This report describes a new approach to prepare atom thick metal–sulfide–graphene nanosheets produced by the subsequent annealing of crosslinked carbon–metal film formed at the water–hexane interface. A bipyridine dithiol (BPD) layer self-assembled in the water–hexane hydrophilic/hydrophobic biphasic medium was used to encapsulate metal ions (M²⁺) (M = Co or Ni). Subsequently, the BPD–M²⁺ film was crosslinked using UV-light. Then the resultant carbon–metal nanosheets were annealed at high temperature under N₂, transforming these molecular sheets into a homogeneous nano-crystalline metal–sulfide–graphene hybrids (MSGH). This approach can produce semi-transparent conducting films having marked conductivity dependence on the number of nanosheets in a stack. The suggested strategy opens up broad prospects toward the MSGH architecture using a simple process with new properties for new applications such as energy conversion/storage and electronics.