Extremely bulky β-diketiminate complexes of calcium(II) and ytterbium(II)

Brant Maitland; Andreas Stasch; Cameron Jones

doi:10.1071/CH21283

Extremely bulky β-diketiminate complexes of calcium(II) and ytterbium(II)

Brant Maitland, Andreas Stasch^*, Cameron Jones^*

^*Corresponding author for this work

School of Chemistry

Research output: Contribution to journal › Article › peer-review

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Abstract

The potassium salt of an extremely bulky β-diketiminate, [K(^Ar*Nacnac)] (^Ar*Nacnac = [(^Ar*NCMe)₂CH]-; Ar^* = C₆H₂Me{C(H)Ph₂}₂-4,2,6) was reacted with either CaI₂ or YbI₂(THF)₂, which afforded [(^Ar*Nacnac)MI] (M = Ca or Yb). These are the first examples of structurally characterised, donor solvent free, N-arene substituted β-diketiminato calcium/ytterbium complexes that incorporate a terminal iodide ligand. Reduction of [(^Ar*Nacnac)CaI] with sodium metal gave a complex product mixture, from which a few crystals of the β-diketiminate C-H activated product, [{Ca(μ-^Ar*Nacnac^-H)}₂], were obtained and crystallographically characterised. In an attempt to form a terminal ytterbium hydride compound, treatment of [(^Ar*Nacnac)YbI] with K[HBEt₃] gave a good yield of the contact ion pair compound [(^Ar*Nacnac)Yb(HBEt₃)].

Original language	English
Article number	CH21283
Journal	Australian Journal of Chemistry
Volume	Online Early
Early online date	18 Feb 2022
DOIs	https://doi.org/10.1071/CH21283
Publication status	E-pub ahead of print - 18 Feb 2022

Keywords

β‐diketiminate
Bulky ligand
Calcium
C–H activation
Metal hydrides
Metal–metal bonding
Reduction
Ytterbium

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10.1071/CH21283Licence: CC BY-NC-ND

Maitland_2022_AJC_Bulky_CC
Copyright © 2022 The Author(s) (or their employer(s)). Published by CSIRO Publishing. This is an open access article distributed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International License (CC BY-NC-ND).
Final published version, 0.99 MBLicence: CC BY-NC-ND

CCDC 2118520 - 2118523: Experimental Crystal Structure Determination
Maitland, B. (Creator), Stasch, A. (Creator) & Jones, C. (Creator), Cambridge Crystallographic Data Centre, 2022
DOI: 10.5517/ccdc.csd.cc293hc9, https://dx.doi.org/10.5517/ccdc.csd.cc293hdb and 2 more links, https://dx.doi.org/10.5517/ccdc.csd.cc293hfc, https://dx.doi.org/10.5517/ccdc.csd.cc293hgd (show fewer)
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@article{afd6bf91599c4fa5ad2c6b6a2a29c76e,

title = "Extremely bulky β-diketiminate complexes of calcium(II) and ytterbium(II)",

abstract = "The potassium salt of an extremely bulky β-diketiminate, [K(Ar*Nacnac)] (Ar*Nacnac = [(Ar*NCMe)2CH]-; Ar* = C6H2Me{C(H)Ph2}2-4,2,6) was reacted with either CaI2 or YbI2(THF)2, which afforded [(Ar*Nacnac)MI] (M = Ca or Yb). These are the first examples of structurally characterised, donor solvent free, N-arene substituted β-diketiminato calcium/ytterbium complexes that incorporate a terminal iodide ligand. Reduction of [(Ar*Nacnac)CaI] with sodium metal gave a complex product mixture, from which a few crystals of the β-diketiminate C-H activated product, [{Ca(μ-Ar*Nacnac-H)}2], were obtained and crystallographically characterised. In an attempt to form a terminal ytterbium hydride compound, treatment of [(Ar*Nacnac)YbI] with K[HBEt3] gave a good yield of the contact ion pair compound [(Ar*Nacnac)Yb(HBEt3)]. ",

keywords = "β‐diketiminate, Bulky ligand, Calcium, C–H activation, Metal hydrides, Metal–metal bonding, Reduction, Ytterbium",

author = "Brant Maitland and Andreas Stasch and Cameron Jones",

note = "This research was supported by the Australian Research Council.",

year = "2022",

month = feb,

day = "18",

doi = "10.1071/CH21283",

language = "English",

volume = "Online Early",

journal = "Australian Journal of Chemistry",

issn = "0004-9425",

publisher = "CSIRO",

}

TY - JOUR

T1 - Extremely bulky β-diketiminate complexes of calcium(II) and ytterbium(II)

AU - Maitland, Brant

AU - Stasch, Andreas

AU - Jones, Cameron

N1 - This research was supported by the Australian Research Council.

PY - 2022/2/18

Y1 - 2022/2/18

N2 - The potassium salt of an extremely bulky β-diketiminate, [K(Ar*Nacnac)] (Ar*Nacnac = [(Ar*NCMe)2CH]-; Ar* = C6H2Me{C(H)Ph2}2-4,2,6) was reacted with either CaI2 or YbI2(THF)2, which afforded [(Ar*Nacnac)MI] (M = Ca or Yb). These are the first examples of structurally characterised, donor solvent free, N-arene substituted β-diketiminato calcium/ytterbium complexes that incorporate a terminal iodide ligand. Reduction of [(Ar*Nacnac)CaI] with sodium metal gave a complex product mixture, from which a few crystals of the β-diketiminate C-H activated product, [{Ca(μ-Ar*Nacnac-H)}2], were obtained and crystallographically characterised. In an attempt to form a terminal ytterbium hydride compound, treatment of [(Ar*Nacnac)YbI] with K[HBEt3] gave a good yield of the contact ion pair compound [(Ar*Nacnac)Yb(HBEt3)].

AB - The potassium salt of an extremely bulky β-diketiminate, [K(Ar*Nacnac)] (Ar*Nacnac = [(Ar*NCMe)2CH]-; Ar* = C6H2Me{C(H)Ph2}2-4,2,6) was reacted with either CaI2 or YbI2(THF)2, which afforded [(Ar*Nacnac)MI] (M = Ca or Yb). These are the first examples of structurally characterised, donor solvent free, N-arene substituted β-diketiminato calcium/ytterbium complexes that incorporate a terminal iodide ligand. Reduction of [(Ar*Nacnac)CaI] with sodium metal gave a complex product mixture, from which a few crystals of the β-diketiminate C-H activated product, [{Ca(μ-Ar*Nacnac-H)}2], were obtained and crystallographically characterised. In an attempt to form a terminal ytterbium hydride compound, treatment of [(Ar*Nacnac)YbI] with K[HBEt3] gave a good yield of the contact ion pair compound [(Ar*Nacnac)Yb(HBEt3)].

KW - β‐diketiminate

KW - Bulky ligand

KW - Calcium

KW - C–H activation

KW - Metal hydrides

KW - Metal–metal bonding

KW - Reduction

KW - Ytterbium

U2 - 10.1071/CH21283

DO - 10.1071/CH21283

M3 - Article

SN - 0004-9425

VL - Online Early

JO - Australian Journal of Chemistry

JF - Australian Journal of Chemistry

M1 - CH21283

ER -

Extremely bulky β-diketiminate complexes of calcium(II) and ytterbium(II)

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CCDC 2118520 - 2118523: Experimental Crystal Structure Determination

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