scholarly journals Softening the Donor-Set: From [Cu(P^P)(N^N)][PF6] to [Cu(P^P)(N^S)][PF6]

Inorganics ◽  
2019 ◽  
Vol 7 (1) ◽  
pp. 11 ◽  
Author(s):  
Isaak Nohara ◽  
Alessandro Prescimone ◽  
Catherine Housecroft ◽  
Edwin Constable
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Spectroscopic Data ◽  
1H Nmr Spectroscopy ◽  
Variable Temperature ◽  
Synthesis And Characterization ◽  
Single Crystal Structures ◽  
Roesy Spectrum ◽  
Vt Nmr

We report the synthesis and characterization of [Cu(P^P)(N^S)][PF6] complexes with P^P = bis(2-(diphenylphosphino)phenyl) ether (POP) or 4,5-bis(diphenylphosphino)-9,9- dimethylxanthene (xantphos) and N^S = 2-(iso-propylthio)pyridine (iPrSpy) or 2-(tert-butylthio)pyridine (tBuSpy). The single crystal structures of [Cu(POP)(iPrSPy)][PF6] and [Cu(POP)(tBuSPy)][PF6] have been determined and confirm a distorted tetrahedral copper(I) centre and chelating P^P and N^S ligands in each complex. Variable temperature (VT) 1H and 31P{1H} NMR spectroscopy reveals dynamic behavior with motion of the POP backbone in [Cu(POP)(iPrSPy)][PF6] and [Cu(POP)(tBuSPy)][PF6] frozen out at 238 K. VT NMR spectroscopic data including EXSY peaks in the ROESY spectrum of [Cu(xantphos)(tBuSPy)][PF6] at 198 K reveal that two conformers exist in an approximate ratio of 5:1. Replacing bpy by the N^S ligands shifts the Cu+/Cu2+ oxidation to a higher potential. The copper(I) compounds are weak emitters in the solid state with PLQY values of <2%. These values are similar to those for [Cu(POP)(bpy)][PF6] and [Cu(xantphos)(bpy)][PF6] in the solid state.

scholarly journals Synthesis and characterization of new Oxazine , Thiazine and Pyrazol derived from chalcones

2014 ◽  
Vol 11 (2) ◽  
pp. 477-485 ◽  
Author(s):  
Baghdad Science Journal
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrazine Hydrate ◽  
Elemental Analysis ◽  
Potassium Hydroxide ◽  
1H Nmr Spectroscopy ◽  
Room Temperature ◽  
Potassium Hydroxide Solution ◽  
Synthesis And Characterization ◽  
Heterocyclic Derivatives

In this study, chalcones were synthesis by condensing 2-acetylpyridine with aromatic aldehyde derivatives in dilute ethanolic potassium hydroxide solution at room temperature according to Claisen-Schmidt condensation. After that, new heterocyclic derivatives such as Oxazine, Thiazine and Pyrazol were synthesis by reaction between chalcones with urea, thiourea and hydrazine hydrate respectively scheme 1. All these compounds wrer characterization by FTIR, 1H-NMR spectroscopy and elemental analysis.

Synthesis and Characterization of Three Novel Nitrogen-containing Macrolides

2011 ◽  
Vol 66 (9) ◽  
pp. 930-934
Author(s):  
Xin Leng ◽  
Bingqin Yang ◽  
Yuanyuan Liu ◽  
Yi Xie ◽  
Jie Tong
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
1H Nmr Spectroscopy ◽  
Mass Spectra ◽  
Synthesis And Characterization ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Preparation Methods ◽  
X Ray

Three novel nitrogen-containing macrolides have been synthesized by esterification. All of them have been characterized by infrared (IR), elemental analysis, mass spectra (MS), and 1H NMR spectroscopy, and their crystal structures were determined by single-crystal X-ray diffraction. The preparation methods and the intermolecular associations based on C-H・・・O hydrogen bonds and π- π stacking interactions are discussed.

Synthesis and Characterization of Indolylfulgide Photochromic Colorants

2013 ◽  
Vol 821-822 ◽  
pp. 522-526
Author(s):  
Ning Ning Lv ◽  
An Guo Sang ◽  
Yan Zhang
Keyword(s):  
Nmr Spectroscopy ◽  
1H Nmr Spectroscopy ◽  
Room Temperature ◽  
Uv Light ◽  
Synthesis And Characterization ◽  
Indole Derivatives ◽  
Thermal Stabilities ◽  
Nmr Data ◽  
New Compounds

This paper describes the synthesis of two photochromic 2-indolyl-fulgides by stobbe condensation of the corresponding 2-acyl-1,3-dimethyl-indole derivatives with diethyl isopropylidene succinate in the presence of hexamethyldisilazane potassium. The overall yields was up to 41% for 3 steps. Both prepared compounds are sensitive to UV light and change colors upon irradiation. And the two fulgides can be switched back and forth 100 times without obvious degradation. Thermal stabilities of the fulgides in acetonitrile at room temperature for 30 days and at 80 °C for 12 h were measured using UV-vis and 1H NMR spectroscopy. The absorption spectra of both forms did not exhibit any sign of degradation. The NMR data indicated that no new compounds were detected. The utilization of these materials for use in photochromic textiles were discussed.

Structural characterization of polyallene in the solid state as studied by variable-temperature high-resolution carbon-13 NMR spectroscopy

1991 ◽  
Vol 24 (8) ◽  
pp. 2011-2014 ◽  
Author(s):  
Kyung Hoon Min ◽  
Hiromichi Kurosu ◽  
Isao Ando ◽  
Takakazu Yamamoto ◽  
Takaki Kanbara
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
High Resolution ◽  
Structural Characterization ◽  
Variable Temperature

Phenylsilane dehydrocoupling and addition to styrene catalyzed by (R-indenyl)Ni(phosphine)(methyl) complexes

2009 ◽  
Vol 87 (1) ◽  
pp. 280-287 ◽  
Author(s):  
Yaofeng Chen ◽  
Davit Zargarian
Keyword(s):  
Solid State ◽  
Nmr Spectra ◽  
Variable Temperature ◽  
Structural Parameters ◽  
Catalytic Cycle ◽  
Synthesis And Characterization ◽  
H Nmr ◽  
Solid State Structures ◽  
Indenyl Complexes

This report describes the synthesis and characterization of the Ni–Me complexes (R-indenyl)Ni(PR′3)Me (R = 1-i-Pr, 1-SiMe3, and 1,3-(SiMe3)2; R′= Me, Ph) and outlines their catalytic reactivities in the dehydrogenative oligomerization of PhSiH3 and its addition to styrene in the absence of initiators/activators. Observation of higher hydrosilylation activities for PPh3-based compounds featuring bulky substituents on the indenyl ligand confirms earlier suggestions that phosphine dissociation is an important component of the catalytic cycle for this reaction. In contrast, oligomerization of PhSiH3 is more facile with PMe3-based precursors and independent of the steric bulk of the indenyl ligand, implying that this reaction does not involve phosphine dissociation. These conclusions are consistent with the variable-temperature 1H NMR spectra of {1,3,-(SiMe3)2-indenyl}Ni(PR′3)Me and various structural parameters observed in the solid-state structures of {1,3,-(SiMe3)2-indenyl}Ni(PPh3)Me, {1,3,-(SiMe3)2-indenyl}Ni(PMe3)Cl, and {1-SiMe3-indenyl}Ni(PMe3)Me.Key words: nickel-indenyl complexes, hydrosilylation, hydrosilane oligomerization.

Synthesis and characterization of dimethyl- and dimethoxyphenylbis(N,N-dialkyldithiocarbamato)tellurium(IV) and chlorodimethyl- and chlorodimethoxyphenyl-(N,N-dialkyldithiocarbamato)tellurium(IV). Crystal structures of Me2Te[S2CNMe2]2 and (p-MeOC6H4)2Te[S2CNMe2]2

1993 ◽  
Vol 71 (1) ◽  
pp. 42-50 ◽  
Author(s):  
Jane H. E. Bailey ◽  
John E. Drake
Keyword(s):  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Variable Temperature ◽  
Reductive Elimination ◽  
Synthesis And Characterization ◽  
Space Group ◽  
Cell Parameters

The compounds Me2Te[S2CNR2]2, Me2TeCl[S2CNR2], (p-MeOC6H4)2Te[S2CNR2]2, and (p-MeOC6H4)2TeCl[S2CNR2], where R = Me, Et, have been prepared and characterised primarily by vibrational and NMR spectroscopy. Variable temperature NMR spectroscopy and qualitative time studies indicate that in solution the dimethoxyphenyltellurium derivatives undergo the reductive-elimination noted for analogous phenyl derivatives but the reductive-elimination does not occur with the dimethyl tellurium derivatives. The crystal structures of Me2Te[S2CNMe2]2, 1, and (p-MeOC6H4)2-Te[S2CNMe2]2, 5, were completed. The cell parameters for 1, which crystallizes as monoclinic in space group P21/n, are a = 13.550(2), b = 13.034(2), c = 17.854(2) Å, β = 106.61(1)°, V = 3021.6(7) Å3, Z = 8, R = 0.0368, and Rw = 0.0402 and for 5, which crystallizes as monoclinic in space group C2/c, are a = 35.36(1), b = 11.063(3), c = 12.778(3) Å, β = 96.16(3)°, V = 4963(3) Å3, Z = 8, R = 0.0627, and Rw = 0.0646.

Synthesis and Characterization of Ni(II) and Pd(II) Complexes Bearing Achiral and Chiral Bidentate Aminophosphine Ligands

2007 ◽  
Vol 72 (4) ◽  
pp. 527-540 ◽  
Author(s):  
David Benito-Garagorri ◽  
Kurt Mereiter ◽  
Karl Kirchner
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Dft Calculations ◽  
Synthesis And Characterization ◽  
X Ray

The synthesis of a range of achiral and chiral bidentate aminophosphine ligands and their complexes with nickel(II) and palladium(II) has been investigated. The ligands and the complexes have been characterized by NMR spectroscopy, and X-ray structures of representative compounds have been determined. In addition, DFT calculations have been performed to investigate different geometries of the nickel(II) complexes in the solid state and in solution.

Sign in / Sign up

Export Citation Format

Share Document