Single crystals of Rh(Si2O)(PO4)(3) and In-4(Si2O).(PO4)(6) were prepared b
y chemical transport reactions in silica tubes and their structures were de
termined. Crystal data of Rh(Si2O)(PO4)(3): triagonal, space group P (3) ov
er bar c1, a = 8.088(3) Angstrom, c = 8.740(2) Angstrom, Z = 2, R(F-2) = 0.
0379, R-W(F-2) = 0.0518 for 601 unique reflections. In-4(Si2O)(PO4)(6): hex
agonal, space group P6(3)/m, a = 8.5149(10) Angstrom, c = 7.7481(12) Angstr
om, Z = 1, R(F-2) = 0.0436, R-W(F-2) = 0.0522 for 509 unique reflections. B
oth of the compounds have hexagonal close packed array of phosphate groups
with metal atoms and SiOSi units in the octahedral interstices, where the S
iOSi units show occupational disorder. The structure of the indium compound
is considered to be a disordered structure of the reported Mo4Si2PbO13 str
ucture, and contains confacial bioctahedral units.