Co(En)\-3MoO\-4 was synthesized by using the method of hydrothermal synthesis and characterized by elemental analysis, IR, ESR and single\|crystal X\|ray methods. It crystallizes in hexagonal space group \%P3C1\% with \{\%a\%=1\^596 4(2) nm\}, \{\%b\%=1\^596 4(2) nm\}, \%c\%=\{0\^993 5(2)\} nm, \%α=β\%=90°, \%γ\%=120°, \%M\%\-c=399\^18, \%V\%=2\^192 6(6) nm\+3, \%D\%\-c=1\^814 g/nm\+3, \%Z\%=6, \%F\%(000)=1 218, \%R\%\-1=0\^070 3, \%R\%\-w=0\^220 7. According to separation of anion which acted on electrostatic potential, the anion and cation ions formed a type of organic and inorganic material.
A layered inner tunnel supramolecular compound 1, [(CuI) 2( o phen) 2], was hydrothermally synthesized and structurally characterized by X ray crystal diffraction. It crystallizes in triclinic system, space group P 1 with a =0.775 9(2) nm, b =0.907 0(2) nm, c =0.918 94(10) nm, α =96 306(14)°, β = 104.567(16)°, γ =109.421(19)°, V =0.576 8(2) nm 3, Z=1, R=0.034 8, wR =0.092 0.
A novel layered compound, [Ni(C 10 H 8N 2) 2V 3O 8 5 ], was hydrothermally synthesized and structurally characterized by single crystal X ray diffraction. The compound crystallizes in monoclinic system, space group P2 1/c with a =1 551 8(3) nm, b =1 476 1(3) nm, c =1 048 3(2) nm, β=92 02(3)°, V = 2 399 8 (8) nm 3, Z=4, R=0 046 7, wR 2= 0 085 9.
A new compound, \[Ni(en)\-3\]\-2\[Ni(en)\-2(H\-2O)\-2\]\[As\-6V\-\{15\}O\-\{42\}\]·4H\-2O, was first prepared by hydrothermal synthesis and characterized by elemental analysis, IR, TGA\|DSC, ESR and single crystal X\|ray diffraction. Crystal data: monoclinic, space group \%C\-c, a\%=1\^523 6(3) nm, \%b\%=2\^051 8(4) nm, \%c\%=2\^395 9(5) nm, \%β=97\^41(3)°, V\%=7\^427(3) nm\+3, \%Z=4, R=0\^057 0, wR\-2=0\^135 7\%. The polyanion consists of six AsO\-3 pyramids and fifteen VO\-5 pyramids. Counterions are complex ions with octahedral structure, which consist of NH\-2CH\-2CH\-2NH\-2 and Ni\+\{2+\}.
