Structure-NMR correlations in halo(ligand)bis(dioximato)cobalt(III) complexes

López, Concepción; Álvarez, Santiago; Soláns, Xavier; Font‐Altaba, M.

doi:10.1021/ic00237a009

Cited by 60 publications

(23 citation statements)

References 5 publications

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“…Z The equatorial Co±N or Cu±N distances in the octahedral or square-planar parts of the trinuclear complexes (8,9) are in accord with the known vicinal dioxime complexes (r Co±N = 1.86±1.94 A Ê , r Cu±N = 1.91± 1.96 A Ê ) [29]. The values concerning interatomic angles for N±Co±N in the trinuclear complex (8) (N±Co±N = 85.47±94.34°) are also comparable to the average N±Co±N angles found in other dioxime complexes (N±Co±N = 83.63±96.43°) [24]. The Pd±S and Pd±N bond distances were longer than values given in the literature [30].…”

Section: Resultssupporting

confidence: 80%

“…The 13 C-NMR spectrum of 7 revealed that, upon replacement of the hydrogen bridges by BF 2 groups, shifts of C=N and C±N carbon atoms up to 0.35±0.52 ppm occured. In the IR spectrum of this complex (7), a downward shift to for the C=N frequencies indicated coordination through the N atoms [24]. In contrast to this downward shift, this BF 2 + -bridged complex exhibited an upward shift to about a 1653 cm ±1 .…”

Section: Resultsmentioning

confidence: 89%

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Synthesis and Characterization of a Novel Macrocyclicvic-Dioxime and Some of its Mono and Trinuclear Complexes

Kanteki̇n

Ocak

Gök

2001

Z. anorg. allg. Chem.

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The (E, E)-dioxime containing a dithia-dioxa-diaza macrocyclic moiety 5,6 : 11,12 : 17,18-tribenzo-2,3-bis(hydroxyimino)-1,4-diaza-7,16-dithia-10,12-dioxacyclooctadecane (H 2 L) has been synthesized in high yield by a 1 + 1 addition of cyanogendi-N-oxide with 2, 3 : 8,9 : 14,15-tribenzo-1,16-diamino-4,13-dithia-7,10-dioxahexadecane (3) which was obtained from condensation reaction with 2-amino thiophenol and 1,2-bis(2-bromoethoxy)benzene, in dichloromethane at ±10°C. Two vic-Dioxime ligands coordinate with Ni(II), Cu(II) and Co(III) through its hydroxyimino nitrogen donor atoms by the loss of the oxime protons. Homo and heterotrinuclear Cu II 3 and Co III Pd II 2 complexes of this ligand have been prepared; their two ligand molecules are connected via hydroxyimino or BF 2 + -bridging groups and two of the metal ions are coordinated by a diaza-dithia mixed donor macrocyclic moiety. The macrocyclic ligand and its transition metal complexes have been characterized on the basis of 1 H-, 13 C-NMR, IR and MS spectroscopy and elemental analysis data. Synthese und Charakterisierung eines neuen vic-Dioxim-Makrocyclus und einiger seiner mono-und trinuklearen MetallkomplexeInhaltsu È bersicht. Das (E,E)-Dioxim mit dem Dithia-dioxodiaza-Makrocyclus 5,6 : 11,12 : 17 : 18-Tribenzo-2,3-bis(hydroxyimino)-1,4-diaza-7,16-dithia-10,12-dioxacyclooctadecan (H 2 L) wurde in hohen Ausbeuten synthetisiert durch 1 + 1 Addition von Dicyan-di-N-oxid mit 2,3 : 8,9 : 14,15-tribenzo-1,16-diamino-4,13-dithia-7,10-dioxahexadecan (3), das durch Kondensationsreaktion von 2-Aminothiophenol und 1,2-Bis(2-bromethoxy)benzol in Dichlormethan bei ±10°C erhalten wurde. Zwei vic-Dioximliganden koordinieren mit Ni II , Cu II bzw. Co III u È ber die Hydroxoimino-Stickstoffatome unter Verlust der Oximprotonen. Homo-und heteronukleare Cu II 3 -und Co III Pd II 2 -Komplexe dieses Liganden wurden dargestellt; ihre beiden Ligandenmoleku È le sind u È ber Hydroxoimino-oder BF 2 + -Bru È cken verbunden und zwei der Metallionen werden durch die N-und S-Donoratome der makrocyclischen Einheit koordiniert. Der makrocyclische Ligand und seine Ûbergangsmetallkomplexe wurden durch 1 H-, 13 C-NMR-, IR-, MS-Spektroskopie sowie durch Elementaranalysen charakterisiert.

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Section: Resultssupporting

confidence: 80%

Section: Resultsmentioning

confidence: 89%

Synthesis and Characterization of a Novel Macrocyclicvic-Dioxime and Some of its Mono and Trinuclear Complexes

Kanteki̇n

Ocak

Gök

2001

Z. anorg. allg. Chem.

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“…The six-coordinate mononuclear Co(III) complex [Co(HL) 2 pyCl] was synthesized as previously reported [23]. The fast atom bombardment mass spectrum of this complex exhibits a molecular ion peak at m/z ¼ 1253 [Mþ1] þ , which supports the proposed structure [24]. In the 1 H-NMR spectrum of the mononuclear Co(III) complex and the resonance of the intramolecular binding O-HÁ Á ÁO protons appear as a singlet at ¼ 16.80 ppm and this shift could easily be identified by deuterium exchange.…”

Section: Resultssupporting

confidence: 58%

The Synthesis and Characterization of a Novel ( E , E )-Dioxime and its Mono- and Heterotrinuclear Complexes Containing an 18-Membered Dioxadithiadiazamacrocycle

Kanteki̇n

Şahinbaş

Ocak

et al. 2003

Journal of Coordination Chemistry

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The novel (E,E )-dioxime, 5,6:17,18-dibenzo-11,12-(4 0 -nitrobenzo)-2,3-bis(hydroxyimino)-7,16-dithia-10,13-dioxa-1,4-diazacyclooctadecane) (H 2 L), has been synthesized from reaction of (E,E )-dichloroglyoxime (1) with 2,3:14,15-dibenzo 8,9-(4 0 -nitrobenzo)-4,13-dithia-7,10-dioxa-1,16-diazahegzadecane (2). The mononuclear Co(III) complex (4) of this dioxime was prepared by oxidation of the cobalt (II) complex. The BF þ 2 -capped Co(III) complex (5) was synthesized by using a precursor Co(III) complex and boron trifluoride dietherate. The heterotrinuclear complexes (6) and (7) were prepared by reaction of (5) with NiCl 2 Á 6H 2 O and CdCl 2 Á H 2 O, respectively. In addition, the homotrinuclear Cu(II) complex (8), has also been prepared by the reaction of this dioxime with CuCl 2 Á H 2 O. The structures of the dioxime and its complexes were identified by using elemental analysis, 1 H-and 13 C-NMR, IR, and mass spectral data.

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“…It is known that protonation of the heterocyclic bases as well as their coordination to metal ions having a labile coordination sphere lead to deshielding of the amine protons [16]. However, the presence of the cobaloxime ring-current has an opposite effect [14,17]. The magnitude of this induced shift (ca.…”

Section: 43smentioning

confidence: 99%

Spectroscopic and X-Ray Investigation of Cobalt(III) Complexes with 2-Oximinocarboxylic Acids

Lampeka

Uzakbergenova

Skopenko

1993

Zeitschrift Für Naturforschung B

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Mixed complexes of Co(III) with 2-oximinopropionic (H 2A) or 2-oximino-3-phenylpropionic (H 2B) acid and different amine (imidazole, benzimidazole, pyridine, yS-picoline, y-picoline) are reported. Characterization of the complexes was based upon ele mental analysis, conductivity and JR, 'H N M R, and electronic absorption spectra, and X-ray diffraction analysis. The organic ligands behave as 0 ,N donors via the carboxyl oxygen and the oxime nitrogen atoms. A trans-octahedral structure has been assigned to the bis(2-oximinocarboxylato)bis(am ine)cobalt(III) on the basis of 'H N M R data.The crystal and molecular structures of the complexes rra«5-[bis(2-oximinopropionato)bis-(imidazole)]-(I) and ^•a«5'-[bis(2-oximinopropionato)bis(pyridine)]cobalt(III) (II) were deter mined. I crystallizes in space group P 2/« with a = 14.167(2), b = 8.774(_1), c = 14.785(2)Ä, ß = 113.37(1)°, Z = 4, Dca)c = 1.568 g e m '3. II crystallizes in space group P 1 with a = 9.122(2), b = 10.038(2), c = 11.759(2) A, a = 69.95(1)°, ß = 67.47(2)°, y = 69.49(2)°, Z = 2, Dcalc = 1.547 g-cm~3. The structures were refined to unweighted R factors of 0.036 and 0.028, respec tively. The coordination sphere around Co is pseudo-octahedral with the 2-oxim inopropionato ligands occupying four equatorial positions, and the amines in axial po sitions.

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Structure-NMR correlations in halo(ligand)bis(dioximato)cobalt(III) complexes

Cited by 60 publications

References 5 publications

Synthesis and Characterization of a Novel Macrocyclicvic-Dioxime and Some of its Mono and Trinuclear Complexes

Synthesis and Characterization of a Novel Macrocyclicvic-Dioxime and Some of its Mono and Trinuclear Complexes

The Synthesis and Characterization of a Novel ( E , E )-Dioxime and its Mono- and Heterotrinuclear Complexes Containing an 18-Membered Dioxadithiadiazamacrocycle

Spectroscopic and X-Ray Investigation of Cobalt(III) Complexes with 2-Oximinocarboxylic Acids

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