Abstract
A family of NaY zeolite-supported iridium clusters was prepared by reductive carbonylation of Ir(CO)2(acac) sorbed in the zeolite pores to form Ir6(CO)16, which was decarbonylated by treatment in He. This method allowed preparation of samples with Ir contents as high as 33.0 wt.%. Extended X-ray absorption fine structure spectra of the decarbonylated samples indicate that the clusters are well approximated as octahedral Ir6 in the zeolite cages. The high loadings of clusters in the zeolite allowed characterization of the hydride ligands on the clusters by 1H NMR spectroscopy and inelastic neutron scattering spectroscopy. These ligands exist on the clusters even in the absence of H2 in the gas phase, presumably equilibrated with OH groups on the zeolite. The data indicate both terminal and bridging hydride ligands on the clusters. The H/Ir atomic ratio is estimated to be approximately 0.01 on the basis of the 1H NMR data and thermogravimetric analysis of the sample.
Original language | English |
---|---|
Pages (from-to) | 1553-1568 |
Number of pages | 16 |
Journal | Zeitschrift fur Physikalische Chemie |
Volume | 220 |
Issue number | 12 |
DOIs | |
State | Published - 2006 |
Externally published | Yes |
Funding
This research was supported by the U.S. Department of Energy, Office of Energy Research, Office of Basic Energy Sciences, Division of Chemical Sci- ences, Contract FG02-87ER13790 (FL, BCG) and FG02-04ER15600 (BCG, JE). We acknowledge the Stanford Synchrotron Radiation Laboratory (SSRL), which is operated by Stanford University for the U.S. Department of Energy, Office of Basic Energy Science, for access to time on beam line 4-1B. The X-ray absorption data were analysed with the software XDAP [19].
Funders | Funder number |
---|---|
Division of Chemical Sci- ences | FG02-04ER15600, FG02-87ER13790 |
Office of Basic Energy Sciences | |
Office of Energy Research | |
U.S. Department of Energy |
Keywords
- EXAFS spectroscopy
- H NMR spectroscopy
- IINS spectroscopy
- Iridium
- Supported iridium clusters
- Zeolite NaY