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首页> 外文学位 >Synthesis and characterization of metal complexes containing tetrazolate, poly(tetrazolyl)borate, and aryl pentazole ligands as high energy density materials.
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Synthesis and characterization of metal complexes containing tetrazolate, poly(tetrazolyl)borate, and aryl pentazole ligands as high energy density materials.

机译：包含四唑酸酯，聚四唑基硼酸酯和芳基戊唑配体作为高能量密度材料的金属配合物的合成和表征。

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摘要

Heavier alkaline earth metal tetrazolates have been prepared as crystals containing aqua ligands and as anhydrous powders, and have been characterized by spectral and analytical methods. Potassium bis(tetrazolyl)borate complexes K(BH2(RCN4)2)(H2O)n (R = H, Me, NMe2, and NiPr2) and their 18-crown-6 adducts have been synthesized. In the solid state, complexes where R = H and Me have B-N bonds to the nitrogen atoms proximal to the tetrazolyl ring core carbon atom, whereas those with R = NMe2 and NiPr2 possess isomeric B-N bonds to the nitrogen atoms distal to the core carbon. With small R groups, the bis(tetrazolyl)borate ligands adopt bridging mu 2 coordination modes to the [18-crown-6]+ fragments, while with larger R groups, they adopt chelating kappa3-N,N',H coordination modes in the 18-crown-6 adducts. Bis(5-methyltetrazolyl)borate complexes of lithium and heavier alkaline earth metals have been prepared. The new group 2 metal complexes have been structurally characterized. Crystals of sodium cyano(tetrazolyl)borate complexes with or without methanol ligands have been prepared. The methanol ligands are lost rapidly from crystals of Na(H2B(CN)(HCN4))(CH3OH) and Na(H2B(CN)(MeCN 4))(CH3OH)˙(CH3OH) at 23°C once they are isolated from the solutions.;All of the new complexes mentioned above are air stable and thermally stable between 210°C and 325°C. They are insensitive toward impact, friction, and electrostatic discharge. The new complexes have potential use as propellants or secondary energetic materials; the barium tetrazolates may behave as primary energetic materials. The group 2 metal complexes are good candidates for colorants in pyrotechnic compositions. The potassium and sodium complexes can serve as starting materials to make other high nitrogen content bis(tetrazolyl)borate and cyano(tetrazolyl)borate complexes, respectively.;A series of rhenium isocyanate complexes (eta5-C 5H5)Re(CO)(NCO)(N2Ar) has been obtained by treatment of the specific rhenium aryldiazenido complexes [(eta5-C 5H5)Re(CO)2(N2Ar)][BF4] (Ar = 4-methoxyphenyl, 2,4-dimethoxyphenyl, 3,4,5-trimethoxyphenyl, 2-trifluoromethylphenyl, and phenyl) with sodium azide. Treatment of CpRe(CO)2(THF) with Et2NC6H5N5 made in situ affords the isocyanate complex (eta5-C5H 5)Re(CO)(NCO)(N2C6H5NEt2) and the methoxycarbonyl complex (eta5-C5H 5)Re(CO)(COOCH3)(N2C6H5NEt 2). The attempted preparation of rhenium aryl pentazole complexes does not proceed to form the desired products.
机译：较重的碱土金属四唑酸盐已制备为含水配体的晶体和无水粉末，并已通过光谱和分析方法进行了表征。已经合成了双（四唑基）硼酸钾配合物K（BH2（RCN4）2）（H2O）n（R = H，Me，NMe2和NiPr2）及其18冠-6加合物。在固态下，R = H和Me的配合物在靠近四唑基环核心碳原子的氮原子上具有B-N键，而R = NMe2和NiPr2的配合物在核心碳远端的氮原子上具有异构B-N键。对于较小的R基团，双（四唑基）硼酸酯配体对[18-crown-6] +片段采用桥接mu 2配位模式，而对于较大的R基团，它们采用螯合的kappa3-N，N'，H配位模式。 18冠6加合物。已经制备了锂和较重的碱土金属的双（5-甲基四唑基）硼酸盐络合物。新的第2组金属络合物已进行了结构表征。制备具有或不具有甲醇配体的氰基（四唑基）硼酸钠配合物的晶体。分离出来的Na（H2B（CN）（HCN4））（CH3OH）和Na（H2B（CN）（MeCN 4））（CH3OH）·（CH3OH）晶体迅速失去甲醇配体上述所有新的配合物在210°C至325°C的温度下均具有空气稳定性和热稳定性。它们对冲击，摩擦和静电放电不敏感。新的配合物具有潜在的推进剂或次级含能材料的用途。四唑酸钡可作为主要的高能材料。第2族金属络合物是烟火组合物中着色剂的良好候选者。钾和钠的配合物可以分别用作制备其他高氮含量的双（四唑基）硼酸酯和氰基（四唑基）硼酸酯配合物的原料。一系列iso异氰酸酯配合物（eta5-C 5H5）Re（CO）（NCO ）（N2Ar）是通过处理特定的芳基二氮杂ido络合物[（eta5-C 5H5）Re（CO）2（N2Ar）] [BF4]（Ar = 4-甲氧基苯基，2,4-二甲氧基苯基，3,4 1,5-三甲氧基苯基，2-三氟甲基苯基和苯基）与叠氮化钠。用原位制备的Et2NC6H5N5处理CpRe（CO）2（THF）得到异氰酸酯络合物（eta5-C5H 5）Re（CO）（NCO）（N2C6H5NEt2）和甲氧羰基络合物（eta5-C5H 5）Re（CO）（ COOCH3）（N2C6H5NEt 2）。 preparation芳基戊唑配合物的尝试制备并未形成所需的产物。

著录项

  • 作者

    Lu, Dongmei.;

  • 作者单位

    Wayne State University.;

  • 授予单位 Wayne State University.;
  • 学科 Chemistry Inorganic.
  • 学位 Ph.D.
  • 年度 2010
  • 页码 177 p.
  • 总页数 177
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

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