High‐Pressure Synthesis, Crystal Structure, and Characterization of Zn2PN3 – A New catena‐Polynitridophosphate
High‐Pressure Synthesis, Crystal Structure, and Characterization of Zn2PN3 – A New catena‐Polynitridophosphate
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DOI：
10.1002/zaac.201000403
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发表时间：
2011-03
期刊：
影响因子：
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通讯作者：
S. Sedlmaier;M. Eberspächer;W. Schnick
中科院分区：
文献类型：
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作者：
S. Sedlmaier;M. Eberspächer;W. Schnick
采用多砧组件，以 Zn3N2 和 P3N5 为原料，在高压高温条件（1200 °C，8 GPa）下合成相纯链状聚硝基磷酸锌 Zn2PN3。其以无色微晶粉末形式获得。 Zn2PN3（Cmc21，编号 36，a = 937.847(6)，b = 547.696(4)，c = 492.396(3) pm，Z = 4，Rp = 0.0110，wRp = 0.0141）的晶体结构已通过 Rietveld 方法使用原子参数从粉末 X 射线衍射数据中精炼出来同型 Mg2PN3 作为起始值。链状聚硝基磷酸盐链阴离子通过 N 配位 Zn2+ 离子相互连接，平行运行 [001]，链周期 P = 2，拉伸因子 fs = 0.88。记录了 Zn2PN3 的 FT-IR 和拉曼光谱并指定了相关谱带。固态 31P MAS NMR 谱在 δ = 42.8 处产生单共振。此外还给出了 Zn2PN3 热行为的说明。
Phase-pure zinc catena-polynitridophosphate Zn2PN3 was synthesized by means of high-pressure high-temperature conditions (1200 °C, 8 GPa) starting from Zn3N2 and P3N5 utilizing a multianvil assembly. It was obtained as a colorless, microcrystalline powder. The crystal structure of Zn2PN3 (Cmc21, no. 36, a = 937.847(6), b = 547.696(4), c = 492.396(3) pm, Z = 4, Rp = 0.0110, wRp = 0.0141) has been refined from powder X-ray diffraction data by the Rietveld method using the atomic parameters of isotypic Mg2PN3 as starting values. Interconnected by N-coordinated Zn2+ ions, the catena-polynitridophosphate chain anions run parallel [001] with a chain periodicity P = 2 and a stretching factor fs = 0.88. FT-IR and Raman spectra of Zn2PN3 were recorded and relevant bands were assigned. The solid-state 31P MAS NMR spectrum yielded a single resonance at δ = 42.8. In addition an account of the thermal behavior of Zn2PN3 is given.