Inorg. Chem. 1992, 31, 2255-2264 Table IV. Crystallographic Data for C1Fe"'(OEPOAc).CH2CI2
C39H48C13FeN402 a = 10.238 (2) A b = 13.301 (2) A c = 15.088 (3) A a = 77.610 (2)" j3 = 71.820 (2)O y = 75.430 (2)' z = 2 V = 1868.5 (6)
" R=
fw = 767.0 Pi, triclinic T = 130K A(Cu Ka) = 1.54178 A r(Cu Ka) = 5.574 dcald,Mgm-' = 1.360 transm factors 0.63-0.87 Ra = 0.051 Rwa= 0.053
ZllFol- l~,ll/F0land Rw= CIIF,I
- IFc11w1/2/~I~ow1/21.
purple, crystalline product obtained after recrystallization from chloroform-hexane. UV-vis (Amax): 388, 506, 544, 642 nm. X-ray Crystdographic Studies. A suitable crystal of ClFe"'(0EPOAc).CH2Cl2was obtained by slow diffusion of hexane through a 2-mm layer of methanol into a dichloromethane solution of the complex in a 5 mm diameter tube. A crystal was mounted on a glass fiber with silicone grease and positioned in the cold stream of a Siemens P3/RA diffractometer. Only random fluctuations (
