Synthesis And Crystal Structures Of [Sn{2-[(Me3si)(2)C]C5h4n}R] [R = C6h2pr3i,4,6 1 Or Ch(Pph2)(2) 2], Two Novel Heteroleptic Tin(Ii) Compounds Derived From [Sn-{2-[(Me3si)(2)C]C5h4n}Cl], And For [{Sn(C6h2pr3i-2,4,6)(2)}(3)] 3, A Structural Redetermination

JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS(1998)

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摘要
Two novel, monomeric heteroleptic tin(II) derivatives, [Sn{2-[(Me3Si)(2)C]C5H4N}R] [R = C6H2Pr3i,-2,4,6 1 or CH(PPh2)(2) 2], have been prepared, characterised by multinuclear NMR spectroscopies and their molecular structures determined by single crystal X-ray diffraction. Both compounds were prepared from the corresponding heteroleptic tin(II) chloro-analogue, [Sn{2-[(Me3Si)(2)C]C5H4N}Cl], and thus demonstrate the utility of this compound as a precursor to further examples of heteroleptic tin(II) derivatives: such compounds are often unstable with respect to ligand redistribution. In each case, the central tin(II) is three-co-ordinate, Crystals of trimeric [{Sn(C6H2Pr3i-2,4,6)(2)}(3)] 3 were found to undergo a solid state phase transition, which may be ascribed to ordering of the ligand isopropyl groups. At 220 K the unit cell is orthorhombic, space group Pna2(1), compared with monoclinic, space group P2(1)/c, for the same crystals at 298 K, in which there is an effective tripling of the now b (originally c) axis. This result illustrates the extreme crowding generated by this bulky aryl ligand.
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crystal structure
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