AN X-RAY AND C-13 CP MAS NMR-STUDY OF C,C-LINKED BIPYRAZOLES AND BISPYRAZOLYLMETHANES

被引：20
作者：
MONGE, MA
PUEBLA, EG
ELGUERO, J
TOIRON, C
MEUTERMANS, W
SOBRADOS, I
机构：
[1] CSIC,INST QUIM,JUAN CIERVA 3,E-28006 MADRID,SPAIN
[2] UNIV COMPLUTENSE MADRID,FAC QUIM,CSIC,INST CIENCIA MAT,DIFRACC RAYOSX LAB,E-28040 MADRID,SPAIN
[3] CSIC,INST CIENCIA MAT,E-28006 MADRID,SPAIN
来源：
SPECTROCHIMICA ACTA PART A-MOLECULAR AND BIOMOLECULAR SPECTROSCOPY | 1994年 / 50卷 / 04期
关键词：
D O I：
10.1016/0584-8539(94)80010-3
中图分类号：
O433 [光谱学];
学科分类号：
0703 ; 070302 ;
摘要：
4,4'-Methylene-bispyrazole (1) crystallizes in the P2(1)/n space group with Z = 4, a = 5.4199(8) angstrom, b = 16.194(6) angstrom, c = 8.381(5) angstrom, beta = 98.18(5)degrees. 4,4'-Methylene-bis (3,5-dimethylpyrazole) (2) crystallizes in the Pbca space group with Z = 8, a = 8.350(3) angstrom, b = 16.078(3) angstrom and c = 17.154(5) angstrom. Finally, 3,3'-bipyrazole (4) crystallizes in the P2(1)/n space group with Z = 2, a = 5.465(2) angstrom, b = 5.491(3) angstrom, c = 10.058(4) angstrom and beta = 92.88(2)degrees. The packing adopted by molecules 1 and 2 is related to the disposition of the pyrazole rings. In compound 4, all the molecules are joined to their neighbors by two double hydrogen bond systems forming zig-zag chains. Using solid state C-13 NMR spectroscopy, no dynamic proton transfer was observed in these crystals, and not on those of 3,5,3',5'-tetramethyl-4,4'-bipyrazole (3) either.
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页码：727 / 734
页数：8
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