A twist on Hellwinkel’s salt, [P(2,2′-biphenyl)2]+[P(2,2′-biphenyl)3]–

2018 ◽  
Vol 96 (6) ◽  
pp. 526-533 ◽  
Author(s):  
Khatera Hazin ◽  
Derek P. Gates
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Spiro Compound ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Isolation And Characterization

Treating PCl5 with C12H8Li2, generated from either C12H10, C12H8Br2, or C12H8I2, affords three products in different ratios depending on the source of the lithiated biphenyl. Hellwinkel’s salt [P(C12H8)2][P(C12H8)3] ([1][2]) and another product [P(C12H8)(C24H16)][P(C12H8)3] ([1′][2]) were obtained by reacting PCl5 with 2,2′-dilithiobiphenyl [Route A: 2.5 equiv.; obtained from biphenyl, n-BuLi, and TMEDA; Route B: 3.0 equiv.; obtained from 2,2′-diiodobiphenyl and n-BuLi; Route C: 4.0 equiv.; obtained from 2,2′-dibromobiphenyl and n-BuLi]. The synthesis, isolation, and characterization of the chiral spiro-compound [1′][2] and the characterization of the pentavalent phosphorane [P(C12H8)2(C12H9)] (3) are reported. The complex [1′][2] was characterized by 31P{1H} NMR spectroscopy, X-ray crystallography, and mass spectrometry. The pentavalent compound (3) was characterized by 31P{1H} NMR spectroscopy and X-ray crystallography.

Preparation, Crystal Structure and Spectroscopic Characterization of [Ga(OH)(SO4)(terpy)(H2O)] · H2O (terpy=2,2’:6’,2-Terpyridine): The First Characterized Gallium(III) Sulfato Complex

2004 ◽  
Vol 59 (3) ◽  
pp. 291-297 ◽  
Author(s):  
Andreas Sofetis ◽  
Giannis S. Papaefstathiou ◽  
Aris Terzis ◽  
Catherine P. Raptopoulou ◽  
Theodoros F. Zafiropoulos
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Good Yield ◽  
Spectroscopic Data ◽  
Spectroscopic Characterization ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr

The reaction of Ga2(SO4)3·18H2O and excess 2,2′:6′,2″-terpyridine (terpy) in MeOH / H2O leads to [Ga(OH)(SO4)(terpy)(H2O)]·H2O (1·H2O] in good yield. The structure of the complex has been determined by single-crystal X-ray crystallography. The GaIII atom in 1·H2O is 6-coordinate and ligation is provided by one terdentate terpy molecule, one monodentate sulfate, one terminal hydroxide and one terminal H2O molecule; the coodination polyhedron about the metal is described as a distorted octahedron. There is an extensive hydrogen-bonding network in the crystal structure which generates corrugated layers parallel to bc. The new complex was characterized by IR and 1H NMR spectroscopy. The spectroscopic data are discussed in terms of the nature of bonding

Structural determination and characterization of copper and zinc bis-glycinates with X-ray crystallography and mass spectrometry

2010 ◽  
Vol 63 (19) ◽  
pp. 3335-3347 ◽  
Author(s):  
Sanjit Konar ◽  
Kevin Gagnon ◽  
Abraham Clearfield ◽  
Charles Thompson ◽  
Jennifer Hartle ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Structural Determination ◽  
X Ray ◽  
X Ray Crystallography ◽  
Copper And Zinc

[Zn(phen)2(CX3COO)]+, X = H orCl; Influence of X on the Coordination Mode of the Carboxylate Group (phen = 1,10-Phenanthroline)

2005 ◽  
Vol 60 (10) ◽  
pp. 1049-1053 ◽  
Author(s):  
Zeanab Talaei ◽  
Ali Morsali ◽  
Ali R. Mahjoub
Keyword(s):  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Coordination Mode ◽  
Bidentate Ligand ◽  
Carboxylate Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Coordinate Geometry ◽  
C Nmr

Two new ZnII(phen)2 complexes with trichloroacetate and acetate anions, [Zn(phen)2(CCl3COO)- (H2O)](ClO4) and [Zn(phen)2(CH3COO)](ClO4), have been synthesized and characterized by elemental analysis, IR, 1H NMR, 13C NMR spectroscopy. The single crystal X-ray data of these compounds show the Zn atoms to have six-coordinate geometry. From IR spectra and X-ray crystallography it is established that the coordination of the COO− group is different for trichloroacetate and acetate. The former acts as a monodentate whereas the latter acts as a bidentate ligand.

Synthesis and crystal structures of three novel benzimidazole/benzoindolizine hybrids

2016 ◽  
Vol 71 (3) ◽  
pp. 231-239 ◽  
Author(s):  
Roumaissa Belguedj ◽  
Sofiane Bouacida ◽  
Hocine Merazig ◽  
Ali Belfaitah ◽  
Aissa Chibani ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Dipolar Cycloaddition ◽  
Dimethyl Acetylenedicarboxylate ◽  
X Ray ◽  
X Ray Crystallography ◽  
Dimethyl Maleate

AbstractThree benzoindolizine derivatives, 1, 2, and 3, were obtained via 1,3-dipolar cycloaddition. The reaction of 1-(2′-benzimidazolylmethyl)isoquinolinium ylides with dimethyl acetylenedicarboxylate gave a mixture of pyrrolo[2,1-a]isoquinoline-1,2-dicarboxylate (1) and 1,10b-dihydropyrrolo[2,1-a]isoquinoline-1,2-dicarboxylate (2) derivatives containing a benzimidazole moiety. The reaction of this isoquinolinium N-ylide with dimethyl maleate gave an unexpected 2,3-dihydropyrrolo[2,1-a]isoquinoline-1,2-dicarboxylate (3). The structures of all reported compounds have been examined by X-ray crystallography, mass spectrometry, and NMR spectroscopy.

scholarly journals Synthesis and characterization of a new bis-NHC palladium complex and its catalytic activity in the Mizoroki–Heck reaction

2020 ◽  
Vol 44 (11-12) ◽  
pp. 684-688
Author(s):  
Can Feng ◽  
Cheng-xin Liu ◽  
Yu-fang Wang ◽  
Jin Cui ◽  
Ming-jie Zhang
Keyword(s):  
Palladium Complex ◽  
Coupling Reaction ◽  
Aryl Halides ◽  
Heck Coupling ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Excellent Stability ◽  
C Nmr

A new bis- N-heterocyclic carbene palladium complex, (C13H9N2F2)2PdCl2, is synthesized by a three-step reaction and characterized by 1H NMR and 13C NMR spectroscopy as well as by X-ray crystallography. This new bis- N-heterocyclic carbene palladium complex has excellent stability and is capable of efficiently catalyzing the Mizoroki–Heck coupling reaction of aryl halides with acrylates.

Nine- and Eight-Vertex Polyhedral Dicarbaborane Chemistry: New arachno and hypho Dicarbaboranes from arachno-4,5-C2B7H13: Isolation and Characterization of the [arachno-4,5-C2B7H12]- and [hypho-7,8-C2B6H13]- Anions, and of the Neutral Ligand Derivatives exo-6-(MeNC)-arachno-4,5-C2B7H11 and exo-5-L-hypho-4,9-C2B7H13 (L = NMe3 and NEt3)

1994 ◽  
Vol 59 (7) ◽  
pp. 1584-1595 ◽  
Author(s):  
Tomáš Jelínek ◽  
Josef Holub ◽  
Bohumil Štíbr ◽  
Xavier L. R. Fontaine ◽  
John D. Kennedy
Keyword(s):  
Nmr Spectroscopy ◽  
Selective Removal ◽  
High Yield ◽  
Two Dimensional ◽  
Neutral Ligand ◽  
Tertiary Amines ◽  
Proton Sponge ◽  
H Nmr ◽  
Isolation And Characterization

Deprotonation of neutral arachno-4,5-C2B7H13 (1) either with 1, 8-(NMe2)2C10H6 (proton sponge, PS) or with a mixture of aqueous K2CO3 and [NMe4]Cl leads to the isolation in high yield of the [arachno-4,5-C2B7H12]- anion (2). Isostructural with this anion is the ligand derivative exo-6-(MeNC)-arachno-4,5-C2B7H11 (3), which is prepared in 20% yield from the reaction between arachno-4,5-C2B7H13 and MeNC in dichloromethane. Under comparable conditions compound 1 with tertiary amines gives the first representatives of the nine-vertex hypho family of dicarbaboranes, the ligand derivatives exo-5-(NR3)-hypho-4,9-C2B7H13 (4a and 4b, where R = Me and Et, respectively) in moderate yields (20 - 55%), whereas the reaction between 1 and aqueous NaCN results in the selective removal of one boron vertex to yield the eight-vertex [hypho-7,8-C2B6H13]- anion (5) in 61% yield. All compounds isolated were characterized by 11B and 1H NMR spectroscopy, with two-dimensional and selective decoupling techniques giving unambiguous assignments.

Synthesis and Characterization of Tetrakis(pentafluoroethyl)germane

Synthesis ◽  
2017 ◽  
Vol 49 (11) ◽  
pp. 2389-2393 ◽  
Author(s):  
Stefanie Pelzer ◽  
Beate Neumann ◽  
Hans-Georg Stammler ◽  
Nikolai Ignat’ev ◽  
Reint Eujen ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Diffraction Analysis ◽  
Spectroscopic Characterization ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Comprehensive Characterization

This paper describes the synthesis and comprehensive characterization of tetrakis(pentafluoroethyl)germane. In addition to a complete NMR spectroscopic characterization, including the rarely used 73Ge NMR spectroscopy, Ge(C2F5)4 was studied by IR spectroscopy, mass spectrometry as well as X-ray diffraction analysis. A 73Ge NMR investigation as well as an X-ray diffraction study of the related germane Ge(CF3)4 are also included.

1,2-Bis(1-aryl-3-alkyltriazen-3-yl)ethanes and related compounds

1998 ◽  
Vol 76 (1) ◽  
pp. 125-135 ◽  
Author(s):  
Donald L Hooper ◽  
Ian R Pottie ◽  
Marc Vacheresse ◽  
Keith Vaughan
Keyword(s):  
Nmr Spectroscopy ◽  
Line Broadening ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Ir And Nmr Spectroscopy ◽  
Diazonium Coupling ◽  
Significant Line ◽  
Related Compounds ◽  
C Nmr

A series of novel bistriazenes, the 1,2-bis(1-aryl-3-methyltriazen-3-yl)ethanes, Ar-N T N-NMe-CH2CH2-NMe-N T N-Ar, have been synthesized by diazonium coupling with N,N'-dimethylethylenediamine. These bistriazenes are stable crystalline compounds and have been unequivocally characterized by IR and NMR spectroscopy (1H and 13C), and elemental analysis. The structures of two compounds in the series have been confirmed by X-ray crystallography. The 1H NMR spectra show significant line broadening of the N-methyl resonances arising from the restricted rotation around the N2-N3 bond of the triazene units. The presence of strongly electron-withdrawing groups on the aryl ring restricts the rotation to the point where the N-methyl signals of the rotamers are distinct even at room temperature; four resonances of the N-methyl signal are clearly evident and these can be assigned to the anti-anti, syn-syn, and syn-anti conformations of the bistriazene. Diazonium coupling with N,N'-diethylethylenediamine affords the N,N'-diethyl homologues of the bistriazenes, which have been similarly characterized. As model compounds to assist in spectroscopic analysis, a series of related triazenes, the 1-(1-aryl-3-methyltriazen-3-yl)-N,N-dimethyl-2-ethanamines, were prepared by diazonium coupling with N,N,N'-trimethylethylenediamine. These dialkyltriazenes exist mainly as oils, but characterization was achieved by IR, 1H NMR, and 13C NMR spectroscopy, also showing the presence of two rotamers in solution when strongly electron-withdrawing substituents are bonded to the aryl moiety.Key words: triazene, bistriazene, diazonium, ethylenediamine, molecular dynamics, NMR.

Sign in / Sign up

Export Citation Format

Share Document