Korean Journal of Crystallography (한국결정학회지)

Korean Crystallographic Association (한국결정학회)
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Synthesis and Structure Dinitroethylenediamine Palladium(II)

Dinitroethylenediamine Palladium(II)의 합성 및 결정구조 연구

  • Namgung Hae (Department of Bio & Nano-Chemistry, Kookmin University)
  • 남궁해 (국민대학교 자연대학 생명나노화학전공)
  • Published : 2004.12.01
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Abstract

The crystal structure of Dinitroethylenediaminepalladium(II), $Pd(C_2H_8N_2)(NO_2)_2$, has been determined by X-ray crystallography. Crystal data: a=7.425(3), b=8.480(4), c=11.885(2) ${\AA}$, Orthorhombic, $A2_1ma$ (Space Group No=36), Z=4, V=748.3(4) ${\AA}^3,\;D_c=2.295 gcm^{-3},\;{\mu}=2.457mm^{-1}$. The structure was solved by Patterson method and refined by full matrix least-square methods using unit weights. The final R and S values were $R_1=0.0306,\;R_w=0.0802,\;R_{all}=0.0320,\;and\;S=1.166)$ for the observed 377 reflections. Bond lengths and angles of palladium complex are similar to the previously reported data. The complex structure is one dimensional Reiset's salt type analogue showing zigzag chain of Pd-Pd length and angle of 3.762(2) ${\AA}$ and $161.41(5)^{\circ}$. The complex molecules are linked through inter-and intramolecular hydrogen bonds of 3.05(1) and 3.15(1) ${\AA}$ between oxygen and nitrogen.

Dinitroethylenediaminepalladium(II), $Pd(C_2H_8N_2)\;(NO_2)_2$의 결정구조는 a=7.425(3), b=8.480(4), c=11.885(2)${\AA}$, 사방정계(Orthorhombic), 공간군 $A2_1ma$, 공간군 번호 36이며, Z=4, V=748.3(4)${\AA}^3,\;D_c=2.295\;gcm^{-3},\;{\mu}=2.457mm^{-1}$이었다. 구조분석은 중금속법으로 풀었으며, 최소 자승법으로 정밀화하였고, 최종 신뢰도 값들은 377개의 회절반점에 대하여 $(R_1=0.0306,\;R_w=0.0802,\;R_{all}=0.0320,\;S=1.166)$이었다. 최종 분석한 착염의 결합거리와 각들은 기존에 알려진 해당 자료들에 상응하였다. 착염의 구조는 Reiset's salt type 유사체와 같은 일차원 구조로써 c축을 따라서, Pd-Pd 거리가 3.762(2) $(\AA)$이고, 각 $161.41(5)^{\circ}$인 지그재그 사슬구조를 형성하고 있다. 사슬내에서나 사슬간에는 질소와 산소사이에 각각 3.05(1)과 3.15(1) ${\AA}$인 수소결합으로 연결되어 있다.

Keywords

References

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