有机锡胂酸化合物的合成及结构研究
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摘要
在第一章中，比较全面的介绍了有机锡氧簇的合成、表征、结构和应用，最后，指明了本课题的选题意义，概括了本研究工作所取得的成果。
在第二章中，利用九种不同的芳基胂酸与三苯基化合物在溶剂热条件下合成了18个锡氧簇化合物，它们可以分四类：[(PhSn)_3(RAsO_3)_3(μ_3-O)(OH)(R'O)_2]_2Sn(A)、[(PhSn)_3(4-NO_2-C_6H_4AsO_3)_2(RAsO_3H)(μ_3-O)(R'O)_2]_2(B)、[(PhSn)_3(2，4-Cl_2-C_6H_3AsO_3)_3(μ_3-O)(R'O)_3]_2Sn(C)和[Sn_3Cl_3(μ_3-O)(R'O)_3]_2(RAsO_3)_4(D)。
A和B类型化合物的结构中都包含两个[Sn_3(μ_3-O)(μ_2-OR')_2]单元。而C和D类型化合物的结构中都包含两个[Sn_3(μ_3-O)(μ_2-OR')_3]单元。本章研究表明胂酸和有机锡先驱体会影响有机锡的结构。
在第三章中，利用烷基胂酸和三苯基化合物在溶剂热条件下合成了7个锡氧簇化合物：
[Sn_3Cl_3(μ_3-O)(R'O)_3]_2(RAsO_3)_4[R=n-Bu，R'=Et(3-1)；R=n-Pr，R'=Et(3-2)；R=Bz，R'=Et(3-3)；R=n-Pr，R'=Me(3-4)和R=4-NO_2-Bz，R'=Et(3-5)]和[(PhSn)_3(RAsO_3)_3(μ_3-O)(OH)(R'O)_2]_2Sn[R=n-Pr，R'=Et(3-6)和R=4-NO_2-Bz，R'=Et(3-7)]。
化合物(3-1)-(3-5)具有相似的结构，结构中都包含两个[Sn_3(μ_3-O)(μ_2-OR')_2]单元。而化合物(3-6)和(3-7)具有相似的结构，结构中都包含两个[Sn_3(μ_3-O)(μ_2-OR')_3]单元。本章研究了化合物(3-2)-(3-7)的氢键C-H…Cl，C-H…O和C-H…π。
在第四章中，以鼓状锡氧簇为先驱体和不同的胂酸反应，合成了7个有机锡氧簇：
[(n-BuSn)_5(μ_3-O)(OH)(R'O)_3(RAsO_3)_4(RAsO_3H)][R=2-NO_2-C_6H_4，R'=Me(4-1a和4-1b)]，[(n-BuSn)_3(RAsO_3)(μ_3-O)(CH_3CO_2)_3(R'O)_2]_2[R=2，4-(NO_2)_2-C_6H_3，R'=Me(4-2)]，[(n-BuSn)_3(RAsO_3)_2(RAsO_3H)(μ_3-O)(R'O)_2]_2[R=4-NO_2-C_6H_4，R'=Me(4-3)]和[(n-BuSn)_3(RAsO_3)_3(μ_3-O)(OH)(R'O)_2]_2Sn[R=C_6H_5CH_2，R'=Me(4-4)，C_6H_5CH_2，R'=H(4-5)和C_6H_5，R'=H(4-6)]。
化合物(4-1)是五核的有机锡氧簇，(4-2)和(4-3)为六核有机锡氧簇，而(4-4)-(4-6)为七核锡氧簇。
在第五章中，合成了两个聚合的二烷基锡胂酸化合物，[n-Bu_2Sn(4-OH-3-NO_2-C_6H_3AsO_3)]_n(5-1)和[n-Bu_2Sn(4-Me-C_6H_4SO_3)(4-NO_2-C_6H_4AsO_3H)]_n(5-2)。
第六章是结论。
In the first chapter, the syntheses, the structures and application of organotin oxo clustersare concisely introduced. At the end of this chapter, we pointed out the importance of thesearch project and summarized the important results obtained in the thesis.
In the second chapter, reactions of Ph_3SnOH or Ph_3SnCl with the arylarsonic acids give18 Sn-O cluster compounds. These compounds can be classified into four types: type A:[(PhSn)_3(RAsO_3)_3(μ_3-O)(OH)(R'O)_2]_2Sn; type B: [(PhSn)_3(RAsO_3)_2(RAsO_3H)(μ_3-O)(R'O)_2]_2;type C: [(PhSn)_3(RAsO_3)_3(μ_3-O)(R'O)_3]_2Sn; type D: [Sn_3Cl_3(μ_3-O)(R'O)_3]_2(RAsO_3)_4. Thestructures of A and B contain [Sn_3(μ_3-O)(μ_2-OR')_2] building block, while in C and D, thestannoxane cores are built by utilizing two [Sn_3(μ_3-O)(μ_2-OR')_3] building block. Thesyntheses, structures, and structural interrelationship of these diverse organostannoxanecompounds are discussed.
In the third chapter, reactions of Ph_3SnCl or Ph_3SnOH with the alkylarsonic acids haveled to seven organotin arsonate clusters: [Sn_3Cl_3(μ_3-O)(R'O)_3]_2(RAsO_3)_4 [R=n-Bu, R'=Et(3-1); R=n-Pr, R'=Et(3-2); R=Bz, R'=Et (3-3); R=n-Pr, R'= Me (3-4) and R =4-NO_2-Bz, R' = Et (3-5)] and [(PhSn)_3(RAsO_3)_3(μ_3-O)(OH)(R'O)_2]_2Sn [R = n-Pr, R' = Et(3-6) and R = 4-NO_2-Bz, R' = Et (3-7)]. Two types of structural units, [Sn_3(μ_3-O)(μ_2-OR')_3]for compounds (3-1)-(3-5) and [Sn_3(μ_3-O)(μ_2-OR')_2] for compounds (3-6) and (3-7), wereobtained by subtle changes of the organotin precursors. For the first time, hydrogen-bondinginteractions such as C-H…Cl, C-H…O and C-H…πwere investigated in the crystal structures oftin alkylarsonate clusters (3-2)-(3-7).
In the fourth chapter, treatment of the acetate drum, [n-BuSn(O)O_2CMe]_6, with differentarsonic acids gave seven organotin arsonate clusters: [(n-BuSn)_5(μ_3-O)(OH)(R'O)_3(RAsO_3)_4(RAsO_3H)] [R = 2-NO_2-C_6H_4, R' = Me (4-1a and 4-1b)],[(n-BuSn)_3(RAsO_3)(μ_3-O)(CH_3CO_2)_3(R'O)_2]_2 [R = 2,4-CNO_2)_2-C_6H_3, R' = Me (4-2)],[(n-BuSn)_3(RAsO_3)_2(RAsO_3H)(μ_3-O)(R'O)_2]_2 [R = 4-NO_2-C_6H_4, R' = Me (4-3)] and[(n-BuSn)_3(RAsO_3)_3(μ_3-O)(OH)(R'O)_2]_2Sn [R = C_6H_5CH_2, R' = Me (4-4), C_6H_5CH_2, R' = H(4-5) and C_6H_5, R' = H (4-6)]. The pentanuclear motif of (4-1a) and (4-1a), was firstly foundin organotin compounds. However, the structures of (4-2) and (4-3) present examples ofhexanuclear organotin-oxygen clusters. The heptanuclear structures of (4-4)-(4-6) arecomposed of two [Sn_3(μ_3-O)(μ_2-OR')_2] units connected via hydroxyl and arsonate ligands to asingle tin. The results reveal that the employment of the organotin precursors in syntheses oforganotin-oxygen arsonate clusters is very effective.
In the fifth chapter, the polymeric organotin arsonates [n-Bu_2Sn(4-OH-3-NO_2-C_6H_3AsO_3)]_n (5-1) and[n-Bu_2Sn(4-Me-C_6H_4SO_3)(4-NO_2-C_6H_4AsO_3H)]_n (5-2) have been successfully isolated.
The sixth chapter is the conclusions.
在第二章中，利用九种不同的芳基胂酸与三苯基化合物在溶剂热条件下合成了18个锡氧簇化合物，它们可以分四类：[(PhSn)_3(RAsO_3)_3(μ_3-O)(OH)(R'O)_2]_2Sn(A)、[(PhSn)_3(4-NO_2-C_6H_4AsO_3)_2(RAsO_3H)(μ_3-O)(R'O)_2]_2(B)、[(PhSn)_3(2，4-Cl_2-C_6H_3AsO_3)_3(μ_3-O)(R'O)_3]_2Sn(C)和[Sn_3Cl_3(μ_3-O)(R'O)_3]_2(RAsO_3)_4(D)。
A和B类型化合物的结构中都包含两个[Sn_3(μ_3-O)(μ_2-OR')_2]单元。而C和D类型化合物的结构中都包含两个[Sn_3(μ_3-O)(μ_2-OR')_3]单元。本章研究表明胂酸和有机锡先驱体会影响有机锡的结构。
在第三章中，利用烷基胂酸和三苯基化合物在溶剂热条件下合成了7个锡氧簇化合物：
[Sn_3Cl_3(μ_3-O)(R'O)_3]_2(RAsO_3)_4[R=n-Bu，R'=Et(3-1)；R=n-Pr，R'=Et(3-2)；R=Bz，R'=Et(3-3)；R=n-Pr，R'=Me(3-4)和R=4-NO_2-Bz，R'=Et(3-5)]和[(PhSn)_3(RAsO_3)_3(μ_3-O)(OH)(R'O)_2]_2Sn[R=n-Pr，R'=Et(3-6)和R=4-NO_2-Bz，R'=Et(3-7)]。
化合物(3-1)-(3-5)具有相似的结构，结构中都包含两个[Sn_3(μ_3-O)(μ_2-OR')_2]单元。而化合物(3-6)和(3-7)具有相似的结构，结构中都包含两个[Sn_3(μ_3-O)(μ_2-OR')_3]单元。本章研究了化合物(3-2)-(3-7)的氢键C-H…Cl，C-H…O和C-H…π。
在第四章中，以鼓状锡氧簇为先驱体和不同的胂酸反应，合成了7个有机锡氧簇：
[(n-BuSn)_5(μ_3-O)(OH)(R'O)_3(RAsO_3)_4(RAsO_3H)][R=2-NO_2-C_6H_4，R'=Me(4-1a和4-1b)]，[(n-BuSn)_3(RAsO_3)(μ_3-O)(CH_3CO_2)_3(R'O)_2]_2[R=2，4-(NO_2)_2-C_6H_3，R'=Me(4-2)]，[(n-BuSn)_3(RAsO_3)_2(RAsO_3H)(μ_3-O)(R'O)_2]_2[R=4-NO_2-C_6H_4，R'=Me(4-3)]和[(n-BuSn)_3(RAsO_3)_3(μ_3-O)(OH)(R'O)_2]_2Sn[R=C_6H_5CH_2，R'=Me(4-4)，C_6H_5CH_2，R'=H(4-5)和C_6H_5，R'=H(4-6)]。
化合物(4-1)是五核的有机锡氧簇，(4-2)和(4-3)为六核有机锡氧簇，而(4-4)-(4-6)为七核锡氧簇。
在第五章中，合成了两个聚合的二烷基锡胂酸化合物，[n-Bu_2Sn(4-OH-3-NO_2-C_6H_3AsO_3)]_n(5-1)和[n-Bu_2Sn(4-Me-C_6H_4SO_3)(4-NO_2-C_6H_4AsO_3H)]_n(5-2)。
第六章是结论。
In the first chapter, the syntheses, the structures and application of organotin oxo clustersare concisely introduced. At the end of this chapter, we pointed out the importance of thesearch project and summarized the important results obtained in the thesis.
In the second chapter, reactions of Ph_3SnOH or Ph_3SnCl with the arylarsonic acids give18 Sn-O cluster compounds. These compounds can be classified into four types: type A:[(PhSn)_3(RAsO_3)_3(μ_3-O)(OH)(R'O)_2]_2Sn; type B: [(PhSn)_3(RAsO_3)_2(RAsO_3H)(μ_3-O)(R'O)_2]_2;type C: [(PhSn)_3(RAsO_3)_3(μ_3-O)(R'O)_3]_2Sn; type D: [Sn_3Cl_3(μ_3-O)(R'O)_3]_2(RAsO_3)_4. Thestructures of A and B contain [Sn_3(μ_3-O)(μ_2-OR')_2] building block, while in C and D, thestannoxane cores are built by utilizing two [Sn_3(μ_3-O)(μ_2-OR')_3] building block. Thesyntheses, structures, and structural interrelationship of these diverse organostannoxanecompounds are discussed.
In the third chapter, reactions of Ph_3SnCl or Ph_3SnOH with the alkylarsonic acids haveled to seven organotin arsonate clusters: [Sn_3Cl_3(μ_3-O)(R'O)_3]_2(RAsO_3)_4 [R=n-Bu, R'=Et(3-1); R=n-Pr, R'=Et(3-2); R=Bz, R'=Et (3-3); R=n-Pr, R'= Me (3-4) and R =4-NO_2-Bz, R' = Et (3-5)] and [(PhSn)_3(RAsO_3)_3(μ_3-O)(OH)(R'O)_2]_2Sn [R = n-Pr, R' = Et(3-6) and R = 4-NO_2-Bz, R' = Et (3-7)]. Two types of structural units, [Sn_3(μ_3-O)(μ_2-OR')_3]for compounds (3-1)-(3-5) and [Sn_3(μ_3-O)(μ_2-OR')_2] for compounds (3-6) and (3-7), wereobtained by subtle changes of the organotin precursors. For the first time, hydrogen-bondinginteractions such as C-H…Cl, C-H…O and C-H…πwere investigated in the crystal structures oftin alkylarsonate clusters (3-2)-(3-7).
In the fourth chapter, treatment of the acetate drum, [n-BuSn(O)O_2CMe]_6, with differentarsonic acids gave seven organotin arsonate clusters: [(n-BuSn)_5(μ_3-O)(OH)(R'O)_3(RAsO_3)_4(RAsO_3H)] [R = 2-NO_2-C_6H_4, R' = Me (4-1a and 4-1b)],[(n-BuSn)_3(RAsO_3)(μ_3-O)(CH_3CO_2)_3(R'O)_2]_2 [R = 2,4-CNO_2)_2-C_6H_3, R' = Me (4-2)],[(n-BuSn)_3(RAsO_3)_2(RAsO_3H)(μ_3-O)(R'O)_2]_2 [R = 4-NO_2-C_6H_4, R' = Me (4-3)] and[(n-BuSn)_3(RAsO_3)_3(μ_3-O)(OH)(R'O)_2]_2Sn [R = C_6H_5CH_2, R' = Me (4-4), C_6H_5CH_2, R' = H(4-5) and C_6H_5, R' = H (4-6)]. The pentanuclear motif of (4-1a) and (4-1a), was firstly foundin organotin compounds. However, the structures of (4-2) and (4-3) present examples ofhexanuclear organotin-oxygen clusters. The heptanuclear structures of (4-4)-(4-6) arecomposed of two [Sn_3(μ_3-O)(μ_2-OR')_2] units connected via hydroxyl and arsonate ligands to asingle tin. The results reveal that the employment of the organotin precursors in syntheses oforganotin-oxygen arsonate clusters is very effective.
In the fifth chapter, the polymeric organotin arsonates [n-Bu_2Sn(4-OH-3-NO_2-C_6H_3AsO_3)]_n (5-1) and[n-Bu_2Sn(4-Me-C_6H_4SO_3)(4-NO_2-C_6H_4AsO_3H)]_n (5-2) have been successfully isolated.
The sixth chapter is the conclusions.
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