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• W2041777072 abstract "Reactions of [Ni6(CO)12]2- (1) with R2SbBr (R = Me, Et, iPr) and R2SbCl (R = tBu, p-FC6H4) have given rise to the new [Ni10(SbR)2(CO)18]2- complexes (R = Me (3), Et (4), iPr (5), tBu (6), p-FC6H4 (7)) as the only major Ni−Sb product in each reaction (30−55% yields isolated as [NMe4]+ salts). These dianions, each of which has a crystallographically imposed inversion center, possess a common noncentered 1,12-Ni10Sb2 icosahedral cage that is surrounded by a 20-vertex ligand polyhedron composed of 10 terminal, 4 doubly bridging, and 4 triply bridging COs and the two Sb-attached R substituents. The formulation of each dianion was unambiguously established from X-ray crystallographic and infrared studies. An elemental analysis of [NMe4]2[3] substantiated its stoichiometry; magnetic susceptibility measurements conclusively showed this salt to be diamagnetic at room temperature. Cyclic voltammetric measurements of 3 and 5 in acetonitrile solutions similarly displayed only irreversible oxidation waves at ca. +0.60 V. A negative-ion electrospray ionization (ESI) mass spectrum of [NMe4]2[5] revealed the doubly charged ion-parent (M2-) signal for the dianion (5) as well as 11 other assigned doubly charged high-range m/z signals. In light of the previously known phenylstibinidene [Ni10(SbPh)2(CO)18]2- (2) prepared from reactions of 1 with either PhSbCl2 or Ph2SbCl, reactions of 1 with PhMeSbX (X = Br, I) were carried out; only 3 was isolated. Limiting slow-exchange 13C{1H} spectra were obtained at −60 °C for both 3 and 5 in acetone-d6; a variable-temperature line-shape analysis of the terminal-bridge carbonyl exchange process in 5 gave an estimated activation energy of 52.5 kJ/mol. One achieved objective was to assess the resulting steric effects due to a systematic change of the Sb-attached R substituents upon both the geometries of the common empty 1,12-Ni10Sb2 cage and the encapsulating 20-vertex ligand polyhedron. Another goal was to determine the possible existence for E = Sb of the other two hypothetical [Ni9(ER)3(CO)15]2- and [Ni8(ER)4(CO)12]2- dianions containing empty 1,2,12-Ni9E3 and 1,2,9,12-Ni8E4 icosahedral cages, respectively; previous work had shown the existence of all three electronically equivalent (isolobal) dianions for E = P and As but only 2 for E = Sb with R = Ph. Despite extensive efforts to detect such species, no evidence for their existence was uncovered. However, a neutral 34-electron Ni2(CO)4(μ2-SbtBu2)2 dimer (8) containing a planar Ni2Sb2 core was isolated as a side product and structurally characterized; this dimer is the first example of a stibinido-bridged analogue of the known 34-electron Ni2(CO)4(μ2-PR2)2-type dimer. A structural/bonding analysis with other 34-, 32-, and 30-electron Ni2(μ2-ER2)2 dimers (E = P, As) containing analogous planar Ni2E2 rings provides a self-consistent basis that a strong Ni−Ni‘ bonding interaction between two Ni(I) plays a dominant role in dictating the observed geometry of each of these ligand-bridged dimers. This comparison also indicates that an essential ingredient for the existence of 8 as a stable entity is the bulky Sb-attached tBu substituents which apparently protect the dimer from air oxidation." @default.
• W2041777072 created "2016-06-24" @default.
• W2041777072 creator A5026095654 @default.
• W2041777072 creator A5027855129 @default.
• W2041777072 date "1997-04-01" @default.
• W2041777072 modified "2023-10-14" @default.
• W2041777072 title "New Nickel−Antimony Carbonyl Clusters: Stereochemical Analyses of the [Ni₁₀(SbR)₂(CO)₁₈]²^- Dianions (R = Me, Et, <i>ⁱ</i>Pr, <i>^t</i>Bu, <i>p</i>-FC₆H₄) Containing Empty 1,12-Ni₁₀Sb₂ Icosahedral Cages and of the Unprecedented Stibinido-Bridged 34-Electron Ni₂(CO)₄(μ₂-Sb<i>^t</i>Bu₂)₂ Dimer¹" @default.
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• W2041777072 doi "https://doi.org/10.1021/om960966c" @default.
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