1H, 13C, 15N NMR and 13C, 15N CPMAS studies of cobalt(III)-chloride-pyridine complexes, spontaneous py→Cl substitution in trans-[Co(py)4Cl2]Cl, and a new synthesis of mer-[Co(py)3Cl3]

被引：15
|
作者：
Pazderski, Leszek [1 ]
Surdykowski, Andrzej [1 ]
Pazderska-Szablowicz, Malgorzata [1 ]
Sitkowski, Jerzy [2 ,3 ]
Kozerski, Lech [2 ,3 ]
Kamienski, Bohdan [3 ]
Szlyk, Edward [1 ]
机构：
[1] Nicholas Copernicus Univ, Fac Chem, PL-87100 Torun, Poland
[2] Natl Drug Inst, PL-00725 Warsaw, Poland
[3] Polish Acad Sci, Inst Organ Chem, PL-01224 Warsaw, Poland
来源：
CENTRAL EUROPEAN JOURNAL OF CHEMISTRY | 2008年 / 6卷 / 01期
关键词：
Co(III) complexes; pyridine complexes; N-15; NMR; CPMAS; NMR coordination shifts;
D O I：
10.2478/s11532-007-0063-3
中图分类号：
O6 [化学];
学科分类号：
0703 ;
摘要：
trans-[Co(py)(4)Cl-2]Cl center dot 6H(2)O, mer-[Co(py)(3)Cl-3] and mer-[Co(py)(3)(CO3)Cl] were studied by UV-Vis, far-IR and H-1, C-13, N-15 NMR. The formation of Co-N bonds lead to variable in sign and magnitude changes of H-1 NMR chemical shifts, heavily dependent on proton position, coordination sphere geometry and character of auxiliary ligands. C-13 nuclei were deshielded upon Co(III) coordination, while N-15 NMR studies exhibited ca. 85-110 ppm shielding effects (ca. 15-25 ppm more expressed for nitrogens trans to N than trans to Cl or O). C-13 and N-15 CPMAS spectra revealed a slight inequivalency of formally identical Co-py bonds in trans-[Co(py)(4)Cl-2]Cl center dot 6H(2)O and mer-[Co(py)(3)Cl-3], suggesting for the latter complex an existence of distortion isomers. In chloroform, a spontaneous trans-[Co(py)(4)Cl-2]Cl -> mer-[Co(py)(3)Cl-3] + py reaction was monitored by H-1 NMR and UV-Vis. This process of py -> Cl substitution allowed the design of a more convenient and efficient method of mer-[Co(py)(3)Cl-3] preparation.
引用
收藏
页码：55 / 64
页数：10
相关论文
共 50 条
  • [41] 1H, 13C and 15N NMR study of 2-alkylnitrosoamino-4-nitropyridines and N-oxides:: An example on restricted inversion of sp3 nitrogen
    Laihia, K.
    Puszko, A.
    Kolehmainen, E.
    Lorenc, J.
    JOURNAL OF MOLECULAR STRUCTURE, 2007, 831 (1-3) : 203 - 208
  • [42] Ring-chain tautomerism in 2-substituted 1,2,3,4-tetrahydroquinazolines A 1H, 13C and 15N NMR study
    Sinkkonen, J
    Zelenin, KN
    Potapov, AKA
    Lagoda, IV
    Alekseyev, VV
    Pihlaja, K
    TETRAHEDRON, 2003, 59 (11) : 1939 - 1950
  • [43] 1H, 13C and 15N NMR spectral analysis of substituted 1,2,3,4-tetrahydro-pyrido [1,2-a]pyrimidines
    Girreser, Ulrich
    Bluhm, Ullvi
    Clement, Bernd
    Heber, Dieter
    MAGNETIC RESONANCE IN CHEMISTRY, 2013, 51 (11) : 714 - 721
  • [44] Letter to the Editor:: Assignment of the 1H, 13C and 15N resonances of the catalytic domain of the rat 2′,3′-cyclic nucleotide 3′-phosphodiesterase
    Kozlov, G
    Lee, J
    Gravel, M
    Ekiel, I
    Braun, PE
    Gehring, K
    JOURNAL OF BIOMOLECULAR NMR, 2002, 22 (01) : 99 - 100
  • [45] Letter to the Editor: Assignment of the 1H, 13C and 15N resonances of the catalytic domain of the rat 2′,3′-cyclic nucleotide 3′-phosphodiesterase
    Guennadi Kozlov
    John Lee
    Michel Gravel
    Irena Ekiel
    Peter E. Braun
    Kalle Gehring
    Journal of Biomolecular NMR, 2002, 22 : 99 - 100
  • [46] Bis(diethyldithiocarbamato)pyridinezinc(II) and -copper(II) clathrates M(Edtc)2Py • nL (L = CH2Cl2 and CHCl3; n=1 and 0.5):: Molecular and crystal structures and EPR and high-resolution solid-state (13C, 15N) NMR spectra
    Ivanov, AV
    Kritikos, M
    Antsutkin, ON
    Forshling, V
    Lund, A
    Lutsenko, IA
    RUSSIAN JOURNAL OF COORDINATION CHEMISTRY, 1999, 25 (08) : 543 - 555
  • [47] 1H, 13C and 15N resonance assignments of the ERK2 binding domain of the MAPK phosphatase MKP-3
    Farooq, A
    Zeng, L
    Zhou, MM
    JOURNAL OF BIOMOLECULAR NMR, 2001, 19 (02) : 195 - 196
  • [48] The crystal and molecular structure of potassium aquapentachloroiridate(III) and the 1H, 13C, 15N NMR coordination shifts in iridium(III) chloride complexes with 2,2′-bipyridine or 1,10-phenanthroline
    Pazderski, Leszek
    Tousek, Jaromir
    Wojtczak, Andrzej
    Sitkowski, Jerzy
    Kozerski, Lech
    Szlyk, Edward
    POLYHEDRON, 2008, 27 (14) : 3067 - 3078
  • [49] SYNTHESIS AND STRUCTURE-ANALYSIS OF STABLE TUNGSTEN ALKYLIDYNE COMPLEX, CL(CO)2(PY)2WC-C6H4-N(CH3)2
    LEE, KS
    SHU, DZ
    ZUBKOWSKI, J
    ABSTRACTS OF PAPERS OF THE AMERICAN CHEMICAL SOCIETY, 1993, 205 : 145 - INOR
  • [50] Rotation isomers of bis(diethyldithiocarbamato)zinc(II) adduct with pyridine, Zn(EDtc)2•Py:: ESR, 13C and 15N CP/MAS NMR and single-crystal X-ray diffraction studies
    Ivanov, AV
    Mitrofanova, VI
    Kritikos, M
    Antzutkin, ON
    POLYHEDRON, 1999, 18 (15) : 2069 - 2078
12345