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  • Title: Polymorphism and spin crossover in mononuclear Fe(II) species containing new dipyridylamino-substituted s-triazine ligands.
    Author: Ross TM, Moubaraki B, Neville SM, Batten SR, Murray KS.
    Journal: Dalton Trans; 2012 Feb 07; 41(5):1512-23. PubMed ID: 22143200.
    Abstract:
    Four new dipyridylamino-substituted s-triazine ligands DBB (N(2),N(2),N(4),N(4)-tetrabenzyl-N(6),N(6)-di(pyridin-2-yl)-1,3,5-triazine-2,4,6-triamine), DDB (N(2),N(2),N(4),N(4)-tetrabutyl-N(6),N(6)-di(pyridin-2-yl)-1,3,5-triazine-2,4,6-triamine), DCCl (6-chloro-N(2),N(2)-dicyclohexyl-N(4),N(4)-di(pyridin-2-yl)-1,3,5-triazine-2,4-diamine) and DDT (N(2),N(2),N(4),N(4)-tetraphenyl-N(6),N(6)-di(pyridin-2-yl)-1,3,5-triazine-2,4,6-triamine), have been incorporated into eight new, 0D Fe(II) compounds of type [Fe(II)(NCX)(2)(L)(2)]·Solvent (where NCX = NCS(-), NCSe(-) or N(CN)(2)(-)). The polymorphic compounds α-trans-[Fe(II)(NCS)(2)(DBB)(2)] (1) and β-trans-[Fe(II)(NCS)(2)(DBB)(2)] (2) display, respectively, a relatively abrupt, complete, one-step spin transition with T(½) ~ 170 K, and a more gradual, complete, one-step spin transition with T(½) ~ 300 K. Gradual, one-step spin transitions are observed for trans-[Fe(II)(N(CN)(2))(2)(DBB)(2)]·2CH(3)CH(2)OH (3) and trans-[Fe(II)(NCSe)(2)(DCCl)(2)]·2CH(3)OH (6) with T(½) ~ 280 K for both, while the one-step spin transition observed for a desolvated sample of trans-[Fe(II)(NCSe)(2)(DDB)(2)]·2CH(3)OH (4) is relatively abrupt, showing hysteresis with T(½↑) = 285 K and T(½↓) = 275 K. The compounds cis-[Fe(II)(NCS)(2)(DDB)(2)] (5) and trans-[Fe(II)(NCS)(2)(DDT)(2)]·4CH(2)Cl(2) (7) remain high spin, while structural data on trans-[Fe(II)(NCSe)(2)(DDT)(2)]·4CH(2)Cl(2) (8) suggests a spin transition at low temperatures. It is likely that distortion of the Fe(II)N(6) octahedron, intermolecular interactions and molecular conformation are crucial in deciding both the T(½) and abruptness of the spin transition for these species, although the nature of their influence varies. Variable temperature powder X-ray diffraction measurements on the polymorphs 1 and 2 reveal anisotropy in the unit cell parameters as the spin transition occurs.
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