Synthesis and Characterization of Bidentate Isonitrile Iron Complexes

Divalent iron complexes trans-[FeBr2(BINC)2], [Cp*FeCl(BINC)] (Cp* = Me5C5) and [FeBr2(CNAr3NC)2] with chelat-ing bis(isonitrile) ligands BINC (bis(2-isocyanophenyl)phenylphosphonate) and CNAr3NC (2,2’’-diisocyano-3,5,3’’,5’’tetramethyl-1,1’:3’,1’’-terphenyl) have been prepared and characterized. Their subsequent reduction yields di- and trinuclear compounds [Fe3(BINC)6], [Cp*Fe(BINC)]2, [Fe(CNAr3NC)2]2 and [K(Et2O)]2[Fe(CNAr3NC)2]2. The molecular structures of all new species were determined by X-ray crystallography. The molecular structures are compared to related iron carbonyl complexes. The complexes were further characterized by NMR and IR spectroscopy, and the electrochemical properties of selected compounds were analyzed by UV-Vis-NIR spectroelectrochemistry. <br>

Download Full-text

Synthesis and characterization of manganese complexes of the dibenzophospholyl ligand

Canadian Journal of Chemistry ◽

10.1139/v01-124 ◽

2001 ◽

Vol 79 (9) ◽

pp. 1321-1329 ◽

Cited By ~ 11

Author(s):

Andreas Decken ◽

Melanie A Neil ◽

Frank Bottomley

Keyword(s):

Mass Spectrometry ◽

Ir Spectroscopy ◽

Phosphorus Atom ◽

Manganese Complexes ◽

Synthesis And Characterization ◽

Carbonyl Complexes ◽

X Ray ◽

Manganese Carbonyl

Manganese carbonyl complexes bearing dibenzophospholyl (DBP) and 1-phenyldibenzophosphole (Ph-DBP) ligands have been prepared. Reaction of Li-DBP with Mn(CO)5Br gave (µ2-DBP)(µ2-Br)Mn2(CO)8, while reaction of bis(1,1'-dibenzophospholyl) and Mn2(CO)10 yielded (µ2-DBP)2Mn2(CO)8. The phosphine adducts (Ph-DBP)Mn2(CO)9 and (Ph-DBP)2Mn2(CO)8 were obtained by reaction of Ph-DBP and Mn2(CO)10. The ligands are σ-bonded through the phosphorus atom in all complexes. The compounds were characterized by 1H, 13C, and 31P NMR and IR spectroscopy, mass spectrometry, and X-ray diffraction.Key words: dibenzophospholyl, dibenzophosphole, manganese, heterocycle.

Download Full-text

Preparation and characterization of a new series of Cr(II) hydroborates

Canadian Journal of Chemistry ◽

10.1139/v95-139 ◽

1995 ◽

Vol 73 (7) ◽

pp. 1126-1134 ◽

Cited By ~ 18

Author(s):

Michel Dionne ◽

Shoukang Hao ◽

Sandro Gambarotta

Keyword(s):

Trinuclear Complex ◽

Synthesis And Characterization ◽

Crystal Data ◽

X Ray ◽

X Ray Crystallography ◽

Quadruple Bond ◽

Quadruple Bonds ◽

Reaction Proceeds

The synthesis and characterization of a new series of mono-, di-, and trinuclear Cr(II) borohydride compounds is described. The reaction of CrCl2(TMEDA) with two equivalents of NaBH4 afforded the thermally unstable (TMEDA)Cr(BH4)2 (1), which was converted by treatment with pyridine into the octahedral monomeric (Py)4Cr(BH4)2 (2). The reaction proceeds via formation of an intermediate trinuclear complex {[(TMEDA)(Py)Cr(η2-BH4)]2[(Py)2Cr(η2-BH4)2]}(µ,η1-BH4)2 (3), which was isolated and characterized by X-ray crystallography. Reaction of 1 and 2 with both CO2 and RN=C=NR (R = Cy, iPr) afforded hydride insertion and formation of the corresponding diamagnetic lantern-type Cr(II) formate (HCO2)4Cr2Py2 (4) and formamidinate compounds [RNC(H)NR]2Cr2(µ-BH)4 (R = Cy (5a), iPr (5b)), respectively, with supershort Cr—Cr quadruple bonds. The structures of 1, 2, 3, and 5b were elucidated by X-ray analysis. Crystal data are as follows. 1: C6H24N2B2Cr, monoclinic, Cc, a = 8.517(2) Å, b = 15.921(5) Å, c = 9.624(2) Å, β = 115.59(1)°, Z = 4, R = 0.022, Rw = 0.029; 2: C28H44N4B2O2Cr, monoclinic, P21/n, a = 12.021(1) Å, b = 15.555(1) Å, c = 15.723(1) Å, β = 90.13(2)°, Z = 4, R = 0.074, Rw = 0.086; 3: C32H76N8B6Cr3, monoclinic, P21/n, a = 8.515(1) Å, b = 14.525(1) Å, c = 18.286(2) Å, β = 91.38(1)°, Z = 2, R = 0.051, Rw = 0.060; 5b: C21H49N6BCr2, monoclinic, C2/c, a = 17.000(1) Å, b = 9.033(1) Å, c = 19.160(1) Å, β = 105.579(9)°, Z = 4, R = 0.069, Rw = 0.078. Keywords: divalent chromium, borohydride, Cr—Cr quadruple bond.

Download Full-text

Synthesis and characterization of a new aroylhydrazone ligand and its cobalt(III) complexes: X-ray crystallography and in vitro evaluation of antibacterial and antifungal activities

Journal of Molecular Structure ◽

10.1016/j.molstruc.2018.10.061 ◽

2019 ◽

Vol 1178 ◽

pp. 544-553 ◽

Cited By ~ 13

Author(s):

Nimya Ann Mathews ◽

Anitha Jose ◽

M.R. Prathapachandra Kurup

Keyword(s):

Synthesis And Characterization ◽

In Vitro Evaluation ◽

Antifungal Activities ◽

X Ray ◽

X Ray Crystallography ◽

Antibacterial And Antifungal Activities ◽

Antibacterial And Antifungal

Download Full-text

Synthesis and characterization of the binuclear diamido titanium chalcogenides [(Ar)NCH2CH2CH2N(Ar)]2Ti(µ-E)2 (E = Se, Te)

Canadian Journal of Chemistry ◽

10.1139/v02-052 ◽

2002 ◽

Vol 80 (11) ◽

pp. 1524-1529 ◽

Cited By ~ 2

Author(s):

Tianle Zhang ◽

Warren E Piers ◽

Masood Parvez

Keyword(s):

Solid State ◽

Key Words ◽

Synthesis And Characterization ◽

Catalyst Precursor ◽

Tellurium Atom ◽

Titanium Complex ◽

X Ray ◽

X Ray Crystallography ◽

Atom Source

Reaction of McConville's chelating amido titanium complex [(Ar)NCH2CH2CH2N(Ar)]Ti(CH3)2 (Ar = 2,6-i-Pr2C6H3) with either elemental Se or the tellurium atom source Te=PBu3 resulted in the formation of bis-µ-chalcogenido dimers [(Ar)NCH2CH2CH2N(Ar)]2Ti(µ-E)2 (E = Se, 2; Te, 3) with concommitant loss of EMe2. The dimers 2 and 3 were characterized spectroscopically and via X-ray crystallography. The two compounds are isostructural in the solid state. The tellurido dimer 3 may also be synthesized by reduction of the diamido dichloride [(Ar)NCH2CH2CH2N(Ar)]2TiCl2 with NaHg amalgam followed by treatment with Te=PBu3. This dimer is unreactive toward further Te=PBu3 or stannanes such as HSnBu3. Unlike decamethyltitanocene derivatives, the diamido complex is not an effective catalyst precursor for the heterohydrodecoupling of Te=PBu3 and HSnBu3.Key words: diamido titanium complexes, selenides, tellurides.

Download Full-text

CAAC Boranes. Synthesis and characterization of cyclic (alkyl) (amino) carbene borane complexes from BF3 and BH3

Beilstein Journal of Organic Chemistry ◽

10.3762/bjoc.6.82 ◽

2010 ◽

Vol 6 ◽

pp. 709-712 ◽

Cited By ~ 16

Author(s):

Julien Monot ◽

Louis Fensterbank ◽

Max Malacria ◽

Emmanuel Lacôte ◽

Steven J Geib ◽

...

Keyword(s):

Silica Gel ◽

Synthesis And Characterization ◽

Gel Chromatography ◽

Nmr Analysis ◽

X Ray ◽

X Ray Crystallography ◽

In Situ Formation ◽

Silica Gel Chromatography

In situ formation of two cyclic (alkyl) (amino) carbenes (CAACs) followed by addition of BF3•Et2O provided the first two examples of CAAC–BF3 complexes: 1-(2,6-diisopropylphenyl)-3,5,5-trimethyl-3-phenylpyrrolidin-2-ylidene trifluoroborane, and 2-(2,6-diisopropylphenyl)-3,3-dimethyl-2-azaspiro[4.5]decan-1-ylidene trifluoroborane. These CAAC–BF3 complexes are robust compounds that are stable to ambient laboratory conditions and silica gel chromatography. They were characterized by spectroscopy and X-ray crystallography. In contrast, a CAAC complex with borane (BH3) was readily formed in situ according to 1H and 11B NMR analysis, but did not survive the workup conditions. These results set the stage for further studies of the chemistry of CAAC boranes.

Download Full-text

Synthesis and characterization of technetium(V) and (VII) complexes with bidentate nitrogen donor ligands. X-ray molecular structures of tetrabutylammonium bis(1,2-diimidobenzene)oxotechnetium(V) and tris(1,2-diimidobenzene)technetium(VII) pertechnetate

Inorganica Chimica Acta ◽

10.1016/s0020-1693(00)86834-6 ◽

1992 ◽

Vol 202 (2) ◽

pp. 191-196 ◽

Cited By ~ 24

Author(s):

Thomas I.A. Gerber ◽

Hanelie J. Kemp ◽

Jan G.H. du Preez ◽

Giuliano Bandoli ◽

Alessandro Dolmella

Keyword(s):

Molecular Structures ◽

Donor Ligands ◽

Synthesis And Characterization ◽

Nitrogen Donor Ligands ◽

X Ray ◽

Nitrogen Donor

Download Full-text

Synthesis and characterization of novel bioactive 1,2,4-oxadiazole natural product analogs bearing the N-phenylmaleimide and N-phenylsuccinimide moieties

Beilstein Journal of Organic Chemistry ◽

10.3762/bjoc.9.259 ◽

2013 ◽

Vol 9 ◽

pp. 2202-2215 ◽

Cited By ~ 26

Author(s):

Catalin V Maftei ◽

Elena Fodor ◽

Peter G Jones ◽

M Heiko Franz ◽

Gerhard Kelter ◽

...

Keyword(s):

Natural Product ◽

Synthesis And Characterization ◽

Aminobenzoic Acid ◽

One Pot ◽

X Ray ◽

X Ray Crystallography ◽

Quisqualic Acid ◽

Oxobutanoic Acid

Taking into consideration the biological activity of the only natural products containing a 1,2,4-oxadiazole ring in their structure (quisqualic acid and phidianidines A and B), the natural product analogs 1-(4-(3-tert-butyl-1,2,4-oxadiazol-5-yl)phenyl)pyrrolidine-2,5-dione (4) and 1-(4-(3-tert-butyl-1,2,4-oxadiazol-5-yl)phenyl)-1H-pyrrole-2,5-dione (7) were synthesized starting from 4-(3-tert-butyl-1,2,4-oxadiazol-5-yl)aniline (1) in two steps by isolating the intermediates 4-(4-(3-tert-butyl-1,2,4-oxadiazol-5-yl)phenylamino)-4-oxobutanoic acid (3) and (Z)-4-(4-(3-tert-butyl-1,2,4-oxadiazol-5-yl)phenylamino)-4-oxobut-2-enoic acid (6). The two natural product analogs 4 and 7 were then tested for antitumor activity toward a panel of 11 cell lines in vitro by using a monolayer cell-survival and proliferation assay. Compound 7 was the most potent and exhibited a mean IC50 value of approximately 9.4 µM. Aniline 1 was synthesized by two routes in one-pot reactions starting from tert-butylamidoxime and 4-aminobenzoic acid or 4-nitrobenzonitrile. The structures of compounds 1, 2, 4, 5 and 6 were confirmed by X-ray crystallography.

Download Full-text

Synthesis and Characterization of Tetrakis(pentafluoroethyl)germane

Synthesis ◽

10.1055/s-0036-1589005 ◽

2017 ◽

Vol 49 (11) ◽

pp. 2389-2393 ◽

Cited By ~ 3

Author(s):

Stefanie Pelzer ◽

Beate Neumann ◽

Hans-Georg Stammler ◽

Nikolai Ignat’ev ◽

Reint Eujen ◽

...

Keyword(s):

Mass Spectrometry ◽

Nmr Spectroscopy ◽

Ir Spectroscopy ◽

Diffraction Analysis ◽

Spectroscopic Characterization ◽

Synthesis And Characterization ◽

X Ray Diffraction ◽

X Ray ◽

Comprehensive Characterization

This paper describes the synthesis and comprehensive characterization of tetrakis(pentafluoroethyl)germane. In addition to a complete NMR spectroscopic characterization, including the rarely used 73Ge NMR spectroscopy, Ge(C2F5)4 was studied by IR spectroscopy, mass spectrometry as well as X-ray diffraction analysis. A 73Ge NMR investigation as well as an X-ray diffraction study of the related germane Ge(CF3)4 are also included.

Download Full-text