Hydration behaviour of POPC/C12-Bet mixtures investigated by sorption gravimetry, 31P NMR spectroscopy and X-ray diffraction

Cyclometallated compounds have been extensively studied, in particular those with palladium and platinum. This is because of their possible applications in medicinal chemistry, as anticancer or antimicrobial agents; in some cases, with similar results as cisplatin, carboplatin or oxaliplatin. What is also remarkable is their use as homogeneous catalysts, for example, in cross coupling reactions such as Suzuki–Miyaura or Mizoroki–Heck. Herein, we report the synthesis of different thiosemicarbazone ligands, which will be reacted with a palladium or platinum salt, to give the corresponding cyclometallated compounds; in addition, their reactivity with bis(diphenylphosphino)methane (dppm) will be studied. Characterization has been carried out by elemental analysis, IR spectroscopy, 1H and 31P NMR spectroscopy. Additionally, 1c has been studied by X-ray diffraction.

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Tetraphosphorus tetraselenide: crystalline and amorphous phases analysed by X-ray diffraction, Raman and magic angle spinning 31P NMR spectroscopy and differential scanning calorimetry

Journal of Non-Crystalline Solids ◽

10.1016/0022-3093(95)00093-3 ◽

1995 ◽

Vol 188 (1-2) ◽

pp. 93-97 ◽

Cited By ~ 1

Author(s):

Jonathan D. Sarfati ◽

Gary R. Burns ◽

Keith R. Morgan

Keyword(s):

Differential Scanning Calorimetry ◽

31P Nmr ◽

Magic Angle Spinning ◽

Magic Angle ◽

31P Nmr Spectroscopy ◽

X Ray Diffraction ◽

Scanning Calorimetry ◽

X Ray ◽

Amorphous Phases ◽

Angle Spinning

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Synthesis, Characterization, and Crystal Structures of [Cu(ca2en)(PPh3)(X)] (X = Cl, Br, I, NCS, N3) Complexes

Australian Journal of Chemistry ◽

10.1071/ch02113 ◽

2003 ◽

Vol 56 (4) ◽

pp. 323 ◽

Cited By ~ 26

Author(s):

Guido Kickelbick ◽

Mehdi Amirnasr ◽

Aliakbar D. Khalaji ◽

Saeed Dehghanpour

Keyword(s):

Infrared Spectroscopy ◽

Nmr Spectroscopy ◽

31P Nmr ◽

Mixed Ligand ◽

Bond Breaking ◽

31P Nmr Spectroscopy ◽

Distorted Tetrahedron ◽

Nmr Studies ◽

X Ray ◽

Elemental Analyses

Novel mixed-ligand copper(I) complexes, [Cu(ca2en)(PPh3)X] (ca2en = N,N′-bis(trans-cinnamaldehyde)-1,2-diaminoethane, X = Cl (1), Br (2), I (3), NCS (4), N3 (5)), have been synthesized and characterized by 1H and 31P NMR spectroscopy, infrared spectroscopy, and elemental analyses. The single crystal X-ray structures of complexes (1)–(5) have been determined. All five complexes reveal discrete monomeric structures in the crystal. The geometry around the copper atom is in each case a distorted tetrahedron, with the distortion most pronounced in (3). The NCS− and N3− are coordinated as terminal ligands and the NCS− ligand is N-bonded in (4). Dynamic 31P NMR studies show partial bond breaking in solution.

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Synthetic and Structural Study of peri-Substituted Phosphine-Arsines

Molecules ◽

10.3390/molecules26237222 ◽

2021 ◽

Vol 26 (23) ◽

pp. 7222

Author(s):

Brian A. Chalmers ◽

D. M. Upulani K. Somisara ◽

Brian A. Surgenor ◽

Kasun S. Athukorala Arachchige ◽

J. Derek Woollins ◽

...

Keyword(s):

Decomposition Product ◽

31P Nmr ◽

31P Nmr Spectroscopy ◽

Dispersion Forces ◽

State Structure ◽

X Ray Diffraction ◽

X Ray ◽

X Ray Crystallography ◽

Donor Acceptor ◽

Tertiary Arsine

A series of phosphorus-arsenic peri-substituted acenaphthene species have been isolated and fully characterised, including single crystal X-ray diffraction. Reactions of EBr3 (E = P, As) with iPr2PAcenapLi (Acenap = acenaphthene-5,6-diyl) afforded the thermally stable peri-substitution supported donor–acceptor complexes, iPr2PAcenapEBr23 and 4. Both complexes show a strong P→E dative interaction, as observed by X-ray crystallography and 31P NMR spectroscopy. DFT calculations indicated the unusual As∙∙∙As contact (3.50 Å) observed in the solid state structure of 4 results from dispersion forces rather than metallic interactions. Incorporation of the excess AsBr3 in the crystal structure of 3 promotes the formation of the ion separated species [iPr2PAcenapAsBr]+Br− 5. A decomposition product 6 containing the rare [As6Br8]2– heterocubane dianion was isolated and characterised crystallographically. The reaction between iPr2PAcenapLi and EtAsI2 afforded tertiary arsine (BrAcenap)2AsEt 7, which was subsequently lithiated and reacted with PhPCl2 and Ph2PCl to afford cyclic PhP(Acenap)2AsEt 8 and acyclic EtAs(AcenapPPh2)2 9.

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Third Generation Buchwald Precatalysts with XPhos and RuPhos: Multigram Scale Synthesis, Solvent-Dependent Isomerization of XPhos Pd G3 and Quality Control by 1H- and 31P-NMR Spectroscopy

Molecules ◽

10.3390/molecules26123507 ◽

2021 ◽

Vol 26 (12) ◽

pp. 3507

Author(s):

Svitlana O. Sotnik ◽

Artem M. Mishchenko ◽

Eduard B. Rusanov ◽

Andriy V. Kozytskiy ◽

Konstantin S. Gavrilenko ◽

...

Keyword(s):

Quality Control ◽

Nmr Spectra ◽

31P Nmr ◽

Impurity Content ◽

31P Nmr Spectroscopy ◽

Third Generation ◽

X Ray Diffraction ◽

Simple Method ◽

Spectra Analysis ◽

X Ray

The third generation Buchwald precatalysts Pd(ABP)(Phos)(OMs) (also known as Phos Pd G3)) with XPhos and RuPhos were prepared in multigram scale by a modified procedure (ABP = fragment of C-deprotonated 2-aminobiphenyl, XPhos = 2-dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl, RuPhos = 2-dicyclohexylphosphino-2′,6′-diisopropoxybiphenyl, OMs− = CH3SO3−). The 1H- and 31P-NMR spectra of the title complexes and some impurities, measured by various 1D and 2D techniques, were analyzed in detail. The solvent-dependent isomerization of Pd(ABP)(XPhos)(OMs) was studied by NMR, and the X-ray structures of two isomers were determined. The impurities in precatalysts, such as Pd(ABP)(HABP)(OMs) (HABP—neutral 2-aminobiphenyl coordinated to Pd2+ in N-monodentate mode) and PdCl2(XPhos)2, were identified and characterized by single crystal X-ray diffraction. A simple method for the quick quality control (QC) of the precatalysts, suitable for routine use, was proposed. The method was based on the assessment of the impurity content on the basis of the 1H-NMR spectra analysis.

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Substituent effects in phosphine ligands

Suid-Afrikaanse Tydskrif vir Natuurwetenskap en Tegnologie ◽

10.4102/satnt.v30i1.267 ◽

2011 ◽

Vol 30 (1) ◽

Author(s):

C. Alicia Renison ◽

D. Bradley G. Williams ◽

Alfred J. Muller

Keyword(s):

Nmr Spectroscopy ◽

High Resolution ◽

Molecular Modelling ◽

31P Nmr ◽

Substituent Effects ◽

Phosphine Ligands ◽

31P Nmr Spectroscopy ◽

Electronic Effects ◽

X Ray ◽

X Ray Crystallography

The study illustrates the use of the P-atom to evaluate steric and electronic effects in P-containing organic compounds. The work involves the synthesis of substituted triarylphosphines and their corresponding Rh Vaska complexes. High resolution X-ray crystallography, molecular modelling, 31P NMR spectroscopy and IR will be used to quantify substituent effects.

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