Supporting Information : On the Existence of AgM 9 ( VO 4 ) 6 I ( M = Ba , Pb )

(M = Ba, Pb) Erik V. Johnstone1,* Daniel J. Bailey,1 M.C. Stennett,1 J. Heo2,3 and Neil C. Hyatt1 1 University of Sheffield, Materials Science and Engineering Department, Sheffield, S10 2TN, England. 2 Department of Materials Science and Engineering, Pohang University of Science and Technology (POSTECH), Pohang, Gyeongbuk 790-784, South Korea 3 Division of Advanced Nuclear Engineering, Pohang University of Science and Technology (POSTECH), Pohang, Gyeongbuk 790-784, South Korea

Stoichiometric amounts of PbO, V 2 O 5 , and AgI (9:3:1), respectively, were batched to yield a final reacted composition of AgPb 9 (VO 4 ) 6 I and were processed and reacted as reported in the main text.The batched powders were pulverized and mixed as a slurry with isopropanol with an agate mortar and pestle.After drying, the resulting powders were pressed at 2 tonnes into ~ 250 mg, 6mm disk pellets.Pellets were reacted in air in a box furnace or in sealed quartz tubes (10 mm O.D., 8 mm I.D., 180 length) in an alumina tube furnace at 700 °C for 5 hr.
The resulting products were analyzed by PXRD (Figure S1), which were comparable to those starting from Pb 3 (VO 4 ) 2 and AgI.The SEM/EDX analysis of the sectioned portion of the pellet reacted in a sealed quartz tube is presented in         Yamanaka, J. Alloy Compd., 384 (2004), pp. 300-302.
Figure S1.Measured PXRD patterns for "AgPb 9 (VO 4 ) 6 I" starting from either Pb 3 (VO 4 ) 2 or PbO and V 2 O 5 with AgI reacted at 700 °C for 5 hr in sealed quartz tubes or in air.The PXRD pattern of β-Pb 3 (VO 4 ) 2 is given for comparison.

Figure S2 .
Figure S2.Back-scattering electron (BSE) SEM image at x2000 magnification and EDX map of V (teal), Pb (blue), I (yellow), and Ag (pink) present in AgPb 9 (VO 4 ) 6 I produced from PbO, V 2 O 5 , and AgI, and reacted at 700 °C for 5 hr in a sealed quartz tube.

Figure S4 .
Figure S4.EDX map of Ag (pink) and I (yellow) showing the presence of AgI and Ag metal in "AgPb 9 (VO 4 ) 6 I" reacted at 700 °C for 5 hr in a sealed quartz tube.

Figure S5 .
Figure S5.A) BSE image (x2000; scale bar length = 30 µm) showing point of measurement on "AgPb 9 (VO 4 ) 6 I" reacted at 700 °C for 5 hr in a sealed quartz tube; B) Red-Green-Blue EDX mixed map of Pb (blue), V (red), and I (green) indicating the presence of an overlapping area (white) corresponding to Pb-V-I phase; C) Resulting EDX spectrum of measured point of interest indicating the presence of Pb, V, and I peaks.