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  • Analytical Chemistry and Spectroscopy  (11)
  • 1H NOESY  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Solution structures of [IrH2(1,5-cyclooctadiene) (bisphosphine)](CF3SO3) complexes. Homo- and heteronuclear long-range couplings from hydride and phosphorus spins to cyclooctadiene protons (1993)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 31 (1993), S. 677-684 
    Details
    ISSN: 0749-1581
    Keywords: Hydrogenation catalysts ; Indium hydrides ; Chiral phosphines ; 3D Solution structures ; Long-range H,H ; P,H couplings ; NOESY ; 1D-COSY{31P} ; Selective COSY and TOCSY ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The solution structures of the two all-cis stereoisomers of [IrH2(COD)((-)-chiraphos)](CF3SO3) and the four all-cis stereoisomers of [IrH2(COD)((-)-norphos)](CF3SO3) [COD = cycloocta-1,5-diene, (-)-chiraphos = 2S,3S-bis(diphenyl- phosphino)butane, (-)-norphos = 2R,3R-bis(diphenylphosphino)norbornene] were assigned on the basis of various one- and two-dimensional correlation methods. The rationalization of a specifically observed scalar coupling interaction between one of the hydrides and a methylene proton of the cyclooctadiene moiety required an assignment of all the relevant protons including their stereochemical relationship. Analogous long-range coupling pathways were also found for the heteronuclear interactions nJ(P,H) and an interpretation of the origin of these scalar couplings is provided in the form of an expansion of the known geometric dependence of allylic and homoallylic couplings.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260310714
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  • 2
    Electronic Resource
    Electronic Resource
    183W NMR spectroscopy of W(VI) imidoaryl and imidoalkyl complexes using inverse detection based on non-specific long-range interactions (1994)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 32 (1994), S. 235-241 
    Details
    ISSN: 0749-1581
    Keywords: 183W NMR ; Inverse detection ; W(VI) imidophenyl compounds ; 14,15N NMR ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 183W NMR spectra for a series of octahedral W(VI) imidophenyl, ‘W≡NPh’ and W(VI) imidoethyl, ‘W≡NEt,’ complexes were obtained using inverse detection based on non-specific long-range interactions. The metal couples to both the ortho and para protons of the NPh moiety (four and six bonds, respectively). The 183W shift is shown to be sensitive to the nature of the ligand and the coordination number. The effect of geometric isomerism on δ183W is shown to be several hundred ppm. Some δ14N and δ15N and 1J(183W,15N) data are reported. A number of new geometric isomers, involving the position of the NR ligand with respect to the remaining ligands, have been identified.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260320409
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  • 3
    Electronic Resource
    Electronic Resource
    Platinum-phosphine cluster chemistry: New potentials from 195Pt-31P{1H} triple-resonance spectroscopy (1991)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 29 (1991), S. S11 
    Details
    ISSN: 0749-1581
    Keywords: HMQC ; Multiple-quantum ; Platinum ; Clusters ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Platinum-phosphorus heteronuclear multiple-quantum coherence spectroscopy has been employed for the characterization of platinum-phosphine cluster compounds. Rules are developed for the interpretation of these spectra, whose appearance depends on the chosen pulse-sequence, phase-cycling and whether direct or remote platinum-phosphorus coupling constants have been selected. Spectral editing according to the different isotopomers (with respect to 195Pt) is possible when complete evolution of multiple-quantum coherence is allowed. This method offers a substantial advantage in the characterization of larger cluster compounds.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260291305
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  • 4
    Electronic Resource
    Electronic Resource
    Solution structure of [(triphos*)RhH2(AuPPh3)3][PF6]2 deduced by one- and two-dimensional 1H{31P} and 1H{103Rh} double-resonance techniques (1991)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 29 (1991), S. S73 
    Details
    ISSN: 0749-1581
    Keywords: Gold-rhodium clusters ; Hydrides ; Dynamic processes ; Double resonance ; 103Rh—1H heteronuclear correlations ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The application of 1H{31P} and 1H{103Rh} double-resonance techniques for the elucidation of the solution structure of the metalla-tetrahedrane clusters of the [(triphos*)RhH2(AuPPh3)3][PF6]2 type, with the chiral tripodal phosphine triphos* [RRR/SSS- or RRS/SSR-1,1,1,-tris(methylphenylphosphinomethyl)ethane] is described. Variable-temperature studies revealed three types of dynamic processes, i.e. rapid rotation of the trigold moiety (AuPPh3)3, mutual exchange of the diastereotopic hydrides and slow rotation of the RRS/SSR-triphos* unit in one diastereomer.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260291314
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  • 5
    Electronic Resource
    Electronic Resource
    Structure of two stereoisomers of Pt(trans-MeO2CCH=CHCO2Me)2[P(cyclohexyl)3]: Complete assignment of the 11 non-equivalent tricyclohexylphosphine protons using DQF-COSY and 13C, 1H two-dimensional methods (1991)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 29 (1991), S. 113-119 
    Details
    ISSN: 0749-1581
    Keywords: 2D NMR ; DQF-COSY ; C,H inverse correlation ; Tricyclohexylphosphine ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 1H NMR spectrum of the Pt(0) complex Pt(trans-MeO2CCH=CHCO2Me)2[P(cyclohexyl)3] was measured and the structures of the two isomeric forms, which differ with respect to olefin coordination, were assigned. The structural study made use of a complete analysis of the 11 non-equivalent protons of the P(cyclohexyl)3 in one isomer, and this was accomplished via DQF-COSY and 13C,1H inverse heteronuclear correlation methods.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260290204
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  • 6
    Electronic Resource
    Electronic Resource
    New Pt … H—N bonds characterized by 15N-filtered and 2D NOESY 1H NMR spectroscopy (1992)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 30 (1992), S. 548-551 
    Details
    ISSN: 0749-1581
    Keywords: NOESY ; 15N-filtered ; Pt-amine complexes ; Cyclometallation ; Pt … H—N interactions ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: New Pt … H—N bonding modes in two cycloplatinated complexes, [Pt(C6H4CH2NMe2-2-C,N)(C6H4CH2NMe2H-2-C,H)Br] (1) and [Pt(1-C10H6NMe2-8-C,N)(1-C10H6NMe2H-8-C,H)Br] (2), were characterized by 15N-filtered and 2D NOESY 1H measurements. Both 1 and 2 show markedly different interactions of an RNMe2H+ group with a platinum centre; the 1J(15N,1H) values of 69 and 59 Hz for 1 and 2, respectively, are considerably less than those of the related free and protonated organic amine systems. The corresponding 1J(195Pt,1H) values are 72 and 180 Hz, respectively. An approach both to understanding and recognizing these Pt … H—N interactions is presented.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260300616
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  • 7
    Electronic Resource
    Electronic Resource
    Structural elucidation of germine esters isolated from Veratrum nigrum L. Total assignment of 1H and 13C nuclear magnetic resonances by two-dimensional NMR techniques (1991)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 29 (1991), S. 100-112 
    Details
    ISSN: 0749-1581
    Keywords: 2D NMR ; Phase-sensitive DQF-COSY and ROESY ; Heteronuclear 13C-1H long-range correlation ; Steroid alkaloid ; Germine esters ; Anti-hypertension ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The application of two-dimensional phase-sensitive COSY, ROESY and 13C-1H shift correlation spectroscopy in the structural elucidation and stereochemical assignment of the steroidal alkaloids 15-(2-methylbutyryl)germine, 3-(2-hydroxy-2-methylbutyryl)-15-(2-methylbutyryl)germine and 16-(2-methylbutyryl)germine is reported. It is shown that two-dimensional 13C-1H heteronuclear long-range correlation spectroscopy is an invaluable method for the stereochemical assignment of proton resonances which overlap in 1H NMR and homonuclear correlation spectra.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260290203
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  • 8
    Electronic Resource
    Electronic Resource
    2D NOESY studies on [Pd(η3-C10H15){(R)( + )-BINAP}]+ defining the relative spatial orientation of the phenyl and π-allyl moieties (1991)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 29 (1991), S. 197-203 
    Details
    ISSN: 0749-1581
    Keywords: [Pd(η3-C10H15){(R)(+)-BINAP}](CF3SO3) ; Three-dimensional solution structure ; 2D NOESY NMR studies ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 2D NOESY, COSY and 31P,1H correlation measurements have been carried out on the optically active β-pineneallyl-(R)(+)-BINAP palladium complex, [Pd(η3-C10H15){(R)(+)-BINAP}](CF3SO3). The ortho protons of the four non-equivalent phenyl rings have been assigned, as have the 15 protons of the β-pineneallyl. The 2D NOE data show selective interactions of the phenyl ortho protons with different sections of the allyl ligand, thereby contributing to our knowledge of the three-dimensional solution structure of this cationic complex.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260290302
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  • 9
    Electronic Resource
    Electronic Resource
    183W-1H long-range shift correlation and 1H NOESY studies on tungsten(II) hydrido-pyrazolylborate complexes (1993)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 31 (1993), S. 58-62 
    Details
    ISSN: 0749-1581
    Keywords: Tungsten(II) hydrido-pyrazolylborate complexes ; 183W-1H long-range shift correlation ; 1H NOESY ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 183W NMR spectra for several tungsten carbonyl complexes were recorded using heteronuclear multiple-quantum spectroscopy. The measurements involved the use of both one-bond and long-range coupling constants, with the latter technique demonstrating a general approach to obtaining 183W spectra in Tp′ [Tp′ = tris(3,5-dimethylpyrazolyl)borohydride] and Cp tungsten compounds. Differences in the 183W chemical shifts between the Tp′ and Cp complexes are explained in terms of σ-donor and π-acceptor capabilities of the ligands. It is suggested that the very small 1J(183W,1H) value of 7 Hz in WH(Tp′)(CO)3 arises from an interaction of an H+ with a [W(Tp′)(CO)3]- orbital with a relatively large d-component. For WH(Tp′)(CO)(PHC≡CMe) (3), the very lowfield hydride chemical shift, δ = 10.8, is suggested to arise, in part, from anisotropic effects. 1H NOESY measurements on 3 show that the hydride lies in a deshielding region with respect to both the acetylene and two pyrazolylborate rings, the acetylene is bent such that the CH3 and Ph groups move toward one another and there is a second isomer of 3, presumably related to the geometry of the coordinated acetylene with respect to the W—C≡O bond.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260310112
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  • 10
    Electronic Resource
    Electronic Resource
    Two-dimensional NMR studies of Pt(2-methallyl)(SnCl3)(styrene). Recognition and interpretation of simultaneous exchange processes via 1H noesy (1989)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 27 (1989), S. 355-359 
    Details
    ISSN: 0749-1581
    Keywords: 2D NMR ; π-Allyl ; Ligand exchange ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 1H NMR spectrum of Pt[η3-CH2C(CH3)CH2](SnCl3)(PhCH=CH2) (1), which is complicated by the existence of two isomers, has been interpreted using (195Pt, 1H)-INVERSE, J-resolved, COSY-90 and NOESY two-dimensional methods. The two isomers are shown to be involved in slow exchange processes, and one intermediate in the exchange, Pt[CH2C(CH3)CH2](SnCl3)33- (4), has been identified and characterized via 1H, 13C, 119Sn and 195Pt spectroscopy. NOESY measurements show that neither 1 nor 4 is involved in an η3 →η1 isomerization, so that 4 must be involved in the dynamics with 1 via loss of a tin-containing fragment, presumably SnCl3-. Uncoordinated PhCH=CH2 has been detected in solution and shown to exchange with the complexed PhCH=CH2 in both isomers of 1.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260270411
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