SYNTHESIS, CRYSTAL AND MOLECULAR-STRUCTURE, AND SPECTROSCOPIC CHARACTERIZATION OF 5-(1-HYDROXYCYCLOHEXYLTHIO)-1,3,4-THIADIAZOLE-2-THIONE

被引：8

作者：

ANTOLINI, L ^{[1
]}

CORNIA, A ^{[1
]}

FABRETTI, AC ^{[1
]}

SCHENETTI, L ^{[1
]}

机构：

[1] UNIV MODENA,DIPARTIMENTO CHIM,VIA G CAMPI,I-41100 MODENA,ITALY

来源：

JOURNAL OF THE CHEMICAL SOCIETY-PERKIN TRANSACTIONS 2 | 1993年 / 03期

关键词：

D O I：

10.1039/p29930000417

中图分类号：

O62 [有机化学];

学科分类号：

070303 ; 081704 ;

摘要：

2,5-Dimercapto-1,3,4-thiadiazole (DMTDA), when dissolved in cyclohexanone, interacts strongly with the solvent and the title monothiohemiacetal (MTH) is formed. MTH has been characterized in the solid state by means of X-ray diffraction, IR spectroscopy and thermogravimetric analysis, and in cyclohexanone solution by means of NMR spectroscopy. The title compound crystallizes in the triclinic space group P1- (No. 2), with cell dimensions a = 6.481 (1), b = 9.322(l), c = 9.553(l) angstrom, alpha = 72.31 (1), beta = 89.74(1), gamma = 80.83(1)-degrees and Z = 2. The structure was solved by direct methods and least-squares refinement of structural parameters led to a conventional R factor of 0.041 for 1074 independent reflections. In the solid state, MTH easily undergoes decomposition with loss of cyclohexanone.

引用

页码：417 / 420

页数：4

共 46 条

[1] TABLES OF BOND LENGTHS DETERMINED BY X-RAY AND NEUTRON-DIFFRACTION .1. BOND LENGTHS IN ORGANIC-COMPOUNDS [J].

ALLEN, FH ;

KENNARD, O ;

WATSON, DG ;

BRAMMER, L ;

ORPEN, AG ;

TAYLOR, R .

JOURNAL OF THE CHEMICAL SOCIETY-PERKIN TRANSACTIONS 2, 1987, (12) :S1-S19

[2] SYNTHESIS, CRYSTAL AND MOLECULAR-STRUCTURE, AND MAGNETIC-PROPERTIES OF BIS[TRIS(MU-3,5-DIAMINO-1,2,4-TRIAZOLE-N1,N2)TRIS(THIOCYANATO-N)NICKEL(II)]NICKEL(II) HEXAHYDRATE [J].

ANTOLINI, L ;

FABRETTI, AC ;

GATTESCHI, D ;

GIUSTI, A ;

SESSOLI, R .

INORGANIC CHEMISTRY, 1990, 29 (01) :143-145

[3] MICROWAVE SPECTRA OF ISOTOPIC 1,3,4-THIADIAZOLES . MOLECULAR STRUCTURE OF 1,3,4-THIADIAZOLE [J].

BAK, B ;

NYGAARD, L ;

PEDERSEN, EJ ;

RASTRUPA.J .

JOURNAL OF MOLECULAR SPECTROSCOPY, 1966, 19 (03) :283-&

[4]

BATS JW, 1976, ACTA CRYSTALLOGR B, V23, P2866

[5] PREPARATION, CHARACTERIZATION, AND STRUCTURAL ASPECTS OF TRANSITION-METAL COMPLEXES WITH 4,7,10-TRIOXA-1,13-DITHIA[13](2,5)-1,3,4-THIADIAZOLOPHANE [J].

BONOMO, R ;

BOTTINO, F ;

FRONCZEK, FR ;

MAMO, A ;

PAPPALARDO, S .

INORGANIC CHEMISTRY, 1989, 28 (26) :4593-4598

[6]

BUSEV AI, 1974, J ANAL CHEM-USSR+, V29, P433

[7]

BUSEV AI, 1987, ZH ANAL KHIM, V29, P1134

[8]

CHO SG, 1988, ACTA CRYSTALLOGR C, V44, P769

[9] CRYSTAL AND MOLECULAR STRUCTURE OF 5-AMINO-2-THIOL-1,3,4-THIADIAZOLE [J].

DOWNIE, TC ;

HARRISON, W ;

RAPER, ES .

ACTA CRYSTALLOGRAPHICA SECTION B-STRUCTURAL CRYSTALLOGRAPHY AND CRYSTAL CHEMISTRY, 1972, B 28 (MAY15) :1584-&

[10] SYNTHESIS, CRYSTAL AND MOLECULAR-STRUCTURE AND MAGNETIC-PROPERTIES OF BIS[(MU-HYDROXO)BIS(MU-2,5-DIAMINO-1,3,4-THIADIAZOLE-N-1, N-2-CHLOROAQUA(2,5-DIAMINO-1,3,4-THIADIAZOLE-N-1)COBALT(II)-O,N-1, N-1]-COBALT(II) DICHLORIDE DIHYDRATE [J].

FABRETTI, AC ;

MALAVASI, W ;

GATTESCHI, D ;

SESSOLI, R .

INORGANICA CHIMICA ACTA, 1992, 195 (02) :157-161

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