ChemInform Abstract: Phosphole Complexes of Copper(I) Halides. Investigations of Structure and Bonding by X-Ray Crystallography, IR Spectroscopy, and CP/MAS 31P NMR Spectroscopy.

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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Gel-to-inverted hexagonal (Lβ-HII) phase transitions in phosphatidylethanolamines and fatty acid-phosphatidylcholine mixtures, demonstrated by 31P-NMR spectroscopy and X-ray diffraction

Biochimica et Biophysica Acta (BBA) - Biomembranes ◽

10.1016/0005-2736(82)90245-0 ◽

1982 ◽

Vol 690 (1) ◽

pp. 117-123 ◽

Cited By ~ 99

Author(s):

Derek Marsh ◽

John M. Seddon

Keyword(s):

Phase Transitions ◽

Fatty Acid ◽

Nmr Spectroscopy ◽

31P Nmr ◽

31P Nmr Spectroscopy ◽

X Ray Diffraction ◽

X Ray

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Synthesis, Spectroscopic Characterization, and Structure of closo-1,10-B10H8F22- and Related Fluorinated Derivatives of B10H102-

Collection of Czechoslovak Chemical Communications ◽

10.1135/cccc19971310 ◽

1997 ◽

Vol 62 (8) ◽

pp. 1310-1324 ◽

Cited By ~ 5

Author(s):

Sergei V. Ivanov ◽

Svetlana M. Ivanova ◽

Susie M. Miller ◽

Oren P. Anderson ◽

Nikolai T. Kuznetsov ◽

...

Keyword(s):

Nmr Spectroscopy ◽

Ir Spectroscopy ◽

Single Crystal ◽

Spectroscopic Characterization ◽

X Ray ◽

X Ray Crystallography ◽

Fluorinated Derivatives ◽

Derivatives Of

The treatment of salts of the B10H102- anion with the commercially available N-fluoro reagent 1-chloromethyl-4-fluoro-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate) (F-TEDA) resulted in the formation of fluorinated derivatives of this ten-vertex borane dianion. The effects of changing the solvent, temperature, and reagent stoichiometry were studied. The derivatives 1-B10H9F2-, 2-B10H9F2-, 1,2-B10H8F22-, 1,6-B10H8F22-, 1,10-B10H8F22-, and 1,2,10-B10H7F32- were examined by a combination of 11B and 19F NMR spectroscopy and by IR spectroscopy. The salt [Ph4P]2[1,10-B10H8F2] . 3 CH2Cl2 was structurally characterized by single-crystal X-ray crystallography: C51H48B10Cl6F2P2, monoclinic, C2/c, a = 13.8134(9), b = 19.141(1), c = 21.136(1) Å, β = 91.546(1)°, Z = 4, T = -100 °C, R = 0.077.

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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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Synthesis and X-ray Diffraction Study of thiosemicarbazone Palladacycles with dppm

Proceedings ◽

10.3390/proceedings2020062013 ◽

2021 ◽

Vol 62 (1) ◽

pp. 13

Author(s):

Marcos Rúa-Sueiro ◽

Paula Munin-Cruz ◽

Francisco Reigosa ◽

José M. Vila ◽

Juan M. Ortigueira

Keyword(s):

Nmr Spectroscopy ◽

31P Nmr ◽

Antimicrobial Agents ◽

Cross Coupling ◽

31P Nmr Spectroscopy ◽

Coupling Reactions ◽

X Ray Diffraction ◽

X Ray ◽

Cross Coupling Reactions ◽

Platinum Salt

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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