9H-9-Silafluorene with two alkoxy groups underwent dehydro-coupling in the presence of [Pt(dmpe)(2)] (dmpe: 1,2-bis(dimethylphosphino)ethane) to produce tetrasilaplatinacyclopentanes having four silafluorenylene units. Ligand exchange of the persilylated platinacycles with non-substituted silafluorene released tetrasilane dihydrides with two pairs of pi-stacked biphenylene units. [Ni(dmpe)(2)] catalyzes the dehydrogenative polycondensation of 2,7-dibutoxy-9H-9-silafluorene to produce the poly(1,1-silafluorene).