一些含碲杂多化合物的研究
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摘要
本论文由以下四部分组成：
第一部分：前言
介绍了杂多化合物的基本概念、发展历史、基本结构、分类及将来的发展方向，并对以第Ⅵ_A族元素Te为杂原子的的多金属氧酸盐的研究现状进行了文献总结。
第二部分：过渡金属配合物连接的碲钨杂多酸盐的合成与表征
首次合成了含有Anderson-Evan杂多阴离子结构的无机-有机碲钨杂多酸盐复合物Na_2[Co(phen)_3]_2[TeW_6O_(24)]·25.16H_2O(1)和Na_2[Ni(phen)_3]_2[TeW_6O_(24)]·22H_2O(2)(phen=phenanthroline)，通过组成分析、IR、UV、TG等方法对其进行了表征，并通过X单晶衍射测定其结构。通过单晶X射线分析表明，化合物1属单斜品系，空间群P2(1)／n，晶胞参数a=9.903(2)(?)，b=23.761(7)(?)，c=21.092(5)(?)，V=4962(2)(?)~3，Z=2，Dc=2.218g／cm~3，R_1=0.0364；化合物2属三斜晶系，空间群P-1，晶胞参数a=11.329(4)(?)，b=16.148(6)(?)，c=16.367(6)(?)，V=2477.7(15)(?)~3，Z=1，Dc=2.182g／cm~3，R_1=0.0630。
第三部分：Na_2(en){[Ni(en)_2(H_2O)]_2[Te_(0.8)W_(6.2)O_(24)])·8H_2O和Na_2{[Cu(en)_2]_2[Te_(0.8)W_(6.2)O_(24)]}·12H_2O的合成与表征
首次合成了两种特殊的，含有Anderson-Evan结构的无机-有机复合物Na_2(en){[Ni(en)_2(H_2O)]_2[Te_(0.8)W_(6.2)O_(24)]}·8H_2O和Na_2{[Cu(en)_2]_2[Te_(0.8)W_(62)O_(24)]}·12H_2O(en=ethylenediamine)，通过X射线分析了化合物晶体的晶体结构并通过组成分析、IR、UV、TG等方法对其进行了表征。
第四部分：含有镧系元素的碲钼杂多化合物的合成与表征
本文合成了一系列含有镧系元素的碲钼杂多化合物[Ln(H_2O)_7]_2[TeMo_6O_(24)]·6H_2O(Ln=La，Pr，Sm)和[Ce(H_2O)_6]_2[TeMo_6O_(24)]·6H_2O，通过X射线分析了化合物晶体的晶体结构，使用化学分析、元素分析、IR、TG方法对其进行了表征。
This dissertation is composed of four parts as following:
Part one: Review
In this part, the history, structure, classification and future opportunities of heteropoly compounds were reviewed and the research state of heteropoly compounds containing the VI_A elements Te as heteroatom was summarized.
Part two: Synthesis and Characterization of Tungstotellurate Linked by Transition Metal Complex Fragments.
In this part, two novel organic-inorganic hybrid tungstotellurate Na_2[Co(phen)_3]_2[TeW_6O_(24)]·25.16H_2O and Na_2[Ni(phen)_3]_2[TeW_6O_(24)]·22H_2O(2) (phen = phenanthroline)have been synthesized and characterized by the elemental analyses, infrared spectra, thermal analyses, and single-crystal X-ray diffraction. The compound 1 crystallizes in the monoclinic system, space group P2 (1)/n with a= 9.903(2) A, b = 23.761(7) A, c = 21.092(5) A, V= 4962(2) A~3, Z=2, Dc = 2.218g/cm~3, R_1 = 0.0364; The compound 2 crystallizes in the monoclinic system, space group P-1 with 11.329(4) A, b=16.148(6 ) A, c=16.367(6) A, V=2477.7(15) A~3, Z=1, Dc=2.182g/cm~3 , R_1= 0.0630= The X-ray structure analysis reveals that both the compounds contain Anderson-Evans type anion.
Part three: Synthesis and Characterization of Organic-Inorganic Hybrid of Na_2(en){[Ni(en)_2(H_2O)]_2[Te_(0.8)W_(6.2)O_(24)]}·8H_2O andNa_2{[Cu(en)_2]_2[Te_(0.8)W_(6.2)O_(24)]}·12H_2O
In this part, the title compounds, Na_2(en){[Ni(en)_2(H_2O)]_2[Te_(0.8)W_(6.2)O_(24)]}·8H_2O and Na_2{[Cu(en)_2]2[Te_(0.8)W_(6.2)O_(24)]}·12H_2O (en = ethylenediamine) were synthesized and reported for the first time and were characterized by using single-crystal X-ray diffraction, chemical analysis, IR and TG.
Part four: Synthesis and Characterization a series of Heteropolymolybdate with Te~(6+) containing Lanthanide.
In this part, four compounds of heteropolymolybdate with Te~(6+) containing lanthanide were synthesized and reported for the first time. The physical and chemical properties of these new heteropoly compounds were studied by using chemical analysis, elementary analysis, infrared spectra, thermal analyses, and single-crystal X-ray diffraction.
第一部分：前言
介绍了杂多化合物的基本概念、发展历史、基本结构、分类及将来的发展方向，并对以第Ⅵ_A族元素Te为杂原子的的多金属氧酸盐的研究现状进行了文献总结。
第二部分：过渡金属配合物连接的碲钨杂多酸盐的合成与表征
首次合成了含有Anderson-Evan杂多阴离子结构的无机-有机碲钨杂多酸盐复合物Na_2[Co(phen)_3]_2[TeW_6O_(24)]·25.16H_2O(1)和Na_2[Ni(phen)_3]_2[TeW_6O_(24)]·22H_2O(2)(phen=phenanthroline)，通过组成分析、IR、UV、TG等方法对其进行了表征，并通过X单晶衍射测定其结构。通过单晶X射线分析表明，化合物1属单斜品系，空间群P2(1)／n，晶胞参数a=9.903(2)(?)，b=23.761(7)(?)，c=21.092(5)(?)，V=4962(2)(?)~3，Z=2，Dc=2.218g／cm~3，R_1=0.0364；化合物2属三斜晶系，空间群P-1，晶胞参数a=11.329(4)(?)，b=16.148(6)(?)，c=16.367(6)(?)，V=2477.7(15)(?)~3，Z=1，Dc=2.182g／cm~3，R_1=0.0630。
第三部分：Na_2(en){[Ni(en)_2(H_2O)]_2[Te_(0.8)W_(6.2)O_(24)])·8H_2O和Na_2{[Cu(en)_2]_2[Te_(0.8)W_(6.2)O_(24)]}·12H_2O的合成与表征
首次合成了两种特殊的，含有Anderson-Evan结构的无机-有机复合物Na_2(en){[Ni(en)_2(H_2O)]_2[Te_(0.8)W_(6.2)O_(24)]}·8H_2O和Na_2{[Cu(en)_2]_2[Te_(0.8)W_(62)O_(24)]}·12H_2O(en=ethylenediamine)，通过X射线分析了化合物晶体的晶体结构并通过组成分析、IR、UV、TG等方法对其进行了表征。
第四部分：含有镧系元素的碲钼杂多化合物的合成与表征
本文合成了一系列含有镧系元素的碲钼杂多化合物[Ln(H_2O)_7]_2[TeMo_6O_(24)]·6H_2O(Ln=La，Pr，Sm)和[Ce(H_2O)_6]_2[TeMo_6O_(24)]·6H_2O，通过X射线分析了化合物晶体的晶体结构，使用化学分析、元素分析、IR、TG方法对其进行了表征。
This dissertation is composed of four parts as following:
Part one: Review
In this part, the history, structure, classification and future opportunities of heteropoly compounds were reviewed and the research state of heteropoly compounds containing the VI_A elements Te as heteroatom was summarized.
Part two: Synthesis and Characterization of Tungstotellurate Linked by Transition Metal Complex Fragments.
In this part, two novel organic-inorganic hybrid tungstotellurate Na_2[Co(phen)_3]_2[TeW_6O_(24)]·25.16H_2O and Na_2[Ni(phen)_3]_2[TeW_6O_(24)]·22H_2O(2) (phen = phenanthroline)have been synthesized and characterized by the elemental analyses, infrared spectra, thermal analyses, and single-crystal X-ray diffraction. The compound 1 crystallizes in the monoclinic system, space group P2 (1)/n with a= 9.903(2) A, b = 23.761(7) A, c = 21.092(5) A, V= 4962(2) A~3, Z=2, Dc = 2.218g/cm~3, R_1 = 0.0364; The compound 2 crystallizes in the monoclinic system, space group P-1 with 11.329(4) A, b=16.148(6 ) A, c=16.367(6) A, V=2477.7(15) A~3, Z=1, Dc=2.182g/cm~3 , R_1= 0.0630= The X-ray structure analysis reveals that both the compounds contain Anderson-Evans type anion.
Part three: Synthesis and Characterization of Organic-Inorganic Hybrid of Na_2(en){[Ni(en)_2(H_2O)]_2[Te_(0.8)W_(6.2)O_(24)]}·8H_2O andNa_2{[Cu(en)_2]_2[Te_(0.8)W_(6.2)O_(24)]}·12H_2O
In this part, the title compounds, Na_2(en){[Ni(en)_2(H_2O)]_2[Te_(0.8)W_(6.2)O_(24)]}·8H_2O and Na_2{[Cu(en)_2]2[Te_(0.8)W_(6.2)O_(24)]}·12H_2O (en = ethylenediamine) were synthesized and reported for the first time and were characterized by using single-crystal X-ray diffraction, chemical analysis, IR and TG.
Part four: Synthesis and Characterization a series of Heteropolymolybdate with Te~(6+) containing Lanthanide.
In this part, four compounds of heteropolymolybdate with Te~(6+) containing lanthanide were synthesized and reported for the first time. The physical and chemical properties of these new heteropoly compounds were studied by using chemical analysis, elementary analysis, infrared spectra, thermal analyses, and single-crystal X-ray diffraction.
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