Treatment of 1-chloro-6-iodohexane or 1-chloro-10-iododecane with lithium tris(pyrazolyl)methanide, followed by potassium thioacetate, affords bifunctional 1-S(acetyl)-tris(pyrazolyl)alkanes (L) (pz)(3)C-(CH2)(n)SAc (n = 6, 1; 10, 2). Magnetic studies of {[(pzTp)Fe-III-(CN)(3)](4)[(NiL)-L-II](4)[OTf](4)}center dot solvent (4, L = 1; 5, L = 2) boxes suggest that -(CH2)(6) chains (4) limit intermolecular interactions while -(CH2)(10) chains in 5 introduce crystallographic disorder and a distribution of relaxation times; 4 and 5 exhibit slow relaxation of the magnetization.