Metallic Macrocycle with a 1,3-Alternate Calix[4]arene Phosphorus Ligand

Sanghoon Kim; Jong Seung Kim; Ok Jae Shon; Shim Sung Lee; Ki Min Park; Sang Ook Kang; Jaejung Ko

doi:10.1021/ic030221g

Metallic Macrocycle with a 1,3-Alternate Calix[4]arene Phosphorus Ligand

Sanghoon Kim, Jong Seung Kim, Ok Jae Shon, Shim Sung Lee, Ki Min Park, Sang Ook Kang, Jaejung Ko

Research output: Contribution to journal › Article › peer-review

18 Citations (Scopus)

Abstract

The preparation of an 1,3-alternate calix[4]arene phosphorus ligand, 25,27-bis(2-(diphenylphosphino)ethoxy)-26,28-bis(1-propyloxy)calix[4]arene (3), is presented. Ligand 3 is obtained in three steps in 64% overall yield. Reaction of 3 with [Rh(cot)₂]BF₄ produced the encapsulated rhodium complex [Rh{(P,P)-diphen-calix[4]arene}]BF₄ (4). As revealed by a single-crystal X-ray diffraction study, the rhodium center has a bent coordination environment with a P-Rh-P angle of 135.66(3)°. Palladation of 3 employing [Pd(MeCN)₄](BF₄)₂ yielded the chelate palladium complex 7 in which the palladium center has a slightly bent configuration. Treatment of the ligand with Pd(cod)Cl₂ and [Pd(η³-C₄H₇)(THF)₂]BF ₄ leads to the isolation of the monometallic complex. Full characterization includes X-ray structural studies of compounds 3, 4, and 6.

Original language	English
Pages (from-to)	2906-2913
Number of pages	8
Journal	Inorganic Chemistry
Volume	43
Issue number	9
DOIs	https://doi.org/10.1021/ic030221g
Publication status	Published - 2004 May 3
Externally published	Yes

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry

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title = "Metallic Macrocycle with a 1,3-Alternate Calix[4]arene Phosphorus Ligand",

abstract = "The preparation of an 1,3-alternate calix[4]arene phosphorus ligand, 25,27-bis(2-(diphenylphosphino)ethoxy)-26,28-bis(1-propyloxy)calix[4]arene (3), is presented. Ligand 3 is obtained in three steps in 64% overall yield. Reaction of 3 with [Rh(cot)2]BF4 produced the encapsulated rhodium complex [Rh{(P,P)-diphen-calix[4]arene}]BF4 (4). As revealed by a single-crystal X-ray diffraction study, the rhodium center has a bent coordination environment with a P-Rh-P angle of 135.66(3)°. Palladation of 3 employing [Pd(MeCN)4](BF4)2 yielded the chelate palladium complex 7 in which the palladium center has a slightly bent configuration. Treatment of the ligand with Pd(cod)Cl2 and [Pd(η3-C4H7)(THF)2]BF 4 leads to the isolation of the monometallic complex. Full characterization includes X-ray structural studies of compounds 3, 4, and 6.",

author = "Sanghoon Kim and Kim, {Jong Seung} and Shon, {Ok Jae} and Lee, {Shim Sung} and Park, {Ki Min} and Kang, {Sang Ook} and Jaejung Ko",

year = "2004",

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doi = "10.1021/ic030221g",

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AU - Kim, Sanghoon

AU - Kim, Jong Seung

AU - Shon, Ok Jae

AU - Lee, Shim Sung

AU - Park, Ki Min

AU - Kang, Sang Ook

AU - Ko, Jaejung

PY - 2004/5/3

Y1 - 2004/5/3

N2 - The preparation of an 1,3-alternate calix[4]arene phosphorus ligand, 25,27-bis(2-(diphenylphosphino)ethoxy)-26,28-bis(1-propyloxy)calix[4]arene (3), is presented. Ligand 3 is obtained in three steps in 64% overall yield. Reaction of 3 with [Rh(cot)2]BF4 produced the encapsulated rhodium complex [Rh{(P,P)-diphen-calix[4]arene}]BF4 (4). As revealed by a single-crystal X-ray diffraction study, the rhodium center has a bent coordination environment with a P-Rh-P angle of 135.66(3)°. Palladation of 3 employing [Pd(MeCN)4](BF4)2 yielded the chelate palladium complex 7 in which the palladium center has a slightly bent configuration. Treatment of the ligand with Pd(cod)Cl2 and [Pd(η3-C4H7)(THF)2]BF 4 leads to the isolation of the monometallic complex. Full characterization includes X-ray structural studies of compounds 3, 4, and 6.

AB - The preparation of an 1,3-alternate calix[4]arene phosphorus ligand, 25,27-bis(2-(diphenylphosphino)ethoxy)-26,28-bis(1-propyloxy)calix[4]arene (3), is presented. Ligand 3 is obtained in three steps in 64% overall yield. Reaction of 3 with [Rh(cot)2]BF4 produced the encapsulated rhodium complex [Rh{(P,P)-diphen-calix[4]arene}]BF4 (4). As revealed by a single-crystal X-ray diffraction study, the rhodium center has a bent coordination environment with a P-Rh-P angle of 135.66(3)°. Palladation of 3 employing [Pd(MeCN)4](BF4)2 yielded the chelate palladium complex 7 in which the palladium center has a slightly bent configuration. Treatment of the ligand with Pd(cod)Cl2 and [Pd(η3-C4H7)(THF)2]BF 4 leads to the isolation of the monometallic complex. Full characterization includes X-ray structural studies of compounds 3, 4, and 6.

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JO - Inorganic Chemistry

JF - Inorganic Chemistry

IS - 9

ER -

Metallic Macrocycle with a 1,3-Alternate Calix[4]arene Phosphorus Ligand

Abstract

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