A 113Cd nuclear magnetic resonance study of some complexes of cadmium with phosphine oxides, sulfides, and selenides

1981 ◽  
Vol 59 (23) ◽  
pp. 3221-3225 ◽  
Author(s):  
Philip A. W. Dean
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Phosphine Oxide ◽  
Nmr Spectra ◽  
Nuclear Magnetic Resonance Study ◽  
Phosphine Oxides ◽  
Cd Spectra ◽  
Magnetic Resonance Study ◽  
Slow Exchange ◽  
Reduced Temperature

113Cd(AsF6)2 has been synthesized from 113CdO by treatment in SO2 with PF5 then AsF5. From the 113Cd-enriched salt have been prepared [Cd(EPR3)4]2+ (E = O, R = C6H11; E = S or Se, R = Ph), [Cd(SP(C6H11)3)x(SeP(C6H11)n−x]2+ (n = 4, x = 0–4; n = 3, x = 0–3), [Cd(EP(o-C6H4Me)3)n]2+ (E = S, n = 4 or 2; E = Se, n = 3 or 2), [Cd(Ph2P(O)(CH2)nP(O)Ph2)3]2+ (n = 1 or 2), and [Cd(Ph2P(O)((CH2)2P(O)Ph2)2)2]2+ in liquid SO2. The reduced temperature slow exchange 31P and 113Cd nmr spectra have been measured and are discussed. The 31P nmr are as expected from previous work on complexes containing 113Cd at natural abundance except that several values of 2J(113Cd—O—31P) have been measured. From the 113Cd spectra the most important shielding sequences observed are [Formula: see text] for [Cd(EP(C6H11)3)4]2+, δ2:1 < δ3:1 < δ4:1 for [Cd(EPR3)n]2+ (E = S or Se, n = 1–4, constant R), and [Formula: see text] for the various phosphine oxide complexes studied.The synthesis of SO2-insoluble Cd(SbF6)2•3(OP(C6H11)3) is reported.

A 19F nuclear magnetic resonance study of the conjugate Brönsted-Lewis superacid HSO3F-SbF5. Part 1

1999 ◽  
Vol 77 (11) ◽  
pp. 1869-1886 ◽  
Author(s):  
Dingliang Zhang ◽  
Markus Heubes ◽  
Gerhard Hägele ◽  
Friedhelm Aubke
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Nmr Spectra ◽  
Nuclear Magnetic Resonance Study ◽  
Magnetic Resonance Study ◽  
Formation Reaction ◽  
H Nmr ◽  
Acid Conjugate ◽  
Nmr Methods ◽  
Cis And Trans

The Brönsted-Lewis superacid HSO3F-SbF5 or "magic acid" is re-investigated by modern 19F NMR methods over a wide concentration range. The system is found to be considerably more complex than had been assumed previously. A total of 13 different anions are identified of which only five have previously been identified in magic acid. With increasing SbF5 contents the concentration of monomeric anions like [SbF6]-, [SbF5(SO3F)]-, cis- and trans-[SbF4(SO3F)2]-, and mer-[SbF3(SO3F)3]- gradually decreases. Except for [Sb2F11]-, which is present in very small concentrations only, the formation of oligomers involves exclusively μ-fluorosulfato bridges. In addition to donor (SO3F)- and acceptor (SbF5) complex formation to give [SbF5(SO3F)]- and possibly ligand redistribution, the solvolysis of SbF5 or SbF4(SO3F) in HSO3F appears to be the principal formation reaction for polyfluorosulfatofluoroantimonate(V) anions. In glass (NMR tubes) the solvolysis product HF is converted to the oxonium ion [H3O]+, which has previously been identified by 1H NMR and structurally characterized as [H3O][Sb2F11] by us.Key words: magic acid, conjugate superacid, fluorosulfuric acid, 19F NMR spectra.

A nuclear magnetic resonance study of Al–Mn quasicrystals and related materials

1987 ◽  
Vol 2 (4) ◽  
pp. 431-435 ◽  
Author(s):  
Keith R. Carduner ◽  
B. H. Suits ◽  
J. A. DiVerdi ◽  
Michael D. Murphy ◽  
David White
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Melt Spinning ◽  
Nmr Spectra ◽  
Nuclear Magnetic Resonance Study ◽  
Magnetic Resonance Study ◽  
Broad Distribution ◽  
Quadrupole Field ◽  
Melt Spinning Technique ◽  
Nuclear Magnetic

Nuclear magnetic resonance (NMR) results are presented for several aluminum alloy samples prepared using the melt-spinning technique including orthorhombic Al6Mn, Al–Mn quasicrystals both with and without doping with Si and Ru, and a T-phase alloy of Al and Pt. With the exception of the orthorhombic material, all of the NMR spectra show a broad distribution of sites. No features unique to the quasicrystal phase are observed. For the orthorhombic material the quadrupole field parameters are found to be ∥VQ∥ − 1.0±0.1 MHz and η = 0.4±0.1.

Synthesis and nuclear magnetic resonance study of the compounds (2-X-1,3-dithiane) (X = H, Me, SiMe3, GeMe3, SnMe3, PbMe3) and their tetracarbonyliron complexes

1978 ◽  
Vol 56 (11) ◽  
pp. 1538-1544 ◽  
Author(s):  
David J. Cane ◽  
William A. G. Graham ◽  
Liviu Vancea
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Nmr Spectroscopy ◽  
Magnetic Resonance ◽  
Energy Barrier ◽  
Nmr Spectra ◽  
Nuclear Magnetic Resonance Study ◽  
Carbonyl Groups ◽  
Magnetic Resonance Study ◽  
Ring Inversion ◽  
C Nmr

A series of (1,3-dithiane)Fe(CO)4 complexes, (2-X-1,3-dithiane)Fe(CO)4, X = H, Me, SiMe3, GeMe3, SnMe3, PbMe3, has been prepared and characterized, and both the complexes and the free ligands studied by 1H and 13C nmr spectroscopy. The energy barrier to ring inversion in (1,3-dithiane)Fe(CO)4, ΔG298†, is 14.7 ± 0.2 kcal mol−1, some 4.4 kcal mol−1 higher than in free 1,3-dithiane.13C nmr spectra showed that within the Fe(CO)4 moiety, rapid averaging of carbonyl groups occurs down to at least −80 °C.

A phosphorus-31 nuclear magnetic resonance spectroscopic study of complexes of zinc with some phosphine oxides, sulfides, and selenides

1983 ◽  
Vol 61 (8) ◽  
pp. 1800-1805 ◽  
Author(s):  
Philip A. W. Dean ◽  
Geetha K. Carson
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Spectroscopic Study ◽  
Mixed Oxide ◽  
Ligand Exchange ◽  
Nmr Spectra ◽  
Zinc Complexes ◽  
Phosphine Oxides ◽  
Cadmium Complexes ◽  
Slow Exchange

Zn(SbF6)2 in liquid SO2 has been shown to act as an acceptor towards a variety of phosphine oxides, sulfides, and selenides, forming complexes which have been characterized in solution using 31P nmr. Slow-exchange 31P nmr spectra are reported for the complexes ZnLn2+ (n = 6, L2 = Ph2P(O)CH2P(O)Ph2 or L3 = (Ph2P(O)(CH2)2)2P(O)Ph; n = 4, L2 = Ph2P(E)CH2P(E)Ph2 (E = O, S, or Se) or bidentate (Ph2P(E)CH2)3CMe (E = S or Se), or L = (C6H11)3PE (E = O, S, or Se) or R3PE (E = S or Se, R = Ph or o-C6H4Me); n = 3, L3 = (Ph2P(E)(CH2)2)2P(E)Ph (E = S or Se) or L = R3PE (E = S or Se, R = C6H11, Ph, or o-C6H4Me); n = 2, L = R3PE (E = S or Se, R = o-C6H4Me or, perhaps, C6H11); n = 1 (possibly), L = (o-C6H4Me)3PS), and partial spectra for [Zn(SeP(C6H11)3)x(SP(C6H11)3)n−x]2+ (n = 3 or 4). No evidence was found for the mixed oxide-chalcogenide species [Zn(EP(C6H11)3)x(OP(C6H11)3)4−x]2+. In most cases the 31P nmr spectra are very similar to those reported earlier for the corresponding cadmium complexes. However, in most instances where comparison could be made it was found that the rate of intermolecular ligand exchange was less for the zinc complexes than for their cadmium counterparts. (Complexes with (Ph2P(O)(CH2)2)2P(O)Ph and Ph2P(O)(CH2)2P(O)Ph2 arc exceptional in being more labile for zinc than cadmium.)

Sesquiterpene alkaloids from Tripterygiumwilfordii (Hook): a nuclear magnetic resonance study of 1-desacetylwilfordine, 1-desacetylwilfortrine, and 2-debenzoyl-2-nicotinoylwilforine

1990 ◽  
Vol 68 (3) ◽  
pp. 371-374 ◽  
Author(s):  
Li Ya ◽  
George M. Strunz ◽  
Larry A. Calhoun
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Chemical Shift ◽  
Nmr Spectra ◽  
Nuclear Magnetic Resonance Study ◽  
Chemical Shift Assignments ◽  
Magnetic Resonance Study ◽  
Root Extracts ◽  
C Nmr ◽  
Nuclear Magnetic

1-Desacetylwilfordine, 8, 1-desacetylwilfortrine, 9, and 2-debenzoyl-2-nicotinoylwilforine, 10, have been isolated from root extracts of the Chinese medicinal and insecticidal plant Tripterygiumwilfordii. Analysis of the 1H and 13C NMR spectra of 8 and 10, with the aid of COSY, HCCOSY, and COLOC experiments, has allowed unambiguous chemical shift assignments of all protons and carbons of these alkaloids. Keywords: alkaloids, sesquiterpene, Celastraceae, Tripterygium, NMR.

Hindered Rotation in Poly(N-acyl)iminoalkylenes - A 13C Nuclear Magnetic Resonance Study

1995 ◽  
Vol 50 (9) ◽  
pp. 1404-1411 ◽  
Author(s):  
Bernabé L. Rivas ◽  
Klaus Albert ◽  
Kurt E. Geckeler ◽  
Ernst Bayer
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Cationic Polymerization ◽  
Nmr Spectra ◽  
Nuclear Magnetic Resonance Study ◽  
Side Chain ◽  
Magnetic Resonance Study ◽  
Hindered Rotation ◽  
13C Nuclear Magnetic Resonance ◽  
C Nmr

AbstractPoly(N-acetyl)iminoethylene. poly(N-propionyl)iminoethylene and poly(N-acetyl)-2,2-dimethyliminoethylene were prepared by cationic polymerization in solution of 2-methyl- 2-oxazoline, 2-ethyl-2-oxazoline, and 2,4,4-trimethyl-2-oxazoline respectively. The 13C NMR spectra of the polymers obtained showed different sets of shifts for the carbon atoms of the backbone as well as for the N-acylimino side chain due to the restricted rotation of the Nacylimino group. The temperature dependence of the N-acylimino side chain signals showed a different coalescence behaviour depending on the substituents at both the main and the side chain.

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