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DOI: 10.1006/jssc.2001.9380

Synthesis And X-ray Powder Diffraction Study Of New Phosphates In The Cu3(PO4)2–Sr3(PO4)2 System: Sr1.9Cu4.1(PO4)4, Sr3Cu3(PO4)4, Sr2Cu(PO4)2, And Sr9.1Cu1.4(PO4)7

A. Belik, A. Malakho, B. Lazoryak, S. Khasanov
Published 2002 · Chemistry

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Abstract New phosphates, Sr 1.9 Cu 4.1 (PO 4 ) 4 , Sr 2 Cu(PO 4 ) 2 , and Sr 9.1 Cu 1.4 (PO 4 ) 7 , were found in the Cu 3 (PO 4 ) 2 –Sr 3 (PO 4 ) 2 system at 900°C under air. Sr 1.9 Cu 4.1 (PO 4 ) 4 crystallizes in an orthorhombic system with a =15.3695(7) A, b =10.3652(4) A, and c =7.9425(4) A. Crystal structures of Sr 9.1 Cu 1.4 (PO 4 ) 7 , Sr 2 Cu(PO 4 ) 2 , and the known phase, Sr 3 Cu 3 (PO 4 ) 4 , were refined by the Rietveld method from X-ray diffraction data: space group R 3 m , a =10.6119(1) A, c =19.7045(2) A, and Z =3 for Sr 9.1 Cu 1.4 (PO 4 ) 7 ; space group C 2/ m , a =11.5155(1) A, b =5.07543(6) A, c =6.57487(7) A, β =106.3563(6)°, and Z =2 for Sr 3 Cu(PO 4 ) 2 ; and space group P 2 1 / c , a =9.2010(1) A, b =4.94104(4) A, c =17.8998(3) A, β =122.8952(9)°, and Z =2 for Sr 3 Cu 3 (PO 4 ) 4 . A second-harmonic generation study confirmed that the structures of all four compounds have the center of symmetry. Sr 3 Cu 3 (PO 4 ) 4 is isotypic with Ca 3 Cu 3 (PO 4 ) 4 . Copper cations in Sr 3 Cu 3 (PO 4 ) 4 have square planar and trigonal bipyramidal coordination and strontium cations have octahedral and ninefold coordination. Sr 2 Cu(PO 4 ) 2 is isotypic with Ba 2 Cu(PO 4 ) 2 . Copper cations in Sr 2 Cu(PO 4 ) 2 have square planar coordination and strontium cations have ninefold coordination. Sr 9.1 Cu 1.4 (PO 4 ) 7 is structurally related to β -Ca 3 (PO 4 ) 2 and Sr 3 (PO 4 ) 2 . A portion of copper cations in Sr 9.1 Cu 1.4 (PO 4 ) 7 fully occupies the trigonal-distorted octahedral site M 5. The structure of Sr 9.1 Cu 1.4 (PO 4 ) 7 has some disordered elements: (1) strontium cations in the M 3 site statistically occupy four positions near the center of symmetry; (2) orientation disordering of the P1O 4 tetrahedra is observed; (3) the M 4 site is occupied by 0.05Sr 2+ +0.2Cu 2+ +0.75□; and (4) copper cations in the M 4 site are slightly displaced from the threefold axis with distances between positions about 0.94 A. Formation of solid solutions Sr 9.1− x Ca x Cu 1.4 (PO 4 ) 7 (0≤ x ≤9.1), Sr 2− x Ba x Cu(PO 4 ) 2 (0≤ x ≤2), and Sr 3− x Ba x Cu 3 (PO 4 ) 4 (0≤ x ≤1.5) was shown.
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