Chemical Crystallography (Chemistry Research and by Bryan L. Connelly

By Bryan L. Connelly

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A diagram of [Mn(dipic)(bpy)]. (Reproduced by permission from reference 124). 32 A. Alvin Holder, C. Lesley Lewis-Alleyne, Don vanDerveer et al. The X-ray crystal structure of [Mn(chedam)(bpy)]·H2O is shown in Figure 22. The structure contains monomeric [Mn(dicarboxylate)(bpy)H2O] units in which the Mn(II) ions have very irregular six-coordinate geometry. 19(5)8) ligands. 23 In this unique structure, [(dipic)2(Hdipic)2FeII3(OH2)4] crystallizes in the centrosymmetric space group P2l/n. The asymmetric unit contains half a molecule located on a crystallographic inversion center on Fe(1) as shown on Figure 23 and a crystallization water molecule in general position.

5H2O and other known seven-coordinate dipicolinato-vanadium(V) complexes with ternary peroxo or hydroxylamido ligands. H2O is shown. [VO2(dipicOH)]- exists as a discrete mononuclear unit with the vanadium atom in a distorted trigonal bipyramidal coordination environment. The pyridine nitrogen atom (N1) and two oxygen atoms (O1, O2) of the VO2 group coordinate to the vanadium center and occupy the distorted equatorial plane, while two carboxylate oxygen atoms occupy the axial positions. 022(4) Å above the least squares equatorial plane through O1, O2, and N1.

The bond angles about the vanadium(V) suggested either a distorted square-pyramidal or trigonal-bipyramidal structure shown in Figure 13. 85°. 283. 105 The bond distances and angles in these structures may be compared to the corresponding structural features of the Cs[VO2(dipic)]100 and Na[VO2(dipic-OH)],81, 99 and Na[VO2(dipic-NH2)] (see Table 4). From the values in this table it is clear that the V=O and V-O bond lengths are virtually identical, showing that substitution in the 4-position of the pyridine ring does not affect those bonds.

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