Reaction of (toluene)iron complex I with CH2:CHCH2Br in KOH gave 60% triallyltoluene iron complex II. Similar allylation of [FeCp(h6-mesitylene)] with CH2:CHCH2Br in DME gave an allyl complex along with demetalated product 1,3,5-C6H3[C(CH2CH:CH2)3]3 (III). Regioselective hydroboration of III with (Me2CHCHMe)2BH in THF followed by alk. oxidn. with 30% H2O2/NaOH gave hygroscopic polyol 1,3,5-C6H3[C(CH2CH2CH2OR)3]3 (IV); R = H). Nonaarylmetalation of IV with [FeCp(h6-p-MeC6H4F)][PF6] in the presence of K2CO3/(Bu4N)Br in THF/DMSO gave title complex IV [R = Fe(h6-p-MeC6H4)] (V). The cyclic voltammetry of V and crystal structure of III were discussed.