Factors Affecting Solution Properties of Vanadium(V) Compounds:  X-ray Structure of β-cis-NH4[VO2(EDDA)]1

Crans, Debbie C.; Keramidas, Anastasios D.; Mahroof-Tahir, Mohammad; Anderson, Oren P.; Miller, Matthew J.

doi:10.1021/ic951270z

Cited by 44 publications

(37 citation statements)

References 44 publications

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“…The O-V-O angle in the VO 2 moiety is similar to those previously reported for related complexes with nitrogen trans to the oxo groups, for example, the a-cis isomer of the EDTA complex [24] and b-cis isomer of the EDDA complex. [18] Other authors [25] also found a rather similar type of isomerism and used the notation cis-and trans-phenolates. Hereafter we will use the a-cis and b-cis notation; however, as will be clear below, in solution the V V ±Rpyr 2 en system is much more complex, because several a-cis and b-cis complexes form.…”

Section: Introductionmentioning

confidence: 84%

“…The white precipitate was filtered, washed with water, ethanol, and diethyl ether, and dried under vacuum. Yield: 60 %; elemental analysis calcd (%) for C 18 ). From the solution of the filtrate, kept at room temperature for two weeks, colorless crystals were collected and characterized by Xray diffraction.…”

Section: Synthesis Of the Ligandsmentioning

confidence: 99%

“…The molecule is neutral with one of the pyridinium nitrogens protonated, and corresponds to the symmetrical isomer, sometimes designated by a-cis (see below). [18] In complex 4 the HRpyr 2 en À ligand coordinates the VO 2 + moiety by means of two phenolate-O À and two amine-N atoms forming a quite distorted octahedral coordination polyhedron. This is due both to the specific constraints of the VO 2 fragment and to the tetradentate coordination, which imposes stereochemical strain, but overall the coordination geometry of this compound is rather similar to other monomeric V V O 2 complexes.…”

Section: Introductionmentioning

confidence: 99%

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N,N′‐Ethylenebis(pyridoxylideneiminato) and N,N′‐Ethylenebis(pyridoxylaminato): Synthesis, Characterization, Potentiometric, Spectroscopic, and DFT Studies of Their Vanadium(IV) and Vanadium(V) Complexes

Correia¹,

Pessoa²,

Duarte³

et al. 2004

Chemistry A European J

128

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The Schiff base N,N'-ethylenebis(pyridoxylideneiminato) (H 2 pyr 2 en, 1) was synthesized by reaction of pyridoxal with ethylenediamine; reduction of H 2 pyr 2 en with NaBH 4 yielded the reduced Schiff base N,N'-ethylenebis-(pyridoxylaminato) (H 2 Rpyr 2 en, 2); their crystal structures were determined by X-ray diffraction. The totally protonated forms of 1 and 2 correspond to H 6 L 4 + , and all protonation constants were determined by pH-potentiometric and Supporting information for this article is available on the WWW under http://www.chemeurj.org/ or from the author. Some additional X-ray data for 1, 2, 4, and 9 (SI-1); further discussion of IR spectra (

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Section: Introductionmentioning

confidence: 84%

Section: Synthesis Of the Ligandsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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N,N′‐Ethylenebis(pyridoxylideneiminato) and N,N′‐Ethylenebis(pyridoxylaminato): Synthesis, Characterization, Potentiometric, Spectroscopic, and DFT Studies of Their Vanadium(IV) and Vanadium(V) Complexes

Correia¹,

Pessoa²,

Duarte³

et al. 2004

Chemistry A European J

128

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“…10 In solution ethylenediaminediacetate (EDDA) ligand forms two isomers of similar stability with vanadium(V), a symmetric α-cis complex and an asymmetric β-cis complex. 10,14 In a previous paper, 15 we reported that the vanadium complex of propylenediaminetetraacetate (PDTA) ligand was determined to have α-cis structure in solid. The anion [VO 2 PDTA] 3− has a slightly irregular octahedral geometry in which two oxo ligands are cis to each other as shown in EDTA, 7,8 and EDDA complexes.…”

Section: Introductionmentioning

confidence: 99%

NMR Studies on the Isomerization of Vanadium(V)-Propylenediaminetetraacetate Complex in Solution

2004

Bulletin of the Korean Chemical Society

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In this paper we have determined the thermodynamic parameters for the isomerization between the α-cis and the β-cis isomers in vanadium(V)-propylenediaminetetraacetate complex in water by 51 V NMR spectroscopy. In addition, the effects of organic solvents (methanol, formamide and dimethylsulfoxide) and inorganic salts (NaCl, NaClO 4 and NH 4 Cl) on the isomerization in solution have been investigated.

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“…But ethylenediaminediacetate (EDDA) is known to form a β-cis structure (2) with vanadium(V). 11 According to the solution studies, 11,12 EDDA forms α-cis and β-cis isomers with vanadium(V) while EDTA forms only the α-cis isomer with vanadium(V). The steric hindrance makes stable the α-cis form of the isomers because the substitution of an acetate group on nitrogen increases steric bulk.…”

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confidence: 99%

Synthesis and Crystal Structure of Triammonium(Propylenediamonetetraacetato)dioxovanadate(V) Monohydrate Complex

2002

Bulletin of the Korean Chemical Society

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Vanadium has been recognized to play important roles in biological systems. 1 Recently it is reported that bis(maltolato)oxovanadium(IV) complex is a potent insulin mimic agent.2,3 The structure, stability and lability of vanadium(V) compounds are important to the mechanisms by which these compounds act in biological systems and in part have contributed to the mechanisms by which vanadate mimics insulin action. 4 But the chemistry of vanadium has not much known yet. Of the representative vanadium(V) complexes, the crystal structures of vanadium(V) complexes with oxalate (Ox), 5,6 ethylenediaminetetraacetate (EDTA), 7,8 nitrilotriacetate (NTA), 9 and N-(2-hydroxyethylimino)diacetate 10 ligands have been studied by X-ray crystallography. Vanadium(V)-EDTA complexes are confirmed to have a α-cis structure (1), in which the anion has an irregular octahedral geometry with VO 2 core. But ethylenediaminediacetate (EDDA) is known to form a β-cis structure (2) with vanadium(V). 11 According to the solution studies, 11,12 EDDA forms α-cis and β-cis isomers with vanadium(V) while EDTA forms only the α-cis isomer with vanadium(V). The steric hindrance makes stable the α-cis form of the isomers because the substitution of an acetate group on nitrogen increases steric bulk.In this paper we report the synthesis of a new vanadium (V) complex, triammonium (propylenediaminetetraacetato)-dioxovanadate(V) monohydrate, as well as its crystal structure determined by X-ray crystallography. Propylenediaminetetraacetate (PDTA) is similar to EDTA in structure. PDTA has an asymmetric carbon on ethylenic backbone according to the substitution of a methyl group, while EDTA has a symmetric structure. Experimental SectionMaterials. All reagent grade chemicals were used without further purification. Ammonium metavanadate (NH 4 VO 3 ) and propylenediaminetetraacetic acid (H 4 PDTA) were purchased from Aldrich Chemical Company.Preparation of vanadium(V) complex. The reaction of NH 4 VO 3 (0.02 mole, 2.34 g), H 4 PDTA (0.02 mole, 6.13 g) and 25% ammonia water (0.03 mole, 2.0 mL) in 100 mL water produced a yellow solution which was concentrated by passing a stream of dry air at room temperature. Ethanol was added and the resulting solution was kept in a refrigerator. The pale yellow crystals were formed and then filtered. The yield was 30%. The single crystals were obtained by dissolving the powders in water and keeping the solution in a refrigerator for several days. The chemical formula, VN 5 O 11 -C 11 H 28 , of the complex was obtained from the elemental analysis. Analytical data (%) are in the range of good agreement (calculated: C, 28.89; H, 6.17; N, 15.32. found: C, 28.83; H, 6.10; N, 15.26).X-Ray measurements. Preliminary experiments and data collection for X-ray crystal structure determination were performed on a Enraf-Nonius CAD4/Turbo diffractometer using Mo K α radiation (λ = 0.71069 Å). A small single crystal, 0.5 × 0.5 × 0.5 mm, was glued to a glass fiber with an epoxy resin. 25 reflections in the diverse reciprocal space were center...

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Factors Affecting Solution Properties of Vanadium(V) Compounds: X-ray Structure of β-cis-NH₄[VO₂(EDDA)]¹

Cited by 44 publications

References 44 publications

N,N′‐Ethylenebis(pyridoxylideneiminato) and N,N′‐Ethylenebis(pyridoxylaminato): Synthesis, Characterization, Potentiometric, Spectroscopic, and DFT Studies of Their Vanadium(IV) and Vanadium(V) Complexes

N,N′‐Ethylenebis(pyridoxylideneiminato) and N,N′‐Ethylenebis(pyridoxylaminato): Synthesis, Characterization, Potentiometric, Spectroscopic, and DFT Studies of Their Vanadium(IV) and Vanadium(V) Complexes

NMR Studies on the Isomerization of Vanadium(V)-Propylenediaminetetraacetate Complex in Solution

Synthesis and Crystal Structure of Triammonium(Propylenediamonetetraacetato)dioxovanadate(V) Monohydrate Complex

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