Preparation, properties and structure of some intermediate nido- and arachno-monocarbaboranes

1981 ◽  
Vol 46 (10) ◽  
pp. 2345-2353 ◽  
Author(s):  
Karel Baše ◽  
Bohumil Štíbr ◽  
Jiří Dolanský ◽  
Josef Duben
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
Nmr Spectra ◽  
Liquid Ammonia ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Starting Compound

The 6-N(CH3)3-6-CB9H11 carbaborane reacts with sodium in liquid ammonia with the formation of 6-CB9H12- which was used as a starting compound for preparing the 4-CB8H14, 9-L-6-CB9H13 (L = (CH3)2S, CH3CN and P(C6H5)3), 1-(η5-C5H5)-1,2-FeCB9H10-, and 2,3-(η5-C5H5)2-2,31-Co2CB9H10- carboranes. The 4-CB8H14 compound was dehydrogenated at 623 K to give 4-(7)-CB8H12 carborane. Base degradation of 6-N(CH3)3-6-CB9H11 in methanol resulted in the formation of 3,4-μ-N(CH3)3CH-B5H10. The structure of all compounds was proposed on the basis of their 11B and 1H NMR spectra and X-ray diffraction was used in the case of the transition metal complexes.

G. Schmid-R. Greese • Tetraschwefeltetraimid als Ligand in Übergangsmetallkomplexen / Tetrasulfur Tetraimide as Ligand in Transition Metal Complexes

1982 ◽  
Vol 37 (5) ◽  
pp. 620-626 ◽  
Author(s):  
Günter Schmid ◽  
Richard Greese ◽  
R. Boese
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
X Ray ◽  
H Nmr

Tetrasulfur tetraimide reacts with (THF)M(CO)5 (M = Cr, W) to form isolable complexes of the type (S4N4H4)M(CO)5 (1) and (S4N4H4)[M(CO)5]2 (2) respectively, 1H NMR and X-ray investigations show the metal to be coordinated to sulfur atoms. In solution partially dissociation of M(CO)5 moieties is observed leading to different equilibria. They are studied by 1H NMR

Syntheses and Structure Investigations of 3d Transition Metal Complexes with a Flexible N4O2-Donor Hexadentate Schiff-Base Ligand

2017 ◽  
Vol 70 (5) ◽  
pp. 581 ◽  
Author(s):  
Kyle J. Howard-Smith ◽  
Alexander R. Craze ◽  
Mohan Badbhade ◽  
Christopher E. Marjo ◽  
Timothy D. Murphy ◽  
...  
Keyword(s):  
Schiff Base ◽  
Transition Metal ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
Schiff Base Ligand ◽  
High Resolution Mass Spectrometry ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Investigations

The syntheses and structure investigations of four new 3d transition metal complexes (1–4) with a flexible N4O2-donor hexadentate Schiff-base ligand are described; three complexes (1, 2, and 4) of FeIII, CoIII, and CuII metal ions have been investigated by UV-vis, FT-IR, high-resolution mass spectrometry (HR-MS), and scanning electron microscopy–electron dispersive spectroscopy, as well as single crystal X-ray diffraction. The X-ray structure of NiII complex 3 is also reported. The molecular structures of the complexes (1–3) demonstrate distorted octahedral coordination geometry, each exhibiting 1 : 1 (M : L) ratios and the CuII complex 4 shows a trinuclear structure with a CuII : L ratio of 3 : 2 in the solid state, which has been proven by X-ray diffraction. On the other hand, a mononuclear species of the CuII complex is formed in solution, which has been identified by electrospray ionization HR-MS.

scholarly journals Darstellung neuer Monofluorphosphine und einiger ihrer Übergangsmetallkomplexe; Einkristall-Röntgenstrukturanalyse eines Platin(II)-Komplexes / Preparation of New Monofluorophosphines and Some of their Transition Metal Complexes; Single Crystal X-Ray Diffraction Study of a Platinum(II) Complex

1993 ◽  
Vol 48 (7) ◽  
pp. 875-885 ◽  
Author(s):  
Thomas G. Meyer ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Single Crystal ◽  
Diffraction Study ◽  
Structure Analysis ◽  
Transition Metal Complexes ◽  
Classical Method ◽  
X Ray Diffraction ◽  
X Ray

The reaction of lithiated precursors with PCl2F led to a number of monofluorophosphines, including the known di-tert-butylmonofluorophosphine, 1. Bis(phenylethinyl)monofluorophosphine (2) was accessible only via this route (the classical method of synthesizing 2 by chlorine/fluorine exchange is impossible, because the corresponding chlorophosphine is unknown). Bis(2-methoxyphenyl)fluorophosphine (5) was prepared via the organolithium/PCl2F route. The NMR results for 5 thus prepared were inconsistent with previous reports, implying that the previously reported synthesis of 5 is in error. From 5 a cis-dichloroplatinum(II) complex (6) was synthesized and subjected to a single crystal X-ray structure analysis, confirming the expected planar coordination. From bis(2,3-dimethoxynaphthyl)monofluorophosphine (7) a rhodium(I) (8) and an iron(0)tetracarbonyl complex (9) were prepared. An iron(0)tetracarbonyl complex (11) was synthesized from bis(9-anthryl)monofluorophosphine (10) which was found to be stable to redox disproportionation.

Optisch aktive Übergangsmetall-Komplexe, 84 [1] Substituenten-Effekte in Diastereomerengleichgewichten von quadratisch-pyramidalen Mo-Komplexen / Optically Active Transition Metal Complexes, 84 [1] Substituent Effects in Diastereomer Equilibria of Square-Pyramidal Mo Complexes

1983 ◽  
Vol 38 (7) ◽  
pp. 852-857 ◽  
Author(s):  
Henri Brunner ◽  
Beate Schönhammer
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
Nmr Spectra ◽  
Substituent Effects ◽  
Optically Active ◽  
Asymmetric Induction ◽  
Chiral Ligand ◽  
H Nmr ◽  
Active Transition

Amidinato complexes with sub­stituents R at the cyclopentadienyl and R′ in the p-position of the phenyl at the asym­metric C atom were synthesized and characterized. The diastereomers differing in their 1H NMR spectra were partly separated by fractional crystallization. After equilibration with respect to the labile Mo configuration the diastereomer ratio, a measure for the asymmetric induction from the chiral ligand on the formation of the two Mo configura­tions at equilibrium, was determined by 1H NMR integration. The diastereomer ratio decreases for substituents R′ = F and R = CH3, and increases for R' = OCH3, com­pared to the unsubstituted compound.

Heavy transition metal complexes of biologically important molecules. I. The crystal and molecular structure of trans-dichloro(bis(isopropyl)-sulfoxide-S)(1-methylcytosine-N)platinum(II)

1976 ◽  
Vol 54 (1) ◽  
pp. 53-58 ◽  
Author(s):  
Colin James Lyne Lock ◽  
Robert Anthony Speranzini ◽  
John Powell
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Metal Complexes ◽  
Single Crystal ◽  
Least Squares ◽  
Transition Metal Complexes ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray

The crystal and molecular structure of trans-dichloro(bis(isopropyl)sulfoxide-S)(1-methylcytosine-N)platinum(II) has been determined by single crystal X-ray diffraction. The crystals are triclinic with a = 16.205(5), b = 8.078(2), c = 6.776(2) Å, α = 106.53(2), β = 96.35(2), γ = 98.54(2)°. The space group is [Formula: see text] and there are two molecules per unit cell. A total of 2294 independent reflections, of which 2023 were observed, were examined on a Syntex [Formula: see text] diffractometer. The structure was refined by full matrix least squares analysis to an R2 value of 0.0427. The ligands form a rough square around the platinum atom with Pt—Cl(1), 2.304(3), Pt—Cl(2), 2.287(4), Pt—S, 2.232(2), Pt—N, 2.058(7). Distances within the ligands are normal. The plane of the cytosine ring is at 84.4° to the plane formed by the ligands around platinum.

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