Study on the Acid-Induced Ring-Expansion of an Oxaphosphirane Complex with an Electron-Withdrawing C-Substituent

2017 ◽  
Vol 70 (4) ◽  
pp. 442 ◽  
Author(s):  
Cristina Murcia García ◽  
Gregor Schnakenburg ◽  
Rainer Streubel

A study on the acid-induced ring-expansion reaction of the first oxaphosphirane complexes bearing an electron-withdrawing C-substituent is described. The stereoselectively obtained 1,3,4-dioxaphospholane complexes 4a–c, representing the first examples of such fluorinated ligands, were unambiguously characterized by multinuclear NMR, elemental analysis, mass spectrometry, and single-crystal X-ray diffraction studies.

2016 ◽  
Vol 71 (1) ◽  
pp. 81-84 ◽  
Author(s):  
Eugen Weisheim ◽  
Hans-Georg Stammler ◽  
Norbert W. Mitzel

AbstractThe reaction of 1,3,5-triethynyl-1,3,5-trimethyl- 1,3,5-trisilacyclohexane with (dimethylamino)trimethylstannane afforded 1,3,5-tris[(trimethylstannyl)ethynyl]- 1,3,5-trimethyl-1,3,5-trisilacyclohexane with tin-functionalised ethynyl groups. The compound was characterized by single-crystal X-ray diffraction, elemental analysis, mass spectrometry, NMR and FT-IR spectroscopy.


2010 ◽  
Vol 65 (5) ◽  
pp. 556-564 ◽  
Author(s):  
Victoria Lachkova ◽  
Sabi Varbanov ◽  
Walter Frank ◽  
Helmut Keck

Three new N-phosphinoyl-substituted aminomethanephosphonic acids have been synthesized and characterized: dimethylphosphinoylmethyl-imino-bis(methanephosphonic acid) (1), [3-(dimethylphosphinoyl)-propyl]-imino-bis(methanephosphonic acid) (2), and N-benzyl-Ndimethylphosphinoylmethyl- aminomethanephosphonic acid (3). The latter was isolated as a hydrochloride 3 ・ HCl. The acids have been prepared via Moedritzer-Irani reaction from the corresponding dimethylphosphinoyl-substituted primary and secondary aliphatic amines. Their structures have been confirmed by elemental analysis, IR, 1H, 31P{1H}, 13C{1H} NMR spectroscopy, electrospray ionization mass spectrometry, and single-crystal X-ray diffraction.


Molbank ◽  
10.3390/m1110 ◽  
2020 ◽  
Vol 2020 (1) ◽  
pp. M1110 ◽  
Author(s):  
Rebeca González-Fernández ◽  
Javier Borge ◽  
Pascale Crochet ◽  
Victorio Cadierno

The synthesis of a series of arene-osmium(II) complexes containing phosphinite-type ligands, namely, [OsCl2(η6-p-cymene){R2PO(CH2)nPh}] (R = Ph, n = 1 (4a), 2 (4b), 3 (4c); R = iPr, n = 1 (5a), 2 (5b), 3 (5c)) and [OsCl2(η6-benzene){iPr2PO(CH2)2Ph}] (7), is presented. All these compounds were characterized by elemental analysis and multinuclear NMR spectroscopy (31P{1H}, 1H and 13C{1H}), and the structure of [OsCl2(η6-p-cymene){Ph2PO(CH2)3Ph}] (4c) unequivocally confirmed through a single-crystal X-ray diffraction study. Attempts to generate the tethered species [OsCl2{η6:κ1(P)-C6H5(CH2)nOPR2}] by intramolecular exchange of the coordinated arene in 4-5a-c or 7, upon thermal or MW heating, failed.


2012 ◽  
Vol 67 (6) ◽  
pp. 589-593 ◽  
Author(s):  
Daniel Winkelhaus ◽  
Beate Neumann ◽  
Norbert W. Mitzel

The reaction of (C6F5)2BCl with 8-lithio-N,N-dimethyl-1-naphthylamine (1) afforded the fivemembered ring system 8-bis(pentafluorophenyl)boryl-N,N-dimethyl-1-naphthylamine (2) with an intramolecular dative B-N bond. The compound was characterised by elemental analysis, NMR spectroscopy and single-crystal X-ray diffraction.


2020 ◽  
Author(s):  
Viktoria Leonhardt ◽  
Stefanie Fimmel ◽  
Ana-Maria Krause ◽  
Florian Beuerle

<div><div><div><p>A trigonal-bipyramidal covalent organic cage compound serves as an efficient host to form stable 1:1-complexes with C60 and C70. Fullerene encapsulation has been comprehensively studied by NMR and UV/Vis spectroscopy, mass spectrometry as well as single-crystal X-ray diffraction. Exohedral functionalization of encapsulated C60 via threefold Prato reaction revealed high selectivity for the symmetry-matched all-trans-3 addition pattern.</p></div></div></div>


Crystals ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 982
Author(s):  
Devaraj Pandiarajan ◽  
Thomas Fox ◽  
Bernhard Spingler

The coordination chemistry of butane-2,3-dione bis (2′-pyridylhydrazone) towards the divalent first-row transition metals zinc and iron has been explored. Depending upon the conditions, the ligand in the six complexes was found to be either neutral, mono, or doubly deprotonated. The zinc(II) and iron(II) complexes were fully characterized by elemental analysis, mass spectrometry, and X-ray diffraction methods.


Author(s):  
Sergei V. Voitekhovich ◽  
Berthold Kersting ◽  
Oleg A. Ivashkevich

The dinuclear nickel(II) complex [Ni2LmClO4] + , where Lm represents a 24-membered macrocyclic hexaaza-dithiophenolate ligand, reacts with 5-(4-pyridyl)tetrazole (PyrCN4H) to give the dinuclear complex [Ni2Lm(PyrCN4)]+ . The new complex was both isolated as perchlorate or tetraphenylborate salts and characterised by elemental analysis and IR spectroscopy. The structure of [Ni2Lm(PyrCN4)]BPh4 ⋅ MeCN was determined by single crystal X-ray diffraction, showing that tetrazolate units are in a N2,N3-bridging mode to generate dioctahedral N3Ni(µ-S)2(µ-N4CPyr)NiN3 core.


2020 ◽  
Vol 42 (2) ◽  
pp. 249-249
Author(s):  
Guo Jun Wu Guo Jun Wu

[Cu(L)(AIP)·1.5H2O]n (1) [L= 3,5-di(benzimidazol-1-yl)pyridine, H2AIP= 5-aminoisophthalic acid] was prepared by the solvothermal reaction, which was characterized by single-crystal X–ray diffraction, infrared spectroscopy, and elemental analysis. 1 exhibits an infinite two dimensional [Cu(AIP)]n sheet parallel to (0 1 1) crystal plane. Furthermore, complex 1 displays good photocatalytic degradation of methyl blue (MB).


2018 ◽  
Vol 6 (2) ◽  
pp. 132-136
Author(s):  
Pramod Kumar Yadav

The title compound azobenzene-4, 4′-dicarbonyl chloride has been synthesized in distilled dichlomethane and characterized by elemental analysis (C, H, N), IR and NMR (1H & 13C) studies. The crystal and molecular structure was further confirmed using single crystal X-ray diffraction analysis. It was crystallized in triclinic crystal system with space group P-1. The centrosymmetrically related molecules held together via C–H---O secondary interaction result in molecular aggregation of the compound.  Int. J. Appl. Sci. Biotechnol. Vol 6(2): 132-136


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