Hydrothermal synthesis, structures, and properties: Indium hydrogen phosphates (MIn)-In-I(HPO4)(2) (M-I = K, Rb, and NH4)статья
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Дата последнего поиска статьи во внешних источниках: 18 июля 2013 г.
Аннотация:Mixed hydrogen phosphates KIn(HPO4)(2) (I), beta(2)-RbIn(HPO4)(2) (II), and (NH4)In(HPO4)(2) (III) were prepared in the In2O3-MH2PO4-H3PO4-HF, In2O3-M2CO3-H3PO4-HF (where M = K or Rb), and In2O3(NH4)Cl-H3PO4 systems under hydrothermal conditions (200degreesC, 20 atm, 96 h). The phosphates were characterized by IR and Raman spectroscopy, thermal analysis, and electron probe microanalysis. The structure of compound II was established by single-crystal X-ray diffraction analysis. The crystal structures of compounds I and III were determined by the Rietveld method. All compounds crystallized in the monoclinic system (space group P2(1)/c, Z= 4); a = 9.6232(1) Angstrom, b = 8.2573(1) Angstrom, c = 9.4571(1) Angstrom, beta = 115.72(1)degrees, R-p = 0.0465, R-wp = 0.0619 for I; a = 9.705(2) Angstrom, b = 8.367(2) Angstrom, c = 9.528(2) Angstrom, beta = 116.60(3)degrees, R-1 = 0.0503, wR(2) = 0.1464 for II; a = 9.6651(1) Angstrom, b = 8.2763(1) Angstrom, c = 9.5964(1) Angstrom, beta = 116.146(1)degrees, R-p = 0.0380, R-wp = 0.0553 for III. The structures of indium hydrogen phosphates can be described as a mixed framework {In[HPO4](2)}(3infinity)(-) of octahedra and tetrahedra. Large cavities in the framework are occupied by monovalent cations. Second-harmonic-generation measurements demonstrated that the crystal structures of compounds I-III have a center of symmetry.