Di-μ-iodo-bis[diiodobis(triphenylphosphine oxide)bismuth(III)]

Lazarini, F.; Milićev, S.

doi:10.1107/s0567740876009072

Cited by 16 publications

(5 citation statements)

References 4 publications

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“…All of them having metal−metal bonding (2.673−2.889 Å) and ranging from d 3 −d 3 to d 6 −d 6 electronic configurations, are listed in Table . Conversely, this is the most typical isomer for edge-sharing complexes of Bi III and Sb III which are, apparently, nonmetal−metal bonded, with monodentate and bidentate phosphines, and phosphine oxide ligands . The same type of ligand distribution occurs rather often for the ESBO compounds of V III , V IV , Ti III , Ti IV , and Nb IV38 with a metal-to-metal separation of more than 3.28 Å.…”

Section: Resultsmentioning

confidence: 84%

Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 3. Novel Structures with Diethylphosphido-bridges and Terminal Diethylphosphines

1998

Inorg. Chem.

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The interaction between octachlorodirhenium anions and diethylphosphine has been shown to strongly depend on reaction conditions, mainly the nature of the solvent and the amount of phosphine. As a result, novel dirhenium products with oxidation states ranging from Re(II) to Re(IV) have been obtained. The reaction of [Re(2)Cl(8)](2)(-) with an excess of PEt(2)H in dichloromethane or acetonitrile led to the first example of a face-sharing complex of rhenium(IV) with three phosphido-bridges, namely [Bu(n)(4)N][Re(2)(&mgr;-PEt(2))(3)Cl(6)] (1). The unusual edge-sharing Re(2)(&mgr;-PEt(2))(2)Cl(4)(PEt(2)H)(4) (2) complex of rhenium(III) with C(i)() core symmetry, containing both terminal phosphines and phosphido-bridges, has been obtained by carrying out the reaction with an excess of PEt(2)H in a benzene (or propanol) - HCl mixture at room temperature. A new example of the 1,2,7,8-type of dirhenium(II) complex, Re(2)Cl(4)(PEt(2)H)(4) (3), having diethylphosphine ligands located cis on each Re atom, has been isolated from the reaction of [Re(2)Cl(8)](2)(-) with PEt(2)H in an ethanol-HCl medium. The solid-state structures of complexes 1-3 have been investigated by X-ray crystallography. Complexes 1 and 2 both crystallized in two forms: [Bu(n)(4)N][Re(2)(&mgr;-PEt(2))(3)Cl(6)] 1a, P2(1)/n with a = 10.482(1) Å, b = 16.512(2) Å, c = 23.986(2) Å, beta = 93.637(8) degrees, and Z = 4; [Bu(n)(4)N][Re(2)(&mgr;-PEt(2))(3)Cl(6)].1.5 C(7)H(8) 1b, C2/c with a = 38.746(9) Å, b = 10.322(2) Å, c = 27.277(3) Å, beta = 110.35(1) degrees, and Z = 8; Re(2)(&mgr;-PEt(2))(2)Cl(4)(PEt(2)H)(4) 2a, P2(1)/n with a = 11.081(3) Å, b = 11.029(3) Å, c = 15.627(2) Å, beta = 90.05(1) degrees, and Z = 2; 2b, P2(1)/c with a = 16.094(3) Å, b = 15.193(3) Å, c = 15.548(3) Å, beta = 100.98(3) degrees, and Z = 4. X-ray data for complex Re(2)Cl(4)(PEt(2)H)(4) 3 are as follows: P2(1)/n with a = 10.445(2) Å, b = 10.113(3) Å, c = 13.473(2) Å, beta = 102.17(2) degrees, and Z = 2. Three bridging &mgr;-PEt(2) groups in the face-sharing complex 1 span a short metal-metal distance of 2.4060(6) Å, averaged over 1a and 1b, with a small Re-PEt(2)-Re angle of 61.34(7) degrees. The rhenium-rhenium bond length in the edge-sharing complex 2 is 2.7545(7) Å, averaged over 2a and 2b, while the bridging Re-PEt(2)-Re angle is 72.16(6) degrees, and the P-Re-P angle for the terminal phosphine ligands is 87.11(7) degrees. The Re-Re bond distance in 3, 2.2533(8) Å, is typical for triply bonded dirhenium complexes, and the P-Re-P angle for the cis phosphine groups is 93.12(6) degrees.

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Section: Resultsmentioning

confidence: 84%

Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 3. Novel Structures with Diethylphosphido-bridges and Terminal Diethylphosphines

1998

Inorg. Chem.

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“…By contrast, far fewer reports have appeared with phosphine chalcogenide ligands. A number of phosphine oxide complexes of arsenic (III), antimony(III) and bismuth(III) halides (X = Cl, Br, I) have been reported, 6,7 of which [SbCl 3 (OPPh 3 ) 2 ], 8 [SbCl 3 (dppmO 2 )], 9 and [Bi 2 I 6 (OPPh 3 ) 4 ], 10 have been crystallographically characterised. Recent reports have shown that AsF 3 and SbF 3 form hydrolytically unstable complexes with phosphine oxides, but BiF 3 does not.…”

Section: Introductionmentioning

confidence: 99%

Formation of M4Se4 cuboids (M = As, Sb, Bi) via secondary pnictogen–chalcogen interactions in the co-crystals MX3·SeP(p-FC6H4)3 (M = As, X = Br; M = Sb, X = Cl; M = Bi, X = Cl, Br)

et al. 2012

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The reactions of the group 15 trihalides, MX(3) (M = As, Sb, Bi; X = Cl, Br), with the phosphine selenide SeP(p-FC(6)H(4))(3) result in the formation of co-crystals of formula MX(3)·SeP(p-FC(6)H(4))(3). No reaction was observed with MI(3) (M = As, Sb, Bi). The structures of MX(3)·SeP(p-FC(6)H(4))(3) (M = As, X = Br 2; M = Sb, X = Cl 3; M = Bi, X = Cl 5; M = Bi, X = Br 6) have been established, and are isomorphous, crystallising in the cubic I23 space group. All the structures feature a primary MX(3) unit, which has three weak secondary MSe interactions to SeP(p-FC(6)H(4))(3) molecules. However, each of these SeP(p-FC(6)H(4))(3) molecules bridges three MX(3) molecules, resulting in the generation of an M(4)Se(4) (M = As, Sb, Bi) distorted cuboid linked by the pnictogen-chalcogen interactions. Four opposing corners of the cuboid are occupied by the M atom (M = As, Sb, Bi) of an MX(3) pyramid, and the other four by the selenium atom of the phosphine selenide.

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“…Ionization potentials and electron affinities of the metal are taken from Vedeneev, Gurvich, Kondrat'ev Medvedev & Frankevich (1962). ( Lazarini & Mili6ev (1976). (f) Lazarini, Goli~ & Pelizzi (1976).…”

Section: Introduetlonmentioning

confidence: 99%

“…A number of interesting configurations in the complexes of Sb m or Bi III halides with organic oxobases, (C6Hs)aPO and (C6H5)3AsO, have been determined by crystal structure analysis (Lazarini, Goli~ & Pelizzi, 1975Lazarini & Mili6ev, 1976) or suggested by vibrational spectroscopy (Mili6ev & Had~i, 1977). The crystal structure determination of SbCIa[(C6Hs)3PO] 2 is reported here.…”

mentioning

confidence: 99%

Trichlorobis(triphenylphosphine oxide)antimony(III)

Golič¹,

Milićev²

1978

Acta Crystallogr Sect B

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Introduetlon. A number of interesting configurations in the complexes of Sb m or Bi III halides with organic oxobases, (C6Hs)aPO and (C6H5)3AsO, have been determined by crystal structure analysis (Lazarini, Goli~ & Pelizzi, 1975Lazarini & Mili6ev, 1976) or suggested by vibrational spectroscopy (Mili6ev & Had~i, 1977). The crystal structure determination of SbCIa[(C6Hs)3PO] 2 is reported here. The complex SbBra[(C6Hs)aPOI 2 is isomorphous, as shown by powder diffraction data and vibrational spectra (Mili6ev & Had~i, 1977).Crystals of SbCIa[(C6Hs)3PO] 2 were obtained by the method of Mili6ev & Had~.i (1977). The unit-cell parameters were determined by single crystal diffractometry. A unique set of 5032 reflections was measured in the range 1.5 < 0 < 30 ° on an Enraf-Nonius CAD-4 diffractometer with 09-20 scan and Mo Ka~ radiation [graphite monochromator, 2 = 0.7107 A, t = 20 (1)°C]. A crystal ground to a sphere (r --0.2 mm) was used for intensity measurements. 2713 reflections having I > 3o(1) were taken as observed. The * To whom correspondence should be addressed. intensities were corrected for Lorentz, polarization and absorption (# = 11.5 cm -1) effects.The structure was solved from a Patterson summation and successive Fourier syntheses. Because of the stoichiometry an Sb as well as a C1 atom should be expected in a special position. Just one peak on the twofold axis belonging to the Sb was observed and an additional peak of half the intensity expected for the C1 atom was found in the general position. Consequently the C1 atom with a population parameter of 0.5 was placed in this position. Population parameters of both CI atoms, positional parameters and anisotropic temperature factors of all non-hydrogen atoms were included in the refinement of the structure. The H-atom parameters were calculated and included in the structure factor calculation (with an isotropic temperature factor U = 0.07 A 2) but not refined. The function minimized in the least-squares procedure was Y w(IFol -P Fcl)2. The weighting scheme applied was as follows:

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Di-μ-iodo-bis[diiodobis(triphenylphosphine oxide)bismuth(III)]

Cited by 16 publications

References 4 publications

Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 3. Novel Structures with Diethylphosphido-bridges and Terminal Diethylphosphines

Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 3. Novel Structures with Diethylphosphido-bridges and Terminal Diethylphosphines

Formation of M4Se4 cuboids (M = As, Sb, Bi) via secondary pnictogen–chalcogen interactions in the co-crystals MX3·SeP(p-FC6H4)3 (M = As, X = Br; M = Sb, X = Cl; M = Bi, X = Cl, Br)

Trichlorobis(triphenylphosphine oxide)antimony(III)

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