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Synthesis, structural and IR spectral studies of lanthanide (Nd, Sm) phenyl- and 2-pyridylthiolates supported by bulky 2,6-diisopropylphenyl substituted β-diketiminate ligand. / Mironova, Olga A.; Sukhikh, Taisiya S.; Konchenko, Sergey N. et al.
In: Polyhedron, Vol. 159, 01.02.2019, p. 337-344.Research output: Contribution to journal › Article › peer-review
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TY - JOUR
T1 - Synthesis, structural and IR spectral studies of lanthanide (Nd, Sm) phenyl- and 2-pyridylthiolates supported by bulky 2,6-diisopropylphenyl substituted β-diketiminate ligand
AU - Mironova, Olga A.
AU - Sukhikh, Taisiya S.
AU - Konchenko, Sergey N.
AU - Pushkarevsky, Nikolay A.
N1 - Publisher Copyright: © 2018 Elsevier Ltd
PY - 2019/2/1
Y1 - 2019/2/1
N2 - Lanthanide triiodides LnI3 (Ln = Nd, Sm) were synthesized by an improved method and used for the synthesis of complexes with β-diketiminate (nacnac) ligand [Ln(LDipp)I2(THF)2] (LDipp = HC(C(NDipp)Me)2 −, Dipp = 2,6-Diisopropylphenyl; Ln = Nd, 1a; Sm, 1b). These complexes were crystallized as solvates with THF or toluene, depending on the solvent, while the Nd complex 1a was also shown to reversibly lose one of coordinated THF molecules upon recrystallization from toluene at elevated temperatures. The diiodide complexes 1 were used as convenient precursors to thiolate complexes of the types [Ln(LDipp)(SPh)2(THF)] (Nd, 2a; Sm, 2b) and [Ln(LDipp)(S-2-Py)2] (Nd, 3a; Sm, 3b), obtained by salt metathesis reactions with KSPh and KS(2-Py), respectively. The phenylthiolate complexes 2 have formal coordination number (CN) of 6, where the 6th position is occupied by a Ph ring which is placed close to the Ln centre and plays a role of a ligand even in the presence of THF. The pyridilthiolates 3 have CN of 6 and contain no coordinated THF molecules. All compounds were characterized by single crystal X-ray diffraction, elemental analysis, IR spectroscopy. IR bands characteristic for all types of ligands in the complexes are discussed.
AB - Lanthanide triiodides LnI3 (Ln = Nd, Sm) were synthesized by an improved method and used for the synthesis of complexes with β-diketiminate (nacnac) ligand [Ln(LDipp)I2(THF)2] (LDipp = HC(C(NDipp)Me)2 −, Dipp = 2,6-Diisopropylphenyl; Ln = Nd, 1a; Sm, 1b). These complexes were crystallized as solvates with THF or toluene, depending on the solvent, while the Nd complex 1a was also shown to reversibly lose one of coordinated THF molecules upon recrystallization from toluene at elevated temperatures. The diiodide complexes 1 were used as convenient precursors to thiolate complexes of the types [Ln(LDipp)(SPh)2(THF)] (Nd, 2a; Sm, 2b) and [Ln(LDipp)(S-2-Py)2] (Nd, 3a; Sm, 3b), obtained by salt metathesis reactions with KSPh and KS(2-Py), respectively. The phenylthiolate complexes 2 have formal coordination number (CN) of 6, where the 6th position is occupied by a Ph ring which is placed close to the Ln centre and plays a role of a ligand even in the presence of THF. The pyridilthiolates 3 have CN of 6 and contain no coordinated THF molecules. All compounds were characterized by single crystal X-ray diffraction, elemental analysis, IR spectroscopy. IR bands characteristic for all types of ligands in the complexes are discussed.
KW - IR spectroscopy
KW - Lanthanides
KW - Mixed-ligand complexes
KW - Thiolates
KW - β-Diketiminates
KW - LN
KW - ALKYL
KW - MAIN-GROUP
KW - POLYMERIZATION
KW - RARE-EARTH COMPLEXES
KW - CLUSTERS
KW - beta-Diketiminates
KW - YTTERBIUM
KW - PRECURSORS
KW - CHALCOGENOLATE COMPLEXES
KW - ACTINIDE METALS
UR - http://www.scopus.com/inward/record.url?scp=85059071851&partnerID=8YFLogxK
U2 - 10.1016/j.poly.2018.12.011
DO - 10.1016/j.poly.2018.12.011
M3 - Article
AN - SCOPUS:85059071851
VL - 159
SP - 337
EP - 344
JO - Polyhedron
JF - Polyhedron
SN - 0277-5387
ER -
ID: 18067621