X-ray crystal structure of the trifluoroacetylcobalt complex CF3COCo(CO)3(PPh3) – Implications for the relationship between structure and reactivity toward migratory insertion of carbon monoxide in cobalt alkyl complexes

2009 ◽  
Vol 362 (1) ◽  
pp. 113-116 ◽  
Author(s):  
Nanda Gunawardhana ◽  
Stephen L. Gipson ◽  
Andreas Franken
1988 ◽  
Vol 43 (10) ◽  
pp. 1256-1262 ◽  
Author(s):  
Hans-Friedrich Klein ◽  
Goetz Lull ◽  
Birgit Rodenhäuser ◽  
Gerhard Cordier ◽  
Helmut Paulus

Mononuclear cobalt(o) complexes containing olefin and trimethylphosphane ligands Co(olefin)(PMe3)3 (olefin = C2H4 (1), C3H6 (2), cyclopentene (3), trans-1,2-diphenylethene (4), tetrafluorobenzo-bicyclo-(2.2.2)-octadiene (5)), are obtained from CoCl2 by reaction with magnesium in the presence of the ligands or by substitution of 3 with olefin. X-ray crystal structure determinations of 4 and 5 show a distorted tetrahedral arrangement of ligands around the cobalt atom. Chemical and spectroscopic properties are consistent with a paramagnetic valence state of the compounds in solution. By reaction with carbon monoxide a dicobalt complex is formed, while azobenzene gives paramagnetic Co(N2Ph2)(PMe3)2.


2000 ◽  
Vol 55 (11) ◽  
pp. 1095-1098
Author(s):  
Mutlaq Al-Jahdali ◽  
Paul K. Baker ◽  
Michael B. Hursthouse ◽  
Simon J. Coles

Reaction of [MI2(CO)(NCMe)(η2-EtC2Et)2] (M = Mo,W) with one equivalent of 2,2' -bipyridine (bipy) in CH2C12 at room temperature gives either the neutral complex, [MoI2(CO)(bipy)- (η2-EtC2Et)] (1) or the cationic complex, [WI(CO)(bipy)(η2-EtC2Et)2]I (2). The neutral molybdenum complex 1, has been crystallographically characterised, and has a pseudo-octahedral geometry with the iodo-ligand trans to the 3-hexyne, and with the bipy, carbon monoxide and other iodo-ligand occupying the equatorial face. 13C NMR studies show the 3-hexyne is donating four electrons to the molybdenum in 1.


2008 ◽  
Vol 63 (3) ◽  
pp. 345-348 ◽  
Author(s):  
Artem A. Babaryk ◽  
Igor V. Zatovsky ◽  
Nikolay S. Slobodyanik ◽  
Ivan V. Ogorodnyk

A new complex phosphate K1.84Fe1.42Nb0.58(PO4)3 has been synthesized by the self-flux technique. The X-ray single crystal structure and magnetic properties were studied. The compound crystallizes in the cubic system with space group P213 (a = 9.9404(10) Å ) and belongs to the langbeinite structure type. The structure contains [M2P3O18] building units. “Closed” fragments [M8P9O60] provide space for location of two potassium atoms. Antiferromagnetic interactions were detected at low temperatures which originate from superexchange through a M(1)-O-P-O-M(2) pathway with corresponding J = −5.5(1) cm−1. The relationship between the UV/vis absorption and the structure is discussed.


Crystals ◽  
2019 ◽  
Vol 9 (11) ◽  
pp. 561 ◽  
Author(s):  
Tatsuya Tanaka ◽  
Chiaki Tsuboi ◽  
Kazuaki Aburaya ◽  
Fumiko Kimura ◽  
Masataka Maeyama ◽  
...  

We previously reported on a method for X-ray single-crystal structure determination from a powder sample via a magnetically oriented microcrystal suspension (MOMS). The method was successfully applied to orthorhombic microcrystals (L-alanine, P212121). In this study, we apply this method to monoclinic microcrystals. Unlike most of the orthorhombic MOMSs, monoclinic MOMSs exhibit two or four orientations with the same magnetic energy (we refer to this as twin orientations), making data processing difficult. In this paper, we perform a MOMS experiment for a powder sample of monoclinic microcrystal (α-glycine, P21/n) to show that our method can also be applied to monoclinic crystals. The single-crystal structure determined in this work is in good agreement with the reported one performed on a real single crystal. Furthermore, the relationship between the crystallographic and magnetic susceptibility axes is determined.


1994 ◽  
Vol 47 (6) ◽  
pp. 1043 ◽  
Author(s):  
D Anastasiou ◽  
EM Campi ◽  
H Chaouk ◽  
GD Fallon ◽  
WR Jackson ◽  
...  

Rhodium- catalysed reactions of o- or p- cyano-N-allylanilines with H2/CO give N- arylpyrrolidine aldehydes resulting from a double hydroformylation sequence. In contrast reactions of o- or p-methyl-N-allylanilines or N- allylaniline itself with H2/CO give ' dimeric ' compounds resulting from self-condensation reactions of an initially formed hydroformylation product together with varying amounts of the double hydroformylation product. Similar reactions of o-cyano-N-but-3-enylanilines give low yields of double hydroformylation products and major products arising from hydrogenation or cross coupling of intermediate enamines. The structure of one of these products, N-2-cyanophenyl-5-(N′-2-cyanophenyl-3-methyl-pyrrolidin-2-yl)-1,2,3,4-tetrahydropyridine (17) (IUPAC name: 2-[5-{1-(2-cyanophenyl)-3-methylpyrrolidin-2-yl}-1,2,3,4-tetrahydropyridin-1-yl] benzonitrile ) was confirmed by an X-ray single-crystal structure determination.


Author(s):  
David H. Farrar ◽  
Brian F.G. Johnson ◽  
Jack Lewis ◽  
J. Nicola Nicholls ◽  
Paul R. Raithby ◽  
...  

1993 ◽  
Vol 48 (6) ◽  
pp. 785-793 ◽  
Author(s):  
Hans-Friedrich Klein ◽  
Michael Helwig ◽  
Michael Karnop ◽  
Herbert König ◽  
Birgit Hammerschmitt ◽  
...  

Mononuclear cobalt(0) complexes Co(η2-azaolefin)(PMe3)3 (azaolefin = benzo[c]cinnoline (1), p-dimethylamino-phenyl(phenyl)diazene (2), 1/2 diazobenzene (3), bis(p-tolyl)diazene (4), bis(p-fluorphenyl)diazene (5), bis(p-trifluoromethyl-phenyl)diazene (6), phenylisocyanate (7)) are obtained from Co(cyclo-C5H8)(PMe3)3 by substitution of the olefin. X-ray crystal structure determinations of 1 and 7 show tetrahedral arrangements of ligands around the cobalt atom. By reaction with carbon monoxide carbonyl(phosphine)cobalt(0) complexes are formed. 7 catalyses the cyclotrimerization of phenylisocyanate, while with CoCl(PMe3)3 as a catalyst the cyclic dimer of phenylisocyanate is selectively formed. A convenient synthesis for CoCl(PMe3)3 is described.


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