The Crystal and Molecular Structure of Piperidinothiosemicarbazide

Piperidinothiosemicarbazide의 結晶 및 分子構造

  • Koo, Chung Hoe (Department of Chemistry, College of Natural Sciences, Seoul National University) ;
  • Kim Hoon Sup (Department of Chemistry, College of Natural Sciences, Seoul National University) ;
  • Chang Chong Hwan (Department of Chemistry, College of Natural Sciences, Seoul National University)
  • 구정회 (서울大學校 自然科學大學 化學科) ;
  • 김훈섭 (서울大學校 自然科學大學 化學科) ;
  • 장종환 (서울大學校 自然科學大學 化學科)
  • Published : 1975.04.30

Abstract

The crystal structure of piperidinothiosemicarbazide, $C_6H_{13}N_3S$, has been determined by single crystal X-ray analysis. The space group is P21/c with four molecules in the unit cell of dimensions $a=14.68{\pm}0.04,\;b=4.59{\pm}0.02,\;c=12.92{\pm}0.04{\AA}\;and\;{\beta}=109.4{\pm}0.2^{\circ}$. Three-dimensional photographic intensities were estimated visually. The structure has been solved by an interpretation of a Patterson synthesis and refined by block-diagonal least-squares methods to give a final R value of 0.14 for 378 observed independent reflections. There are two independent hydrogen bonds in the structure. One of them is of the type N-H${\ldots}$S with the length 3.28 and $3.39{\AA}$, and another is of the type N-H${\ldots}$N with the length $3.03{\AA}$. Apart from the hydrogen bonding system the molecules are held together in the crystal by van der Waals forces.

피페리디노티오세미카르바지드의 결정구조가 X-선을 이용한 단결정 해석에 의하여 해명되었다. 공간군은 $P2_1/c$이며 단위세포는 4분자를 포함하고 있고, 단위세포는 4분자를 포함하고 있고, 세포상수는 $a=14.68{\pm}0.04,\;b=4.59{\pm}0.02,\;c=12.92{\pm}0.04{\AA},\;{\beta}=109.4{\pm}0.2^{\circ}$이다. 3차원적인 회절반점의 강도는 목측에 의하여 얻었다. 결정구조는 패터슨 함수의 해석으로 밝혔고, 원자좌표치는 최소자승법으로 정밀화하였으며 378개의 독립적인 회절반점에 대한 최종 R값은 0.14이었다. 수소결합에는 $N-H{\cdot}{\cdot}{\cdot}S$ 형과 $N-H{\ldots}N$형의 두종류가 있다. $N-H{\ldots}S$형의 길이는 3.28 및 $3.39{\AA}$이고, $N-H{\ldots}N$형의 길이는 $3.03{\AA}$이다. 수소결합외의 분자들을 연결하는 힘은 van der Wasls힘이다.

Keywords

References

  1. J. Korean Chem. Soc. v.17 C. H. Koo;H. S. Kim;H. S. Shin;Y. Lee
  2. Nature v.150 A. J. C. Wilson
  3. Computing Methods and the Phase Problem in X-ray Crystal Structure Analysis D. W. J. Cruickshank
  4. International Table for X-ray Crystallography v.III
  5. IBM 1130 Data Reduction Program, Technical Reports R. Shiono
  6. IBM 1130 Least Squares Program, Technical Report R. Shiono
  7. Acta. Cryst. v.B26 R. Restivo;G. J. Palenik
  8. Acta Cryst. v.B25 E. J. Gabe;M. R. Taylor;J. P. Glusker;J. A. Minkin;A. L. Patterson
  9. Acta Cryst. v.B25 P. Domiano;G. F. Gasparri;M. Nardelli;P. Sgarabotto
  10. Acta Cryst. v.B29 R. E. Wagner;W. Jensen;W. Wadsworth;Q. Johnson