A series of tetrakis (alkylthio) tetraselenafulvalene compounds (TTC n-TSeF, n= 1–15) were prepared by a one-step reaction between dialkyl disulfide and tetralithiated TSeF. Molecular properties (redox potentials and optical absorptions in solution) and solid-state properties (thermal behaviors, electric conductivities, and molecular and crystal structures for n= 1 and 10) were studied. TTC n-TSeF compounds are weak electron donor molecules and ...