Synthesis, Crystal Structure And Characterization Of Hybrid Transition Metal Borate And Phosphate

A new organic-inorganic hybrid transition metal pentaborate and two phosphate compounds were synthesized by hydrothermal methods. The structures of these compounds were determined by single crystal X-ray diffraction. FT-IR spectrum, Raman spectrum, elemental analysis and thermal analysis were also used for characterization.( 1 ) A n o v e l o r g a n i c - i n o r g a n i c c o p p e r p e n t a b o r a t e [Cu(C3N2H4)4][Cu(CH3COO)2(C3N2H4)2(H2O)2][B5O6(OH)4]2 was synthesized by hydrothermal methods, which crystallizes in triclinic system, space group _P , a=6.2480(14)?, b=11.5671(17)?, c=11.7791(19)?,α=83.084(9)°,β=75.721(8)°,γ=66.685(6)°, V=1120.9(3)?3, Z=1. The structure of this compound consists of [Cu(C3N2H4)4]2+ cation, [Cu(CH3COO)2(C3N2H4)2(H2O)2] neutral cluster and two isolated [B5O6(OH)4]- polyanions. The isolated anions form infinite anionic layers with eight-membered boron rings along ab plane by hydrogen bonds. Moreover, the copper-centered octahedrons are connected by common oxygen atom and form an infinite chain. The metal chains are further intercalated with the anionic layers via hydrogen bonding interaction, forming a three-dimensional framework.(2) A new organically templated cobalt phosphate supramolecule [Co(H2O)6]2[HPO4]4·2(H3NCH2CH2NH3) was synthesized hydrothermally. It crystallizes in monoclinic system, space group P2(1)/c, a=6.271(3)?, b=16.367(8)?, c=14.736(8)?,β=91.405(7)°, V=1512.2(3)?3, Z=2,ρ=1.850g/cm3. The fundamental building blocks of the crystal structure consist of two cobalt octahedrons, four isolated PO3(OH) tetrahedras and two diprotonated ethylenedimaine molecules. The cobalt octahedrons and PO3(OH) tetrahedras are linked together via hydrogen bonding interaction, forming a pseudo-open framework with alternatively deposited one-dimensional channels. Protonated ethylenediamine molecules reside in the spacing of the framework and compensate the charge balance.(3) An organic phosphate (H3NCH2CH2NH3)(HPO4) was prepared under hydrothermal conditions. It crystallizes in monoclinic system, space group P2(1)/c, a=7.4858(17)?, b=11.776(3)?, c=7.9980(18)?,β=110.225(3)°, V=661.6(3)?3, Z=4,ρ=1.587g/cm3. The structure consists of phoshpate tetrahedras and protonated ethylenediamine molecules. The HPO4 tetrahedras are linked together by hydrogen bonds, forming infinite chains, which are further connected with ethylenediamine molecules by H bonds to construct a three-dimensional structure.(4) The hydrothermal synthesis of organic-inorganic metal borate and phosphate was discussed.