[cis,cis,trans-RuCl2(CO)2{Ph2P(CH2CH2O)nCH2CH2PPh2-P,P'}]m (n = 4, 5; m = 1, 2, ...) Metallacrown Ethers. X-ray Crystal Structures of cis,cis,trans-RuCl2(CO)2{Ph2P(CH2CH2O)4CH2CH2PPh2-P,P'}, a Complex Which Exhibits Rotational Isomers in the Solid State, and [cis,cis,trans-RuCl2(CO)2{.mu.-Ph2P(CH2CH2O)4CH2CH2PPh2-P,P'}]2, an Unusual Dimetallacrown Ether

Gray, Gary M.; Varshney, Ashima; Duffey, Christina H.

doi:10.1021/om00001a036

Cited by 31 publications

(25 citation statements)

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“…This is particularly true for cis,cis,trans-[ RuCI2 ( CO)2 { Ph2 P ( CH2 CH2 O),, CH2 CH2 PPh2 -P, P' } ] metallacrown ethers because the preparation of these complexes requires the simultaneous addition of dilute solutions of [RuClz(CO)3(th0] and the ligand (Gray, Varshney & Duffey, 1995). Other Ru n precursors are unsuitable for this reaction because they are generally polymeric and insoluble.…”

Section: Commentmentioning

confidence: 99%

fac-Tricarbonyldichloro(tetrahydrofuran)ruthenium(II)

Gray¹,

Duffey²

1996

Acta Crystallogr C

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In the fac- [RuClz(CO) 3(thO] complex, the Ru ll has slightly distorted octahedral coordination geometry with the carbonyl ligands in a facial arrangement and the thf trans to one of the carbonyls. The dihedral angle between the least-squares plane of the thf and the leastsquares plane through the four ligands cis to the thf is 90.56 (23) °. The torsion angles about the RuH--O(thf) bond indicate that the thf ring nearly bisects the angles between cis Cl and carbonyl ligands. CommentThe complex,, (I), first reported in 1989 (Reddy, Whitten, Redmill, Varshney & Gray, 1989), is a useful starting material for the synthesis of cis,cis,trans-[RuClz(CO)2(phosphine)2] complexes. This is particularly true for cis,cis,trans-[ RuCI2 ( CO)2 { Ph2 P ( CH2 CH2 O),, CH2 CH2 PPh2 -P, P' } ] metallacrown ethers because the preparation of these complexes requires the simultaneous addition of dilute solutions of [RuClz(CO)3(th0] and the ligand (Gray, Varshney & Duffey, 1995). Other Ru n precursors are unsuitable for this reaction because they are generally polymeric and insoluble. The fac-[RuCl2(CO)3(thO] complex was initially reported as [RuC12(CO)3].0.75thf based on elemental analysis (Reddy, Whitten, Redmill, Varshney & Gray, 1989). The fractional stoichiometry seemed unlikely, and one reason for obtaining a crystal structure of the complex was to determine the amount of thf present. Other points of interest in the crystal structure are the coordination geometry at the Ru iI center and the conformation of the thf ring.An ORTEPII (Johnson, 1976) drawing of fac-[RuC12(CO)3(thf)] is shown in Fig. 1. The coordination geometry of Ru is slightly distorted octahedral, as indicated by the dihedral angles between the three leastsquares planes through the Ru and the atoms coordinated to it (90.7, 89.4 and 92.2°). The carbonyl ligands are in a facial arrangement and the thf is trans to one of the carbonyls. The thf ring (04, C4, C5, C6, C7) has an envelope conformation with 04, C4, C5 and C7 forming the base and C5, C6 and C7 forming the flap. The displacement ellipsoid of C7 of thf is elongated relative to this plane, suggesting that, as expected, the ring is conformationally flexible. The dihedral angles between the least-squares plane of the thf (04, C4, C5, C6, C7) and the least-squares planes containing the Ru, the thf O atom, one of the cis carbonyl C atoms, one of the cis C1 ligands and the trans carbonyl C atom (Ru, Cll, 04, C 1, C3 35.0°; Ru, C12, 04, C2, C3 127.2 °) indicate that the thf experiences repulsive interactions with the ligands cis to it. This potential strain is relieved by a rotation of the thf around the Ru--O4 bond to move C4 into the space between C12 and C 1, and C7 into the space between C11 and C2. The dihedral angle between the least-squares plane of thf (04, C4, C5, C6, C7) and that formed by the Ru, the two C1 ligands and the two cis carbonyl C atoms (Ru, Cll, C12, C1, C2) is 90.56 °. This unusual arrangement is consistent with literature reports of other thf complexes

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Section: Commentmentioning

confidence: 99%

fac-Tricarbonyldichloro(tetrahydrofuran)ruthenium(II)

Gray¹,

Duffey²

1996

Acta Crystallogr C

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“…Bis(imidazol-1-yl), bis(pyrazol-1-yl), and bis(benzimidazol-1-yl) polyether type compounds react with K 2 [PtCl 4 ] to yield square planar dichloro{bis(azolyl)polyether}platina(II) type complexes (1)(2)(3)(4)(5)(6)(7). In addition, L1 and L2 react with K 2 [PtI 6 ] to yield the respective diiodoplatinum(II) complexes 8 and 9 via reductive elimination.…”

Section: Discussionmentioning

confidence: 99%

“…The synthesis of several such metallacrown ethers has been described with, frequently, phosphorus or nitrogen donor moieties as the ligating units connecting the metal to the polyether backbone [2][3][4][5][6]. Furthermore, the propensity of metallacrown ethers to bind metal cations in the ring cavity has been demonstrated [1,7].…”

Section: Introductionmentioning

confidence: 99%

Synthesis, characterization and X-ray crystal structures of polyether and ethylene bridged bis(azolyl) platinum(II) complexes

Kelly

Gómez‐Ruiz

Steinborn

et al. 2008

Transition Met Chem

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The preparation of platinum(II) complexes of the types [PtCl 2 {Y(CH 2 CH 2 O) x CH 2 CH 2 Y}] (Y: imidazol-1-yl, im; pyrazol-1-yl, pz or benzimidazol-1-yl, bim) and [PtI 2 {im(CH 2 CH 2 O) x CH 2 CH 2 im}] with varying ligand backbone length (x between 0 and 3) is described. A new bis(pyrazol-1-yl) polyether compound, pz(CH 2 CH 2 O) 2 CH 2 -CH 2 pz, is reported. Spectroscopic characterization of the complexes is discussed. Two crystal structures of the general formula [PtCl 2 {im(CH 2 CH 2 O) x CH 2 CH 2 im}] (x is 1 or 3) are also reported.Abbreviations bim Benzimidazol-1-yl im Imidazol-1-yl pz Pyrazol-1-yl

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“…For N-heterocyclic carbene ligands and their complexes, see: Herrmann (2002); Hahn & Jahnke (2008). For details of bisphosphine polyether ligands, see: Alcock et al (1976); Powell et al (1981); Gray et al (1995). For mixed NHC metallacrown ether ligands, see: Nielsen et al (2003); Liu et al (2007); Wang et al (2005).…”

Section: Related Literaturementioning

confidence: 99%