By　the　solvothermal　reaction　of　a　triangular　ligand,　2,4,6-tris-(4-carboxyphenoxy)-1,3,5-triazine　(H(3)tcpt)　with　Zn(NO3)(2)center　dot　6H(2)O　in　N,　N＇-dimethylacetamide/acetonitrile/H2O　(v/v/v　=　1　:　1　:　1)　mixed　solvents,　a　two-fold,　interpenetrated,　three-dimensional　(3D),　porous　metal-organic　framework,　[Zn-2(tcpt)OH]center　dot　solvents　(1　center　dot　solvents),　with　a　rare,　paddlewheel　secondary　building　unit　(SBU),　Zn-2(COO)(3),　was　synthesized　and　characterized.　It　was　found　that　a　single　3D　structure　of　1　forms　when　two-dimensional　layers,　which　are　constructed　by　tcpt(3-)　bonding　with　the　paddlewheel　SBUs,　are　linked　by　-OH　groups　along　the　axial　sites　of　the　SBUs.　Compared　with　the　reported　Zn(II)-based　partners　with　this　ligand,　synthesis　conditions,　particularly　the　solvents　used,　clearly　played　a　key　role　in　the　formation　of　different　SBUs,　thereby　resulting　in　distinct　MOFs　with　the　same　ligand.　In　particular,　1　features　good　water　and　thermal　stability　and　can　withstand　acidic　aqueous　solutions　with　pH　values　ranging　from　5　to　12.　In　addition,　1　displays　good　adsorption　ability　towards　H-2　(2.21　wt%　at　77　K　and　1　atm)　and　can　selectively　adsorb　CO2　from　CH4　and　N-2,　in　spite　of　its　relatively　low　void　volume　(36.8%),　suggesting　potential　applications　in　gas　storage　and　separation.