TY - JOUR
T1 - The synthesis and crystal structure of [NiL(NCS)2] (L = 3-hydroxyethyl-1,3,5,8,12-pentaazacyclotetradecane)
AU - Hay, Robert W.
AU - Cromie, Thomas J.
AU - Lightfoot, Philip
PY - 1997/1/1
Y1 - 1997/1/1
N2 - The reaction of H2CO and H2NCH2CH2OH with the nickel(II) complex of 1,9-diamino-3,7-diazanonane (2,3,2-tet) in the presence of Et3N gives the nickel(II) complex of the macrocycle 3-hydroxyethyl-1,3,5,8,12-pentaazacyclotetradecane (L), which can be readily isolated as the perchlorate salt. The reaction of KCNS with the perchlorate salt in aqueous solution gives [NiL(NCS)2] and the crystal structure of this complex has been determined. The complex is octahedral and trans with the two N-bonded thiocyanates in the axial sites with Ni - NCS bond lengths of 2.106 and 2.145 Å. The equatorial sites are occupied by N2, N5, N8 and N12 with Ni - N bond distances of 2.053 to 2.076 Å, which are typical for octahedral nickel(II) complexes. The ligand has a trans III configuration of the sec-NH centres, leading to chair six-membered rings and gauche five-membered rings. The hydroxyethyl group on N3 is axial. There is no evidence for hydrogen-bonding interactions involving the hydroxyethyl group in the crystal lattice.
AB - The reaction of H2CO and H2NCH2CH2OH with the nickel(II) complex of 1,9-diamino-3,7-diazanonane (2,3,2-tet) in the presence of Et3N gives the nickel(II) complex of the macrocycle 3-hydroxyethyl-1,3,5,8,12-pentaazacyclotetradecane (L), which can be readily isolated as the perchlorate salt. The reaction of KCNS with the perchlorate salt in aqueous solution gives [NiL(NCS)2] and the crystal structure of this complex has been determined. The complex is octahedral and trans with the two N-bonded thiocyanates in the axial sites with Ni - NCS bond lengths of 2.106 and 2.145 Å. The equatorial sites are occupied by N2, N5, N8 and N12 with Ni - N bond distances of 2.053 to 2.076 Å, which are typical for octahedral nickel(II) complexes. The ligand has a trans III configuration of the sec-NH centres, leading to chair six-membered rings and gauche five-membered rings. The hydroxyethyl group on N3 is axial. There is no evidence for hydrogen-bonding interactions involving the hydroxyethyl group in the crystal lattice.
UR - http://www.scopus.com/inward/record.url?scp=0006018777&partnerID=8YFLogxK
U2 - 10.1023/A:1018575632645
DO - 10.1023/A:1018575632645
M3 - Article
AN - SCOPUS:0006018777
SN - 0340-4285
VL - 22
SP - 510
EP - 512
JO - Transition Metal Chemistry
JF - Transition Metal Chemistry
IS - 5
ER -