Due to thiolate's fast and robust coordination, crystallographically resolved thiolate-ligated metal-organic frameworks (MOFs) are hard to obtain. Following the previous success of the masked synthetic strategy to achieve single-crystal Pb-thiolate connected MOFs, thioester-protected hexathiotriphenylene (HVaTT) was employed in this work to assemble with a Zn(II) centre to yield the first example of a first-row transition-metal based crystallographically resolved metal-tetrathiolate connected MOF, HTT-Zn. HTT-Zn features a 3D anionic framework connected by tetrahedral [ZnS