Synthese und Charakterisierung von Halogen-phosphor(III)- Derivaten des 8-Hydroxychinolins. Röntgenstrukturanalyse von 8-[Phenyl(chloro)-phosphito]-chinolin/ Synthesis and Characterization of Halogen-phosphorus(III) Derivatives of 8-Hydroxyquinoline. X -Ray Structure Analysis of 8-[Phenyl(chloro)phosphito]-quinoline

1993 ◽  
Vol 48 (1) ◽  
pp. 85-89 ◽  
Author(s):  
Lin Yang ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Study ◽  
Elemental Analysis ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Compounds ◽  
Derivatives Of

The reaction of 8 -trimethylsiloxyquinoline, 2 with PCl3, PhPCl2, and PhPF2 has furnished the corresponding 8 -quinolyl halophosphite derivatives, 3-5 . The synthesis of two metal complexes, 8 and 9, of 4 with Au(I) and Pt(II) is described. The new compounds were characterized by elemental analysis and by 1H and 31P NMR spectroscopy. A single crystal X-ray diffraction study of 4 has been conducted; a short intramolecular P ··· N contact (230.9 pm) and a long P-Cl bond (218.7 pm) were observed.

Synthesis and Characterization of the nido-Platinaborane 7,7-(PPh3)2-7-PtB10H11-11-OC(O)Me

2011 ◽  
Vol 66 (4) ◽  
pp. 387-391
Author(s):  
Jinling Miao ◽  
Yong Nie ◽  
Haiyan Chen ◽  
Daqi Wang ◽  
Markus Enders ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Chain Structure ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

The reaction of closo-B10H102− with PtCl2(PPh3)2 in the presence of MeCOSH afforded the title platinaborane nido-7,7-(PPh3)2-7-PtB10H11-11-OC(O)Me (1), which has been characterized by IR and NMR spectroscopy, MS, elemental analysis, and single-crystal X-ray diffraction. In contrast to the known products having exo-polyhedral Pt-S-C-O-B ring(s) from the same reaction with Ph- COSH, compound 1 has a B-acetoxy group on the open PtB4 face of the nido-PtB10 cluster. The structure of 1 features both intramolecular/intermolecular C-H· · ·O hydrogen bonds and intramolecular C-H· · ·H-B dihydrogen bonds, which link the molecules into a 1-D chain structure.

The Reaction of Cp*ReH6, Cp* = C5Me5, with Monoborane to Yield a Novel Rhenaborane. Synthesis and Characterization of arachno-Cp*ReH3B3H8

2002 ◽  
Vol 67 (6) ◽  
pp. 808-812 ◽  
Author(s):  
Sundargopal Ghosh ◽  
Alicia M. Beatty ◽  
Thomas P. Fehlner
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Diffraction Study ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray

The rhenaborane Cp*ReH3B3H8, which is generated by the reaction of Cp*ReH6 with BH3·THF, has been characterized spectroscopically in solution and by a single-crystal X-ray diffraction study in the solid state as a hydrogen-rich arachno-metallatetraborane.

N-alkyl-2-(1,2-diferrocenylvinyl)-4,5-dihydrooxazolinium salts, multi-component synthesis and breaking of their heterocyclic systems

2016 ◽  
Vol 88 (12) ◽  
pp. 1129-1142 ◽  
Author(s):  
Jessica J. Sánchez García ◽  
Marcos Flores-Alamo ◽  
Mark E. Martínez Klimov ◽  
Elena I. Klimova
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Alkyl Iodides ◽  
New Compounds ◽  
C Nmr

AbstractA new multicomponent method for the synthesis of N-alkyl-2-(Z-1,2-diferrocenylvinyl)-4,5-dihydrooxazolinium salts 3a–f, 5-(N-alkyl-2′,3′-diferrocenyl-acryloylamido)-3-aza-3-alkylpentanols 4a–d, (E)-N-alkyl-N-(2-morpholinoethyl)-2,3-diferrocenylacrylamides 9a,b,e,f and (E)-N-alkyl-N-(2-piperidinoethyl)-2,3-diferrocenylacrylamides 10a,c from reactions of 2,3-diferrocenylcyclopropenone 1 with bis-1,4-N,O-nucleophiles in the presence of triethyloxonium tetrafluoroborate, alkyl iodides, morpholine, piperidine and Et3N is described. The characterization of the new compounds was done by IR, 1H- and 13C-NMR spectroscopy, mass-spectrometry, elemental analysis and X-ray diffraction studies.

scholarly journals Half-Sandwich Arene-Osmium(II) Complexes with Phosphinite Ligands

Molbank ◽  
10.3390/m1110 ◽  
2020 ◽  
Vol 2020 (1) ◽  
pp. M1110 ◽  
Author(s):  
Rebeca González-Fernández ◽  
Javier Borge ◽  
Pascale Crochet ◽  
Victorio Cadierno
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Study ◽  
Elemental Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
Intramolecular Exchange ◽  
Multinuclear Nmr Spectroscopy ◽  
Half Sandwich

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.

Synthesis and Characterization of 3-Chloropropyl-substituted o- Carboranes: Crystal Structures of 1,2-(1,3-Propanediyl)-o-carborane, 1-(3-Chloropropyl)-o-carborane and 1,2-Bis(3-chloropropyl)-ocarborane

2013 ◽  
Vol 68 (7) ◽  
pp. 804-810 ◽  
Author(s):  
Deqian Bian ◽  
Yong Nie ◽  
Jinling Miao ◽  
Zhenwei Zhang ◽  
Ping Lu
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Main Product ◽  
Total Yield ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

The reactions of the lithio-o-carborane Li2C2B10H10 with ClCH2CH2CH2Br were studied under various conditions. While the main product is the known exo-polyhedrally cyclized 1,2- (1,3-propanediyl)-o-carborane (2), the expected 3-chloropropyl-substituted carborane products 1- (ClCH2CH2CH2)C2B10H11 (3) and 1,2-(ClCH2CH2CH2)2C2B10H10 (4) can be obtained in a total yield of 22%. In the presence of CuCl, the same reaction proceeded rather slowly and gave compound 3and bis(o-carborane) (5) in small yields, with the recovery of the starting o-C2B10H12. Compounds 2- 4were characterized by means of IR and NMR spectroscopy and mass spectrometry, as well as by single-crystal X-ray diffraction.

An Intramolecular Boron Nitrogen Lewis Acid Base Pair on a Rigid Naphthyl Backbone

2012 ◽  
Vol 67 (6) ◽  
pp. 589-593 ◽  
Author(s):  
Daniel Winkelhaus ◽  
Beate Neumann ◽  
Norbert W. Mitzel
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Lewis Acid ◽  
Elemental Analysis ◽  
Base Pair ◽  
Ring System ◽  
X Ray Diffraction ◽  
Acid Base ◽  
X Ray ◽  
Boron Nitrogen

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.

Synthesis and Characterization of Tetraphenylphosphonium Tetraazidoborate

2002 ◽  
Vol 57 (6) ◽  
pp. 621-624 ◽  
Author(s):  
Wolfgang Fraenk ◽  
Heinrich Nöth ◽  
Thomas M. Klapötke ◽  
Max Suter
Keyword(s):  
Single Crystal ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray

AbstractTetraphenylphosphonium tetraazidoborate, [P(C6H5)4][B(N3)4], was obtained from B(N3)3 - in situ prepared from BH3 · O(C2H5)2 and HN3 - and [P(C6H5)4][N3]. Recrystallization from an acetonitrile / hexane mixture yielded colorless crystals in 60% yield. The molecular structurewas determined by single crystal X-ray diffraction and the [B(N3)4]- anionwas shown to possess S4 symmetry.

Synthesis and Characterization of Three Novel Nitrogen-containing Macrolides

2011 ◽  
Vol 66 (9) ◽  
pp. 930-934
Author(s):  
Xin Leng ◽  
Bingqin Yang ◽  
Yuanyuan Liu ◽  
Yi Xie ◽  
Jie Tong
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
1H Nmr Spectroscopy ◽  
Mass Spectra ◽  
Synthesis And Characterization ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Preparation Methods ◽  
X Ray

Three novel nitrogen-containing macrolides have been synthesized by esterification. All of them have been characterized by infrared (IR), elemental analysis, mass spectra (MS), and 1H NMR spectroscopy, and their crystal structures were determined by single-crystal X-ray diffraction. The preparation methods and the intermolecular associations based on C-H・・・O hydrogen bonds and π- π stacking interactions are discussed.

scholarly journals Synthesis and Characterization of New Diiron and Diruthenium μ-Aminocarbyne Complexes Containing Terminal S-, P- and C-Ligands

2007 ◽  
Vol 62 (3) ◽  
pp. 427-438 ◽  
Author(s):  
Vincenzo G. Albano ◽  
Luigi Busetto ◽  
Fabio Marchetti ◽  
Magda Monari ◽  
Stefano Zacchini ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Diffraction Study ◽  
Coordination Mode ◽  
Bond Cleavage ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dithiocarbamate Ligand ◽  
High Yields

The diiron aminocarbyne complexes [Fe2{μ-CN(Me)(R)}(μ-CO)(CO)(NCMe)(Cp)2][SO3CF3] (R = Xy1, 1a; R = Me, 1b; R = CH2Ph, 1c; Xy1 = 2,6-Me2C6H3) undergo replacement of the coordinated nitrile by halides, diethyldithiocarbamate, and dicyanomethanide to give [Fe2{μ-CN(Me) (R)}(μ-CO)(CO)(X)(Cp)2] complexes (R = Me, X = Br, 4a; R = Me, X = I, 4b; R = CH2Ph, X = Cl, 4c; R = CH2Ph, X = Br, 4d; R = CH2Ph, X = I, 4e; R = Xy1, X = SC(S)NEt2, 5a; R = Me, X = SC(S)NEt2, 5b; R = Xy1, X = CH(CN)2, 7), in good yields. The molecular structure of 5a shows an unusual η1 coordination mode of the dithiocarbamate ligand. Similarly, treatment of [M2{μ-CN(Me) (R)}(μ-CO)(CO)(NCMe)(Cp)2][SO3CF3] (M = Fe, R = Xy1, 1a; M = Fe, R = Me, 1b; M = Ru, R = Xy1, 2a; M = Ru, R = Me, 2b) with a series of phosphanes generates the cationic complexes [M2{μ- CN(Me)(R)}(μ-CO)(CO)(P)(Cp)2][SO3CF3] (M = Fe, R = Xy1, P = PPh2H, 6a; M = Fe, R = Xy1, P = PPh3, 6b; M = Fe, R = Xy1, P = PMe3, 6c; M = Fe, R = Me, P = PMe2Ph, 6d; M = Fe, R = Me, P = PPh3, 6e; M = Fe, R = Me, P = PMePh2, 6f; M = Ru, R = Xy1, P = PPh2H, 6g; M = Ru, R = Me, P = PPh2H, 6h), in high yields. The molecular structure of 6a has been elucidated by an X-ray diffraction study. The reactions of [Fe2{μ-CN(Me)(Xyl)}(μ-CO)(CO)(NCR′)(Cp)2][SO3CF3] [R′ = Me, 1a; R′ = tBu, 3] with PhLi and PPh2Li yield [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(Ph)(Cp)2] (8) and [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(PPh2)(Cp)2] (9), respectively. The molecular structure of 8 has been ascertained by X-ray diffraction. Conversely, the reaction of 1a with MeLi generates the aminoalkylidene compound [Fe2{C(Me)N(Me)(Xy1)}(μ-CO)2(CO)(Cp)2] (10).Finally, the acetone complex [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(OCMe2)(Cp)2][SO3CF3] (12) reacts with lithium acetylides to give complexes [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(C≡CR)(Cp)2] (R = p-C6H4Me, 11a; R = Ph, 11b; R = SiMe3, 11c), in high yields. Filtration through alumina of a solution of 11a in CH2Cl2 results in hydration of the acetylide group and C-Si bond cleavage, affording [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO){C(O)Me}(Cp)2] (12).

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