bis(2,6-di-t-butyl-4-methylphenoxo)bis(diethylether)ytterbium(II) | 124206-22-0

• 分子结构分类: 有机化合物 - 苯类化合物 - 苯和取代衍生物
• 英文名称: bis(2,6-di-t-butyl-4-methylphenoxo)bis(diethylether)ytterbium(II)
• 英文别名: 2,6-ditert-butyl-4-methylphenolate;ethoxyethane;ytterbium(2+)
• CAS: 124206-22-0
• 化学式: C₃₈H₆₆O₄Yb
• 分子量: 759.98
• InChiKey: TWDWDOZXPDUPFP-UHFFFAOYSA-L

计算性质

• 辛醇/水分配系数(LogP)：
  None
• 重原子数：
  None
• 可旋转键数：
  None
• 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：

  bis(2,6-di-t-butyl-4-methylphenoxo)bis(diethylether)ytterbium(II) 在 tetrahydrofuran 作用下， 以 正己烷 为溶剂， 以79%的产率得到
  参考文献：
  名称：

  Synthesis and¹⁷¹Yb-{¹H} nuclear magnetic resonance spectra of ytterbium(II) aryloxides [Yb(OR′)₂(L)_n][(L)_n=(OEt₂)₂, (thf)₂, (thf)₃, (pyridine)₂or Me₂PCH₂CH₂PMe₂] and [{Yb(µ-OR′)(X)}₂](X = OR′ or NR₂)(R′= C₆H₂Bu^t₂-2,6-Me-4, R = SiMe₃, thf = tetrahydrofuran)

  摘要：

  Crystalline homo- and hetero-leptic ytterbium(II) aryloxides derived from bulky 2,6-di-tert-bityl-4-methylphenol (R'OH) were prepared as follows: (a) [Yb(OR')(2)(OEt(2))(2)] 1 from 2 R'OH and [Yb(NR(2))(2)(OEt(2))(2)] I (R = SiMe(3)); (b) [{Yb(OR')(mu-OR')}(2)] 2 by desolvating 1 or from [{Yb(NR(2))(mu-NR(2))}(2)] II and 4 R'OH; and (c) [{Yb(NR(2))(mu-OR')}(2)] 3 from II and 2 R'OH or II and 2. Single-crystal X-ray diffraction studies established complex 1 to be monomeric with a distorted tetrahedral configuration and 2 to be dimeric with asymmetrically bridging -OR' ligands. Complexes 1-3 were characterised by multinuclear (H-1,C-13, Si-29 and Yb-171) NMR spectroscopy and elemental (C, H, N) analysis. Variable-temperature H-1 and C-13 NMR spectral data for 2 led to Delta G(double dagger) for the terminal/bridge -OR' site-exchange process. The known aryloxide [Yb(OR')(2)(thf)(3)] 4 was obtained from 1 and an excess of tetrahydrofuran (thf); reacting 1 with the appropriate stoichiometric amount of thf, pyridine (py) or 1.2-bis(dimethylphosphino) ethane (dmpe) yielded [Yb(OR')(2)(thf)(2)] 5, [Yb(OR')(2)(py)(2)] 6 or [Yb(OR')(2)(dmpe)] 7, respectively. The delta [Yb-171-{H-1}] NMR spectral data for complexes 4-7 showed that displacement of diethyl ether from 1 (delta 238 at 193 K) by another neutral coligand had a marked effect on the magnitude of the chemical shift, ranging from delta 286 at 233 K for 4 to delta 999 at 296 K for 7.

  DOI：

  10.1039/dt9950001435
• 作为产物：
  描述：

  、 2,6-二叔丁基-4-甲基苯酚 以 乙醚 为溶剂， 以67%的产率得到bis(2,6-di-t-butyl-4-methylphenoxo)bis(diethylether)ytterbium(II)
  参考文献：
  名称：

  Synthesis and¹⁷¹Yb-{¹H} nuclear magnetic resonance spectra of ytterbium(II) aryloxides [Yb(OR′)₂(L)_n][(L)_n=(OEt₂)₂, (thf)₂, (thf)₃, (pyridine)₂or Me₂PCH₂CH₂PMe₂] and [{Yb(µ-OR′)(X)}₂](X = OR′ or NR₂)(R′= C₆H₂Bu^t₂-2,6-Me-4, R = SiMe₃, thf = tetrahydrofuran)

  摘要：

  Crystalline homo- and hetero-leptic ytterbium(II) aryloxides derived from bulky 2,6-di-tert-bityl-4-methylphenol (R'OH) were prepared as follows: (a) [Yb(OR')(2)(OEt(2))(2)] 1 from 2 R'OH and [Yb(NR(2))(2)(OEt(2))(2)] I (R = SiMe(3)); (b) [{Yb(OR')(mu-OR')}(2)] 2 by desolvating 1 or from [{Yb(NR(2))(mu-NR(2))}(2)] II and 4 R'OH; and (c) [{Yb(NR(2))(mu-OR')}(2)] 3 from II and 2 R'OH or II and 2. Single-crystal X-ray diffraction studies established complex 1 to be monomeric with a distorted tetrahedral configuration and 2 to be dimeric with asymmetrically bridging -OR' ligands. Complexes 1-3 were characterised by multinuclear (H-1,C-13, Si-29 and Yb-171) NMR spectroscopy and elemental (C, H, N) analysis. Variable-temperature H-1 and C-13 NMR spectral data for 2 led to Delta G(double dagger) for the terminal/bridge -OR' site-exchange process. The known aryloxide [Yb(OR')(2)(thf)(3)] 4 was obtained from 1 and an excess of tetrahydrofuran (thf); reacting 1 with the appropriate stoichiometric amount of thf, pyridine (py) or 1.2-bis(dimethylphosphino) ethane (dmpe) yielded [Yb(OR')(2)(thf)(2)] 5, [Yb(OR')(2)(py)(2)] 6 or [Yb(OR')(2)(dmpe)] 7, respectively. The delta [Yb-171-{H-1}] NMR spectral data for complexes 4-7 showed that displacement of diethyl ether from 1 (delta 238 at 193 K) by another neutral coligand had a marked effect on the magnitude of the chemical shift, ranging from delta 286 at 233 K for 4 to delta 999 at 296 K for 7.

  DOI：

  10.1039/dt9950001435

文献信息

• Four-and five-co-ordinate lanthanide (<scp>II</scp>) aryloxides: X-ray structures of the bis(2,6-di-t-butyl-4-methylphenoxo)ytterbium(<scp>II</scp>) complexes [Yb(OAr)₂(L)₂] and [Yb(OAr)₂(L′)₃][ArC₆H₂Bu^t₂-2,6-Me-4, L = tetrahydrofuran (thf) or OEt₂, L′= thf]
  作者：Glen B. Deacon、Peter B. Hitchcock、Stephen A. Holmes、Michael F. Lappert、Peter MacKinnon、Russell H. Newnham

  DOI：10.1039/c39890000935

  日期：——
• Synthesis and characterisation of lanthanide(<scp>II</scp>) aryloxides including the first structurally characterised europium(<scp>II</scp>) compound [Eu(OC₆H₂Bu^t₂-2,6-Me-4)₂(thf)₃]·thf (thf = tetrahydrofuran)
  作者：Johannes R. van den Hende、Peter B. Hitchcock、Stephen A. Holmes、Michael F. Lappert、Wing-Por Leung、Thomas C. W. Mak、Sanjiv Prashar

  DOI：10.1039/dt9950001427

  日期：——

  The lanthanide(II) aryloxide complexes [Yb(OC(6)H(2)Bu(2)(t)-2,6-Me-4)(2)(OEt(2))(2)] 1, [Yb(OC(6)H(3)Bu(2)(t)- 2,6)(2)(thf)(3)] 2, [Yb(OC(6)H(2)Bu(3)(t)-2,4,6)(2)(thf)(3)] 3, [Sm(OC(6)H(2)Bu(2)(t)-2,6-Me-4)(2)(thf)(3)] 4, [Eu(OC(6)H(2)Bu(2)(t)- 2,6-Me-4)(2)(thf)(3)].thf 5, [Yb(OC(6)H(2)Bu(2)(t)-2,6-Me-4)(2)(thf)(3)] 6 and [Yb(OC(6)H(2)Bu(2)(t)-2,6-Me-4)l(thf)(x)] 7 (thf = tetrahydrofuran) have been synthesized. Each of the complexes 1-3 was prepared by the reaction of 2 equivalents of the appropriate potassium aryloxide with Ybl(2) in diethyl ether (1) or thf (2 or 3). Complexes 4-6 were prepared by the reaction of 2 equivalents of K(OC(6)H(2)Bu(2)(t)-2,6-Me-4) with Lnl(2)(thf)(2) (Ln = Sm, Eu or Yb) in thf. Reacting Ybl(2) with 1 equivalent of K(OC(6)H(2)Bu(2)(t)-2,6-Me-4) in thf yielded complex 7 as the main product, but Yb-171-H-1} NMR spectroscopy showed that 6 and [Ybl(2)(thf)(4)] 8 were also formed. The crystal structure of complex 5 reveals that it adopts a distorted trigonal-bipyramidal conformation with (i) apical thf oxygens [O(4)-Eu-O(5) 178.6(2)degrees, Eu-O(4) 2.590(5) and Eu-O(5) 2:573(5) Angstrom]; (ii) the equatorial O(1), O(2) and O(3) thf coplanar; and (iii) Eu-O(1) 2.321(5), Eu-O(2) 2.337(5) and Eu-O(3) 2.515(6) Angstrom. The crystal structure of complex 8 showed there to be an octahedral arrangement around the metal, the molecule lying on a crystallographic inversion centre, with angles l-Yb-O(1) 90.1(2), l-Yb-O(2) 91.4(2) and O(1)-Yb-O(2) 88.9(3)degrees, and bond lengths Yb-l 3.103(1). Yb-O(1) 2.399(9) and Yb-O(2) 2.373(8) Angstrom.