Synthesis and X-ray structural analysis of a unique Co-crystallization complex of [NaSal]2DB24C8 and [KSal]2DB24C8

Momany, Cory; Hackert, Marvin L.; Sharma, Jyotsna; Poonia, N. S.

doi:10.1007/bf00665367

Cited by 9 publications

(4 citation statements)

References 20 publications

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“…For these reasons DB24C8 was a logical choice to try to create a mixed Na/K complex in which the two metal ions occupy similar coordination environments. The first reported structure of a mixed-metal Na/K crown complex appeared in Momany et al (1987), featuring DB24C8 and the anion salicylate. In that structure, although cocrystallized, each metal cation complexed separately with its own crown and anions, thus affording a good opportunity to compare Na/K differential complexation tendencies.…”

Section: Discussionmentioning

confidence: 99%

“…1), and X is a chelating organic anion such as 2-hydroxybenzoate (sal), 2,6-dihydroxybenzoate (HOsal), 3,5-dinitrobenzoate (dnb), 2-nitrophenolate (onp), 2,4-dinitrophenolate (dnp), and 2,4,6-trinitrophenolate (pic). X-ray analysis of the first mixed-cation complex synthesized, that in which X = sal, revealed it to be a homogeneous cocrystallization of the metallic complexes [Na(sal)]2(DB24C8) and [K(sal)]2(DB24CS) (Momany, Hackert, Sharma, & Poonia, 1987). In that structure, the coordination environments of the two cations differ significantly between the two complexes, primarily in that the conformation of the crown molecule is flat in the di-K complex and distinctly puckered in the di-Na complex.…”

Section: Introductionmentioning

confidence: 99%

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Dipotassium and sodium/potassium crystalline picrate complexes with the crown ether 6,7,9,10,12,13,20,21,23,24,26,27-dodecahydrodibenzo[b,n][1,4,7,10,13,16,19,22]octaoxacyclotetracosin (dibenzo-24-crown-8)

Gallagher¹,

Taylor²,

Ernst³

et al. 1991

Acta Crystallogr Sect B

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The crystal structures of the dipotassium and the mixed sodium/potassium picrate complexes with the crown ether dibenzo-24-crown-8 (DB24C8) were solved and found to be nearly identical. (I): NaKpicz(DB24C8), [NaK(C6H2N307)2(C24H3208)], Mr = 966.8, triclinic, P1, a = 8-164 (2), b = 9.960 (2), c= 13. structure. Na + is able to occupy an environment similar to that of K + under the conditions of these crystals, a situation not previously observed in the chemistry of crown ethers or macrocylic multidentates.

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Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Dipotassium and sodium/potassium crystalline picrate complexes with the crown ether 6,7,9,10,12,13,20,21,23,24,26,27-dodecahydrodibenzo[b,n][1,4,7,10,13,16,19,22]octaoxacyclotetracosin (dibenzo-24-crown-8)

Gallagher¹,

Taylor²,

Ernst³

et al. 1991

Acta Crystallogr Sect B

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“…A well-known example is that of dibenzo-24-crown-8, which binds two sodium ions in its cavity. 52 The solution NMR analysis of [CoL 8 (OH)] 2+ in the absence and presence of Na + indicated a significant conformational change upon complexation. In terms of the torsional angles discussed previously, ω 2 must be gauche in the absence of bound guest ion if NOE peaks between the aromatic protons and the methyl group are to be observed.…”

Section: Discussionmentioning

confidence: 98%

“…It is also not unusual for large crown ethers to complex two cations. A well-known example is that of dibenzo-24-crown-8, which binds two sodium ions in its cavity …”

Section: Discussionmentioning

confidence: 99%

Crown Ether Appended Cyclam Receptors for Cationic Guests

Bernhardt

Hayes

2002

Inorg. Chem.

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A series of crown ether appended macrocyclic amines has been prepared comprising benzo-12-crown-4, benzo-15-crown-5, or benzo-18-crown-6 attached to a diamino-substituted cyclam. The Co(III) complexes of these three receptors have been prepared and characterized spectroscopically and structurally. Crystal structures of each receptor in complex with an alkali metal ion and structures of the benzo-12-crown-4 and benzo-15-crown-5-receptors without guest ions are reported. 2D NMR and molecular mechanics modeling have been used to examine conformational variations upon guest ion complexation. Addition of cations to these receptors results in an appreciable anodic shift in the Co(III/II) redox potential, even in aqueous solution, but little cation selectivity is observed. Evidence for complex formation has been corroborated by (23)Na and (7)Li NMR spectroscopy and electrospray mass spectrometry.

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Supramolecular Chemistry Based on Frustrated Lewis Pairs – Reactions of an Al/P FLP with Potassium Formate and Cesium Fluoride

Uhl

Lange

Hepp

et al. 2018

Zeitschrift anorg allge chemie

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Reactions of the Al/P‐based frustrated Lewis pair Mes2P–C(AltBu2)=C(H)–Ph (1) with the Brønstedt acids HBr, HI, and HCO2H resulted in the formation of the corresponding HX adducts Mes2(H)P–C[Al(X)tBu2]=C(H)–Ph [X = Br (4), I (5), OC(H)O (6)]. Despite the well‐known sensitivity of Al–C bonds towards protolysis, the products were isolated in good yields. Short intramolecular distances between H and Br, I or O are consistent with the presence of P–H···X hydrogen bonds. Treatment of 1 with potassium formate or CsF yielded in poor to moderate yields the adducts Mes2P–C(AltBu2)=C(H)Ph·(KO2CH) (7) and Mes2P–C(AltBu2)=C(H)Ph·(CsF) (8). The potassium compounds required the presence of additional solvent molecules to obtain isolable crystalline products. Two monomeric units were joined by interactions of each K+ cation with two formate anions. Supramolecular entities resulted by the additional coordination of the K+ cations to solvent molecules (7a, toluene; 7b, 1,2‐difluorobenzene; 7c, THF), weak contacts to a mesityl group and in case of 7b and 7c to a tBu group and the P atom. The CsF adduct 8 crystallizes as a double‐stranded chain with the coordination of the Cs+ cation to F–, a mesityl group (η6), a Ph group (η6; leads to an infinite chain), and a tBu group (connects two chains to a double strand) of two different neighboring molecules. The Cs–F bond length is with 274.7(1) pm comparatively short, and the adduct may be viewed as a CsF molecule trapped by the FLP functionality.

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Synthesis and X-ray structural analysis of a unique Co-crystallization complex of [NaSal]2DB24C8 and [KSal]2DB24C8

Cited by 9 publications

References 20 publications

Dipotassium and sodium/potassium crystalline picrate complexes with the crown ether 6,7,9,10,12,13,20,21,23,24,26,27-dodecahydrodibenzo[b,n][1,4,7,10,13,16,19,22]octaoxacyclotetracosin (dibenzo-24-crown-8)

Dipotassium and sodium/potassium crystalline picrate complexes with the crown ether 6,7,9,10,12,13,20,21,23,24,26,27-dodecahydrodibenzo[b,n][1,4,7,10,13,16,19,22]octaoxacyclotetracosin (dibenzo-24-crown-8)

Crown Ether Appended Cyclam Receptors for Cationic Guests

Supramolecular Chemistry Based on Frustrated Lewis Pairs – Reactions of an Al/P FLP with Potassium Formate and Cesium Fluoride

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