High-pressure synthesis using the multianvil press is one of the most important synthetic strategies to prepare structurally versatile materials. Multianvil press is an instrument which employs quasi-hydrostatic compression of the samples and could generate pressure upto 25 GPa. Borates, gallates, germanates are the most widely researched group of compounds in the widespread field of high-pressure chemistry. Here, we focus on bringing out a synthetic strategy that clicked in preparing the first-of-its-kind mixed transition metal borate M5B12O25(OH) where M = Co and V possessing shared occupancies. The Co-V mixed borate, Co5-xVxB12O25(OH)crystallizes in tetragonal crystal system with space group I41/acd.