Kinetics and mechanism of the reaction of palladium(II) complexes of o-(diphenylphosphino)thioanisole and o-(diphenylphosphino)selenoanisole with nucleophiles thiocyanate and iodide. Carbon-13 NMR spectroscopy of the methyl-heteroatom complexes and x-ray structural characterization of diiodobis[o-(diphenylphosphino)benzenethiolato]dipalladium(II)

The reaction of OP(NH-t-Bu)3 with 1 equiv. of ZnMe2 generates the dimeric eight-membered ring {MeZn[(µ-NH-t-Bu)(µ-N-t-Bu)P(NH-t-Bu)(µ-O)]}2 (5) and the cubane {[MeZn]3[OP(N-t-Bu)3][OP(NH-t-Bu)3]} (6), which contains the first known trisimidophosphate trianion. A related complex {Zn[ZnMe]2[OP(N-t-Bu)(NH-t-Bu)2][OP(N-t-Bu)3]} (7) is obtained by the reaction of OP(NH-t-Bu)3 with ZnMe2 in a 2:3 molar ratio. The treatment of OP(NHMe)3 with 1 equiv. of ZnMe2 produces the oxide-templated cluster {Zn4(µ4-O)[OP(NMe)(NHMe)2]4[OP(NMe)2(NHMe)]}2 (8). Each half of this centrosymmetric dimer contains a tetrahedral arrangement of four 4-coordinate Zn2+ ions surrounding the central µ4-O2- anion. The reaction of SP(NH-t-Bu)3 with ZnMe2 in a 1:1 molar ratio generates the dimer {MeZn(µ-S)(µ-N-t-Bu)P(NH-t-Bu)2}2 (10), which has a ladder-type structure. When a 2:1 molar ratio of the same reagents is employed, the bis(N,S)-chelated complex {Zn[(µ-S)(µ-N-t-Bu)P(NH-t-Bu)2]2} (11) is obtained. The monomeric N,N′-chelated complex {MeZn[(µ-N-t-Bu)(µ-NSiMe3)P(NH-t-Bu)2]} (12) results from the reaction of Me3SiNP(NH-t-Bu)3 with 1 equiv. of dimethylzinc. All new compounds have been characterized by multinuclear (1H, 13C, and 31P) NMR spectroscopy and, in the case of 5, 6, 7, 8, and 10, by X-ray structural determinations.Key words: zinc, phosphate, imido ligands, sulfur.

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Structural Characterization of Organometallic Sandwich Intercalates of Tin and Zirconium Dichalcogenides by X-ray and Neutron Diffraction and Solid State 2H NMR Spectroscopy

Inorganic Chemistry ◽

10.1021/ic00102a027 ◽

1994 ◽

Vol 33 (24) ◽

pp. 5515-5521 ◽

Cited By ~ 10

Author(s):

Heng-Vee Wong ◽

John S. O. Evans ◽

Stephen Barlow ◽

Susan J. Mason ◽

Dermot O'Hare

Keyword(s):

Solid State ◽

Nmr Spectroscopy ◽

Neutron Diffraction ◽

Structural Characterization ◽

2H Nmr ◽

X Ray ◽

2H Nmr Spectroscopy

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Synthesis and molecular structure of [Rh(η5-C5H5)(coe)(PtBu2H)] (coe=cis-cyclooctene)

Zeitschrift für Naturforschung B ◽

10.1515/znb-2019-0041 ◽

2019 ◽

Vol 74 (5) ◽

pp. 455-457 ◽

Cited By ~ 1

Author(s):

Hans-Christian Böttcher ◽

Peter Mayer ◽

Daniel Beck

Keyword(s):

Molecular Structure ◽

Nmr Spectroscopy ◽

Single Crystals ◽

Structural Characterization ◽

Title Compound ◽

Good Yield ◽

X Ray Diffraction ◽

X Ray

AbstractThe synthesis and structural characterization of the new olefinic complex [Rh(η5-C5H5)(coe)(PtBu2H)] (2, coe = cis-cyclooctene) is reported. The title compound was easily prepared in good yield by a thermolytic approach using [Rh(η5-C5H5)(coe)2] (1) and the secondary phosphane in toluene under reflux conditions. The compound 2 has been characterized by NMR spectroscopy and microanalysis. Single crystals of 2 were grown from n-hexane and the molecular structure has been established by X-ray diffraction.

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Magneto-Structural Characterization of Metallocene-Bridged Nitronyl Nitroxide Diradicals by X-Ray, Magnetic Measurements, Solid-state NMR Spectroscopy, and Ab Initio Calculations

Chemistry - A European Journal ◽

10.1002/chem.200305349 ◽

2004 ◽

Vol 10 (6) ◽

pp. 1355-1365 ◽

Cited By ~ 13

Author(s):

Christian Sporer ◽

Henrike Heise ◽

Klaus Wurst ◽

Daniel Ruiz-Molina ◽

Holger Kopacka ◽

...

Keyword(s):

Solid State ◽

Nmr Spectroscopy ◽

Ab Initio Calculations ◽

Ab Initio ◽

Structural Characterization ◽

Solid State Nmr ◽

Magnetic Measurements ◽

Nitronyl Nitroxide ◽

X Ray

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Synthesis and Structural Characterization of Metal Complexes of 2-Formylpyrrole 4N-Methylthiosemicarbazone (4ML1) and 2-Acetyl- pyrrole 4N-Methylthiosemicarbazone (4ML2). The X-Ray Crystal Structures of [Ni(4ML1-H)2], [Pd(4ML1-H)2] and [Cd(4ML2)2I2]

Zeitschrift für Naturforschung B ◽

10.1515/znb-2001-0301 ◽

2001 ◽

Vol 56 (3) ◽

pp. 219-228 ◽

Cited By ~ 6

Author(s):

Ruben Alonso ◽

Elena Bermejo ◽

Rosa Carballo ◽

Alfonso astiñeiras ◽

Teresa Pérez

Keyword(s):

Mass Spectrometry ◽

Nmr Spectroscopy ◽

Elemental Analysis ◽

Structural Characterization ◽

X Ray ◽

Group 12 ◽

New Compounds ◽

Group 10 Metals ◽

C Nmr

Abstract Reaction of 4N-methyl-2-[1-(pyrrol-2-yl)methylidene]hydrazinecarbothioamide (4ML1 and 4N-methyl-2-[1-(pyrrol-2-yl)-ethylidene]hydrazine carbothioamide (4ML1) with zinc(II), cadmium(II) and mercury(II) halides afforded complexes with formulas [M(L)X2] [(L; M; X) =(4ML1; Cd; Cl) (4), (4ML1; Hg; Cl, Br, I) (7 - 9), (4ML2; Cd; Cl) (17), (4ML2; Hg; Cl, Br, I) (20 - 22)] or [M(L)2X2] [(L; M; X) = (4ML1; Zn; Cl, Br, I) (1 - 3), (4ML1; Cd; Br, I) (5, 6), (4ML2; Zn; Cl, Br, I) (14 - 16), (4ML2; Cd; Br, I) (18, 19)]. Reaction of 4ML1 with salts of copper(II), nickel(II), palladium(II) and platinum(II) afforded complexes of formula [M(4ML1-H)2] (10 -13). Crystals of 11, 12 and 19 were studied by X-ray diffractometry, and all new compounds were characterized by elemental analysis, mass spectrometry, and IR, electronic and 1H and 13C NMR spectroscopy and, when pertinent and allowed by the solubility of the compound, 113Cd or 199Hg NMR spectroscopy. In the complexes of Group 12 metals, both ligands are neutral and S-monodentate. In the complexes of copper or Group 10 metals, 4ML1 is monodeprotonated and S,N-bidentate.

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