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Data for Direct solid state NMR observation of the 105Pd nucleus in inorganic compounds and palladium metal systems
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Hooper, Thomas J. N., Partridge, Thomas A., Rees, Gregory J., Keeble, Dean Samuel, Powell, Nigel A., Smith, Mark E., Mikheenko, Iryna P., Macaskie, Lynne E., Bishop, Peter T. and Hanna, John V. (2018) Data for Direct solid state NMR observation of the 105Pd nucleus in inorganic compounds and palladium metal systems. [Dataset]
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README(Hooper_PCCP c8cp02594k_105Pd data).docx - Supplemental Material Available under License Creative Commons Attribution 4.0. Download (18Kb) |
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Archive (ZIP) (Data files)
Hooper_PCCP_data.zip - Published Version Available under License Creative Commons Attribution 4.0. Download (43Mb) |
Abstract
The ability to clearly relate local structure to function is desirable for many catalytically relevant Pd-containing systems. This report represents the first direct 105Pd solid state NMR measurements of diamagnetic inorganic (K2Pd(IV)Cl6, (NH4)2Pd(IV)Cl6 and K2Pd(IV)Br6) complexes, and micron- and nano-sized Pd metal particles at room temperature, thereby introducing effective 105Pd chemical shift and Knight shift ranges in the solid state. The very large 105Pd quadrupole moment (Q) makes the quadrupole parameters (CQ, ηQ) extremely sensitive to small structural distortions. Despite the well-defined high symmetry octahedral positions describing the immediate Pd coordination environment, 105Pd NMR measurements can detect longer range disorder and anisotropic motion in the interstitial positions. The approach adopted here combines high resolution X-ray pair distribution function (PDF) analyses with 105Pd, 39K and 35Cl MAS NMR, and shows solid state NMR to be a very sensitive probe of short range structural perturbations. Solid state 105Pd NMR observations of ∼44–149 μm Pd sponge, ∼20–150 nm Pd black nanoparticles, highly monodisperse 16 ± 3 nm PVP-stabilised Pd nanoparticles, and highly polydisperse ∼2–1100 nm biomineralized Pd nanoparticles (bio-Pd) on pyrolysed amorphous carbon detect physical differences between these systems based on relative bulk:surface ratios and monodispersity/size homogeneity. This introduces the possibility of utilizing solid state NMR to help elucidate the structure–function properties of commercial Pd-based catalyst systems.
| Item Type: | Dataset | ||||||
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| Subjects: | Q Science > QD Chemistry | ||||||
| Divisions: | Faculty of Science > Physics | ||||||
| Type of Data: | Zip | ||||||
| Library of Congress Subject Headings (LCSH): | Inorganic compounds, Palladium, Magnetic resonance imaging, Nanoparticles, Catalysts | ||||||
| Publisher: | Department of Physics, University of Warwick | ||||||
| Official Date: | 14 September 2018 | ||||||
| Dates: |
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| Date of first compliant deposit: | 14 September 2018 | ||||||
| Status: | Not Peer Reviewed | ||||||
| Publication Status: | Published | ||||||
| Media of Output: | .txt .par .info .png File .temp | ||||||
| Access rights to Published version: | Open Access | ||||||
| Copyright Holders: | University of Warwick | ||||||
| Description: | This data directory contains the raw data files for all the data presented in the Physical Chemistry Chemical Physics manuscript entitled “Direct Solid State NMR Observation of the 105Pd Nucleus in Inorganic Compounds and Palladium Metal Systems“, (manuscript no. c8cp02594k). The directory is seperated into subdirectories with names following the format below: Hooper_PCCP_data\FigX&Y_[type] where FigX&Y denotes that the actual data utliised in Figures X and Y, and [type] provides further information about the type of data that it represents. Each subdirectory is then separated into folders denoting the material system that the data was investigating with folders named with the following shorthand convention for each sample: e.g. K2PdBr6 = K2PdBr6(s), PVPstabPd = PVP stabilised Pd nanoparticles, etc. All MAS and static NMR data (Fig1&2&SI1&SI2_105PdNMR_complexes; Fig3_39KNMR; Fig4_35ClNMR; Fig6&SI3_105PdNMR_metals) is initially categorised by seperating into folders representing the magnetic field strength at which the data was acquired (i.e. either 7.05T, 9.40T, 11.7T, 14.1T or 20.0T). These MAS and static NMR data are predominantly in the form of raw Bruker TopSpin data folders with some 7.05T data saved as text files (due to aquisition on a Varian-Chemagnetics spectrometer controlled by SPINSIGHT software). For the 105Pd VOCS NMR measurements the raw data of each individual spectrum that contributes to the cumulative/total spectrum has been included. The spectrometer frequency of each spectrum has been appended to the end of the VOCS file names in brackets (i.e. 170125_300(26.63MHz)) to differentiate between them. (N.B. the file names of NMR data begin with the date followed by an arbitrary number X such as YYMMDD_X). The PDF data (Fig5_PDF) is given as a text file and the produced structure is included as a CIF file, while the TEM images (Fig7_TEM) are given as JPG or PNG files. |
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