7] Further details of the crystal structure investlgations are available on request from the Director of the Cambridge Crystallographic Data Centre, 12 Union Road, GB-Cambridge CB2 1EZ (UK), on quoting the full journal citation. [8] Crbslal data for 4b: C,,H,,BrF,N,O,OsP,S, triclinic, Pi, a =11.434(3), h = 13.?18(4). c=13.859(3)& x=98.17(2), 8=100.31(2). y=104.13(2)". V = 2034.2(9) A 3 . Z = 2.pcJ,cd =1.685 g~m -~. p ( M o~J = 43.04cm-'. T = 296K. Of 12316 ddta collected (Siemens P3, 20,,, = 6 0 ) . 11865 were independent and 8878 ucre observed (SaF,). All non-hydrogen atoms were anisotropically refined and phenyl hydrogen atoms were treated as idealized contributions: those ol' the hydrazine molecule were ignored. The phenyl rings were constrained lo rigid planar hexagons. SHELXTL software was used for all calculations At convergence: R ( F ) = 0.0371, R(wF) = 0.0430. [9] CrystAdatafor5b: C,,H,,BrF,N,O,OsP,S. monoclinic, P21/c. a = 11.219(2).h = 14 165(3). r = 25.410(6) A. /I = 93.370(2)", V = 4031.2(15) A', 2 = 4, pcd,Ld = 1.697 gem-', p(MoKr) = 43.44 cm-'. T = 296 K. Of 5774 data collected (Siemens P4,20,,, = 45'). 5272 were independent, and 3701 were observed ( 4 0 E J . All non-hydrogen atoms were anisotropically refined. and hydrogen atonis were idealized except for the diazene hydrogen atoms which were located and refined. SHELXTL software was used for all calculations. R ( F ) = 0.0537, R(n F ) = 0.0624.
