Hoi o i i ( ' ~i i i ~p i ~i ~m ~s
20 (!Vm wpp/wneni S(,rics V d . 54). Springer. Berlin, 1979. [ I l l " H (160.5 Mtlr). 'H (500.1 MHr). and "P (122 M H d NMR data (CDCI,. 25 ('. rel,iti\c intensities i n parentheses): 6("8) = + 46.7(1). + 46.3(1). ('ii + 1 3 1 I, + l0.7(1). -3.1(1) (resonances too broad to observe proton coupling): W H I = + 5.12(2). + 3 16(1). + 3.09(1). + 7.0 to + 7.5 (phenyl):
[I31 Cr!\t.ilIographic data for C,,H,,FeIrO,P, (5). crystal dimensions 0.20 x 0 50 x 0.30 imm, (298(2) K): (i = 10.675(5). h = 10.736(3), L' = 19.221 (7) .&. I ~ x x . y n i x p = 78.?6(4). ;a = 71.69(3) . v = 2045.2(13).&'. z = 2. c r y s ~a ~ 'tun triclinic. space group Pi. pc.3,Ld = 1.576 gcni '. p = 3.762 tiim I. ,,1 = I) 7OO4 T,,,,,, = 0.3470. Structure solution and refinement were carried out w i t h SHELXTL 5.0 (Siemens analytical X-ray Division Madison. WI. 1994). Of 114% reflections collected (3.00 > 211 > 55.0 ) 9424 independent i-cllecci(iiis w r e used in the relinement. Full matrix least squares refinement w;i\ c;irried oiit hy ininimi7ing S > ir(F,fc)'. The final residual values were R ( F ) = 0.1)7.33 for reflections F >2lr(F). wR(F2) = 0.1525. .\ = 1.042. number = 491. Further details of the crystal structure investigation may he oht:iiiieJ from the Director of the Cambridge Crystallographic Data Centre. 1 2 Union Ro;id. GB-Cambridge. CB2 IEZ (UK). on quoting the full journal