fac-[Re(CO)3Cl(N-(di(pyridin-2-yl)methylene)benzohydrazide)] | 640274-44-8

• 英文名称: fac-[Re(CO)3Cl(N-(di(pyridin-2-yl)methylene)benzohydrazide)]
• 英文别名: (4,5-diazafluoren-9-one benzoylhydrazone)chlorotricarbonylrhenium(I)；fac-tricarbonylchloro(di-2-pyridylketonebenzoylhydrazone)rhenium(I)；fac-[Re(CO)₃Cl(N-(di(pyridin-2-yl)methylene)benzohydrazide)]；fac-Re(CO)3(di-2-pyridylketone benzoylhydrazone)Cl
• CAS: 640274-44-8
• 化学式: C₂₁H₁₄ClN₄O₄Re
• 分子量: 608.027
• InChiKey: LLXQKNOPGMFAMN-UHFFFAOYSA-M

计算性质

• 辛醇/水分配系数(LogP)：
  None
• 重原子数：
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• 可旋转键数：
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• 环数：
  None
• sp3杂化的碳原子比例：
  None
• 拓扑面积：
  None
• 氢给体数：
  None
• 氢受体数：
  None

反应信息

• 作为反应物：
  描述：

  fac-[Re(CO)3Cl(N-(di(pyridin-2-yl)methylene)benzohydrazide)] 、 N,N-二甲基甲酰胺 以 N,N-二甲基甲酰胺 为溶剂， 生成 fac-tricarbonylchloro(di-2-pyridylketonebenzoylhydrazone)rhenium(I) dimethylformamide solvate
  参考文献：
  名称：

  fac-三羰基氯（二-2-吡啶基酮苯甲酰腙）铼（I）二甲基甲酰胺溶剂化物的X射线晶体学、光谱和分子传感特性

  摘要：

  摘要 分子传感器 fac-[Re(CO)3(dpkbh)Cl]·DMF (1) 其中 DMF=N,N-二甲基甲酰胺和 dpkbh=di-2-pyridylketonebenzoylhydrazone 在无心三斜空间群 P1 中结晶。结构分析显示 (1) 的两个单元与铼在扭曲的八面体几何形状中，羰基位于面位置，平均 C-Re-C 角为 90°，N,N-双齿 dpkbh 形成六元金属环船形中的铼。分子堆积显示 DMF 与 fac-[Re(CO)3(dpkbh)Cl] 的结合以及 (1) 的螺旋链通过氢键网络互锁。DMF 中 fac-[Re(CO)3(dpkbh)Cl] 的光学测量表明，在 440 和 318 nm 处存在两个互锁的电荷转移带，它们对其周围环境的轻微变化高度敏感。随着浓度的降低，440 nm 处的低能量吸收带的强度增加，当浓度增加时观察到相反的情况。DMF 中 fac-[Re(CO)3(dpkbh)Cl]

  DOI：

  10.1016/j.molstruc.2003.12.038
• 作为产物：
  描述：

  五羰基氯铼(I) 、 二-2-吡啶基酮苯甲酰腙 以 甲苯 为溶剂， 以72%的产率得到fac-[Re(CO)3Cl(N-(di(pyridin-2-yl)methylene)benzohydrazide)]
  参考文献：
  名称：

  fac-三羰基氯（二-2-吡啶基酮苯甲酰腙）铼（I）二甲基甲酰胺溶剂化物的X射线晶体学、光谱和分子传感特性

  摘要：

  摘要 分子传感器 fac-[Re(CO)3(dpkbh)Cl]·DMF (1) 其中 DMF=N,N-二甲基甲酰胺和 dpkbh=di-2-pyridylketonebenzoylhydrazone 在无心三斜空间群 P1 中结晶。结构分析显示 (1) 的两个单元与铼在扭曲的八面体几何形状中，羰基位于面位置，平均 C-Re-C 角为 90°，N,N-双齿 dpkbh 形成六元金属环船形中的铼。分子堆积显示 DMF 与 fac-[Re(CO)3(dpkbh)Cl] 的结合以及 (1) 的螺旋链通过氢键网络互锁。DMF 中 fac-[Re(CO)3(dpkbh)Cl] 的光学测量表明，在 440 和 318 nm 处存在两个互锁的电荷转移带，它们对其周围环境的轻微变化高度敏感。随着浓度的降低，440 nm 处的低能量吸收带的强度增加，当浓度增加时观察到相反的情况。DMF 中 fac-[Re(CO)3(dpkbh)Cl]

  DOI：

  10.1016/j.molstruc.2003.12.038

文献信息

• Coordination of Bidentate Aroylhydrazone-Based N,N-Donor Ligands to the fac-[Re(CO)3]+ Core
  作者：Janvier Mukiza、Thomas I. A. Gerber、Eric C. Hosten

  DOI：10.1007/s10870-014-0524-4

  日期：2014.7

  The reaction of the potentially bidentate aroylhydrazone-based N,N-donor ligands N-(di(pyridin-2-yl)-methylene)benzohydrazide (Hdpmb) and 3-((pyridin-2-yl)methyleneamino)-2,3-dihydro-2-(pyridin-2-yl)quinazolin-4-(1H)one (Hppq) with [Re(CO)5Cl] in alcohol led to the isolation of the neutral complexes fac-[Re(CO)3Cl(Hdpmb)] (1) and fac-[Re(CO)3Cl(Hppq)] (2) respectively. Spectroscopic data and the X-ray crystal structures of the complexes are reported. The cell parameters of the complexes are 1: monoclinic, P21/c, a = 13.7393(9) Å, b = 12.0512(8) Å, c = 13.3543(9) Å, β = 107.105(2)°, V = 2113.4(2) Å3, R 1 = 0.0317, wR 2 = 0.0699; and 2.½ ethanol:monoclinic, P21/c, a = 17.607(1) Å, b = 20.826(1) Å, c = 13.5887(8) Å, β = 101.875(2)°, V = 4876.0(5) Å3, R 1 = 0.0228, wR 2 = 0.0503. The reaction of the potentially bidentate aroylhydrazone-based N,N-donor ligands 3-((pyridin-2-yl)methyleneamino)-2,3-dihydro-2-(pyridin-2-yl)quinazolin-4-(1H)one and N-(di(pyridin-2-yl)-methylene)benzohydrazide (NN) with [Re(CO)5Cl] in alcohol led to the isolation of the neutral complexes fac-[Re(CO)3Cl(NN)].

  潜在的双齿芳酰肼基N,N供体配体N-(二(吡啶-2-基)亚甲基)苯甲酰肼(Hdpmb)和3-((吡啶-2-基)亚甲基氨基)-2,3-二氢-2-(吡啶-2-基)喹唑啉-4-(1H)酮(Hppq)与[Re(CO)5Cl]在醇中反应，分别得到了中性配合物fac-[Re(CO)3Cl(Hdpmb)](1)和fac-[Re(CO)3Cl(Hppq)](2)。报道了这些配合物的光谱数据和X射线晶体结构。配合物的晶胞参数为：1.单斜晶系，P21/c，a=13.7393(9) Å，b=12.0512(8) Å，c=13.3543(9) Å，β=107.105(2)°，V=2113.4(2) Å3，R1=0.0317，wR2=0.0699；2.半乙醇:单斜晶系，P21/c，a=17.607(1) Å，b=20.826(1) Å，c=13.5887(8) Å，β=101.875(2)°，V=4876.0(5) Å3，R1=0.0228，wR2=0.0503。具有潜在双齿芳酰肼基N,N供体配体的3-((吡啶-2-基)亚甲基氨基)-2,3-二氢-2-(吡啶-2-基)喹唑啉-4-(1H)酮和N-(二(吡啶-2-基)亚甲基)苯甲酰肼(NN)与[Re(CO)5Cl]在醇中反应，得到了中性配合物fac-[Re(CO)3Cl(NN)]。
• Optical, electrochemical and structural studies of the first rhenium compound of di-2-pyridylketone benzoylhydrazone (dpkbz) fac-Re(CO)3(dpkbh)Cl
  作者：Mohammed Bakir、Ordel Brown

  DOI：10.1016/s0020-1693(03)00324-4

  日期：2003.9

  The reaction between Re(CO)(5)Cl and di-2-pyridylketone benzoylhydrazone (dpkbh) in refluxing toluene gave fac-Re(CO)(3)(dpkbh)Cl in good yield. Spectroscopic and electrochemical measurements on fac-Re(CO)(3)(dpkbh)Cl revealed strong solvent-solute interaction, as manifested by the sensitivity of its reduction potentials and electronic absorption spectra to solvent variations. Spectroscopic and thermo-optical measurements in polar solvents in the presence of NaBH4 and NaBF4, or NaOH and citric acid reveal reversible interconversion between the low- and high-energy electronic states of fac-Re(CO)(3)(dpkbh)Cl at 440 and 318 nm. Electrochemical measurements on fac-Re(CO)(3)(dpkbh)Cl show irreversible redox processes pointing to electrochemical transformations following the first electronic transfer(s). Crystals of fac-Re(CO)(3)(dpkbh)Cl obtained from an acetonitrile solution of fac-Re(CO)(3)(dpkbh)Cl are centric and crystals of fac-Re(CO)(3)(dpkbh)Cl.dmso obtained from a dmso solutions of fac-Re(CO)(3)(dpkbh)Cl are acentric. Structural studies show non-identical twins of fac-Re(CO)(3)(dpkbh)Cl and fac-Re(CO)(3)(dpkbh)Cl dmso with distorted octahedral coordination about rhenium and the conformation about the amide group is syn- in fac-Re(CO)(3)(dpkbh)Cl and anti- in fac-Re(CO)(3)(dpkbh)Cl-dmso. The packing of molecules shows a web of hydrogen bonds that may account for the stability of different conformations observed in the solid state. (C) 2003 Elsevier B.V. All rights reserved.
• Tricarbonyl Rhenium(I) and Technetium(I) Complexes with Hydrazones Derived from 4,5‐Diazafluoren‐9‐one and 1,10‐Phenanthroline‐5,6‐dione
  作者：Paula Barbazán、Adelheid Hagenbach、Elisabeth Oehlke、Ulrich Abram、Rosa Carballo、Sabina Rodríguez‐Hermida、Ezequiel M. Vázquez‐López

  DOI：10.1002/ejic.201000522

  日期：2010.10

  AbstractTricarbonylrhenium(I) and ‐technetium(I) halide (halide = Cl and Br) complexes of ligands derived from 4,5‐diazafluoren‐9‐one (df) and 1,10‐phenanthroline‐5,6‐dione (phen) derivatives of benzoic and 2‐hydroxybenzoic acid hydrazides have been prepared. The complexes have been characterized by elemental analysis, MS, IR, 1H NMR and absorption and emission UV/Vis spectroscopic methods. The metal centres (ReI and TcI) are coordinated through the nitrogen imine atoms and establish five‐membered chelate rings, whereas the hydrazone groups stand uncoordinated. The 1H NMR spectra suggest the same behaviour in solution on the basis of only marginal variations in the chemical shifts of the hydrazine protons.