| The synthesis of novel inorganic materials has been receiving great attention due to their widespread applications in separation, absorption, ion-exchange, catalysis and remediation of radioactive waste. Recent decades, many groups have commit themselves to the synthesis of novel germanates and vanadates because of not only the diversity of the structures but also the potential applications in different fields. In this thesis, in order to improve the thermal stability of germanates and obtain novel vanadates, eleven novel compounds have been reported, which were synthesized under hydrothermal and sovlothermal conditions by changing and adjusting different factors including the materials, solvents, temperature, concentration and so on. All of the structures were characterized by single crystal X-ray diffraction and their properties were studied by Elemental Analysis, IR, TG .1. Three new nickel complexes [Ni(C3N2H4)6](SO4)(H2O)2 1 ,Ni3(C10N2H8)2(SO4)3(H2O)11 2 and Ni2V4O12.5 (C10N2H8)4 (H3O) 3 have been synthesized under hydrothermal conditions and characterized by IR spectroscopy, powder XRD, TG and single crystal X-ray diffraction. Compound 1 crystallizes in the Trigonal space group P-31c with a = b= 9.0029(9) (?), c = 22.937(4) (?), V = 1610.0(4) (?)3, Z = 2. Compound 2:Triclinic,space group P1, a = 11.1737(11) (?), b = 11.1737(11) (?), c = 11.3668(11) (?),α= 72.8220(10)°,β= 73.3880(10)°,γ= 83.6400(10)°, V = 844.09(14) (?)3, Z = 1. Compound 3:Triclinic,space group P-1, a = 8.995(4) (?), b = 11.282(5) (?), c = 14.966(7) (?),α= 76.262(6)°,β= 81.595(6)°,γ= 68.378(5)°, V = 1368.6(11) (?)3, Z = 2. These three nickel complexes were new and obtained by adjusting the reaction conditions during experiments, which keep different dimensional strctures.2. Two new organic templated 1-D linear vanadium sulfates (C2H10N2)4 [GaV3 (SO4)8(OH)4]·4H2O 4 and [C4H12N2][VIII (OH)(SO4)2]·H2O 5 have been synthesized under solvothermal conditions and characterized by IR spectroscopy, TG and single crystal X-ray diffraction. Compound 4 crystallizes in the Monoclinic space group P2(1)/c, a = 6.8956(15) (?), b = 10.303(2) (?), c = 15.094(3) (?),β= 90.802(3)°,V = 1073.23 (3) (?)3, Z = 1. Compound 5:Monoclinic, P2(1)/c,a = 9.290(4) (?), b = 18.264(7) (?), c = 7.132(3) (?),β= 98.149(8)°, V = 1197.9(8) (?)3, Z = 4. In the structure of compound 4 and 5, the OH and SO4 tetrahedra as bridging ligands connected the VO6 octahedra to generate an infinite chain, and protonated organic amines exist between the chains and involve in the hydrogen bonding interaction to generate a 3D supermolecule structure.3. Three new germanates Ge10O20 (H2O)3 6,Ge7O12(OH)4(C6NH15)0.5(H2O)4 7 and Ge7O12(OH)4(C3NH9)0.25(H2O)5 8 with different topology structures have been synthesized under hydrothermal and solvothermal conditions, and characterized by IR spectroscopy, powder XRD, TG and single crystal X-ray diffraction. Compound 6 crystallizes in the tetragonal space group P4/mcc, a = b = 8.7885(18) (?) , c = 14.490(6) (?), V = 1119.2(6) (?)3, Z = 2. Compound 7: cubic, P-43m,a = 7.7187(1) (?), V = 459.87(1) (?)3, Z = 1. Compound 8: cubic, P-43m, a = 7.7198(6) (?), V = 460.06(6) (?)3, Z = 1. Compound 6 has the same framework as ASU-7, which presents 12-membered-ring channels along the c axis. Compounds 7 and 8 are the same structure and templated by two different organic amines, which are composed of Ge4(OH)4 cubanes and chiral intertwined Ge-O double helices, moreover, 2-D 8-membered-ring channels can be observed in the structure.4. In order to enhance the thermal stability of the germanates, three new microporous aluminogermanates [C4H12N] [AlGe3O8] 9,KAlGe3O8 10和KAl2Ge2O7F 11 with different zeolite topologies have been synthesized under solvothermal condition and characterized by IR spectroscopy, powder XRD, TG and single crystal X-ray diffraction. Compound 9 crystallizes in the tetragonal space group I41/a, a = b = 10.7754(8) (?), c = 9.9116(14) (?), V = 1150.8(2) (?)3, Z = 4. Compound 10: Orthorhombic, Pnma, a = 9.4336(13) (?), b = 8.7068(12) (?), c = 9.8212(14) (?), V = 806. 68 (19) (?)3, Z = 4. Compound 11: tetragonal, I-42d,a = b = 7.3626(4) (?), c = 17.4940(18) (?),V = 948.31(12) (?)3, Z = 4. Compound 9 as an organic templated microporous aluminogermanates has the same topology as GIS zeolite. Compound 10 has the same topology as para zeolite, while compound 11 has the same structure as MON zeolite. Specially, compound 9 shows good thermal stability by calcinations, the structure of inorganic framework is retained when the organic amine is removed by calcinations, which provides potential applications for the zeolite.
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