Reactions of Ru3(CO)12 with Ethyne: Molecular Structure of Ru2(µ-h1,h4:h1,h4-C8H8)(CO)4

1999 ◽  
Vol 52 (5) ◽  
pp. 413 ◽  
Author(s):  
Michael I. Bruce ◽  
Brian W. Skelton ◽  
Natasha N. Zaitseva ◽  
Allan H. White

The reaction between Ru3(CO)12 and ethyne (refluxing tetrahydrofuran, 2 h) produced four binuclear complexes, Ru2(CO)m(C2H2)n [m = 4,n= 4 (1); m = 5,n= 4 (3); m = 7,n= 2 (2), 4 (4)], in low yield. The molecular structure of (1) has been determined by X-ray crystallography and consists of an Ru2(CO)4 group bridged by a C8H8 chain, attached in the µ−η1 ,η4 :η1 ,η4 mode. Structures for the other three complexes are suggested on the basis of their i.r. and mass spectra and similarities with analogous ruthenium complexes obtained from other alkynes.

Author(s):  
Shabana Noor ◽  
Richard Goddard ◽  
Fehmeeda Khatoon ◽  
Sarvendra Kumar ◽  
Rüdiger W. Seidel

AbstractSynthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes with the formula [ZnLn(HL)(µ-OAc)(NO3)2(H2O)x(MeOH)1-x]NO3 · n H2O · n MeOH [Ln = Pr (1), Nd (2)] and the crystal and molecular structure of [ZnNd(HL)(µ-OAc)(NO3)2(H2O)] [ZnNd(HL)(OAc)(NO3)2(H2O)](NO3)2 · n H2O · n MeOH (3) are reported. The asymmetrical compartmental ligand (E)-2-(1-(2-((2-hydroxy-3-methoxybenzylidene)amino)-ethyl)imidazolidin-2-yl)-6-methoxyphenol (H2L) is formed from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation, resulting in a peripheral imidazoline ring. The structures of 1–3 were revealed by X-ray crystallography. The smaller ZnII ion occupies the inner N2O2 compartment of the ligand, whereas the larger and more oxophilic LnIII ions are found in the outer O2O2’ site. Graphic Abstract Synthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes (Ln = Pr, Nd) bearing an asymmetrical compartmental ligand formed in situ from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation are reported.


2018 ◽  
Vol 73 (12) ◽  
pp. 1029-1032
Author(s):  
Peter Mayer ◽  
Hans-Christian Böttcher

AbstractTreatment of THF solutions containing the rhodium(II) complex trans-[RhCl2(PtBu2Ph)2] (1) with [Fe2(CO)9] in the same solvent resulted in the formation of the Vaska-type complex trans-[RhCl(CO)(PtBu2Ph)2] (2) in high yield. The title complex 2 was obtained as pale yellow crystals, characterized by NMR and IR spectroscopy, as well as by microanalyses. Additionally, the molecular structure of 2 has been established by X-ray crystallography. As often reported for similar constituted compounds, the chlorido and carbonyl ligands in crystals of 2 are strongly disordered.


1983 ◽  
Vol 36 (2) ◽  
pp. 253 ◽  
Author(s):  
AC McDonell ◽  
TW Hambley ◽  
MR Snow ◽  
AG Wedd

The salts Ph4As [ReO(SPh)4].MeCN and Ph4As [ReO(SePh)4] have been synthesized and characterized. The crystal and molecular structure of the thiolate compound has been determined by X-ray crystallography which reveals a square-pyramidal arrangement of ligand atoms around the central rhenium atom of the [ReO(SPh)4]- anion. Crystal data: a 9.756(4), b 18.171(3), c 25.684(4) �, space group P212121, Z 4.


1997 ◽  
Vol 75 (10) ◽  
pp. 1336-1339 ◽  
Author(s):  
Yutaka Saitoh ◽  
Take-aki Koizumi ◽  
Kohtaro Osakada ◽  
Takakazu Yamamoto

Bromation of 1,10-phenanthroline with Br2 proceeds smoothly in the presence of S2Cl2 and pyridine to give 3,8-dibromo-1,10-phenanthroline in good yield. Bromation of 2,9-dibutoxy-1,10-phenanthroline with Br2, in an aqueous medium gives 5,6-dibromo-2,9-dibutoxy-1,10-phenanthroline selectively. Similar bromination of 4,7-dibutoxy-1,10-phenanthroline with Br2 gives 3,8-dibromo-4,7-dibutoxy-1,10-phenanthroline, which forms a 1:1 adduct with Cu(NO3)2. Molecular structure of the 1:1 adduct has been determined by X-ray crystallography. Keywords: bromination, 1,10-phenanthroline, 3,8-dibromo-1,10-phenanthroline.


Author(s):  
Rosa María Claramunt ◽  
María Dolores Santa María ◽  
Isabelle Forfar ◽  
Francisco Aguilar-Parrilla ◽  
María Minguet-Bonvehí ◽  
...  

1999 ◽  
Vol 52 (1) ◽  
pp. 51 ◽  
Author(s):  
Martin A. Bennett ◽  
Christopher J. Cobley ◽  
David C. R. Hockless ◽  
Thomas Klettke

Reaction of bis(cycloocta-1,5-diene)platinum(0) with the (alkynyl)phenylsilanes Ph3SiC2But, Ph2Si(C2But)2 and PhSi(C2But)3 gives, respectively, [Pt (Ph3SiC2But)2] (1b), [Pt {Ph2Si(C2But)}]2 (2b), and [Pt {PhSi(C2But)3}]2 (4b), which contain zerovalent platinum atoms coordinated by two alkyne units. Spectroscopic data indicate that (2b) and (4b) contain two PtC4 and two SiC4 tetrahedra joined at the corners. X-Ray crystallography shows that complex (4b) is isostructural and isomorphous with the known nickel analogue, two of the alkyne units being uncoordinated; the central eight-membered ring comprising two silicon, four alkyne carbon and two platinum atoms has an approximate chair conformation. In contrast, the monomer (1b) is isostructural but not isomorphous with the analogous nickel compound (1a); in the crystal there is evidence for a weak intramolecular phenyl-phenyl interaction.


1984 ◽  
Vol 39 (5) ◽  
pp. 668-674 ◽  
Author(s):  
Ernst Otto Fischer ◽  
Rudolf Reitmeier ◽  
Klaus Ackermann

The hexacarbonyl compounds of chromium, molybdenum and tungsten react with the highly nucleophilic agent Li NiPr2 and in a subsequent alkylation with (Et3O)BF4 to give the carbene complexes (CO)5M[C(N′Pr2)OEt] (1, 3, 4). In case of W(CO)6 and Mo(CO)6 the novel biscarbene complexes cis(CO)4M[C(NiPr2)OEt]2 (2, 5) are additionally obtained. Reaction conditions, properties and spectroscopic data of the new compounds are reported. The molecular structure of cis(CO)4W[C(NiPr2)OEt]2 (4) was determined by X-ray crystallography


1984 ◽  
Vol 39 (8) ◽  
pp. 1076-1081 ◽  
Author(s):  
Klaus R. Pörschke ◽  
Richard Mynott ◽  
Carl Krüger ◽  
M. J. Romão

AbstractSynthesis and properties of tris(phosphane)(ethene)nickel(0) complexes (dmpe)(PR3)Ni(C2H4) (R = CH3(4), c-C6H11(5), and C6H5 (6)) are reported. In solution. 4-6 are thermolabile and undergo ligand exchange reactions affording tetrakis(phosphane)nickel(0 ) and bis(phosphane)- (ethene)nickel(0) complexes. 1H, 13C, and 31P NMR data of 4-6 confirm the tetrahedral geometry around nickel. For 6 , the crystal and molecular structure has been determined by X-ray crystallography.


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