M , = 1512.24. orthorhombic. space group P2,2,2,, u = 14.9659(1), h =18.4204(1). c=24.9210(1).& U = 6870.2(1).&', Z = 4 , y,,,,,=1.472g~m-~, F(000) = 3117. !L = 10.11 cm-I. crystal dimensions 0.3 x 0 3x0.4mm. Mo,, radiation (0.71073 A). measurement at 150(2) K. Final R (on F) and wR2 (on F2) were 0 030 and 0 090. respectively, for all 11 760 unique data. Final G O F = 0.95. and the final difference fourier map showed no peak at greater than + 0.891 and less than -0.629 e k 3 . A Flack i parameter of -0.009(8) showed the refinement had been carried out with the correct polarity. 3: C,,H,,DyF,N,,O,,S,. M , = 1570 9X. orthorhombic. space group P 2 , 2 , 2 , , u = 15 7679(4). h = 20.3133(4). ( = 21.7304(4) A, U = 6960.2(3) A'. 2 = 4, pCorr = 1.499 gcm-3. F(000) = 3216. p = 12 55 cm-'. crystal dimensions 0.2 x 0.3 x 0.3 mm. Ma,,radiation (1).71073 A). measurement at 150(2)K Final R (on F ) and 1rR2 (on F 2 ) were 0.042 and 0.1174, respectively, for all 12017 unique data. Final GOF = 1.097. and the final difference fourier map showed no peak at greater than f0.993 and less than -1.088 e k ' . A Flack Y parameter of -0.02119) showed the refinement had been carried out with the correct polarity. Crystal data were collected on a Siemens SMART diffractometer equipped with a CCD (512 x 511 pixels) area detector for all three complexes. The structures were solved by using Patterson methods (SHELXS86) [lo] and refined on F2 using all unique data by full-matrix least-squares (SHELXL93)."" All non-hydrogen atoms have anisotropic displacement parameters with hydrogen atoms generated in ideal positions (riding model). Crystallographic data (excluding structure factors) for the structures reported in this paper have been deposited with the Cambridge Crystallographic Data Centre as supplementary publication no. CUX-179-152. Copies of the data can be obtained free of charge on application to The Director, CCDC. 12 Union Road, Cambridge CB2 1EZ. U K