Inorganic co-ordination polymers—II monoamminedichlorozinc(II)

Block, B. P.; Florentine, R. A.; Simkin, Joseph; Barth-Wehrenalp, G.

doi:10.1016/0022-1902(62)80032-3

Cited by 2 publications

(1 citation statement)

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“…Attempts to grow suitable single crystals for a solid-state determination of 2 failed, but a solution of 2 in dichloromethane at −40 °C rendered a very small fraction of yellow crystals of the ammonia adduct [(H 3 N)Cl 2 Zn{(μ 3 -NH)Ti 3 (η 5 -C 5 Me 5 ) 3 (μ-NH) 2 (μ 3 -N)}] ( 3 ). Complex 3 could not be obtained in a preparative scale experiment since reactions of 2 with an excess of ammonia in dichloromethane gave immediately 1 and a fine white precipitate of [ZnCl 2 (NH 3 ) 2 ]. , Furthermore, we did not observe any reaction between complex 1 and [ZnCl 2 (NH 3 ) 2 ] in dichloromethane or toluene even at high temperatures.…”

Section: Resultsmentioning

confidence: 70%

Cube-Type Nitrido Complexes Containing Titanium and Zinc/Copper

et al. 2006

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Several azaheterometallocubane complexes containing [MTi3N4] cores have been prepared by the reaction of [{Ti(eta5-C5Me5)(mu-NH)}3(mu3-N)] (1) with zinc(II) and copper(I) derivatives. The treatment of 1 with zinc dichloride in toluene at room temperature produces the adduct [Cl2Zn{(mu3-NH)3Ti3(eta5-C5Me5)3(mu3-N)}] (2). Attempts to crystallize 2 in dichloromethane gave yellow crystals of the ammonia adduct [(H3N)Cl2Zn{(mu3-NH)Ti3(eta5-C5Me5)3(mu-NH)2(mu3-N)}] (3). The analogous reaction of 1 with alkyl, (trimethylsilyl)cyclopentadienyl, or amido zinc complexes [ZnR2] leads to the cube-type derivatives [RZn{(mu3-N)(mu3-NH)2Ti3(eta5-C5Me5)3(mu3-N)}] (R = CH2SiMe3 (5), CH2Ph (6), Me (7), C5H4SiMe3 (8), N(SiMe3)2 (9)) via RH elimination. The amido complex 9 decomposes in the presence of ambient light to generate the alkyl derivative [{Me3Si(H)N(Me)2SiCH2}Zn{(mu3-N)(mu3-NH)2Ti3(eta5-C5Me5)3(mu3-N)}] (10). The chloride complex 2 reacts with lithium cyclopentadienyl or lithium indenyl reagents to give the cyclopentadienyl or indenyl zinc derivatives [RZn{(mu3-N)(mu3-NH)2Ti3(eta5-C5Me5)3(mu3-N)}] (R = C5H5 (11), C9H7 (12)). Treatment of 1 with copper(I) halides in toluene at room temperature leads to the adducts [XCu{(mu3-NH)3Ti3(eta5-C5Me5)3(mu3-N)}] (X = Cl (13), I (14)). Complex 13 reacts with lithium bis(trimethylsilyl)amido in toluene to give the precipitation of [{Cu(mu4-N)(mu3-NH)2Ti3(eta5-C5Me5)3(mu3-N)}2] (15). Complex 15 is prepared in a higher yield through the reaction of 1 with [{CuN(SiMe3)2}4] in toluene at 150 degrees C. The addition of triphenylphosphane to 15 in toluene produces the single-cube compound [(Ph3P)Cu{(mu3-N)(mu3-NH)2Ti3(eta5-C5Me5)3(mu3-N)}] (16). The X-ray crystal structures of 3, 8, 9, and 15 have been determined.

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Section: Resultsmentioning

confidence: 70%