引用本文:
王科志, 黄春辉, 翁诗甫, 徐光宪, 韩玉真, 贺存恒, 郑启泰. 协萃络合物结构的研究——二(1-苯基 -3-甲基-4-三氟乙酰基吡唑啉酮-5)-(1，10菲啰啉)合钴(II)的合成、表征与晶体结构的测定[J]. 物理化学学报,
1989, 5(01): 20-26.
doi:
10.3866/PKU.WHXB19890106
Citation: Wang Ke-Zhi, Huang Chun-Hui, Weng Shi-Fu, Xu Guang-Xian, Han Yu-Zhen, He Cun-Heng, Zheng Qi-Tai. Study on Synergistic Extracted Complex——The Synthesis, Characterizaton and Crystal Structure of Bis (1-Pnenyl-3-Methyl-4-Trifluoroacetyl-Pyrazolone-5)Mono (1,10-Phenanthroline) Cobalt (II)[J]. Acta Physico-Chimica Sinica, 1989, 5(01): 20-26. doi: 10.3866/PKU.WHXB19890106
Citation: Wang Ke-Zhi, Huang Chun-Hui, Weng Shi-Fu, Xu Guang-Xian, Han Yu-Zhen, He Cun-Heng, Zheng Qi-Tai. Study on Synergistic Extracted Complex——The Synthesis, Characterizaton and Crystal Structure of Bis (1-Pnenyl-3-Methyl-4-Trifluoroacetyl-Pyrazolone-5)Mono (1,10-Phenanthroline) Cobalt (II)[J]. Acta Physico-Chimica Sinica, 1989, 5(01): 20-26. doi: 10.3866/PKU.WHXB19890106
协萃络合物结构的研究——二(1-苯基 -3-甲基-4-三氟乙酰基吡唑啉酮-5)-(1，10菲啰啉)合钴(II)的合成、表征与晶体结构的测定
摘要:
合成了二(1-苯基-3-甲基-4-三氟乙酰基吡唑啉酮-5)-(1,10菲啰啉)合钴(Ⅱ)混合配体络合物单晶, 由元素分析确定其组成为Co(C_(12)H_3F_3O_2N_2)_2·(C_(12)H_8N_2)。通过溶解性、摩尔电导, 磁性、中红外光谱、远红外光谱、差热、热重分析研究了该化合物的有关性质。
用四园单晶衍射仪, 测定了该络合物的分子及晶体结构。晶体属单斜晶系, P2_(l/o)空间群,晶胞参数为:a=1.0422(3) nm, b=1.6462(2) nm, c=2.0678(3) nm, β=75.86(1)°, V=3.4402(1.6) nm, Z=4, F(000)=1580, d_(calc)=1.50 g cm~(-3), d_(exp.)=1.492g cm~(-3)。
经最小二乘法修正后, 最终偏差因子R=0.0716。配合物中钴的配位数为六, 分子中有四个氧来自两个双齿配体PMTFP, 两个氮原子由phen所提供。
English
Study on Synergistic Extracted Complex——The Synthesis, Characterizaton and Crystal Structure of Bis (1-Pnenyl-3-Methyl-4-Trifluoroacetyl-Pyrazolone-5)Mono (1,10-Phenanthroline) Cobalt (II)
Abstract:
A synergistic extracted complex of bis-(1-phenyl-3-methyl-4-trifluoroacetylpyrazolone-5) mono (1,10-phenanthroline) eobalt(Ⅱ) has been synthesized and studied by solubility, conduetometric method, magnetometry, IR, far-IR, thermo analysis as well as single crystal X-ray diffractometry.
The crystal and molecular structure of the complex was determined by single crystal X-ray diffraction analysis and refined by full-matrix least square to a value of R 0.0716. The complex crystallizes in space group P2_1/c with a=1.0422(3) nm, b=1.6462(2) nm, c=2.0678(3) nm, β=75.86(1)°, V=3.4402(1.6) nm, Z=4, F(000)=1580, d_(calc)=1.50 g cm~(-3), d_(exp.)=1.492 g cm~(-3).
The metal atoms occupy general position in crystal. The crystal is composed of mononuclear complexes containing a six-coordinate cobalt (II) ions. Each PMTFP group coordinates to the central ion through two oxygen atoms bidentately. The phen molecule coordinates through its two nitrogen atoms bond lengths are 0.203, 0.204, 0.205, 0.210 nm for cotalt-oxygen, and 0.212 0.216 nm for cotalt-nitrogen.
The crystal and molecular structure of the complex was determined by single crystal X-ray diffraction analysis and refined by full-matrix least square to a value of R 0.0716. The complex crystallizes in space group P2_1/c with a=1.0422(3) nm, b=1.6462(2) nm, c=2.0678(3) nm, β=75.86(1)°, V=3.4402(1.6) nm, Z=4, F(000)=1580, d_(calc)=1.50 g cm~(-3), d_(exp.)=1.492 g cm~(-3).
The metal atoms occupy general position in crystal. The crystal is composed of mononuclear complexes containing a six-coordinate cobalt (II) ions. Each PMTFP group coordinates to the central ion through two oxygen atoms bidentately. The phen molecule coordinates through its two nitrogen atoms bond lengths are 0.203, 0.204, 0.205, 0.210 nm for cotalt-oxygen, and 0.212 0.216 nm for cotalt-nitrogen.
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