Application of the MAS-J-HMQC experiment to a new pair of nuclei {29Si, 31P}:: Si5O(PO4)6 and SiP2O7 polymorphs

被引:39
作者
Coelho, C
Azais, T
Bonhomme-Coury, L
Maquet, J
Massiot, D
Bonhomme, C
机构
[1] Univ Paris 06, Lab Chim Mat Condensee, UMR 7574, F-75252 Paris 05, France
[2] CNRS, CRMHT, F-45071 Orleans 2, France
关键词
MAS-J-HMQC; J coupling; solid state NMR; Si5O(PO4)(6); SiP2O7; silicophosphate;
D O I
10.1016/j.jmr.2005.11.015
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
We report the results of the two-dimensional MAS-J-HMQC experiment providing scalar correlations between Si-29 and P-31 nuclei in solid state NMR, and we give the first evaluation of the (2)J(Si-O-P) coupling constants (similar to 15 Hz) for a crystalline silicophosphate phase Si5O(PO4)(6). The experiment is applied to the characterization of complex mixtures of SiP2O7 phases, through editing of P-31 spin pairs by the heteronuclear (2)J(P-O-Si) interaction. (c) 2005 Elsevier Inc. All rights reserved.
引用
收藏
页码:114 / 119
页数:6
相关论文
共 24 条
[1]   Measurement of J-couplings between spin-1-2 and quadrupolar nuclei by frequency selective solid-state NMR [J].
Amoureux, JP ;
Trebosc, J ;
Wiench, JW ;
Massiot, D ;
Pruski, M .
SOLID STATE NUCLEAR MAGNETIC RESONANCE, 2005, 27 (04) :228-232
[2]   Determining hydrogen-bond strengths in the solid state by NMR:: the quantitative measurement of homonuclear J couplings [J].
Brown, SP ;
Pérez-Torralba, M ;
Sanz, D ;
Claramunt, RM ;
Emsley, L .
CHEMICAL COMMUNICATIONS, 2002, (17) :1852-1853
[3]   Sol-gel synthesis of humidity-sensitive P2O5-SiO2 amorphous films [J].
D'Apuzzo, M ;
Aronne, A ;
Esposito, S ;
Pernice, P .
JOURNAL OF SOL-GEL SCIENCE AND TECHNOLOGY, 2000, 17 (03) :247-254
[4]   INEPT EXPERIMENTS IN SOLID-STATE NMR [J].
FYFE, CA ;
WONGMOON, KC ;
HUANG, Y ;
GRONDEY, H .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1995, 117 (41) :10397-10398
[5]   1D and 2D solid state NMR investigations of the framework structure of As-synthesized AlPO4-14 [J].
Fyfe, CA ;
Altenschildesche, HMZ ;
Wong-Moon, KC ;
Grondey, H ;
Chezeau, JM .
SOLID STATE NUCLEAR MAGNETIC RESONANCE, 1997, 9 (2-4) :97-106
[6]   P-31 MAS and 2D exchange NMR of crystalline silicon phosphates [J].
Hartmann, P ;
Jana, C ;
Vogel, J ;
Jager, C .
CHEMICAL PHYSICS LETTERS, 1996, 258 (1-2) :107-112
[7]   BIOCERAMICS - FROM CONCEPT TO CLINIC [J].
HENCH, LL .
JOURNAL OF THE AMERICAN CERAMIC SOCIETY, 1991, 74 (07) :1487-1510
[8]   NMR heteronuclear correlation between quadrupolar nuclei in solids [J].
Iuga, D ;
Morais, C ;
Gan, ZH ;
Neuville, DR ;
Cormier, L ;
Massiot, D .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2005, 127 (33) :11540-11541
[9]   INEPT experiments involving quadrupolar nuclei in solids [J].
Kao, HM ;
Grey, GP .
JOURNAL OF MAGNETIC RESONANCE, 1998, 133 (02) :313-323
[10]   Solid phosphoric acid catalyst: A multinuclear NMR and theoretical study [J].
Krawietz, TR ;
Lin, P ;
Lotterhos, KE ;
Torres, PD ;
Barich, DH ;
Clearfield, A ;
Haw, JF .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1998, 120 (33) :8502-8511