M. Kita et al., CRYSTAL-STRUCTURES OF [CO(ACAC)2((CH3)2XCH2CH2NH2)]CLO4 (X=N, P, AS ACAC = 2,4-PENTANEDIONATE ION), Bulletin of the Chemical Society of Japan, 66(6), 1993, pp. 1687-1692
The structures of [Co(acac)2{(CH3)2XCH2CH2NH2}]ClO4 (acac=2,4-pentaned
ionate ion, X=N (complex 1), P (complex 2), and As (complex 3)) with a
series of group 15 donor atoms were determined by the single-crystal
X-ray diffraction method. Crystal data and final R values are: for 1,
orthorhombic, Pba2, a=13.192(2), b=25.504(5), c=11.840(2) angstrom, V=
3984(i) angstrom3, D(m)=1.47(2), D(x)=1.48 g cm-3 and Z=8, R=0.050 for
2684 reflections. For 2, monoclinic, P2(1/c), a=13.953(6), b=25.061(1
0), c=12.079(7) angstrom, beta=92.29(6)-degrees, V=4220(2) angstrom, D
(m)=1.45(3), D(x)=1.45 g cm-3, Z=8, R=0.084 for 5801 reflections. For
3, monoclinic, C2/c, a=28.125(9), b=13.303(1), c=12.647(4) angstrom, b
eta=115.41(4)-degrees, V=4274(2) angstrom3, D(m)=1.50(3), D(x)=1.54 g
cm-3, Z=8, R=0.051 for 3698 reflections. All the complex ions have a s
imilar structure, forming a distorted octahedron with 40, N, and X don
or atoms. The Co-X bond lengths are av. 2.026(8) angstrom for 1, av. 2
.192(3) angstrom for 2, and 2.302(1) angstrom for 3. The Co-O bond len
gths trans to X are av. 1.886(6) angstrom for 1, av. 1.950(5) angstrom
for 2, and 1.928(3) angstrom for 3, which are longer by 0.002(6), 0.0
65(6) and 0.037(4) angstrom, respectively, than the average lengths of
other three Co-O bonds (1: av. 1.884(6), 2: av. 1.885(6), 3: 1.891(4)
angstrom).