30982-88-8Relevant academic research and scientific papers
Syntheses, Structures, and Characterization of Nickel(II) Stibines: Steric and Electronic Rationale for Metal Deposition
Taylor, William V.,Xie, Zhu-Lin,Cool, Nicholas I.,Shubert, Sofia A.,Rose, Michael J.
, p. 10364 - 10374 (2018)
Reactions of the homoleptic and heteroleptic antimony ligands SbiPr3, SbiPr2Ph, SbMe2Ph, and SbMePh2 with NiI2 generate rare NiII stibine complexes in either square planar or trigonal bipyramidal (TBP) geometries, depending on the steric size of the ligands. Tolman electronic parameters were calculated (DFT) for each antimony ligand to provide a tabulated resource for the relative strengths of simple antimony ligands. The electronic absorbance spectra of the square planar complexes exhibit characteristic bands [λmax ≈ 560 nm (17 900 cm-1), ? ≈ 4330 M-1 cm-1] at lower energies compared to the reported phosphine complexes, indicating the weak donor strength of the stibine ligands and resultant low-energy ligand field d→d transitions. The square planar complex Ni(I)2(SbiPr3)2 reacts with CO to form the TBP complex Ni(I)2(SbiPr3)2(CO). Lastly, the complexes were investigated for nickel metal deposition on Si|Cu(100 nm) substrates. The complexes with the strongest donating ligand, SbiPr3, deposited the purest layer of NiCu alloy according to the balanced reaction Ni(I)2(SbIIIiPr3)2 → Ni0 + SbV(iPr3)I2; the iodinated SbV byproduct was unambiguously detected in the supernatant by 1H NMR and mass spectrometry. Complexes with weaker ligands (poor I2 acceptors/scavengers) resulted undesired deposition of iodine and CuI on the surface. This work thus serves as a guide for the design and synthesis of 3d metal complexes with neutral, heavy main-group donors that are useful for metal deposition applications.
Synthesis and properties of new ditertiary stibines based upon o-, m- or p-xylyl and m- or p-phenylene backbones and their complexes with tungsten, iron and nickel carbonyls
Levason, William,Matthews, Melissa L.,Reid, Gillian,Webster, Michael
, p. 51 - 58 (2007/10/03)
High yield syntheses for 1,2-, 1,3-, and 1,4-xylyl distibines (1,2-C6H4(CH2SbMe2)2, 1,3-C6H4(CH2 SbMe2)2, 1,4-C6H4(CH2 SbMe2)2, respectively) from Me2SbCl (conveniently made in situ from Me2PhSb and HClgas) and the appropriate di-Grignard are reported. The 1,3- and 1,4-phenylene distibines, 1,3-C6H4(SbMe2)2 and 1,4-C6H4(SbMe2)2, were made similarly. The new ligands have been characterised by mass spectrometry, 1H and 13C{1H} NMR spectroscopy, and by the preparation of methiodide derivatives. The crystal structures of 1,4-C6H4(CH2 SbMe2)2 and [1,3-C6H4(CH2 SbMe3)2]I2 have been determined. The synthesis of 1,2-C6H4-(CH2 SbPh2)2 has been achieved similarly in modest yield and the distibine converted into the tetra-iodo-derivative 1,2-C6H4(CH2SbPh2 I2)2. The coordination modes available to these ligands have been probed by the synthesis and characterisation of complexes with nickel, iron and tungsten carbonyls. The crystal structure of [{Fe(CO)4}2-{μ-1,3-C6H4 (CH2SbMe2)2}] has been determined. The spectroscopic properties of these carbonyl derivatives have been compared with those of complexes of other antimony ligands, and in some cases with diphosphine and diarsine complexes, to probe the electronic properties of the new ligands.
New Reagents, XXV. lithium and -copper(I); Synthesis and Preparative Applications
Kauffmann, Thomas,Joussen, Rolf,Klas, Norbert,Vahrenhorst, Annemarie
, p. 473 - 478 (2007/10/02)
lithium (1b), quantitatively obtained by organoelement-lithium exchange from bis(diphenylstibino)methane (1a), reacts with aldehydes and ketones to give (β-hydroxyalkyl)diphenylstibanes (2) (39 - 82percent).These compounds are now well accessible. copper(I) (5), quantitatively obtained by transmetalation from 1b, reacts with alkyl iodides to give alkyldiphenylstibanes (3) (45 - 80percent). (Diphenylphosphino)- (4a) and (diphenylarsino)(diphenylstibino)methane (4b) were obtained from 1b in unsatisfactory yields only.
ORGANOSTIBINES AS LIGANDS. SYNTHESIS OF DIMETHYL(Α-PICOLYL)STIBINE, DIMETHYL(8-QUINOLYL)STIBINE, AND (R;S)-METHYLPHENYL(8-QUINOLYL)STIBINE AND SOME TRANSITION METAL DERIVATIVES
Shewchuk, Eric,Wild, Stanley Bruce
, p. 181 - 192 (2007/10/02)
The unsymmetrical mono-tertiary stibines dimethyl(α-picolyl)stibine (picstib), dimethyl(8-quinolyl)stibine (quinstib), and (R; S)-methylphenyl(8-quinolyl)-stibine (R; S-quinstib) have been synthesised and the square-planar complexes , MX2(q
Aqueous electrochemistry of quaternary organoantimony ions
Kok, Gregory L.,Morris, Michael D.
, p. 2146 - 2150 (2008/10/08)
The series of quaternary organoantimony ions, (CH3)m(C6H5)m-4Sb + (m = 1-4), has been studied in aqueous solution using dc polarography, cyclic voltammetry, and controlled potential electrolysis. Tetramethylantimony ion undergoes a single two-electron reduction to trimethylantimony and methane. The other three ions in the series are reduced in two one-electron steps. The first electron transfer involves the formation of an antimony(IV) species which rapidly reacts with the electrode metal to form an organomercury radical and a trivalent organoantimony compound. The organomercury radical disproportionates to form a diorganomercury compound. The second electron transfer gives trivalent organoantimony compounds and hydrocarbons. In two of the three possible cases both methyl and phenyl groups are lost by the antimony. The relative losses are different following the first and second electron transfer. Two factors govern the loss of the hydrocarbon group: the stability of the resulting hydrocarbon radical or carbanion and the stability of the resulting antimony compounds.
