The thermal behavior and morphology of a diblock copolymer of polystyrene and poly(ferrocenyldimethylsilane) (PFS) (M-a = 36000, phi(PS) = 0.308) have been surveyed using small angle X-ray scattering and transmission electron microscopy. As cast films are partly crystalline. The crystal structure is seriously perturbed by the propensity of the molecules to microphase segregation. After annealing above the glass transition temperature of polystyrene both crystallization and definition of the microphase separated domains are improved. The system forms an ordered microphase segregated structure once annealed above the melting temperature of the PFS block. Even then both cylindrical and spherical morphologies are observed and annealing times of a few days do not force the system to develop the long range order generally associated with carefully annealed polystyrene-b-polydiene polymers of comparable molecular weight.