Substituted 1,2-diaza-7-oxaspiro[4,4]nonen-6-ones; Preparation, NMR spectra, and crystal structure

1991 ◽  
Vol 56 (5) ◽  
pp. 973-983 ◽  
Author(s):  
Jaroslav Jonas ◽  
Tadeusz Głowiak ◽  
Zdirad Žák ◽  
Petr Trška ◽  
Ctibor Mazal
Keyword(s):  
Crystal Structure ◽  
Nmr Spectra

Diazomethane adds to substituted 3-methylene-2-(3H)-dihydrofuranones (Ia-Ii) to give the corresponding title dihydropyrazolospirodihydrofuranones (IIa-IIf, IIi,andIIj) or (IIIa, IIIg, and IIIh). NMR spectra of the adducts are discussed in some detail and the crystal structure has been solved for (4R, 5S)-5-benzoyloxy-1,2-diaza-7-oxaspiro[4.4]non-1-en-6-one (IIa).

scholarly journals Heteroleptic [Cu(P^P)(N^N)][PF6] Complexes: Effects of Isomer Switching from 2,2′-biquinoline to 1,1′-biisoquinoline

Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 185
Author(s):  
Nina Arnosti ◽  
Marco Meyer ◽  
Alessandro Prescimone ◽  
Edwin C. Constable ◽  
Catherine E. Housecroft
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Nmr Spectra ◽  
Phenyl Ether ◽  
Quantum Yields ◽  
Dynamic Processes ◽  
Electrochemical Behaviors ◽  
Ambient Temperatures ◽  
Π Stacking

The preparation and characterization of [Cu(POP)(biq)][PF6] and [Cu(xantphos)(biq)][PF6] are reported (biq = 1,1′-biisoquinoline, POP = bis(2-(diphenylphosphanyl)phenyl)ether, and xantphos = (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphane). The single crystal structure of [Cu(POP)(biq)][PF6] 0.5Et2O was determined and compared to that in three salts of [Cu(POP)(bq)]+ in which bq = 2,2′-biquinoline. The P–C–P angle is 114.456(19)o in [Cu(POP)(biq)]+ compared to a range of 118.29(3)–119.60(3)o [Cu(POP)(bq)]+. There is a change from an intra-POP PPh2-phenyl/(C6H4)2O-arene π-stacking in [Cu(POP)(biq)]+ to a π-stacking contact between the POP and bq ligands in [Cu(POP)(bq)]+. In solution and at ambient temperatures, the [Cu(POP)(biq)][PF6]+ and [Cu(xantphos)(biq)]+ cations undergo several concurrent dynamic processes, as evidenced in their multinuclear NMR spectra. The photophysical and electrochemical behaviors of the heteroleptic copper (I) complexes were investigated, and the effects of changing from bq to biq are described. Short Cu···O distances within the [Cu(POP)(biq)]+ and [Cu(xantphos)(biq)]+ cations may contribute to their very low photoluminescent quantum yields.

Nuclear magnetic resonance studies on the anions [M(SnCl3)5Cl]4− (M = Ru, Os) and [Ru(SnCl3)5(MeCN)]3−: the X-ray crystal structure of [N(C2H5)4]4[Ru(SnCl3)5Cl]

1982 ◽  
Vol 60 (11) ◽  
pp. 1304-1316 ◽  
Author(s):  
Louis J. Farrugia ◽  
Brian R. James ◽  
Claude R. Lassigne ◽  
Edward J. Wells
Keyword(s):  
Crystal Structure ◽  
Nuclear Magnetic Resonance ◽  
Nmr Spectroscopy ◽  
Nmr Spectra ◽  
Octahedral Geometry ◽  
Coupling Constants ◽  
Order Effects ◽  
Magnetic Resonance Studies ◽  
X Ray ◽  
Crystallographic Study

The octahedral anions [M(SnCl3)5Cl]4− (M = Ru, Os) have been fully characterized by 119Sn FT nmr spectroscopy. For M = Ru, 117Sn and 115Sn nmr spectra were also recorded, and an X-ray crystallographic study was carried out on the tetraethylammonium salt, isolated as a disolvate from acetonitrile. The Ru—Sn bond lengths indicate some degree of dπ–dπ interactions. The slight distortions from octahedral geometry are discussed in connection with the packing of the chlorine atoms. The Sn nmr spectra reveal the first observed coupling to a 99Ru nucleus (I = 5/2, 12.7% natural abundance), very large 2J(119Sn—117Sn) coupling constants, and the first observed second-order effects on a heteronuclear system. The octahedral anion [Ru(SnCl3)5(MeCN)]3− was also synthesized as the tetraethylammonium salt and characterized spectroscopically.

Polycarboxylate crown ethers from meso-tartaric acid

1991 ◽  
Vol 69 (1) ◽  
pp. 12-19 ◽  
Author(s):  
Frank R. Fronczek ◽  
Richard D. Gandour ◽  
Thomas M. Fyles ◽  
Philippa J. Hocking ◽  
Susan J. McDermid ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Crown Ether ◽  
Tartaric Acid ◽  
Crown Ethers ◽  
Nmr Spectra ◽  
Product Distribution ◽  
Complexing Agents ◽  
Triclinic Space Group ◽  
The Stability ◽  
Ether Synthesis

The synthesis of crown ethers derived from meso-tartaric acid was investigated. The sodium salt of the bis(dimethylamide) of meso-tartaric acid reacted with diethylene glycol ditosylate to give a mixture of 18-crown-6 tetraamide and 27-crown-9 hexaamide crown ethers. The 2R,3S,11S,12R 18-crown-6 isomer crystallized in triclinic space group [Formula: see text] (a = 7.557(2), b = 8.866(2), c = 10.4133(13) Å, α = 94.13(2), β = 95.86(2), γ = 99.26(2)°, R = 0.040 for 2090 observed of 3129 unique reflections). The structures of the remaining products were then assigned from the NMR spectra. The solution conformations of the amide crown ethers were examined by NMR, and provide a rationale for the product distribution obtained. One of the 18-crown-6 isomers and a mixture of the two 27-crown-9 isomers were hydrolyzed to the respective crown ether carboxylic acids, and the stability constants for complexation of cations were determined by potentiometric titration. The meso tetra- and hexacarboxylates are remarkably nonselective and inefficient cation complexing agents, compared to related crown ethers from R,R-(+)-tartaric acid, due to the unfavorable conformational control exerted by the tartaro units. Key words: crown ether synthesis, complexation, crown ether conformation, meso-tartaric acid, crystal structure.

Über Antimon-haltige Heterocyclen, V Antimon(III)-dithiolate mit verbrückten 5-und 8-Ringen/On Heterocyclic Systems Containing Antimony, V Antimony(III) Dithiolates with Bridged 5-and 8 -Membered Rings

1986 ◽  
Vol 41 (11) ◽  
pp. 1455-1460 ◽  
Author(s):  
Harald M. Hoffmann ◽  
Martin Dräger
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Nmr Spectra ◽  
Crystal Structure Analysis ◽  
Coordination Polyhedra ◽  
Starting Point ◽  
C Nmr

Abstract For diamony(III)-trisdithiolates two constitutions (bicyclic B or two bridged monocycles C) are possible. Two synthetical paths to three examples Sb2(XS2)3 with X = CH2CH2 (1), CH2CH2- O - CH2CH2 (2), CH2CH2- S - CH2CH2 (3) are reported. 13C NMR spectra in CDCl3 solution show the constitution C for 2 and 3, and a possible equilibrium C ⇌ 4:1) for 1. This corresponds to the result of a crystal structure analysis (R = 0.027). The constitution C found in solid 1 exhibits expanded coordination polyhedra around the two antimony atoms which indicate a starting point for rearrangement into the constitution B. The two bridged 5-membered rings have different conformations: envelope and half-chair.

[4 + 2]-Cyclodimer of Sabinone: Formation, Crystal Structure, and NMR Spectra.

ChemInform ◽  
2003 ◽  
Vol 34 (52) ◽  
Author(s):  
E. M. Suleimenov ◽  
V. A. Raldugin ◽  
M. M. Shakirov ◽  
I. Yu. Bagryanskaya ◽  
Yu. V. Gatilov ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectra

The Effect of Hydrostatic Pressure on Crystal and Orbital Structures of LaMnO3 and LaMn0.5Ga0.5O3

2010 ◽  
Vol 168-169 ◽  
pp. 441-444 ◽  
Author(s):  
Liudmila E. Gonchar ◽  
Anatoliy E. Nikiforov ◽  
Julia V. Leskova ◽  
Anton A. Firsin ◽  
D.P. Kozlenko
Keyword(s):  
Crystal Structure ◽  
Hydrostatic Pressure ◽  
Nmr Spectra ◽  
Theoretical Study ◽  
Magnetic Interactions ◽  
Ga Doping ◽  
Effect Of Hydrostatic Pressure

The crystal structure of manganite under pressure is investigated. The influence of external hydrostatical pressure is studied. The theoretical study of magnetic interactions and NMR spectra under pressure is carried out. The influence of Ga-doping is discussed.

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