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首页> 外文期刊>Zeitschrift fur Naturforschung, B. A Journal of Chemical Sciences >La3Cu4P4O2 and La5Cu4P4O4Cl2: synthesis, structure and P-31 solid state NMR spectroscopy
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La3Cu4P4O2 and La5Cu4P4O4Cl2: synthesis, structure and P-31 solid state NMR spectroscopy

机译：La3Cu4P4O2和La5Cu4P4O4Cl2：合成，结构和P-31固态NMR光谱

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摘要

The phosphide oxides La3Cu4P4O2 and La5Cu4P4O4Cl2 were synthesized from lanthanum, copper(I) oxide, red phosphorus, and lanthanum(III) chloride through a ceramic technique. Single crystals can be grown in a NaCl/KCl flux. Both structures were refined from single crystal X-ray diffractometer data: I4/mmm, a = 403.89(4), c = 2681.7(3) pm, wR2 = 0.0660, 269 F-2 values, 19 variables for La3Cu4P4O2 and a = 407.52(5), c = 4056.8(7) pm, wR2 = 0.0905, 426 F-2 values, 27 variables for La5Cu4P4O4Cl2. Refinement of the occupancy parameters revealed full occupancy for the oxygen sites in both compounds. The structures are composed of cationic (La2O2)(2+) layers and covalently bonded (Cu4P4)(5-) polyanionic layers with metallic characteristics, and an additional La3+ between two adjacent (Cu4P4)(5-) layers. The structure of La5Cu4P4O4Cl2 comprises two additional LaOCl slabs per unit cell. Temperature-dependent magnetic susceptibility studies revealed Pauli paramagnetism. The phosphide substructure of La3Cu4P4O2 was studied by P-31 solid state NMR spectroscopy. By using a suitable dipolar re-coupling approach the two distinct resonances belonging to the P-2(4-) and the P3- units could be identified.
机译：通过陶瓷技术由镧，氧化铜（I），红磷和氯化镧（III）合成了磷氧化物La3Cu4P4O2和La5Cu4P4O4Cl2。可以在NaCl / KCl助熔剂中生长单晶。两种结构均从单晶X射线衍射仪数据中精炼而成：I4 / mmm，a = 403.89（4），c = 2681.7（3）pm，wR2 = 0.0660、269 F-2值，La3Cu4P4O2的19个变量和a = 407.52 （5），c = 4056.8（7）pm，wR2 = 0.0905，426个F-2值，La5Cu4P4O4Cl2的27个变量。占用参数的细化显示了两种化合物中氧位的完全占用。该结构由具有金属特性的阳离子（La2O2）（2+）层和共价键合（Cu4P4）（5-）聚阴离子层以及两个相邻（Cu4P4）（5-）层之间的附加La3 +组成。 La5Cu4P4O4Cl2的结构每单位晶胞包含两个额外的LaOCl平板。温度相关的磁化率研究表明，宝利顺磁性。通过P-31固态NMR光谱研究了La3Cu4P4O2的磷化物亚结构。通过使用合适的偶极子再耦合方法，可以识别出属于P-2（4-）和P3-单元的两个不同的共振。

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