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Volumn , Issue 17, 2009, Pages 2482-2486

Activator-controlled high temperature in-situ ligand synthesis for the formation of rare earth thiolate amide coordination polymers

Author keywords

C S bond cleavage; Coordination polymers; In situ synthesis; Lanthanides; Thiolates

Indexed keywords

AMIDES; CHELATION; CHEMICAL BONDS; LIGANDS; MERCURY (METAL); RARE EARTHS;

EID: 66549119327     PISSN: 14341948     EISSN: 10990682     Source Type: Journal    
DOI: 10.1002/ejic.200900208     Document Type: Article
Times cited : (15)

References (73)
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    • Referring experiments carried out directly from benzimidazole melts together with Ln elements gave no in situ formation of 2,2'-bibenzimidazole but a previously unknown high-temperature form of benzimidazole itself. It forms on. the surface of the lantlianide metals. We also determined, the crystal structure of this ß-1-H--benzimidazole (5, It can be distinguished from the room temperature a-form by a closer overall packing see Supporting Information and CCDC-716038
    • Referring experiments carried out directly from benzimidazole melts together with Ln elements gave no in situ formation of 2,2'-bibenzimidazole but a previously unknown high-temperature form of benzimidazole itself. It forms on. the surface of the lantlianide metals. We also determined, the crystal structure of this ß-1-H--benzimidazole (5). It can be distinguished from the room temperature a-form by a closer overall packing (see Supporting Information and CCDC-716038).
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    • CCDC-716040 and the Supporting Information contain detailed crystallographic data for 3: C63H43LaN18, M, 1.191.1 gmol-1, crystal, dimensions 0.1 X 0.08 X 0.03 mm; orthorhombic, space group C2221 (No. 20, a, 1673.6(3) pm, b, 1513.5(3) pm, c, 2243.9(4) p.m, T, 200 K, Z, 4, V, 5683,8(2) X 106 pm3, pcálc±, 1.392 g cm-3, 20max, 47.12°, diffractometer Nonius Kappa CCD, Ω-Scan with An, 0,9°, radiation Mo-Ka, wave length γ, 0.71073 ̊, Flack-X Parameter 0,00(6, 21191 measured reflections, 4192 independent reflections, 3614 reflections with I>20[I, refined parameters 372. R 1, 0.0541 for 36.14 with I>20[I, wR2, 0.0953 for all 4192 independent reflections; remaining electron density: +1.45/-0.68 e pm 106
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    • The negative charges of the square antiprismatic ions of 3 are compensated by benzimidazolium cations in a ratio of 1:1 resulting in the overall formula (Bim.H2, La(BbimH)4] for this salt like compound. As no benzimidazole was added, to the reaction, the cations also derive from the C-S bond cleavage but with subsequent protonation instead of recombination to bibenzimidazole. The benzimidazolium cations are non-coordinating. Anionic benzimidazolates are not known for lanthanides today. The cationic character is evident in a reduction of the aromatic character of the ring system, by elongating C-N distances in the imidazole part. This behaviour resembles pyridylbenzimidazolium cations that also compensate the charges of corresponding square antiprismatic Ln-pyridylbenzimidazolate anions.[6c] Further information on the crystal structure of 3 can be deduced, from the Supporting Information
    • [6c] Further information on the crystal structure of 3 can be deduced, from the Supporting Information.
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    • Known are complexes of the Ln elements that are acetylbenzopyranone substituted, on the S atom of 2-merca.ptobenzimidazole. Because of the oxophilicity of the lanthanid.es they are coordinated via O and not S atoms, accordingly: K. B. Gudasi, T. R. Goudar, J. Indian Chem. Soc. 1997, 74, 786-788.
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* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.