Tp*WIVO(S2CNEt2): the Missing Member of the Series

2004 ◽  
Vol 57 (3) ◽  
pp. 269 ◽  
Author(s):  
Aston A. Eagle ◽  
Charles G. Young ◽  
Edward R. T. Tiekink
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Cyclic Voltammetry ◽  
1H Nmr Spectroscopy ◽  
Octahedral Complex ◽  
Synthesis And Characterization ◽  
Oxygen Atom Transfer ◽  
X Ray ◽  
Distorted Octahedral

The missing member of the series Tp*ME(S2CNEt2) (M = Mo, W; E = O, S), namely Tp*WO(S2CNEt2), has been synthesized by oxygen-atom transfer from pyridine N-oxide to Tp*W(S2CNEt2)(CO)2. The air-stable, blue-purple complex was characterized by microanalysis, mass spectrometry (m/z 645 (100%), [M]+), cyclic voltammetry, and IR and 1H NMR spectroscopy. Solutions of the complex are dichroic and solvatochromic. The X-ray crystal structure of the complex revealed a six-coordinate, distorted octahedral complex with axial oxo (W = O 1.680(5) Å), ‘equatorial’ dithiocarbamate (W—S 2.3962(17) and 2.4102(17) Å), and facial tridentate Tp* ligands. The synthesis and characterization of Tp*WCl3 are also reported.

Synthesis and characterization of a new Keggin anion: [BeW12O40]6−

2014 ◽  
Vol 50 (65) ◽  
pp. 9083-9085 ◽  
Author(s):  
Alexander V. Anyushin ◽  
Anton I. Smolentsev ◽  
Dmitry A. Mainichev ◽  
Cristian Vicent ◽  
Artem L. Gushchin ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Cyclic Voltammetry ◽  
Synthesis And Characterization ◽  
Keggin Anion ◽  
X Ray ◽  
Esi Mass Spectrometry

The first berillododecatungstate [BeW12O40]6− has been synthesized and characterized by X-ray analysis, cyclic voltammetry, ESI-mass spectrometry, and 9Be and 183W NMR.

The synthesis and characterization of the pendant-armed ligand N,N′-bis(2′-pyridylmethyl)-1,7-dithia-4,11-diazacyclotetradecane (L4) and crystal structures of L4 and the copper(II) complex [Cu(L4)](ClO4)2 — Crystal structure of the nickel(II) complex of N-(2′-pyridylmethyl)-1,4,7-trithia-11-azacyclotetradecane (L2), [Ni(L2)(CH3CN)](ClO4)2·CH3CN

2006 ◽  
Vol 84 (2) ◽  
pp. 187-195 ◽  
Author(s):  
B CM Chak ◽  
A McAuley
Keyword(s):  
Crystal Structure ◽  
Copper Ion ◽  
Esr Spectra ◽  
Synthesis And Characterization ◽  
Electrochemical Studies ◽  
High Dilution ◽  
Donor Ligand ◽  
X Ray ◽  
Distorted Octahedral

The synthesis and characterization of the mixed donor ligand N,N′-bis(2′-pyridylmethyl)-1,7-dithia-4,11-diazacyclotetradecane (L4) containing two pendant pyridine arms is described. The macrocycle formation involves reaction of N-tosylbis(2-bromoethyl)amine with N-tosylbis(3-mercaptopropyl)amine at high dilution followed by detosylation at the nitrogen atoms using LiAlH4 in view of the presence of the thioether groups. An X-ray study of the ligand shows the sulphur atoms lie exo to the macrocyclic ring. The nickel(II) and copper(II) complexes of L4 have been characterized and the X-ray structure of the Cu(II) ion exhibits a five-coordinate copper ion despite the presence of six available donor atoms. In the case of ligand N-(2-pyridylmethyl)-1,4,7-trithia-11-azacyclotetradecane (L2), with a single pendant N donor, the Ni(II) complex is distorted octahedral with a molecule of acetonitrile in the sixth site. Details of UV–vis, ESR spectra, and electrochemical studies on the complexes are presented.Key words: synthesis, pendant-armed, mixed donor S,N macrocycles, copper, nickel.

Nitridomolybdenum Complexes of Tris(3,5-dimethylpyrazol-1-yl)Hydroborate and the X-Ray Crystal-Structure of {HB(3,5-Me2C3N2H)3)MoN(N3)2

1990 ◽  
Vol 43 (8) ◽  
pp. 1347 ◽  
Author(s):  
CG Young ◽  
F Janos ◽  
MA Bruck ◽  
PA Wexler ◽  
JH Enemark
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Least Squares ◽  
Elemental Analysis ◽  
Bond Distance ◽  
Octahedral Complex ◽  
Fourier Methods ◽  
X Ray ◽  
Distorted Octahedral ◽  
R Value

The reaction of (NEt4)2[MoNCl5] and K{HB(Me2pz)3}[HB(Me2pz)3- = tris (3,5- dimethylpyrazol-1-yl) hydroborate anion] produces both purple, diamagnetic {HB(Me2pz)3}MoNCl2 (1) and yellow, paramagnetic Net4 [{HB(Me2pz)3}MoNCl2] (2) (e.s.r.: {g} 1.961, {a}(95Mo) 57×10-4 cm-1), which have been separately isolated under different conditions. In contrast, the reaction of [ MoN (N3)4]- with Na{HB(Me2pz)3} results in the exclusive formation of red {HB(Me2pz)3} MoN (N3)2 (3). Crystals of (3) are monoclinic and belong to space group P21/n with a 16.440(2), b 8.787(2), c 16.754(2) Ǻ,β 112.47(1)°, V 2236.4 Ǻ3, and Z 4. The structure was solved by Patterson and Fourier methods, followed by least-squares refinement, using 3208 reflections, to a conventional R value of 0.032 ( Rw 0.047). In the distorted octahedral complex the molybdenum(VI) atom is coordinated by a facial HB(Me2pz)3- ligand , a terminal nitrido ligand with a Mo-N bond distance of 1.646(4)Ǻ, and two azide ligands. All complexes have been characterized by elemental analysis, infrared, 1H n.m.r. or e.s.r. spectroscopy, and mass spectrometry. Improved syntheses for the starting materials (NEt4)2 [MoNCl5] and (NEt4)2 [MoNCl4] are also reported.

Synthesis and Characterization of Enantiopure Tribenzotriquinacene Dimers Bearing a Platinum-Diacetylene Unit

Synthesis ◽  
2019 ◽  
Vol 51 (10) ◽  
pp. 2116-2121 ◽  
Author(s):  
Wen-Rong Xu ◽  
Xin-Rui Wang ◽  
Hak-Fun Chow ◽  
Dietmar Kuck
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
31P Nmr ◽  
Synthesis And Characterization ◽  
31P Nmr Spectroscopy ◽  
Enantiomerically Pure ◽  
X Ray ◽  
Esi Mass Spectrometry ◽  
13C And 31P Nmr

A pair of enantiomerically pure metallodimers containing two deeply concave tribenzotriquinacene (TBTQ) units linked by a platinum-diacetylene unit were synthesized. Such linear metal-centered TBTQ dimers are considered as edges of metallosquares and metallocubes that bear four or eight mutually syn-oriented TBTQ bowls at their tips, respectively. The structures of the metallodimers were characterized by 1H, 13C and 31P NMR spectroscopy, ESI mass spectrometry, and circular dichroism. The single X-ray crystal structure of (+)-enantiomer confirmed the absolute configuration of the metallodimers and revealed an edge (tip-to-tip) length of 18.456 Å and an approximated syn-orientation of the two TBTQ bowls in the solid state.

Synthesis and Characterization of a Methanofullerene-4-Fluoro-α-Cyanostilbene Dyad as a Potential Acceptor for Organic Solar Cells

2015 ◽  
Vol 1784 ◽  
Author(s):  
Venkata Neti
Keyword(s):  
Mass Spectrometry ◽  
Cyclic Voltammetry ◽  
Solar Cells ◽  
Organic Solar Cells ◽  
Synthesis And Characterization ◽  
Lumo Energy ◽  
Homo Lumo ◽  
Aryl Ester

ABSTRACTA series of fluorine appended highly conjugated fullerenes were prepared containing fluoro-α-cyanostilbene and aryl ester units. These modified PCBM dyads are fully characterized by NMR, Mass spectrometry, UV-vis, and cyclic voltammetry (Figures 1-4). It was found that the presence of fluoro-α-cyanostilbenes and esters affects the cyclic voltammetry and absorption in the UV-Vis region. The PCBA modified fullerenes significantly influences the HOMO-LUMO energy and wide absorption compared to PCBM.

Darstellung und Charakterisierung von Rubidiumhydrogencyanamid/Synthesis and Characterization of Rubidium Hydrogen Cyanamide

1999 ◽  
Vol 54 (11) ◽  
pp. 1375-1378 ◽  
Author(s):  
Michael Becker ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Liquid Ammonia ◽  
Synthesis And Characterization ◽  
Hydrogen Cyanamide ◽  
X Ray ◽  
Bond Lengths

The synthesis of RbHCN2 was carried out by reaction of cyanamide with rubidium amide in liquid ammonia. The crystal structure has been determinedo by x-ray powder methods (orthorhombic, P21,21,21, a = 7.299(1), b = 9.435(1), c = 9.420(1) Å; Z = 8). The anion is slightly bent (174°) and exhibits two different bond lengths (C-N: 1.17, HN-C: 1.31 Å).

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