Structure de (diméthyl-5,5 diphényl-1,9 tétraaza-3,4,6,7 nonatétraène-1,3,6,8 diolato-1,9-O,O',N,N')nickel(II), [Ni(C19H18N4O2)]

A quantitative analysis is made of the problem of obtaining accurate polarization measurements in Raman microspectroscopy. The introduction of experimentally determined correction factors arising from the optical properties of the beam splitter allows the depolarization by the microscope objective to be studied separately. Correction curves are calculated for the various parameters which characterize the light-excitation path and the light-collection path. These parameters are functions of both the numerical aperture of the objective and the refractive index of the (isotropic) sample. The introduction of these parameters into the expressions for the depolarization ratios of various Raman and resonance Raman bands accounts well for the differences noted between the results of the present microprobe measurements and those obtained with conventional instruments. The values determined here are, within experimental error, in agreement with the calculated results over a large range of depolarization ratios.

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Polarization measurements in Raman microspectroscopy. I—Isotropic samples

Brémard

Laureyns

Merlin

et al. 1987

J Raman Spectroscopy

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Resonance Raman studies of a dioxy-tetraaza-nickel complex containing a cofacial dimeric structure

Bariz

Brémard

Sueur

1986

Journal of Molecular Structure

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Synthesis, Structure, and Solution Reduction Reactions of Volatile and Thermally Stable Mid to Late First Row Transition Metal Complexes Containing Hydrazonate Ligands

et al. 2013

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Treatment of MCl2 (M = Ni, Co, Fe, Mn, Cr) with 2 equiv of the hydrazonate salts K(tBuNNCHCtBuO), K(tBuNNCHCiPrO), or K(tBuNNCMeCMeO) afforded the complexes M(tBuNNCHCtBuO)2 (M = Ni, 65%; Co, 80%; Fe, 83%; Mn, 68%; Cr, 64%), M(tBuNNCHCiPrO)2 (M = Ni, 63%; Co, 86%; Fe, 75%), and M(tBuNNCMeCMeO)2 (M = Ni, 34%; Co, 29%; Fe, 27%). Crystal structure determinations of Co(tBuNNCHCtBuO)2, M(tBuNNCHCiPrO)2 (M = Ni, Co), and M(tBuNNCMeCMeO)2 (M = Ni, Co, Fe) revealed monomeric complexes with tetrahedral geometries about the metal centers. To evaluate the potential of these new complexes as film growth precursors, preparative sublimations, thermogravimetric analyses, solid state decomposition studies, and solution reactions with reducing coreagents were carried out. M(tBuNNCHCtBuO)2 sublime between 120 and 135 °C at 0.05 Torr, whereas M(tBuNNCHCiPrO)2 and M(tBuNNCMeCMeO)2 sublime between 100 and 105 °C at the same pressure. All complexes afforded ≥96% recovery of sublimed material, with ≤3% of nonvolatile residues. The solid state decomposition temperatures were highest for M(tBuNNCHCiPrO)2 (273-308 °C), intermediate for M(tBuNNCHCtBuO)2 (241-278 °C), and lowest for M(tBuNNCMeCMeO)2 (235-250 °C). Treatment of Co(tBuNNCHCtBuO)2 in tetrahydrofuran with hydrazine, BH3(L) (L = NHMe2, SMe2, THF), pinacol borane, and LiAlH4 led to rapid formation of cobalt metal, while analogous reductions of Mn(tBuNNCHCtBuO)2 with BH3(THF), pinacol borane, and LiAlH4 appeared to afford manganese metal. The new complexes M(tBuNNCHCtBuO)2, M(tBuNNCHCiPrO)2, and M(tBuNNCMeCMeO)2 have very promising properties for use as precursors for the growth of the respective metals in atomic layer deposition film growth processes.

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Structure de (diméthyl-5,5 diphényl-1,9 tétraaza-3,4,6,7 nonatétraène-1,3,6,8 diolato-1,9-O,O',N,N')nickel(II), [Ni(C19H18N4O2)]

Cited by 3 publications

References 7 publications

Polarization measurements in Raman microspectroscopy. I—Isotropic samples

Polarization measurements in Raman microspectroscopy. I—Isotropic samples

Resonance Raman studies of a dioxy-tetraaza-nickel complex containing a cofacial dimeric structure

Synthesis, Structure, and Solution Reduction Reactions of Volatile and Thermally Stable Mid to Late First Row Transition Metal Complexes Containing Hydrazonate Ligands

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