Methylene chain length and coordination geometry in triosmium clusters containing diphosphine ligands X-ray crystal structures of [Os3(CO)10{μ-Ph2P(CH2)n}](n = 4 or 5) and [Os3(CO) 8{μ-Ph2PCH2PPh2}2]

Kabir, Shariff E.; Miah, Arzu; Nesa, Lutfun; Uddin, Khabir; Hardcastle, Kenneth I.; Rosenberg, Edward; Deeming, Antony J.

doi:10.1016/0022-328x(94)05276-h

Cited by 31 publications

(21 citation statements)

References 25 publications

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“…The two phosphorus atoms in the dppm ligand are slightly out of the Ru 3 plane, forcing one below and the other above the plane of the Ru 3 cluster [torsion angle: P(1)–Ru(1)–Ru(2)–P(2) = 17.86(6)°], whereas the value of a similar torsion angle in Ru 3 (CO) 10 (dppm) is 19.1(1)°. This also caused the axial carbonyl ligand to be twisted from their normal orthogonal positions 21…”

Section: Resultsmentioning

confidence: 99%

A Straightforward Synthesis of 5‐Methylaaptamine from Eugenol, Employing a 6π‐Electrocyclization Reaction of a 1‐Azatriene

2016

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Aaptamine, isolated from tropical marine sponges of the Demospongiae class, is the most prominent member of a growing family of natural products. Many aaptaminoids have been shown to have interesting biological activity. The efficient access to 5-methylaaptamine, an unnatural analogue of aaptamine, was achieved by using economic and naturally-occurring eugenol as the starting material. The synthesis involved the preparation of a 5-aminoeugenol derivative through successive nitration, O-methylation, and nitro group reduction reactions.

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Section: Resultsmentioning

confidence: 99%

A Straightforward Synthesis of 5‐Methylaaptamine from Eugenol, Employing a 6π‐Electrocyclization Reaction of a 1‐Azatriene

2016

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“…The synthesis and reactivity of triosmium clusters containing bridging diphosphine ligands [Os 3 (CO) 10 {µ-Ph 2 P(CH 2 ) n PPh 2 }] (n = 1-5) have widely been studied during the last decade. [1][2][3][4][5][6][7][8][9][10][11][12][13][14] In particular, the dppm [= bis(diphenylphosphino)methane, Ph 2 PCH 2 PPh 2 ] compound [Os 3 (CO) 10 (µ-dppm)] 1 has attracted considerable attention because of its novel reactivity to give many interesting species and also because of the special ability of dppm to maintain the metal cluster framework intact during chemical reactions. [3][4][5][6][7][8][9][10][11][12][13][14] For example, decarbonylation of 1 in refluxing toluene gives the co-ordinatively unsaturated cluster [Os 3 (µ-H)(CO) 8 {Ph 2 PCH 2 P(Ph)C 6 H 4 }] 2 which reacts with CO to form [Os 3 (µ-H)(CO) 9 {Ph 2 PCH 2 (Ph)C 6 H 4 }], 7 with H 2 to form [Os 3 (µ-H) 2 (CO) 8 (µ-dppm)], 8 with diphenylacetylene to form [Os 3 (CO) 8 (µ-dppm)(PhC᎐ ᎐ ᎐ CPh)] 9 and with [Au(PPh 3 )]PF 6 and HBF 4 to form the cationic clusters [Os 3 (µ-H)(CO) 8 {Ph 2 PCH 2 -P(Ph)C 6 H 4 }(µ-AuPPh 3 )]PF 6 and [Os 3 (µ-H) 2 (CO) 8 {Ph 2 PCH 2 -P(Ph)C 6 H 4 }]BF 4 respectively.…”

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confidence: 99%

Synthesis, structure and reactivity of triosmium clusters derived from the reactions of [Os3(CO)10(μ-dppm)] (dppm = Ph2PCH2PPh2) and [Os3(μ-H)(CO)8{Ph2PCH2P(Ph)C6H4}] with PHPh2

Azam¹,

Hursthouse²,

Islam³

et al. 1998

J. Chem. Soc., Dalton Trans.

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“…The diphosphine groups (e.g. of dppm) adopt monodentate,chelating or edge-bridging coordination modes on the cluster surface [6]. In polynuclear complexes, the dppm ligandhas agreater tendency to act either as amonodentate or as abridging bidentate ligand than as ac helating ligand because of the four-membered ring being strained [6].…”

Section: Discussionmentioning

confidence: 99%

Crystal structure of tetrakis(μ-thiocyanato)bis(μ-(bis(diphenylphosphino) methane-P,P′))tetrasilver(I), Ag4(SCN)4(C25H22P2)2

Jin¹,

Hu²,

Chen³

et al. 2008

Zeitschrift Für Kristallographie - New Crystal Structures

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C54H44Ag4N4P4S4,monoclinic, P12 1 /n1(no. 14), a =12.4531(4) Å, b =16.7286(5) Å, c =13.6948(4) Å, b =98.722(2)°, V =2820.0 Å 3 , Z =2,Rgt(F) =0.031, wRref(F 2 ) =0.062, T =273 K. Source of materialSynthesis of the titlecompound was carried out by stirring the solution of AgSCN (silver thiocyanate)(0.0489 g, 0.3 mmol), bis(diphenylphosphino)methane (dppm; 0.0577g, 0.15 mmol), and quinoline (0.0194 g, 0.15 mmol) in N,N-dimethylformamide (10 ml) for 24 hours at room temperature.After filtration, thefiltrate was allowed to stand at room temperature. Slowevaporation of the colorless solventyielded white crystals. Discussion. The diphosphine groups (e.g. of dppm) adopt monodentate,chelating or edge-bridging coordination modes on the cluster surface [6]. In polynuclear complexes, the dppm ligandhas agreater tendency to act either as amonodentate or as abridging bidentate ligand than as ac helating ligand because of the four-membered ring being strained [6]. The crystal structure determination of the title compound revealed atetranuclear silver(I) cluster. Because of all the thiocyanato ligands are almost linear, each two thiocyanates and two silver atoms form adistortedhexagon. Each silver atom is coordinated by one nitrogenatom of the thiocyanate,one sulfur atom of the other thiocyanate and the phosphorusa tom of the dppm ligand. Ag(1,1A,2,2A)a toms form at etragon whose edgesa re bridged by two dppmligands and two m-thiocyanates. The edges of the tetragonare not equivalent and the distance of the two silver atoms in different hexagons (3.0635(3) Å)is0.14 Å longer than the sum of the covalentr adii (2.88 Å) [ 7], which indicates that there is aweak Ag···Ag interaction.The bond length of S1-Ag1 (2.5683(7) Å)i ss lightly shorter than that of S2-Ag2 (2.6054(6) Å). The bond lengths of N1-Ag2 and N2-Ag1 are 2.231(2) Å and 2.214(2) Å,r espectively. The bond lengths of P1-Ag1and P2-Ag2are 2.3891(6) Å and 2.4087(6) Å,respectively, the average Ag-P bondl ength of 2.399 Å is 0.12 Å shorter than that reportedfor [Ag4(m-dppm)4(m4-i-mnt)2][5]. The angles of N-Ag-P are 127.38(6)°and 139.00(5)°,while the angles of P-Ag-S are 130.36(2)°and 110.93(2)°.H owever, the range of the angles of N-Ag-S is very small, beingb etween 102.24(6)°and 102.35(5)°.

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Methylene chain length and coordination geometry in triosmium clusters containing diphosphine ligands X-ray crystal structures of [Os3(CO)10{μ-Ph2P(CH2)n}](n = 4 or 5) and [Os3(CO) 8{μ-Ph2PCH2PPh2}2]

Cited by 31 publications

References 25 publications

A Straightforward Synthesis of 5‐Methylaaptamine from Eugenol, Employing a 6π‐Electrocyclization Reaction of a 1‐Azatriene

A Straightforward Synthesis of 5‐Methylaaptamine from Eugenol, Employing a 6π‐Electrocyclization Reaction of a 1‐Azatriene

Synthesis, structure and reactivity of triosmium clusters derived from the reactions of [Os3(CO)10(μ-dppm)] (dppm = Ph2PCH2PPh2) and [Os3(μ-H)(CO)8{Ph2PCH2P(Ph)C6H4}] with PHPh2

Crystal structure of tetrakis(μ-thiocyanato)bis(μ-(bis(diphenylphosphino) methane-P,P′))tetrasilver(I), Ag4(SCN)4(C25H22P2)2

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