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含磷（III）和砷（III）中心的杂双环双（叔丁基氨基）环二磷（III）氮烷化合物的合成与结构

Syntheses and structures of heterobicyclic bis(tert-butylamido)cyclodiphosph(III)azane compounds having phosphorus(III) and arsenic(III) centers.

作者信息

Schranz I, Grocholl L P, Stahl L, Staples R J, Johnson A

机构信息

Department of Chemistry, University of North Dakota, Grand Forks, North Dakota 58202-9024, USA.

出版信息

Inorg Chem. 2000 Jul 10;39(14):3037-41. doi: 10.1021/ic991405r.

DOI:10.1021/ic991405r
PMID:11196898
Abstract

Syntheses and single-crystal X-ray diffraction studies of heterobicyclic cyclodiphosphazanes having central phosphorus(III) and arsenic(III) atoms are described. Interaction of PCl3 or AsCl3 with cis-[(tBuNP)2(tBuNLixTHF)2] produced the isomorphous ([(tBuNP)2(tBuN)2]ECl); E = P(1), As(4), respectively. These Cs-symmetric molecules crystallize with two molecules in the monoclinic space group P2(1)/m. Unit cell dimensions of 1 are (293 K) a = 9.777(1) A, b = 11.745(1) A, c = 9.986(2) A, and beta = 97.44(1) degrees; those of 4 are (213 K) a = 9.688(3) A, b = 11.873(3) A, c = 9.975(3) A, and beta = 97.80(3) degrees. When ([(tBuNP)2(tBuN)2]PCl) was treated with NaN3 or LiN(SiMe3)2, ([(tBuNP)2(tBuN)2]PN3)(2) and ([(tBuNP)2(tBuN)2]PN(SiMe3)2)(3), respectively, were obtained. Compound 2 crystallizes in the monoclinic space group P2(1)/m and has until-cell dimensions (213 K) of a = 9496(7) A, b = 12455(7) A, c = 10043(6) A, and beta = 9723(4) degrees, Z = 2.

摘要

描述了含有中心磷（III）和砷（III）原子的杂双环环二磷氮烷的合成及单晶X射线衍射研究。PCl₃ 或 AsCl₃ 与顺式 - [（tBuNP）₂（tBuNLixTHF）₂] 的相互作用分别生成了同构体（[（tBuNP）₂（tBuN）₂]ECl）；E分别为P（1）、As（4）。这些具有Cs对称性的分子在单斜空间群P2（1）/m中以两个分子结晶。1的晶胞参数（293K）为a = 9.777（1）Å，b = 11.745（1）Å，c = 9.986（2）Å，β = 97.44（1）°；4的晶胞参数（213K）为a = 9.688（3）Å，b = 11.873（3）Å，c = 9.975（3）Å，β = 97.80（3）°。当（[（tBuNP）₂（tBuN）₂]PCl）用NaN₃ 或 LiN（SiMe₃）₂ 处理时，分别得到了（[（tBuNP）₂（tBuN）₂]PN₃）（2）和（[（tBuNP）₂（tBuN）₂]PN（SiMe₃）₂）（3）。化合物2在单斜空间群P2（1）/m中结晶，其晶胞参数（213K）为a = 9496（7）Å，b = 12455（7）Å，c = 10043（6）Å，β = 9723（4）°，Z = 2。

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