(4), γ = 101.989(3)°, Z = 2, space group [Formula: see text]. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares procedures to R = 0.048 and Rw = 0.078 for 5508 reflections with I ≥ 3σ(I). The coordination about the Ni atom is distorted trigonal bipyramidal with the two nitrogen atoms from the Me2Ga(N2C5H7)2 ligand occupying equatorial positions. The tridentate Me2Ga(N2C5H7)(OCH2CH2NMe2) ligand is meridionally coordinated with the oxygen in the equatorial and the two nitrogens in the axial positions. Important bond lengths (corrected for libration) are: Ni—N(eq), 2.005(3) and 2.006(3), Ni—O, 1.993(3), Ni—N(pz—ax), 2.072(3), Ni—N(amino), 2.229(3), Ga—O, 1.913(3), Ga—N, 1.971(3)–1.989(3), and Ga—C, 1.961(10)–1.986(6) Å.

Synthesis and characterization of molybdenum–tin complexes derived from the molybdenum tricarbonyl anion, [MeGapz3]Mo(CO)3−, and organotin chlorides. X-ray crystal structure of [MeGapz3]Mo(CO)3SnPh3 (where pz = pyrazolyl, N2C3H3)

1986 ◽  
Vol 64 (2) ◽  
pp. 321-327 ◽  
Author(s):  
Emmanuel C. Onyiriuka ◽  
Steven J. Rettig ◽  
Alan Storr
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Heavy Atom ◽  
Synthesis And Characterization ◽  
Full Matrix ◽  
X Ray ◽  
Tin Complexes ◽  
Interesting Solution ◽  
Single Bonds

The reaction of the molybdenum tricarbonyl anion, [MeGapz3]Mo(CO)3−, with the organotin chlorides, Ph3SnCl, Me3SnCl, and Me2SnCl2, has yielded a series of complexes in which direct Mo—Sn single bonds are featured. The [MeGapz3]Mo(CO)3SnMe2Cl complex shows an interesting solution behavior in which a transition from a 3:4, or piano stool structure, to a 3:3:1, or capped octahedral arrangement, is thought to occur. The 3:3:1 structure has been demonstrated in the solid state for the [MeGapz3]Mo(CO)3SnPh3 compound by means of a crystal structure determination. Crystals of [methyltris(1-pyrazolyl)gallato-N,N,N](triphenylstannyl)tricarbonylmolybdenum are monoclinic, a = 11.4439(8), b = 19.5116(8), c = 15.2686(12) Å β = 111.370(3)°, Z = 4, space group P21/c. The structure was solved by conventional heavy-atom methods and was refined by full-matrix least-squares procedures to R = 0.025 and Rw = 0.031 for 5259 reflections with I ≥ 3σ(I). Important bond lengths include: Mo—Sn = 2.8579(3), Mo—N = 2.239(2)–2.244(2), Mo—C = 1.967(3)–2.000(3), Sn—C = 2.151(3)–2.166(3), Ga—N = 1.920(3)–1.931(3), and Ga—C = 1.943(4) Å.

scholarly journals Synthesis, structure and characterization of a new cadmium(II) iodide containing a tetradentate tripodal amine

2014 ◽  
Vol 10 (5) ◽  
pp. 2728-2736 ◽  
Author(s):  
Kamel Kaabi ◽  
Valeria Ferretti ◽  
Frederic Lefebvre ◽  
Cherif Ben Nasr
Keyword(s):  
Infrared Spectroscopy ◽  
Dft Calculations ◽  
Absorption Bands ◽  
Nmr Spectrum ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Cp Mas Nmr ◽  
13C Cp Mas Nmr ◽  
Distorted Trigonal Bipyramidal

A cadmium(II) iodide compound of the [Cd(L)I]I series, with L = tris(2-aminoethyl)amine, is synthesized and characterized. X-ray structural study shows that the title compound has a slightly distorted trigonal bipyramidal environment where the CdN4I chromophore is bounded by N atoms of L and one iodide. In the structural arrangement, the [Cd(L)I]+ cationic complexes are interconnected via N-H···I hydrogen bonds generated by the uncoordinated I iodide anions to form layers parallel to the (a, c) plane. The 13C CP-MAS NMR spectrum is discussed and the vibrational absorption bands were identified by infrared spectroscopy and DFT calculations.

Neue Oxopnictate AI3MVO4: Darstellung und Kristallstruktur von A3AsO4 (A = K, Rb, Cs) und K3BiO4 / New Oxopnictates AI3MVO4: Synthesis and Crystal Structure of A3AsO4 (A = K, Rb, Cs) and K3BiO4

2002 ◽  
Vol 57 (6) ◽  
pp. 599-604 ◽  
Author(s):  
Franziska Emmerling ◽  
Mamdouh Idilbi ◽  
Caroline Röhr
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Close Packing ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Trigonal Bipyramidal Geometry ◽  
Trigonal Bipyramidal ◽  
Centrosymmetric Dimers ◽  
Distorted Trigonal Bipyramidal

Abstract The title compounds have been synthesized via oxidation of the elemental pnicogenes (M = As, Bi) with the hyperoxides AO2 (A = K, Rb, Cs) and their crystal structures were determined on the basis of single crystal X-ray data. In K3AsO4 (orthorhombic, Cccm, a = 1060:1(1), b = 1135:2(1), c = 1694:0(2) pm, Z = 16) and Cs3AsO4(orthorhombic, Pnma, a = 1254:3(2), b = 902:9(2), c = 658:5(3) pm, Z = 4) isolated tetrahedra [AsO4]3- with distances As-O between 167.0 and 170.5 pm are present, which are arranged in a nearly cubic close packing. The structure of K3BiO4 (triclinic, P1̄, a = 643:18(6), b = 657:27(6), c = 762:41(7) pm, α = 101:724(2)°, β = 96:472(2)°, γ = 105:465(2)°, Z = 2) contains centrosymmetric dimers [O3BiO2BiO3]6-, in which the Bi(V) atoms are surrounded by five O atoms in a distorted trigonal bipyramidal geometry with distances Bi-O in the range of 199.5 to 233.1 pm.

Synthesis and Characterization of o-Carboranylthioether Derivatives

2011 ◽  
Vol 66 (9) ◽  
pp. 947-952
Author(s):  
Meiling Xu ◽  
Yong Nie ◽  
Jinling Miao ◽  
Zhenwei Zhang ◽  
Bin Peng ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Solid State ◽  
Single Crystal ◽  
Uv Light ◽  
Chloroform Solution ◽  
Alkyl Halides ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray

The reactions of the dithiolato-o-carborane salt (Et3NH)2(S2C2B10H10) (2) with alkyl halides BrCH2CH=CH2, BrCH2CH2CH2Cl and C6H5CH2Cl, afford the o-carboranyl-bisthioether derivatives 3a - c, which have been characterized by IR and NMR (1H, 13C, 11B) spectroscopy, mass spectrometry, and single-crystal X-ray diffraction (3c). The photoluminescent properties of the known compound 3c has been investigated. It exhibits a violet (chloroform solution) or blue (solid state) emission when excited with UV light.

Synthesis and Characterization of New Non-aromatic Texaphyrin-type Expanded Porphyrins

1999 ◽  
Vol 03 (02) ◽  
pp. 148-158 ◽  
Author(s):  
SYLVIE MEYER ◽  
MICHAEL C. HOEHNER ◽  
VINCENT LYNCH ◽  
JONATHAN L. SESSLER
Keyword(s):  
Schiff Base ◽  
Solid State ◽  
Good Yield ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Expanded Porphyrins ◽  
Meso Position ◽  
Macrocyclic Structure

The synthesis and X-ray diffraction-based characterization of a texaphyrin-type non-aromatic expanded porphyrin, 13,18,22,27-tetraethyl-14,17,23,26-tetramethyl-20-p-nitrophenyl-3,10,28,29,30,31-hexaazahexacyclo[23.2.1.04,9.112,15.116,19.121,24]untriaconta-2, 4, 5, 7, 10,12,14,16,18,-20,22,24(30),25,27-tetradecaene (1), is reported. This Schiff base macrocycle was prepared in good yield via the 1:1 HCl -catalyzed condensation of a tetrapyrrole dialdehyde precursor, (di(5-formyl-4,4'-diethyl-3,3'-dimethyl-2,2'-bipyrrole)-p-nitrophenylmethine), with 1,2-phenylenediamine. Compound 1 was assigned as being a 26 π-electron non-aromatic benzannulene on the basis of both proton NMR and single-crystal X-ray diffraction analyses. The latter studies, in particular, revealed a non-planar macrocyclic structure co-crystallized with a molecule of water. By varying either the diamine used in the cyclization step and/or the substituent in the meso-position of the tetrapyrrolic precursor, a range of other systems analogous to 1 could be obtained. The resulting systems were found to present good stability both in the solid state and in solution.

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