pentamethylcyclopentadienyl niobium(V) tetrachloride | 80432-35-5

• 分子结构分类: 有机化合物 - 有机杂环化合物 - 氮杂环化合物
• 英文名称: pentamethylcyclopentadienyl niobium(V) tetrachloride
• 英文别名: Cp'NbCl4；(η(5)-C5Me5)NbCl4
• CAS: 80432-35-5
• 化学式: C₁₀H₁₅Cl₄Nb
• 分子量: 369.948
• InChiKey: PAEWIAUVWKFOGV-UHFFFAOYSA-J

计算性质

• 辛醇/水分配系数(LogP)：
  6.02
• 重原子数：
  15
• 可旋转键数：
  0
• 环数：
  1.0
• sp3杂化的碳原子比例：
  0.5
• 拓扑面积：
  0
• 氢给体数：
  0
• 氢受体数：
  0

反应信息

• 作为反应物：
  描述：

  pentamethylcyclopentadienyl niobium(V) tetrachloride 在 sodium amalgam 作用下， 以 甲苯 为溶剂， 以75%的产率得到
  参考文献：
  名称：

  半三明治铌化合物的还原：（五甲基环戊二烯基）铌（III）的叔膦和羰基衍生物

  摘要：

  The reduction of [Nb(eta5-C5Me5)Cl4], (1), with sodium amalgam permitted the isolation of the trivalent niobium chloride [Nb(eta5-C5Me5)Cl2]2 (2) in high yield. The reduction of 1 in the presence of Me2PCH2CH2PMe2 (dmpe) with 1 equiv of sodium amalgam led to the paramagnetic niobium(IV) derivative [Nb(eta5-C5Me5)Cl3(dmpe)] (3), whereas monomeric and paramagnetic niobium(III) complexes of the type [Nb(eta5-C5Me5)Cl2L2] were obtained by using 2 equiv of the reducing agent in the presence of different phosphine ligands, PMe3 (4), PMe2Ph (5), and Me2PCH2CH2PMe2 (6), or by addition of the ligands to toluene solutions of 2. These niobium(III) complexes reacted with carbon monoxide to give pseudo-octahedral diamagnetic species [Nb(eta5-C5Me5)Cl2(CO)2L], where L = PMe3 (7), PMe2Ph (8), and [Nb(eta5-C5Me5)Cl2(CO) (dmpe)] (9). Complexes 3-5 were characterized by H-1 NMR, EPR, and magnetic measurements at room temperature. The H-1, C-13, and P-31 NMR studies of complex 9 indicated a pseudo-octahedral arrangement with both phosphorus atoms occupying one equatorial position trans to chlorine and one axial position trans to the cyclopentadienyl ring.

  DOI：

  10.1021/om00028a037
• 作为产物：
  描述：

  五氯化铌 、 三甲基(1,2,3,4,5-五甲基环戊二烯基)硅烷 以 甲苯 为溶剂， 以70%的产率得到pentamethylcyclopentadienyl niobium(V) tetrachloride
  参考文献：
  名称：

  铌的新型单和双（二烯）配合物的合成和催化，以及双核 [Nb(.mu.-Cl)(C5H5)(s-cis-butadiene)]2 和单核 Nb(C5H5)的 X 射线结构（顺-顺-2,3-二甲基丁二烯)2

  摘要：

  制备物由滴定 NbCl 4 (C 5 R 5 ) 或 R=H、CH 3 和丁烯-2二基-1,4 镁组成。Les diene coordinats de ces complexes sont le dimethyl-2,3 butadiene, l'isoprene et le butadiene

  DOI：

  10.1021/ja00223a018

文献信息

• Half-sandwich imido complexes of niobium and tantalum
  作者：David N. Williams、Jonathan P. Mitchell、Andrew D. Poole、Ulrich Siemeling、William Clegg、David C. R. Hockless、Paul A. O'Neil、Vernon C. Gibson

  DOI：10.1039/dt9920000739

  日期：——

  [Nb(η-C5R5)Cl4] with NMe(SiMe3)2 in acetonitrile. The sterically hindered alkyl- and aryl-imido analogues [Nb(η-C5H5)(NR)Cl2](R = But1c, or C6H3Pri2-2,6 1d), [Nb(η-C5Me5)(N-C6H3Pri2-2,6)Cl2]1e and the tantalum compound [Ta(η-C5Me5)(N-C6H3Pri2-2,6)Cl2]1f are obtained by treatment of [M(η-C5R5)Cl4] with two equivalents of NHR(SiMe3) in chlorocarbon solvent. Crystal structures of 1a, 1c, 1d and 1f show that these complexes

  半夹心methylimido配合物[铌（η-C 5 - [R 5）（NME）氯2 ]（R = H 1a中，或Me 1B）已经被制备治疗[铌（η-C 5 - [R 5）氯4 ]与NMe（SiMe 3）2在乙腈中的溶液。空间位阻的烷基-和芳基-亚氨基类似物[铌（η-C 5 H ^ 5）（NR）氯2 ]（R =卜吨1c中，或C 6 H ^ 3镨我2 -2,6 1D），[Nb的（η-C 5我5）（NC6 ħ 3镨我2 -2,6）氯2 ] 1E和钽化合物[TA（η-C 5我5）（NC 6 H ^ 3镨我2 -2,6）氯2 ] 1F是通过处理而得到的[M（η-C 5 - [R 5）氯4 ]与NHR两个当量（森3在氯烃溶剂）。1a， 1c， 1d和1f的晶体结构表明这些配合物是单核的，具有准线性的亚氨基配体。金属-氮键的距离范围为1.744（3）至1.780（5）Å，与伪三键一致。化合物1A - 1E与
• Syntheses, Structures, and Reactivities of Heterobimetallic Bridging Dinitrogen Complexes Containing Group 6 and Group 4 or 5 Transition Metals¹
  作者：Hiroshige Ishino、Tatsuya Nagano、Shigeki Kuwata、Youhei Yokobayashi、Youichi Ishii、Masanobu Hidai、Yasushi Mizobe

  DOI：10.1021/om000684j

  日期：2001.1.1

  heterobimetallic dinitrogen complexes containing group 6 and group 4 or 5 transition metals were synthesized by the reaction of the tungsten or molybdenum dinitrogen complexes cis-[W(N2)2(PMe2Ph)4] (1) and trans-[M(N2)2(dppe)2] (2) (M = W, Mo) with group 4 or group 5 compounds such as [CpTiCl3], [Cp2M‘Cl2] (M‘ = Ti, Zr, Hf), or [Cp‘M‘Cl4] (Cp‘ = Cp, Cp*; M‘ = Nb, Ta). Crystallographic studies of the complexes thus

  通过钨或钼二氮配合物顺式-[W（N 2）2（PMe 2 Ph）4 ]（1）和反式- [M（N 2）2（dppe）2 ]（2）（M = W，Mo）与第4组或第5组化合物，例如[CpTiCl 3 ]，[Cp 2 M'Cl 2 ]（M'= Ti， Zr，Hf）或[Cp'M'Cl 4 ]（Cp'= Cp，Cp *; M'= Nb，Ta）。如此获得的复合物的晶体学研究，包括[WCl（PMe2 PH）4（μ-N 2）TiCpCl 2 ]和[WCL（PME 2 PH）4（μ-N 2）NbCpCl 3 ]显示，M-N-N-M”芯基本上是线性的，并且所述N个-N键被认为是为具有2.几个μ-N正规键级2种配合物的配体的甲基在该基团也通过二氮络合物的反应得到4或5族金属中心1和2a中（M = W）与所述甲基络合物[Cp 2 ZrMeCl]，[TaMe 3 Cl 2 ]和[NbMe 2 Cl 3 ]。络合物[WCl（dppe）的反应2（μ-N
• Synthesis and characterization of cyclopentadienyl sulfur niobium complexes
  作者：Manuel Gómez、Cristina Hernández-Prieto、Avelino Martín、Miguel Mena、Cristina Santamaría

  DOI：10.1016/j.jorganchem.2019.06.022

  日期：2019.10

  The trinuclear nature of complex 2 has been established by single crystal X-ray diffraction analysis. Thermal treatment of 2 with SiH3Ph generated the dinuclear niobium(IV) complex [Nb2(η5-C5Me5)2Cl2(μ-S)2] (3) in a quantitative way. Likewise, one-pot syntheses of 3 has been developed from reaction of 1, (Me3Si)2S, and SiH3Ph in toluene. A series of dinuclear sulfide niobium(IV) derivatives [Nb2(η5-C5Me5)2R2(μ-S)2]

  甲三金属硫化物簇[Nb的3（η 5 -C 5我5）3氯3（μ 3 -Cl）（μ-S）3（μ 3 -S）]（2）已经从反应合成[Nb的（η 5 -C 5我5）氯4 ]（1）与（ME 3 Si）的2在4 S：3的比例由SiClMe释放3。配合物2的三核性质已通过单晶X射线衍射分析确定。用SiH热处理23博士所产生的双核铌（IV）配合物[Nb的2（η 5 -C 5我5）2氯2（μ-S）2 ]（3以定量的方式）。同样，由1，（Me 3 Si）2 S和SiH 3 Ph在甲苯中的反应开发了3的一锅合成法。一系列的双核硫化物铌（IV）的衍生物[铌2（η 5 -C 5我5）2 - [R 2（μ-S）2 ]（R =我4，Et 5，CH 2 SiMe 3 6，C 3 H 5 7，CH 2 Ph 8，n Bu 9）可以容易地由3与2当量的相应烷基化试剂的反应获得。的单晶X射线衍射分析6和7在所有情况下表现出反式的取代基的布置。
• Synthesis, Structural Characterisation and Reactivity of New Dinuclear Monocyclopentadienyl Imidoniobium and ‐tantalum Complexes − X‐ray Crystal Structures of [{Nb(η ⁵ ‐C ₅ H ₄ SiMe ₃ )Cl ₂ } ₂ (μ‐1,4‐NC ₆ H ₄ N)], [{Ta(η ⁵ ‐C ₅ Me ₅ )Cl ₂ } ₂ (μ‐1,4‐NC ₆ H ₄ N)] and [{Ta(η ⁵ ‐C ₅ Me ₅ )(CH ₂ SiMe ₃ ) ₂ } ₂ (μ‐1,4‐NC ₆ H ₄ N)]
  作者：Antonio Antiñolo、Iván Dorado、Mariano Fajardo、Andrés Garcés、Isabel López‐Solera、Carmen López‐Mardomingo、Marek M. Kubicki、Antonio Otero、Sanjiv Prashar

  DOI：10.1002/ejic.200300530

  日期：2004.3

  R = Me, i = 3 (13); Cp′ = η5-C5H4SiMe3, M = Nb, R = CH2SiMe3, i = 3 (14); Cp′ = η5-C5H4SiMe3, M = Nb, R = CH2Ph, i = 3 (15); Cp′ = η5-C5Me5, M = Ta, R = Me, i = 4 (16); Cp′ = η5-C5Me5, M = Ta, R = CH2SiMe3, i = 4 (17); Cp′ = η5-C5Me5, M = Ta, R = CH2Ph, i = 4 (18)]. The alkylated complexes with other stoichiometries, [M(Cp′)(Me)(X)}2(μ-1,4-NC6H4N)] [Cp = η5-C5H4SiMe3, M = Nb, X = Cl (19); Cp = η5-C5H4SiMe3

  一系列双核单环戊二烯基亚氨基铌和-钽配合物的制备是通过两种不同的合成路线实现的。二亚胺配合物 [M(Cp')Cl2}2(μ-1,i-NC6H4N)] [Cp' = η5-C5H4SiMe3, M = Nb, i = 4 (1); Cp' = η5-C5H4SiMe3, M = Nb, i = 3 (2); Cp' = η5-C5H4SiMe3, M = Nb, i = 2 (3); Cp' = η5-C5Me5, M = Nb, i = 4 (4); Cp' = η5-C5Me5, M = Nb, i = 3 (5); Cp' = η5-C5H4SiMe3, M = Ta, i = 4 (6); Cp' = η5-C5H4SiMe3, M = Ta, i = 3 (7)] 由一当量的三氯前体 [MCl3}2(μ-1,i-NC6H4N)] (M = Nb, Ta, i = 4, 3 或 2)
• Synthesis, Characterization, and Reactivity of Niobium and Tantalum Complexes Bearing Metal−Nitrogen Bonds. X-ray Molecular Structure of [Nb(C₅H₄SiMe₃){NH(CH₂)₂-η-NH₂}Cl₃] and the Novel Tetranuclear Niobium Oxo Derivative [{Nb(C₅H₄SiMe₃)Cl(μ₂-O)}₄(Cl)₂(μ₃-O)]
  作者：M. Carmen Maestre、Cristina Paniagua、Eberhardt Herdtweck、Marta E. G. Mosquera、Gerardo Jiménez、Tomás Cuenca

  DOI：10.1021/om7002927

  日期：2007.8.1

  three-component mixture, the chlorosilyl-substituted cyclopentadienyl titanium compound [Ti(η5-C5H4SiMe2Cl)Cl3], the corresponding mononuclear amido-amino, [NbCpRNH(CH2)2-η-NH2}Cl3] (CpR = Cp‘, 4a; Cp*, 4b), and the dinuclear imido niobium complexes [NbCpRCl2}2(μ-N(CH2)2-η-N)] (CpR = Cp‘, 5a; Cp*, 5b). In contrast, the analogue tantalum complexes thermally degraded, when CpR = Cp‘ at normal temperature, whereas

  环戊二烯基甲硅烷基酰氨基钛化合物的反应钛[Ti η 5 -C 5 H ^ 4森达2 -η-N（CH 2）2 -η-NH 2 }氯2 ]与第5种族金属的单环戊二烯配合物[MCP ř CL 4 ];（M =铌，钽的CP - [R = C 5 H ^ 4森达3（CP'），C 5我5，得到（CP *））双核配合物[的TiCl 2 η 5 -C 5 H ^ 4森达2 -η-N（CH 2）2 -κ-NH 2 } MCP ř氯4 ]（M =铌中，CP [R = CP ' 2a中; *的CP，2B ; M =钽中，CP [R = CP'，3A ; CP =的CP *，3B） 。化合物2演变在室温下，得到的三组分混合物中，氯甲硅烷取代的环戊二烯钛化合物钛[Ti（η 5 -C 5 H ^ 4森达2 Cl）的氯3 ]，相应的单核酰氨基-氨基，[国家预防腐败局ř NH（CH 2）2 -η-NH 2 }氯3