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• W2063579554 abstract "Several novel binuclear HgII complexes of cis,trans,cis-1,2,3,4-tetrakis(diphenylphosphino)cyclobutane (dppcb) have been prepared and characterised by X-ray diffraction methods, NMR spectroscopy (199Hg{1H}, 31P{1H}, 1H), FAB mass spectrometry, IR spectroscopy, elemental analyses and melting points. The tetrahedral coordination of both the HgII centres in the homobimetallic compounds [Hg2L4(dppcb)] (L=Cl− (1), Br− (2), CN− (3), NO3− (4)), synthesised by the reaction of HgL2 with dppcb, is indicated by their solution NMR parameters and is confirmed by the X-ray structures of 1–3. Though the Fermi contact term is not always dominant in determining 1J(Hg,P), the NMR parameters are correlated to the changes in the bond lengths and angles in 1–3. A comparison is given with correlations derived from similar complexes. The reaction of 4 with 2,2′-bipyridine (bipy) or 1,10-phenanthroline (phen) leads to [Hg2(dppcb)(bipy)2](NO3)4 (5) and [Hg2(dppcb)(phen)2](NO3)4 (6). Also, for 5 and 6 the NMR data and FAB mass spectra are in agreement with tetrahedral HgII centres. The treatment of 4 with monophosphines produces trans-[Hg2(NO3)2(dppcb)L′2](NO3)2 (L′=P(CH2Ph)3 (7), P(CH2CH2CN)3 (8), PPh3 (9)). In 7–9 the typical large 1J(Hg,P) values are observed for the monophosphines compared with the corresponding parameters for chelating dppcb, which are reduced due to the five-membered ring formation. In the reaction of 4 with the diphosphine Ph2PCH2PPh2 (dppm) and the subsequent metathesis with LiAsF6, trans-[Hg2(NO3)2(dppcb)(η1-dppm)2](AsF6)2 (10) is formed. The X-ray structure of 10 showing coordinated and dangling phosphorus atoms of dppm is the first complete characterisation of a HgII complex containing two different chelating phosphines. Though in solution the dppm ligands are involved in fast intramolecular end-over-end exchange, the solution structure of 10 corresponds to its solid state structure, which is indicated by unusual 1J(Hg,P) values. Catalytic amounts of HgII convert trans-[Hg2(NO3)2(dppcb)(η1-dppm)2](NO3)2 into trans-[Hg2(NO3)2(dppcb)(η1-P-dppmO)2](NO3)2 (11), where dppmO is Ph2PCH2P(O)Ph2. The X-ray structure of 11 is the first complete characterisation of a HgII compound consisting of chelating phosphine together with phosphinoyl moieties. The solid state structure and the solution NMR parameters of 11 clearly show the presence of a dangling P(O)Ph2 group. The complexes 1–11 illustrate the tendency that polydentate donor ligands often geometrically and entropically restrict the number of accessible structures for HgII. Especially, the X-ray structures of 1–3, 10, and 11 indicate the preference of HgII for tetrahedral and trigonal pyramidal coordinations in compounds containing dppcb." @default.
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• W2063579554 date "2001-04-01" @default.
• W2063579554 modified "2023-09-24" @default.
• W2063579554 title "Solution and solid state behaviour of binuclear mercury(II) compounds containing cis,trans,cis-1,2,3,4-tetrakis(diphenylphosphino)cyclobutane: first X-ray structural characterisation of mercury(II) complexes with two different chelating phosphines" @default.
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• W2063579554 doi "https://doi.org/10.1016/s0277-5387(01)00708-2" @default.
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