Philip Dean | University of Western Ontario (original) (raw)

Papers by Philip Dean

Research paper thumbnail of The <sup>19</sup>F nuclear magnetic resonance spectra of antimony pentafluoride, <i>cis</i>-Sb<sub>3</sub>F<sub>16</sub><sup>−</sup> and higher polyanions Sb<sub><i>n</i></sub>F<sub>5<i>n</i>+1</sub><sup>−</sup>

Canadian Journal of Chemistry, Nov 1, 1970

The resonances in the 19F nuclear magnetic resonance (n.rn.r.), spectrum of antimony pentafluorid... more The resonances in the 19F nuclear magnetic resonance (n.rn.r.), spectrum of antimony pentafluoride have been reassigned and it is shown that the fine structure observed in the spectrum of antimony pentafluoride in various inert solvents can only be explained by considering the effects of magnetic nonequivalence. Solutions of t-butyl fluoride and tetra-n-butylammonium hexafluoroantimonate in excess SbF,/SO,CIF are shown to contain the Sb3F16-and Sb4Fzl-anions which have cis-fluorine bridged structures. The coupling constants and chemical shifts in the n.m.r. spectra of Sb3FI6-, Sb4Fzl-, (SbF,), and 1 :1 and 2:l complexes of SbF, are compared and discussed.

Research paper thumbnail of The reaction of metallothionein with mercuribenzoate. A dialysis and 113Cd-n.m.r. study

Biochemical Journal, Mar 15, 1986

The reaction of metallothionein with mercuribenzoate A dialysis and 113Cd-n.m.r. study*

Research paper thumbnail of A multinuclear (1H, 13C, 113Cd) nuclear magnetic resonance and magnetic circular dichroism spectroscopic study of thiolate complexes of cadmium

Inorganica Chimica Acta, 1981

Appropriate combinations of 'H, 13C and "'Cd NMR have been used to study ca. 0.05 M solutions of ... more Appropriate combinations of 'H, 13C and "'Cd NMR have been used to study ca. 0.05 M solutions of a wide range of 1'3Cd-enriched thiolatocadmates formed from the corresponding poorly soluble cadmium thiolates in the presence of excess thiolate. In addition, MCD spectra have been recorded for dilute, ca. lo-' M, solutions of a representative set of thiolate complexes of cadmium. Cadmium-113 chemical shifts are given for the complexes formed by 31 different thiolates individually in water at ambient probe temperature, and slowexchange 'H and/or 13C and/or '13Cd NMR spectra are reported for several typical complexes at reduced temperature in CD30D. In aqueous solution at ambient probe temperature, ligands with vicinal thiolate groups and-SCH, CHRS (R = H, Me, Et, CH, OH, CH, SO; or CH2S)) form bis(chelate) complexes which have 6od >\ 778 ppm, less shielded than the range for tetrahedral Cd(SR)i

Research paper thumbnail of A mass spectrometric investigation of clusters formed by sodium cations and pentacyanonitrosylferrate(2−) anions in the gas phase, and an exploration of structures of some of the clusters using Density Functional Theory

Inorganica Chimica Acta, 2013

Approximately 50 new cationic and anionic aggregates of general formula [Na x (NP) y ] z (NP 2À =... more Approximately 50 new cationic and anionic aggregates of general formula [Na x (NP) y ] z (NP 2À = pentacyanonitrosylferrate(2À), nitroprusside, [Fe(CN) 5 (NO)] 2À) have been observed mass spectrometrically by electrospraying a methanolic solution of Na 2 (NP)Á2H 2 O, with ion identification using Fourier-transform ion cyclotron resonance, and/or a quadrupole ion trap. Several families of ions have been observed in which the m/z values are the same but the values of z differ between family members. The distribution of species is compared with those of PPh 4 +-containing analogs, reported earlier and augmented here. Density Functional Theory has been used to determine structures and relative energies (after inclusion of zero-point and dispersion energies) of aggregates with y = 1 or 2. In general, isomeric structures occur, but in none of the optimized structures was bonding of Na + to the oxygen or nitrogen atoms of the nitrosyl group of NP 2À observed. A terminal Na + could be associated with as many as three nitrogen atoms from cyanide ligands, while a bridging Na + could be associated with up to six such nitrogen atoms. Association of Na + with two or three nitrogen atoms in a chelating manner was found to result in significant Fe-C-N and C-Fe-C angle bending. On the basis of these structures, and the bonding motifs within them, possible structures of ions with larger values of y are discussed.

Research paper thumbnail of Preparation and carbon-13 nuclear magnetic resonance spectra of arene complexes of mercury(I)

Journal of the Chemical Society, 1973

ABSTRACT

Research paper thumbnail of Synthesis and multinuclear magnetic resonance study of some tin(IV) complexes of pyridine-2-thiolate and related ligands, and the X-ray structural analysis of Sn(C5H4NS)4•C5H5NS

Canadian Journal of Chemistry, Aug 1, 1990

Novel ionic mixed-ligands complexes of the types cis-and trans-[Pt(pz) 2 (Ypy) 2 ](NO 3) 2 (where... more Novel ionic mixed-ligands complexes of the types cis-and trans-[Pt(pz) 2 (Ypy) 2 ](NO 3) 2 (where Ypy is a pyridine derivative and pz = pyrazine) were synthesized and studied mainly in the solid state by IR spectroscopy and in aqueous solution by multinuclear (195 Pt, 1 H and 13 C) magnetic resonance spectroscopy. The trans isomers with ligands containing a methyl group in ortho position on the pyridine ring could not be synthesized. The results of the solution NMR characterization have shown that the isolated compounds are pure. In 195 Pt NMR, the cis complexes containing a methyl group in ortho positions were observed at lower field (average À2337 ppm) than the other cis compounds (average À2427 ppm), which is explained by the solvent effect. The trans isomers were observed at very slightly lower fields (average À2422 ppm) than the equivalent cis complexes (average À2427 ppm). In 1 H NMR, the coupling constants 3 J(195 Pt-1 H Ypy) and 3 J(195 Pt-1 H pz) are larger in the cis compounds ($40 Hz) than in the trans complexes ($31 Hz). A few 4 J(195 Pt-1 H pz) were observed ($16 Hz). In 13 C NMR spectroscopy, the coupling constants 3 J(195 Pt-13 C pz) and 3

Research paper thumbnail of The trifluorosulphur(VI) oxide cation, SOF3 +

Journal of the Chemical Society D Chemical Communications, 1970

ABSTRACT

Research paper thumbnail of π-Arene complexes of cadmium(II) and zinc(II)

Journal of Organometallic Chemistry, 1977

ABSTRACT

Research paper thumbnail of Cadmium binding to metal-free metallothionein: A correlation of UV, CD and 113Cd NMR data and a 113Cd NMR characterization of the binding sites in the reconstituted protein

Inorganica Chimica Acta, 1983

Page 276,1.h. column, under Spectroscopic Measurements, the '13Cd nmr repetition rates for the na... more Page 276,1.h. column, under Spectroscopic Measurements, the '13Cd nmr repetition rates for the native and reconstituted protein should be 2.5 min-' and 28 mine1 respectively and not 2.5 s-' and 8 s-'.

Research paper thumbnail of The solid state structure of arene-mercury(II) complexes from magic-angle spinning carbon-13 NMR and the solution carbon-13 NMR of some complexes of mercury(II) with arenes having bulky aliphatic substituents

Journal of Organometallic Chemistry, Feb 1, 1982

The cross-polarization magic angle spinning 13C NMR spectra of Hg(SbF6)2 - 2 Arene (Arene = C6HMe... more The cross-polarization magic angle spinning 13C NMR spectra of Hg(SbF6)2 - 2 Arene (Arene = C6HMe5, 1,2,4,5-C6H2Me4, 1,2,3,4-C6H2Me4, or C6H6) have been measure.

Research paper thumbnail of Spectroscopic studies of inorganic fluoro-complexes. Part I. The 19F nuclear magnetic resonance and vibrational spectra of hexafluorometallates of Groups IVA and IVB

Journal of the Chemical Society, 1967

Research paper thumbnail of ChemInform Abstract: PREPARATION AND CARBON-13 NUCLEAR MAGNETIC RESONANCE SPECTRA OF ARENE COMPLEXES OF MERCURY(I)

Chemischer Informationsdienst, Dec 11, 1973

ChemInform Abstract Quecksilber(I)-hexafluoroarsenat (I) bildet mit verschiedenen Aromaten in Sch... more ChemInform Abstract Quecksilber(I)-hexafluoroarsenat (I) bildet mit verschiedenen Aromaten in Schwefeldioxid-Lösung die 1:1-Komplexe (II). Mit Benzophenanthren (III) entstehen die Komplexe (IV) und (V). (Raman-und NMR-spektroskopische Angaben).

Research paper thumbnail of ChemInform Abstract: A MULTINUCLEAR (PROTON, CARBON-13, CADMIUM-113) NUCLEAR MAGNETIC RESONANCE AND MAGNETIC CIRCULAR DICHROISM SPECTROSCOPIC STUDY OF THIOLATE COMPLEXES OF CADMIUM

Chemischer Informationsdienst, Jan 5, 1982

ChemInform Abstract (Untersuchungen an einer Vielzahl von Komplexen mit einzähnigen Thiolatligand... more ChemInform Abstract (Untersuchungen an einer Vielzahl von Komplexen mit einzähnigen Thiolatliganden und Dithiolat-Chelatkomplexen)

Research paper thumbnail of Pyridine-2-selenolate and -2-tellurolate as ligands: a multinuclear (77Se, 119Sn, 125Te) magnetic resonance study of some tin(IV) complexes, and X-ray structural analyses of Sn(SPh)2(2-Se-C5H4N-N,Se)2 and Sn(SPh)1.85(2-Se-C5H4N)2.15

Canadian Journal of Chemistry, Nov 1, 1996

Reactions between Sn(E′Ph)n (E′ = S or Se; n = 2 or 4) and the bis(pyridine) dichalcogenides 2,2′... more Reactions between Sn(E′Ph)n (E′ = S or Se; n = 2 or 4) and the bis(pyridine) dichalcogenides 2,2′-(C5H4NE)2 (E = Se or Te), abbreviated py2E2, have been studied using multinuclear (77Se, 119Sn, 125Te) magnetic resonance. In this way the occurrence of the pyridine-2-chalcogenate complexes Sn(E′Ph)4−x(Epy)x (E′ = S or Se; E = Se, x = 1–4; E = Te, x = 1 or 2) has been demonstrated. The pattern of 119Sn NMR chemical shifts for Sn(E′Ph)4−x(Sepy)x (E′ = S or Se, x = 0–4) is consistent with bidentate bonding for the pySe− ligand when x = 1 and 2. The pyTe− ligand is probably bidentate also in all four complexes containing this ligand. As part of the NMR analysis, 77Se and (or) 125Te NMR data were obtained for py2Te2 and for the new mixed dichalcogenides PhE′ER (E′ = S, Se, or Te; E ≠ E′ = Se or Te; R = 2-py or Ph), which were produced in the systems Ph2E′2:R2E2. The complex Sn(SPh)2(Sepy)2 (1) was isolated pure and its structure determined by the single crystal X-diffraction technique. The compound crystallizes in the monoclinic space group P21/n, with unit cell dimensions a = 9.7929(9) Å, b = 22.340(2) Å, c = 11.368(1) Å, β = 108.803(7) °, V = 2354.3(4) Å3, dcalc = 1.837 g cm−3 and Z = 4. Refinement by full-matrix least squares on F2 gave agreement factors R1 = 0.0425 and wR2 = 0.0882 for 2823 independent reflections with F0 ≥ 4σ(F0) and 258 variables. The structure confirms that the PySe− ligand behaves in a chelating manner. The molecule Sn(SPh)2(2-Se-C5H4N-N,Se)2 has a distorted octahedral structure with the PhS− ligands in cis positions and the two Se donor atoms in trans positions. The Sn—Se, Sn—S, and Sn—N distances are 2.6291(8) and 2.6358(8) Å, 2.475(2) and 2.464(2) Å, and 2.325(5) and 2.333(5) Å. The bite angles N-Sn-Se of the chelating ligands are 65.9(1)° and 65.8(1)°. En route to 1, the yellow crystalline compound Sn(SPh)1 85(2-Se-C5H4N)2 15 (2) was isolated. This was shown by 119Sn NMR spectroscopy to contain both Sn(2-Se-C5H4N)2(SPh)2 and Sn(2-Se-C5H4N)3(SPh). The crystal and molecular structure of 2 was determined by single crystal X-ray diffraction techniques. Crystal data: monoclinic, space group P21/n, a = 9.795(2) Å, b = 22.355(4) Å, c = 11.362(2) Å, β = 108.87(3)°, V = 2354.2(8) Å3, dcalc = 1.837 g cm−3, dobs = 1.87(5) g cm−3Z = 4, R1 = 0.0306, wR2 = 0.0651 for 2756 data (F0 ≥ 4σ(F0)) and 258 parameters. Crystallographic evidence for the presence of co-crystallized Sn(2-Se-C5H4N)3(SPh) occurs only in a minor lengthening of one of the two Sn—S bonds, Sn—S(1) (compared with expectation for 1), and an excess of electron density at S(1) when the data are modelled as Sn(2-Se-C5H4N)2(SPh)2. These effects are attributed to a crystallographic disorder of SPh and η1-{2-Se-C5H4N} at the S(1)Ph site, involving isostructural Sn(η2-{2-Se-C5H4N})2({η1-{2-Se-C5H4N})(SPh) and Sn(η2-{2-Se-C5H4N})2(SPh)2. Key words: pyridine-2-selenolate, pyridine-2-tellurolate, tin complexes.

Research paper thumbnail of π-Arene complexes of the main group elements. II. Complexes of cadmium(II) and zinc(II)

Journal of Organometallic Chemistry, Mar 1, 1979

ABSTRACT

Research paper thumbnail of A preparative and 1H and 13C NMR spectroscopic study of mercury(II)-Arene complexes

Journal of Organometallic Chemistry, Nov 1, 1979

... EF Kiefer, WL Waters and DA Carison J. Amer. Chem. Soc. 90 (1968), p. 5127. Full Text via Cro... more ... EF Kiefer, WL Waters and DA Carison J. Amer. Chem. Soc. 90 (1968), p. 5127. Full Text via CrossRef | View Record in Scopus | Cited By in Scopus (11). VI Sokolov, VV Bashilov and OA Reutov Acad. Sci. USSR 197 (1971), p. 184 Dokl. Chem. ; Chem. Abstr. ...

Research paper thumbnail of ChemInform Abstract: Π-ARENE COMPLEXES OF CADMIUM(II) AND ZINC(II)

Chemischer Informationsdienst, May 31, 1977

ChemInform Abstract In Analogie zu den schon bekannten Silber-Arin-Komplexen sind in flüssigem SO... more ChemInform Abstract In Analogie zu den schon bekannten Silber-Arin-Komplexen sind in flüssigem SO2 13C-NMR-spektroskopisch Anzeichen für die Arin-Bildung aus (II) mit (I) und (III) nachzuweisen.

Research paper thumbnail of ChemInform Abstract: (19)F NUCLEAR MAGNETIC RESONANCE SPECTRA OF OCTAHEDRAL FLUOROTHIOCYANATO-N- AND FLUOROCYANATO-N-TITANATES (IV)

Chemischer Informationsdienst, May 7, 1974

Research paper thumbnail of A multinuclear (1H, 13C, 113Cd) nuclear magnetic resonance and magnetic circular dichroism spectroscopic study of thiolate complexes of cadmium

Inorganica Chimica Acta, Sep 1, 1985

Appropriate combinations of 'H, 13C and "'Cd NMR have been used to study ca. 0.05 M solutions of ... more Appropriate combinations of 'H, 13C and "'Cd NMR have been used to study ca. 0.05 M solutions of a wide range of 1'3Cd-enriched thiolatocadmates formed from the corresponding poorly soluble cadmium thiolates in the presence of excess thiolate. In addition, MCD spectra have been recorded for dilute, ca. lo-' M, solutions of a representative set of thiolate complexes of cadmium. Cadmium-113 chemical shifts are given for the complexes formed by 31 different thiolates individually in water at ambient probe temperature, and slowexchange 'H and/or 13C and/or '13Cd NMR spectra are reported for several typical complexes at reduced temperature in CD30D. In aqueous solution at ambient probe temperature, ligands with vicinal thiolate groups and-SCH, CHRS (R = H, Me, Et, CH, OH, CH, SO; or CH2S)) form bis(chelate) complexes which have 6od >\ 778 ppm, less shielded than the range for tetrahedral Cd(SR)i

Research paper thumbnail of ChemInform Abstract: A Multinuclear, (77Se,119Sn,125Te) NMR Spectroscopic Study of the Series Sn(SPh)x(SePh)y(TePh)4-x-y

Chemischer Informationsdienst, 1986

Research paper thumbnail of The <sup>19</sup>F nuclear magnetic resonance spectra of antimony pentafluoride, <i>cis</i>-Sb<sub>3</sub>F<sub>16</sub><sup>−</sup> and higher polyanions Sb<sub><i>n</i></sub>F<sub>5<i>n</i>+1</sub><sup>−</sup>

Canadian Journal of Chemistry, Nov 1, 1970

The resonances in the 19F nuclear magnetic resonance (n.rn.r.), spectrum of antimony pentafluorid... more The resonances in the 19F nuclear magnetic resonance (n.rn.r.), spectrum of antimony pentafluoride have been reassigned and it is shown that the fine structure observed in the spectrum of antimony pentafluoride in various inert solvents can only be explained by considering the effects of magnetic nonequivalence. Solutions of t-butyl fluoride and tetra-n-butylammonium hexafluoroantimonate in excess SbF,/SO,CIF are shown to contain the Sb3F16-and Sb4Fzl-anions which have cis-fluorine bridged structures. The coupling constants and chemical shifts in the n.m.r. spectra of Sb3FI6-, Sb4Fzl-, (SbF,), and 1 :1 and 2:l complexes of SbF, are compared and discussed.

Research paper thumbnail of The reaction of metallothionein with mercuribenzoate. A dialysis and 113Cd-n.m.r. study

Biochemical Journal, Mar 15, 1986

The reaction of metallothionein with mercuribenzoate A dialysis and 113Cd-n.m.r. study*

Research paper thumbnail of A multinuclear (1H, 13C, 113Cd) nuclear magnetic resonance and magnetic circular dichroism spectroscopic study of thiolate complexes of cadmium

Inorganica Chimica Acta, 1981

Appropriate combinations of 'H, 13C and "'Cd NMR have been used to study ca. 0.05 M solutions of ... more Appropriate combinations of 'H, 13C and "'Cd NMR have been used to study ca. 0.05 M solutions of a wide range of 1'3Cd-enriched thiolatocadmates formed from the corresponding poorly soluble cadmium thiolates in the presence of excess thiolate. In addition, MCD spectra have been recorded for dilute, ca. lo-' M, solutions of a representative set of thiolate complexes of cadmium. Cadmium-113 chemical shifts are given for the complexes formed by 31 different thiolates individually in water at ambient probe temperature, and slowexchange 'H and/or 13C and/or '13Cd NMR spectra are reported for several typical complexes at reduced temperature in CD30D. In aqueous solution at ambient probe temperature, ligands with vicinal thiolate groups and-SCH, CHRS (R = H, Me, Et, CH, OH, CH, SO; or CH2S)) form bis(chelate) complexes which have 6od >\ 778 ppm, less shielded than the range for tetrahedral Cd(SR)i

Research paper thumbnail of A mass spectrometric investigation of clusters formed by sodium cations and pentacyanonitrosylferrate(2−) anions in the gas phase, and an exploration of structures of some of the clusters using Density Functional Theory

Inorganica Chimica Acta, 2013

Approximately 50 new cationic and anionic aggregates of general formula [Na x (NP) y ] z (NP 2À =... more Approximately 50 new cationic and anionic aggregates of general formula [Na x (NP) y ] z (NP 2À = pentacyanonitrosylferrate(2À), nitroprusside, [Fe(CN) 5 (NO)] 2À) have been observed mass spectrometrically by electrospraying a methanolic solution of Na 2 (NP)Á2H 2 O, with ion identification using Fourier-transform ion cyclotron resonance, and/or a quadrupole ion trap. Several families of ions have been observed in which the m/z values are the same but the values of z differ between family members. The distribution of species is compared with those of PPh 4 +-containing analogs, reported earlier and augmented here. Density Functional Theory has been used to determine structures and relative energies (after inclusion of zero-point and dispersion energies) of aggregates with y = 1 or 2. In general, isomeric structures occur, but in none of the optimized structures was bonding of Na + to the oxygen or nitrogen atoms of the nitrosyl group of NP 2À observed. A terminal Na + could be associated with as many as three nitrogen atoms from cyanide ligands, while a bridging Na + could be associated with up to six such nitrogen atoms. Association of Na + with two or three nitrogen atoms in a chelating manner was found to result in significant Fe-C-N and C-Fe-C angle bending. On the basis of these structures, and the bonding motifs within them, possible structures of ions with larger values of y are discussed.

Research paper thumbnail of Preparation and carbon-13 nuclear magnetic resonance spectra of arene complexes of mercury(I)

Journal of the Chemical Society, 1973

ABSTRACT

Research paper thumbnail of Synthesis and multinuclear magnetic resonance study of some tin(IV) complexes of pyridine-2-thiolate and related ligands, and the X-ray structural analysis of Sn(C5H4NS)4•C5H5NS

Canadian Journal of Chemistry, Aug 1, 1990

Novel ionic mixed-ligands complexes of the types cis-and trans-[Pt(pz) 2 (Ypy) 2 ](NO 3) 2 (where... more Novel ionic mixed-ligands complexes of the types cis-and trans-[Pt(pz) 2 (Ypy) 2 ](NO 3) 2 (where Ypy is a pyridine derivative and pz = pyrazine) were synthesized and studied mainly in the solid state by IR spectroscopy and in aqueous solution by multinuclear (195 Pt, 1 H and 13 C) magnetic resonance spectroscopy. The trans isomers with ligands containing a methyl group in ortho position on the pyridine ring could not be synthesized. The results of the solution NMR characterization have shown that the isolated compounds are pure. In 195 Pt NMR, the cis complexes containing a methyl group in ortho positions were observed at lower field (average À2337 ppm) than the other cis compounds (average À2427 ppm), which is explained by the solvent effect. The trans isomers were observed at very slightly lower fields (average À2422 ppm) than the equivalent cis complexes (average À2427 ppm). In 1 H NMR, the coupling constants 3 J(195 Pt-1 H Ypy) and 3 J(195 Pt-1 H pz) are larger in the cis compounds ($40 Hz) than in the trans complexes ($31 Hz). A few 4 J(195 Pt-1 H pz) were observed ($16 Hz). In 13 C NMR spectroscopy, the coupling constants 3 J(195 Pt-13 C pz) and 3

Research paper thumbnail of The trifluorosulphur(VI) oxide cation, SOF3 +

Journal of the Chemical Society D Chemical Communications, 1970

ABSTRACT

Research paper thumbnail of π-Arene complexes of cadmium(II) and zinc(II)

Journal of Organometallic Chemistry, 1977

ABSTRACT

Research paper thumbnail of Cadmium binding to metal-free metallothionein: A correlation of UV, CD and 113Cd NMR data and a 113Cd NMR characterization of the binding sites in the reconstituted protein

Inorganica Chimica Acta, 1983

Page 276,1.h. column, under Spectroscopic Measurements, the '13Cd nmr repetition rates for the na... more Page 276,1.h. column, under Spectroscopic Measurements, the '13Cd nmr repetition rates for the native and reconstituted protein should be 2.5 min-' and 28 mine1 respectively and not 2.5 s-' and 8 s-'.

Research paper thumbnail of The solid state structure of arene-mercury(II) complexes from magic-angle spinning carbon-13 NMR and the solution carbon-13 NMR of some complexes of mercury(II) with arenes having bulky aliphatic substituents

Journal of Organometallic Chemistry, Feb 1, 1982

The cross-polarization magic angle spinning 13C NMR spectra of Hg(SbF6)2 - 2 Arene (Arene = C6HMe... more The cross-polarization magic angle spinning 13C NMR spectra of Hg(SbF6)2 - 2 Arene (Arene = C6HMe5, 1,2,4,5-C6H2Me4, 1,2,3,4-C6H2Me4, or C6H6) have been measure.

Research paper thumbnail of Spectroscopic studies of inorganic fluoro-complexes. Part I. The 19F nuclear magnetic resonance and vibrational spectra of hexafluorometallates of Groups IVA and IVB

Journal of the Chemical Society, 1967

Research paper thumbnail of ChemInform Abstract: PREPARATION AND CARBON-13 NUCLEAR MAGNETIC RESONANCE SPECTRA OF ARENE COMPLEXES OF MERCURY(I)

Chemischer Informationsdienst, Dec 11, 1973

ChemInform Abstract Quecksilber(I)-hexafluoroarsenat (I) bildet mit verschiedenen Aromaten in Sch... more ChemInform Abstract Quecksilber(I)-hexafluoroarsenat (I) bildet mit verschiedenen Aromaten in Schwefeldioxid-Lösung die 1:1-Komplexe (II). Mit Benzophenanthren (III) entstehen die Komplexe (IV) und (V). (Raman-und NMR-spektroskopische Angaben).

Research paper thumbnail of ChemInform Abstract: A MULTINUCLEAR (PROTON, CARBON-13, CADMIUM-113) NUCLEAR MAGNETIC RESONANCE AND MAGNETIC CIRCULAR DICHROISM SPECTROSCOPIC STUDY OF THIOLATE COMPLEXES OF CADMIUM

Chemischer Informationsdienst, Jan 5, 1982

ChemInform Abstract (Untersuchungen an einer Vielzahl von Komplexen mit einzähnigen Thiolatligand... more ChemInform Abstract (Untersuchungen an einer Vielzahl von Komplexen mit einzähnigen Thiolatliganden und Dithiolat-Chelatkomplexen)

Research paper thumbnail of Pyridine-2-selenolate and -2-tellurolate as ligands: a multinuclear (77Se, 119Sn, 125Te) magnetic resonance study of some tin(IV) complexes, and X-ray structural analyses of Sn(SPh)2(2-Se-C5H4N-N,Se)2 and Sn(SPh)1.85(2-Se-C5H4N)2.15

Canadian Journal of Chemistry, Nov 1, 1996

Reactions between Sn(E′Ph)n (E′ = S or Se; n = 2 or 4) and the bis(pyridine) dichalcogenides 2,2′... more Reactions between Sn(E′Ph)n (E′ = S or Se; n = 2 or 4) and the bis(pyridine) dichalcogenides 2,2′-(C5H4NE)2 (E = Se or Te), abbreviated py2E2, have been studied using multinuclear (77Se, 119Sn, 125Te) magnetic resonance. In this way the occurrence of the pyridine-2-chalcogenate complexes Sn(E′Ph)4−x(Epy)x (E′ = S or Se; E = Se, x = 1–4; E = Te, x = 1 or 2) has been demonstrated. The pattern of 119Sn NMR chemical shifts for Sn(E′Ph)4−x(Sepy)x (E′ = S or Se, x = 0–4) is consistent with bidentate bonding for the pySe− ligand when x = 1 and 2. The pyTe− ligand is probably bidentate also in all four complexes containing this ligand. As part of the NMR analysis, 77Se and (or) 125Te NMR data were obtained for py2Te2 and for the new mixed dichalcogenides PhE′ER (E′ = S, Se, or Te; E ≠ E′ = Se or Te; R = 2-py or Ph), which were produced in the systems Ph2E′2:R2E2. The complex Sn(SPh)2(Sepy)2 (1) was isolated pure and its structure determined by the single crystal X-diffraction technique. The compound crystallizes in the monoclinic space group P21/n, with unit cell dimensions a = 9.7929(9) Å, b = 22.340(2) Å, c = 11.368(1) Å, β = 108.803(7) °, V = 2354.3(4) Å3, dcalc = 1.837 g cm−3 and Z = 4. Refinement by full-matrix least squares on F2 gave agreement factors R1 = 0.0425 and wR2 = 0.0882 for 2823 independent reflections with F0 ≥ 4σ(F0) and 258 variables. The structure confirms that the PySe− ligand behaves in a chelating manner. The molecule Sn(SPh)2(2-Se-C5H4N-N,Se)2 has a distorted octahedral structure with the PhS− ligands in cis positions and the two Se donor atoms in trans positions. The Sn—Se, Sn—S, and Sn—N distances are 2.6291(8) and 2.6358(8) Å, 2.475(2) and 2.464(2) Å, and 2.325(5) and 2.333(5) Å. The bite angles N-Sn-Se of the chelating ligands are 65.9(1)° and 65.8(1)°. En route to 1, the yellow crystalline compound Sn(SPh)1 85(2-Se-C5H4N)2 15 (2) was isolated. This was shown by 119Sn NMR spectroscopy to contain both Sn(2-Se-C5H4N)2(SPh)2 and Sn(2-Se-C5H4N)3(SPh). The crystal and molecular structure of 2 was determined by single crystal X-ray diffraction techniques. Crystal data: monoclinic, space group P21/n, a = 9.795(2) Å, b = 22.355(4) Å, c = 11.362(2) Å, β = 108.87(3)°, V = 2354.2(8) Å3, dcalc = 1.837 g cm−3, dobs = 1.87(5) g cm−3Z = 4, R1 = 0.0306, wR2 = 0.0651 for 2756 data (F0 ≥ 4σ(F0)) and 258 parameters. Crystallographic evidence for the presence of co-crystallized Sn(2-Se-C5H4N)3(SPh) occurs only in a minor lengthening of one of the two Sn—S bonds, Sn—S(1) (compared with expectation for 1), and an excess of electron density at S(1) when the data are modelled as Sn(2-Se-C5H4N)2(SPh)2. These effects are attributed to a crystallographic disorder of SPh and η1-{2-Se-C5H4N} at the S(1)Ph site, involving isostructural Sn(η2-{2-Se-C5H4N})2({η1-{2-Se-C5H4N})(SPh) and Sn(η2-{2-Se-C5H4N})2(SPh)2. Key words: pyridine-2-selenolate, pyridine-2-tellurolate, tin complexes.

Research paper thumbnail of π-Arene complexes of the main group elements. II. Complexes of cadmium(II) and zinc(II)

Journal of Organometallic Chemistry, Mar 1, 1979

ABSTRACT

Research paper thumbnail of A preparative and 1H and 13C NMR spectroscopic study of mercury(II)-Arene complexes

Journal of Organometallic Chemistry, Nov 1, 1979

... EF Kiefer, WL Waters and DA Carison J. Amer. Chem. Soc. 90 (1968), p. 5127. Full Text via Cro... more ... EF Kiefer, WL Waters and DA Carison J. Amer. Chem. Soc. 90 (1968), p. 5127. Full Text via CrossRef | View Record in Scopus | Cited By in Scopus (11). VI Sokolov, VV Bashilov and OA Reutov Acad. Sci. USSR 197 (1971), p. 184 Dokl. Chem. ; Chem. Abstr. ...

Research paper thumbnail of ChemInform Abstract: Π-ARENE COMPLEXES OF CADMIUM(II) AND ZINC(II)

Chemischer Informationsdienst, May 31, 1977

ChemInform Abstract In Analogie zu den schon bekannten Silber-Arin-Komplexen sind in flüssigem SO... more ChemInform Abstract In Analogie zu den schon bekannten Silber-Arin-Komplexen sind in flüssigem SO2 13C-NMR-spektroskopisch Anzeichen für die Arin-Bildung aus (II) mit (I) und (III) nachzuweisen.

Research paper thumbnail of ChemInform Abstract: (19)F NUCLEAR MAGNETIC RESONANCE SPECTRA OF OCTAHEDRAL FLUOROTHIOCYANATO-N- AND FLUOROCYANATO-N-TITANATES (IV)

Chemischer Informationsdienst, May 7, 1974

Research paper thumbnail of A multinuclear (1H, 13C, 113Cd) nuclear magnetic resonance and magnetic circular dichroism spectroscopic study of thiolate complexes of cadmium

Inorganica Chimica Acta, Sep 1, 1985

Appropriate combinations of 'H, 13C and "'Cd NMR have been used to study ca. 0.05 M solutions of ... more Appropriate combinations of 'H, 13C and "'Cd NMR have been used to study ca. 0.05 M solutions of a wide range of 1'3Cd-enriched thiolatocadmates formed from the corresponding poorly soluble cadmium thiolates in the presence of excess thiolate. In addition, MCD spectra have been recorded for dilute, ca. lo-' M, solutions of a representative set of thiolate complexes of cadmium. Cadmium-113 chemical shifts are given for the complexes formed by 31 different thiolates individually in water at ambient probe temperature, and slowexchange 'H and/or 13C and/or '13Cd NMR spectra are reported for several typical complexes at reduced temperature in CD30D. In aqueous solution at ambient probe temperature, ligands with vicinal thiolate groups and-SCH, CHRS (R = H, Me, Et, CH, OH, CH, SO; or CH2S)) form bis(chelate) complexes which have 6od >\ 778 ppm, less shielded than the range for tetrahedral Cd(SR)i

Research paper thumbnail of ChemInform Abstract: A Multinuclear, (77Se,119Sn,125Te) NMR Spectroscopic Study of the Series Sn(SPh)x(SePh)y(TePh)4-x-y

Chemischer Informationsdienst, 1986