LEWIS-BASE ADDUCTS OF LEAD(II) COMPOUNDS .7. SYNTHETIC AND STRUCTURALSTUDIES OF SOME 1 1 ADDUCTS OF LINEAR POLYAMINES WITH LEAD(II) NITRATE/

Syntheses and room-temperature single-crystal X-ray structure determin ations are recorded for 1:1 adducts of lead(II) nitrate with the linea r multidentate polyamines ethane-1,2-diamine ('en' (= '2')), H2N(CH2)( 2)NH(CH2)(2)NH2 ('dien' = '22') and H2N(CH2)(x)NH(CH2)(y)NH(CH2)(z)NH2 (zyztet = '222tet' (= 'trien'), '232tet', '323tet'). Crystal/refineme nt data are as follows: [(en)Pb(NO3)(2)]((infinity/infinity)) is monoc linic, P2(1)/c, a 5.388(2), b 12.440(5), c 13.123(3) Angstrom, beta 10 2.33(3)degrees, Z = 4 f.u.; R 0.037 for N-o 2698 'observed' (I > 3 sig ma(I)) reflections. [(dien)Pb(NO3)(2)]((infinity/infinity)) is orthorh ombic, Ccma, a 9.800(2), b 10.840(2), c 20.521(5), Z = 8; R 0.045, N-o 991. [(trien)Pb(NO3)(2)]((infinity/infinity)) is orthorhombic, P2(1)2 (1)2(1), a 14.815(3), b 10.975(3), c 8.410(2) Angstrom, Z = 4; R 0.050 , N-o 1360; [(232tet)Pb(NO3)(2)]((infinity/infinity)) is isomorphous, a 14.524(6), b 11.221(1), c 8.860(2) Angstrom, R 0.036, N-o 2371. [(32 3tet)Pb(NO3)(2)]((infinity/infinity)) is monoclinic, P2(1)/c, a 8.195( 4), b 14.407(7), c 13.312(4) Angstrom, beta 91.05(3)degrees, Z = 4; R 0.049: N-o 1644. In general, the degree of complexity of the adduct di minishes as the ligand size increases: whereas the en adduct is a comp act one-dimensional two-stranded polymer with nearly all nitrate oxyge ns involved in tight bridging interactions, the extent of bridging dim inishes in the adducts of the larger amines, until, for the 323tet spe cies, a monomer is obtained involving a lead coordination sphere conta ining the ligand and a pair of bidentate nitrate groups. The 1:2 adduc t with en is also recorded, and is a dimer with quasi-i internal symme try. [(en)(2)Pb(NO3)(2)](2) is monoclinic, P2(1), a 6.661(2), b 14.226 (8), c 13.618(4) Angstrom, beta 96.51(2)degrees; R 0.072, N-o 1713.