Layered Calcium Structures of p-Phosphonic Acid O-Methyl-Calix[6]arene

Thomas Clark; Adam Martin; Mohamed Makha; Alexandre Sobolev; Dian Su; Henry Rohrs; Michael Gross; Colin Raston

doi:10.1021/cg1003484

Layered Calcium Structures of p-Phosphonic Acid O-Methyl-Calix[6]arene

Thomas Clark, Adam Martin, Mohamed Makha, Alexandre Sobolev, Dian Su, Henry Rohrs, Michael Gross, Colin Raston

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

15 Citations (Scopus)

Abstract

Hexamethoxy-calix[6]arene has been fully functionalized with p-phosphonic acid groups on the upper rim in57% yield over three steps and has been authenticated in the solid state by X-ray diffraction as either a nitrate salt or one of two calcium complexes. The latter differ by the ratio of calcium ions per calixarene, either 3:1 or 4:1. In both structures, the coordination sphere of the calcium ions is made up of oxygen atoms from the phosphonic acid groups and from water of crystallization, as part of extended polymeric layers in the extended three-dimensional packing. Hirshfeld surface analysis shows extensive O⋯H and O⋯Ca interactions for the phosphonic acid moieties in both calcium structures. Matrix assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) of the hexaphosphonic acid shows nanoarrays consisting of up to a maximum of 28 calixarene units.

Original language	English
Pages (from-to)	3211-3217
Number of pages	7
Journal	Crystal Growth and Design
Volume	10
Issue number	7
DOIs	https://doi.org/10.1021/cg1003484
Publication status	Published - 7 Jul 2010

Access to Document

10.1021/cg1003484

Cite this

@article{914cb5487ddc41a382cce175e91340a5,

title = "Layered Calcium Structures of p-Phosphonic Acid O-Methyl-Calix[6]arene",

abstract = "Hexamethoxy-calix[6]arene has been fully functionalized with p-phosphonic acid groups on the upper rim in57% yield over three steps and has been authenticated in the solid state by X-ray diffraction as either a nitrate salt or one of two calcium complexes. The latter differ by the ratio of calcium ions per calixarene, either 3:1 or 4:1. In both structures, the coordination sphere of the calcium ions is made up of oxygen atoms from the phosphonic acid groups and from water of crystallization, as part of extended polymeric layers in the extended three-dimensional packing. Hirshfeld surface analysis shows extensive O⋯H and O⋯Ca interactions for the phosphonic acid moieties in both calcium structures. Matrix assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) of the hexaphosphonic acid shows nanoarrays consisting of up to a maximum of 28 calixarene units.",

author = "Thomas Clark and Adam Martin and Mohamed Makha and Alexandre Sobolev and Dian Su and Henry Rohrs and Michael Gross and Colin Raston",

year = "2010",

month = jul,

day = "7",

doi = "10.1021/cg1003484",

language = "English",

volume = "10",

pages = "3211--3217",

journal = "Crystal Growth and Design",

issn = "1528-7483",

publisher = "American Chemical Society",

number = "7",

}

TY - JOUR

T1 - Layered Calcium Structures of p-Phosphonic Acid O-Methyl-Calix[6]arene

AU - Clark, Thomas

AU - Martin, Adam

AU - Makha, Mohamed

AU - Sobolev, Alexandre

AU - Su, Dian

AU - Rohrs, Henry

AU - Gross, Michael

AU - Raston, Colin

PY - 2010/7/7

Y1 - 2010/7/7

N2 - Hexamethoxy-calix[6]arene has been fully functionalized with p-phosphonic acid groups on the upper rim in57% yield over three steps and has been authenticated in the solid state by X-ray diffraction as either a nitrate salt or one of two calcium complexes. The latter differ by the ratio of calcium ions per calixarene, either 3:1 or 4:1. In both structures, the coordination sphere of the calcium ions is made up of oxygen atoms from the phosphonic acid groups and from water of crystallization, as part of extended polymeric layers in the extended three-dimensional packing. Hirshfeld surface analysis shows extensive O⋯H and O⋯Ca interactions for the phosphonic acid moieties in both calcium structures. Matrix assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) of the hexaphosphonic acid shows nanoarrays consisting of up to a maximum of 28 calixarene units.

AB - Hexamethoxy-calix[6]arene has been fully functionalized with p-phosphonic acid groups on the upper rim in57% yield over three steps and has been authenticated in the solid state by X-ray diffraction as either a nitrate salt or one of two calcium complexes. The latter differ by the ratio of calcium ions per calixarene, either 3:1 or 4:1. In both structures, the coordination sphere of the calcium ions is made up of oxygen atoms from the phosphonic acid groups and from water of crystallization, as part of extended polymeric layers in the extended three-dimensional packing. Hirshfeld surface analysis shows extensive O⋯H and O⋯Ca interactions for the phosphonic acid moieties in both calcium structures. Matrix assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) of the hexaphosphonic acid shows nanoarrays consisting of up to a maximum of 28 calixarene units.

UR - http://www.scopus.com/inward/record.url?scp=77956150001&partnerID=8YFLogxK

U2 - 10.1021/cg1003484

DO - 10.1021/cg1003484

M3 - Article

SN - 1528-7483

VL - 10

SP - 3211

EP - 3217

JO - Crystal Growth and Design

JF - Crystal Growth and Design

IS - 7

ER -

Layered Calcium Structures of p-Phosphonic Acid O-Methyl-Calix[6]arene

Abstract

Access to Document

Other files and links

Fingerprint

Cite this