Syntheses and structure of bis(pentamethylcyclopentadienyl)-dithiophosphinato Complexes

Ebels, Jörg; Pietschnig, Rudolf; Nieger, Martin; Niecke, Edgar; Kotila, Sirpa

doi:10.1002/(sici)1098-1071(1997)8:6<521::aid-hc11>3.0.co;2-t

Cited by 8 publications

(6 citation statements)

References 7 publications

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“…As expected, the Li–O term (DME) bonds (1.9621(18) Å) are somewhat shorter than the Li−μ 2 -O(DME) bonds (2.0433(18)–2.2772(18) Å). All Li–O, Li–N, and Li–S distances are in agreement with the analogous distances in other lithium complexes. − Atoms of the Li(1)O(2)Li(1A)O(2A) fragment form a planar ring. The mbt F ligand plane forms an angle equal to 59.57° with the Li 2 O 2 ring.…”

Section: Resultssupporting

confidence: 77%

“…The mbt F ligand plane forms an angle equal to 59.57° with the Li 2 O 2 ring. The Li···Li distance in the complex is 3.161(3) Å, which is characteristic for lithium dimers with bridging DME ligands. , In contrast to complexes 1 and 2 , in a molecule of 3 the four-membered LiNCS metallacycle is almost flat. The dihedral angle between the NLiS and NCS planes is 1.82°.…”

Section: Resultsmentioning

confidence: 95%

“…As expected, the Li− O term (DME) bonds (1.9621(18) Å) are somewhat shorter than ligands. 49,50 In contrast to complexes 1 and 2, in a molecule of 3 the four-membered LiNCS metallacycle is almost flat. The dihedral angle between the NLiS and NCS planes is 1.82°.…”

Section: ■ Introductionmentioning

confidence: 94%

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Unexpected Findings in a Simple Metathesis Reaction of Europium and Ytterbium Diiodides with Perfluorinated Mercaptobenzothiazolates of Alkali Metals

et al. 2020

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In the search for new f–d luminescent complexes of Eu(II) and Yb(II) the metathesis reactions of diiodides of these metals with perfluorinated 2-mercaptobenzothiazolates of alkali metals were studied. It has been found that the reactions of LnI2(THF)2 (Ln = Eu, Yb) with K(mbtF) (mbtF = perfluorinated 2-mercaptobenzothiazolate anion) in DME result in the formation of the nonluminescent complexes Ln(mbtF)2(DME)2 and precipitation of KI in high yields. Single-crystal X-ray diffraction analyses have shown that Eu(mbtF)2(DME)2 has a trans orientation of mbtF ligands, while in the Yb(mbtF)2(DME)2 molecule the ligands occupy cis positions. The DFT calculations and estimations with the invariom model revealed that the complexes have a flexible coordination sphere of Ln2+ ions and a relatively low energy of Ln–mbtF binding. The reactions of the same diiodides with the lithium complex Li(mbtF) are reversible and proceed through the formation of intermediate complexes of unknown structure which have been isolated as noncrystalline solids. The europium product (solid and in DME solution) upon UV excitation exhibited bright luminescence with λ 510 nm. Data from time-resolved photoluminescence (PL) spectroscopy indicated the existence in the intermediate substance of two Eu2+ emission centers with different coordinating environments. Treatment of the solid intermediate product with toluene led to its dissociation onto Ln(mbtF)2(DME)2 and [LiI(DME)] n . The back-replacement of toluene with DME gives again the solutions from which the starting LnI2 and Li(mbtF)(DME) were precipitated by slow evaporation of the solvent. The reversibility of the processes has been confirmed by the reaction of nonluminescent Eu(mbtF)2(DME)2 with LiI in DME medium, which resulted in the same luminescent solution which gave a mixture of EuI2(DME)3 and Li(mbtF).

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Section: Resultssupporting

confidence: 77%

Section: Resultsmentioning

confidence: 95%

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Unexpected Findings in a Simple Metathesis Reaction of Europium and Ytterbium Diiodides with Perfluorinated Mercaptobenzothiazolates of Alkali Metals

et al. 2020

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“…Sulfur-lithium bond lengths are also approximately equal (S(1)-Li(1) 2.494(9); S(2)-Li(1) 2.491(9) A ˚). 25 and [(Cy 2 PS 2 ) 4 Li 5 (OH)] 2 in which the ligands bridge up to four metal centers in four different bonding modes. 26 The homologous tetra-selenium ligand (3) was prepared in an analogous fashion to 2 with an overall 73% yield of crystalline product.…”

Section: Resultsmentioning

confidence: 99%

“…The resultant four membered S(1)−P(1)−S(2)−Li(1) chelate ring is close to planar (sum of internal angles = 356.81°) with a S(1)−Li(1)−S(2) bite angle of 84.2(3)° and a S(1)−P(1)−S(2) angle of 114.34(7)°. Two other lithium dithiophosph(in)ates have been previously crystallographically characterized: (Cp* 2 PS 2 Li.DME) 2 in which the ligand adopts an isobidentate type B coordination mode, and [(Cy 2 PS 2 ) 4 Li 5 (OH)] 2 in which the ligands bridge up to four metal centers in four different bonding modes …”

Section: Resultsmentioning

confidence: 99%

Facile Synthesis of Bis(dichalcogenophosphinate)s and a Remarkable [Li₈(OH)₆]²⁺ Polyhedron

et al. 2010

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The synthesis and characterization of three lithium complexes of novel bis(dichalcogenophosphinate) ligands are reported: (PhP(S) 2 CH 2 CH 2 P(S) 2 Ph)Li 2 (THF) 4 (2), (PhP(Se) 2 CH 2 CH 2 P(Se) 2 Ph)Li 2 (THF) 4 .(PhP(Se) 2 CH 2 CH 2 P(Se) 2 Ph)Li 2 (THF) 6 (3) and [PhP(Te) 2 CH 2 CH 2 P(Te) 2 Ph][Li 8 (OH) 6 (THF) 8 ] (4). The synthetic route to these complexes proceeds via the insertion reaction of elemental chalcogens into the phosphorus-lithium bonds of 1,2-dilithio-1,2-di(phenylphosphine)ethylene (1). X-ray analysis of 2 revealed anisobidentate coordination of the lithiums by the dithiophosphinate groups. In contrast, the diselenophosphinate groups in 3 coordinate the lithium centers in both isobidentate and mono-dentate modes, and the ditellurophosphinate groups in 4 form non-coordinate separate ion pairs. The counter-cation in 4 is shown to be a unique [Li 8 (OH)

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Chemical Shifts and Coupling Constants for C26H46NPS2

Kumar

2014

Chemical Shifts and Coupling Constants for Phosphorus-31

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Syntheses and structure of bis(pentamethylcyclopentadienyl)-dithiophosphinato Complexes

Cited by 8 publications

References 7 publications

Unexpected Findings in a Simple Metathesis Reaction of Europium and Ytterbium Diiodides with Perfluorinated Mercaptobenzothiazolates of Alkali Metals

Unexpected Findings in a Simple Metathesis Reaction of Europium and Ytterbium Diiodides with Perfluorinated Mercaptobenzothiazolates of Alkali Metals

Facile Synthesis of Bis(dichalcogenophosphinate)s and a Remarkable [Li₈(OH)₆]²⁺ Polyhedron

Chemical Shifts and Coupling Constants for C26H46NPS2

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Syntheses and structure of bis(pentamethylcyclopentadienyl)-dithiophosphinato Complexes

Cited by 8 publications

References 7 publications

Unexpected Findings in a Simple Metathesis Reaction of Europium and Ytterbium Diiodides with Perfluorinated Mercaptobenzothiazolates of Alkali Metals

Unexpected Findings in a Simple Metathesis Reaction of Europium and Ytterbium Diiodides with Perfluorinated Mercaptobenzothiazolates of Alkali Metals

Facile Synthesis of Bis(dichalcogenophosphinate)s and a Remarkable [Li8(OH)6]2+ Polyhedron

Chemical Shifts and Coupling Constants for C26H46NPS2

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Facile Synthesis of Bis(dichalcogenophosphinate)s and a Remarkable [Li₈(OH)₆]²⁺ Polyhedron