Bruker SMART-CCD diffractometer (graphite-monochromated Mo Ka -radiation: l 0.71073 ). The structures were solved by direct methods (SHELXTL Version 5.10) and refined by full-matrix leastsquares on F 2 . All non-hydrogen atoms were refined anisotropically. Crystal data for C 20 H 18 N 4 CoP 2 V 2 O 12 (1): Crystal dimensions 0.170 Â 0.070 Â 0.070 mm, monoclinic, space group C2/c (no. 15), a 25.1399( 15), b 8.1532(5), c 15.6510( 10) , b 127.0030(10)8, V 2561.9(3) 3 . Z 4, 1 calcd 1.890 g cm À3 , m(Mo Ka ) 1.552 mm À1 . Of the 6086 reflections measured (2.60 q 23.248), 1832 symmetryindependent reflections were used to solve the structure. Based on all these data and 223 refined parameters, R1 0.0349 (all data), wR2 0.0824, and goodness-of-fit on F 2 is 1.039. Crystal data for C 20 H 18 N 4 NiP 2 V 2 O 12 (2): Crystal dimensions 0.160 Â 0.080 Â 0.050 mm, monoclinic, space group C2/c (no. 15), a 25.025(3), b 8.1660( 12), c 15.610(2) , b 127.477(3)8, V 2531.5(6) 3 . Z 4, 1 calcd 1.913 g cm À3 , m(Mo Ka ) 1.659 mm À1 . Of the 6008 reflections measured (2.05 q 23.278), 1822 symmetry-independent reflections were used to solve the structure. Based on all these data and 223 refined parameters, R1 0.0385 (all data), wR2 0.0876, and goodness-of-fit on F 2 is 1.089. Crystallographic data (excluding structure factors) for the structures reported in this paper have been deposited with the Cambridge Crystallographic Data Centre as supplementary publication nos. CCDC-137922 (1) and CCDC-137923 (2). Copies of the data can be obtained free of charge on application to CCDC,