Polyhydrido Copper Nanoclusters with a Hollow Icosahedral Core: [Cu30H18{E2P(OR)2}12] (E=S or Se; R=nPr, iPr or iBu)
Abstract
Although atomically precise polyhydrido copper nanoclusters are of prime interest for a variety of applications, they have so far remained scarce. Here, we describe the synthesis of a dithiophosphate-protected copper(I) hydride-rich nanocluster (NC), [Cu30H18{S2P(OnPr)2}12] (1H), fully characterized by various spectroscopic methods and single-crystal X-ray diffraction. The X-ray structure of 1H reveals an unprecedented central Cu12 hollow icosahedron. Six faces of this icosahedron are capped by Cu3 triangles, the whole Cu30 core being wrapped by twelve dithiophosphate ligands and the whole cluster has ideal S6 symmetry. The locations of the 18 hydrides in 1H were ascertained by a single-crystal neutron diffraction study. They are composed of three types: capping μ3-H, interstitial μ4-H (seesaw) and μ5-H ligands (square pyramidal), in good agreement with the DFT simulations. The numbers of hydrides and ligand resonances in the 1H NMR spectrum of 1H are in line with their coordination environment in the solid state, retaining the S6 symmetry in solution. Furthermore, two new Se-protected polyhydrido copper nanoclusters, [Cu30H18{Se2P(OR)2}12] (2H: R=iPr 3H: R=iBu) were synthesized from their sulfur relative 1H via ligand displacement reaction and their X-ray structures feature the exceptional case where both the NC shape and size are fully conserved during the course ofmore »
- Authors:
-
[2];
[1]
- National Dong Hwa University, Hualien (Taiwan)
- Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
- Univ. Rennes (France)
- Publication Date:
- Research Org.:
- Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source (SNS)
- Sponsoring Org.:
- USDOE Office of Science (SC), Basic Energy Sciences (BES); Taiwan Ministry of Science and Technology (MOST); French National Research Agency (ANR)
- OSTI Identifier:
- 1783008
- Grant/Contract Number:
- AC05-00OR22725; 106-2113-M-259-010; 108- 2923-M-259-001; x2016-087367
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Chemistry - A European Journal
- Additional Journal Information:
- Journal Volume: 26; Journal Issue: 46; Journal ID: ISSN 0947-6539
- Publisher:
- ChemPubSoc Europe
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; copper; hydride; nanocluster; hollow icosahedron; neutron diffraction; ligand exchange; palladium
Citation Formats
Barik, Subrat Kumar, Huo, Shou‐Chih, Wu, Chun‐Yen, Chiu, Tzu‐Hao, Liao, Jian‐Hong, Wang, Xiaoping, Kahlal, Samia, Saillard, Jean‐Yves, and Liu, C. W. Polyhydrido Copper Nanoclusters with a Hollow Icosahedral Core: [Cu30H18{E2P(OR)2}12] (E=S or Se; R=nPr, iPr or iBu). United States: N. p., 2020.
Web. doi:10.1002/chem.202001449.
Barik, Subrat Kumar, Huo, Shou‐Chih, Wu, Chun‐Yen, Chiu, Tzu‐Hao, Liao, Jian‐Hong, Wang, Xiaoping, Kahlal, Samia, Saillard, Jean‐Yves, & Liu, C. W. Polyhydrido Copper Nanoclusters with a Hollow Icosahedral Core: [Cu30H18{E2P(OR)2}12] (E=S or Se; R=nPr, iPr or iBu). United States. https://doi.org/10.1002/chem.202001449
Barik, Subrat Kumar, Huo, Shou‐Chih, Wu, Chun‐Yen, Chiu, Tzu‐Hao, Liao, Jian‐Hong, Wang, Xiaoping, Kahlal, Samia, Saillard, Jean‐Yves, and Liu, C. W. Thu .
"Polyhydrido Copper Nanoclusters with a Hollow Icosahedral Core: [Cu30H18{E2P(OR)2}12] (E=S or Se; R=nPr, iPr or iBu)". United States. https://doi.org/10.1002/chem.202001449. https://www.osti.gov/servlets/purl/1783008.
@article{osti_1783008,
title = {Polyhydrido Copper Nanoclusters with a Hollow Icosahedral Core: [Cu30H18{E2P(OR)2}12] (E=S or Se; R=nPr, iPr or iBu)},
author = {Barik, Subrat Kumar and Huo, Shou‐Chih and Wu, Chun‐Yen and Chiu, Tzu‐Hao and Liao, Jian‐Hong and Wang, Xiaoping and Kahlal, Samia and Saillard, Jean‐Yves and Liu, C. W.},
abstractNote = {Although atomically precise polyhydrido copper nanoclusters are of prime interest for a variety of applications, they have so far remained scarce. Here, we describe the synthesis of a dithiophosphate-protected copper(I) hydride-rich nanocluster (NC), [Cu30H18{S2P(OnPr)2}12] (1H), fully characterized by various spectroscopic methods and single-crystal X-ray diffraction. The X-ray structure of 1H reveals an unprecedented central Cu12 hollow icosahedron. Six faces of this icosahedron are capped by Cu3 triangles, the whole Cu30 core being wrapped by twelve dithiophosphate ligands and the whole cluster has ideal S6 symmetry. The locations of the 18 hydrides in 1H were ascertained by a single-crystal neutron diffraction study. They are composed of three types: capping μ3-H, interstitial μ4-H (seesaw) and μ5-H ligands (square pyramidal), in good agreement with the DFT simulations. The numbers of hydrides and ligand resonances in the 1H NMR spectrum of 1H are in line with their coordination environment in the solid state, retaining the S6 symmetry in solution. Furthermore, two new Se-protected polyhydrido copper nanoclusters, [Cu30H18{Se2P(OR)2}12] (2H: R=iPr 3H: R=iBu) were synthesized from their sulfur relative 1H via ligand displacement reaction and their X-ray structures feature the exceptional case where both the NC shape and size are fully conserved during the course of ligand exchange. DFT and TD-DFT calculations allow understanding the bonding and optical properties of clusters 1H–3H. In addition, the reaction of 1H with [Pd(PPh3)2Cl2] in the presence of terminal alkynes led to the formation of new bimetallic Cu–Pd alloy clusters [PdCu14H2{S2P(OnPr)2}6(C≡CR)6] (4: R=Ph; 5: R=C6H4F).},
doi = {10.1002/chem.202001449},
journal = {Chemistry - A European Journal},
number = 46,
volume = 26,
place = {United States},
year = {Thu May 07 00:00:00 EDT 2020},
month = {Thu May 07 00:00:00 EDT 2020}
}
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