Darstellung und Kristallstruktur der Addukte [DB‐18C6] · CH3CN · CH3CSOH und [DC‐18C6](CH3CSOH)2sowie der salzartigen Verbindungen [Cs(B‐15C5)2]CH3CSS und [Cs(DB‐18C6)]2S5(DMF)21)

Schnock, M.; Müller, Christian; Böttcher, P.

doi:10.1002/zaac.19966220414

Cited by 6 publications

(1 citation statement)

References 61 publications

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“…To our knowledge, the first X-ray structural analysis of alkali metal thiocarboxylates was reported in 1976 by Borel and Ledesert, who analyzed potassium and rubidium thioacetates . Lithium benzenecarbothioate (PhCOSLi/TMEDA) and cesium thioacetate with crown ether were then reported by Banister et al and Böttcher et al, respectively. Potassium di- and trithiooxalates have also been documented .…”

Section: Introductionmentioning

confidence: 99%

Facile Synthesis and Structure of Heavy Alkali Metal Thiocarboxylates: Structural Comparison with the Selenium and Tellurium Isologues

1999

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Potassium, rubidium, and cesium thiocarboxylates were found to be synthesized by the reaction of thiocarboxylic acid or its O-trimethylsilyl esters with KF, RbF, and CsF. Tetramethylammonium thiocarboxylates were prepared in good yields by the reaction of sodium thiocarboxylates with tetramethylammonium chloride. The structures of potassium benzene-, 2-methoxybenzene-, and 4-methoxybenzenecarbothioates, rubidium 2-methoxybenzenecarbothioate, tetramethylammonium 2-methoxy- and 2-trifluoromethylbenzenecarbothioates, potassium 2-methoxybenzenecarboselenoate, and rubidium 2-methoxybenzenecarbotelluroate were characterized by X-ray structural analysis. All of these alkali metal salts exhibit a dimeric structure in which the oxygen and/or sulfur atom is associated with the metal of the opposite molecule, while the tetramethylammonium thiocarboxylates are monomeric. In potassium 2-methoxybenzenecarbothioate, the two thiocarboxylate groups chelate to the potassium atoms above and below the plane which involves the thiocarboxylate groups. In potassium 4-methoxybenzenecarbothioate, one thiocarboxylate group chelates to potassium. Without exception, the o-methoxy oxygen intermolecularly coordinates to the metal of the opposite molecule. The C-O bond lengths of the thiocarboxylate group are in the range 1.22-1.24 Å, which is slightly longer than those of common thioesters. The C(sp(2))-S distances are in the range 1.70-1.72 Å, which is close to that of a typical C-S single bond and suggests that the negative charge may be somewhat localized on the sulfur atom. The interaction number of the metals with oxygen and sulfur atoms was 7 for K and 8 for both Rb and Cs. The dihedral angle between the thiocarboxyl group and the phenyl ring is substantially increased by the introduction of the o-methoxy group. In these alkali metal thio-, seleno-, and tellurocarboxylates, only cesium 2-methoxybenzenecarbotelluroate showed an intermolecular nonbonding interaction between the cesium and the phenyl ring carbons.

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Section: Introductionmentioning

confidence: 99%

Facile Synthesis and Structure of Heavy Alkali Metal Thiocarboxylates: Structural Comparison with the Selenium and Tellurium Isologues

1999

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A Europium(II) Complex with Benzo‐15‐Crown‐5

Starynowicz

Bukietyńska

2002

Euro J of Inorganic Chem

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Keywords: Europium / Crown compounds / X-ray diffraction / Luminescence / LanthanidesThe present paper reports the crystal structure and luminescent properties of bis(benzo-15-crown-5)europium(II) diperchlorate. The structure is composed of complex bis(benzo-15-crown-5)europium(II) cations and perchlorate anions. The complex cation is centrosymmetric, and the metal ion is surrounded by 10 oxygen atoms of two ligand molecules. The

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Strukturen der Alkalimetallsalze aromatischer, heterocyclischer Amide: Synthese und Struktur von Kronenether‐Addukten der Alkalimetall‐indolide

Heldt

Borrmann

Behrens

2003

Zeitschrift anorg allge chemie

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The synthesis of five alkali metal indolide crown ether complexes is reported. Lithium-indolide(12-crown-4) (1) was synthezised from butyllithium, indole, and 12-crown-4; sodium-indolide(15-crown-5) (2) from sodium metal, indole, and 15-crown-5; potassium-indolide(18-crown-6) (3) from potassium hydride, indole, and 18-crown-6. Rubidium-and cesium-indolide(18-crown-6) (4, 5) were made from Rb-and Cs-hexamethyldisilazide, indole, Einleitung 1) Die Alkalimetall-cyclopentadienide, -indenide und -fluorenide sind bekanntlich wichtige Ausgangsverbindungen für die Synthese von Metallocenen der Haupt-und Nebengruppenelemente. Ohne zusätzliche koordinierende Liganden wie Tetrahydrofuran (THF), Dimethoxyethan (DME), Tetramethylethylendiamin (TMEDA) usw. bilden die Alkalimetall-cyclopentadienide polymere Stapelstrukturen aus [1]. Auch Lithium-indenid kristallisiert in Form einer Multidekker-Struktur [2]. Kronenether sind in besonderem Maße fähig, die polymeren Strukturen der basen-freien Alkali-5) wurden aus Rb-bzw. Cs-hexamethyldisilazid, Indol und 18-Krone-6 erhalten. Die Strukturen von 2, 4 und 5 konnten röntgenographisch bestimmt werden. Die Komplexe 2 und 4 sind einkernig, das Indolid-Anion weist eine η 1 (N)-Koordination zum Metallkation auf. Komplex 5 ist zweikernig mit einem zentralen [CsϪNϪ] 2 -Ring.and 18-crown-6. The structures of 2, 4, and 5 could be determined by X-ray diffraction. The complexes 2 and 4 are mononuclear, the indolide anion shows an η 1 (N)-coordination to the metal cation. Complex 5 is dinuclear with a central [CsϪNϪ] 2 -ring.

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Darstellung und Kristallstruktur der Addukte [DB‐18C6] · CH₃CN · CH₃CSOH und [DC‐18C6](CH₃CSOH)₂sowie der salzartigen Verbindungen [Cs(B‐15C5)₂]CH₃CSS und [Cs(DB‐18C6)]₂S₅(DMF)₂¹)

Cited by 6 publications

References 61 publications

Facile Synthesis and Structure of Heavy Alkali Metal Thiocarboxylates: Structural Comparison with the Selenium and Tellurium Isologues

Facile Synthesis and Structure of Heavy Alkali Metal Thiocarboxylates: Structural Comparison with the Selenium and Tellurium Isologues

A Europium(II) Complex with Benzo‐15‐Crown‐5

Strukturen der Alkalimetallsalze aromatischer, heterocyclischer Amide: Synthese und Struktur von Kronenether‐Addukten der Alkalimetall‐indolide

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