Jm. Harrowfield et al., LEWIS-BASE ADDUCTS OF LEAD(II) COMPOUNDS .16. SYNTHETIC AND STRUCTURAL STUDIES OF SOME ADDUCTS OF 2-AMINOMETHYLPYRIDINE WITH LEAD(II) COMPOUNDS, Australian Journal of Chemistry, 49(10), 1996, pp. 1127-1133
Syntheses and room-temperature single-crystal X-ray structure determin
ations are recorded for 2:1 adducts of 2-aminomethylpyridine ('amp') w
ith lead(II) nitrate and thiocyanate. [(amp)(2)Pb(NO3)(2)](2) is tricl
inic, <P(1)over bar>, a 11.616(4), b 11.145(6), c 7.341(3) Angstrom, a
lpha 83.87(4), beta 89.17(3), gamma 64.12(3)degrees, Z = 1 dimer, R wa
s 0.043 for N-o 3529 independent 'observed' (I > 3 sigma(I)) reflectio
ns. [(amp)(2)Pb(SCN)(2)](2) is also triclinic, <P(1)over bar>, a 12.12
1(9), b 9.301(14), c 8.615(8) Angstrom, alpha 70.11(10), beta 84.00(7)
, gamma 79.38(10)degrees, Z = 1 dimer (R 0.033 for N-o 3467). Both com
plexes are centrosymmetric dimers, the coordination environment is mad
e up in each cas of a pair of N,N'-bidentate bases, one terminally bou
nd anion (O,O'-chelating nitrate or S-bonded thiocyanate) and bridging
anions. In the case of the thiocyanates, these bridge end-on, so that
the lead(II) environment is seven-coordinate PbN5S2; in the nitrate,
the anion chelates through two of its oxygen atoms, bridging via the t
hird, so that the lead(II) environment is nine-coordinate (PbN4O5. A '
problem structure', [(amp)(2)Pb(ClO4)(2)], monoclinic, C2/c (?), a 14.
528(3), b 8.203(3), c 15.495(6) Angstrom, beta 91.14(3)degrees, Z = 4
f.u., R 0.044 for N-o 1775, is also recorded, the crystal seemingly a
disordered aggregate of [(N,N'-amp)(2)Pb(OClO3)(2)] moieties.