Data for Manuscript
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Data for manuscript "“Postsynthetic Bromination of UiO-66 Analogues: Altering Linker Flexibility and Mechanical Compliance”

Dalton Transactions, 2016

Authors:

Ross J. Marshall, Tom Richards, Claire Hobday, Colin F. Murphie, Claire Wilson, Stephen A. Moggach, Thomas D. Bennett, and Ross S. Forgan

Experimental data in Origin format, Bruker NMR format. Data can be accessed by Bruker TopSpin v3.2 NMR software (NMR data) or by OriginPro v8.5 (all other data).

Funded by EPSRC grant EP/L004461/1

CCDC 1418959-1418961 contain the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.

Data available

NMR spectra, Thermogravimetric analysis, powder X-ray diffraction, nanoindentation and nitrogen adsorption.


The data comprise experimental synthesis and characterisation of two porous materials, and their subsequent transformation by addition of bromine. The data also include the effect this modification of the material has on the mechanical properties, specifically the elastic modulus.

 
Data Collection Protocols:

All chemicals and solvents were purchased from Alfa Aesar, Fisher Scientific, Fluorochem, Merck, Sigma-Aldrich, Strem Chemicals and VWR and used without further purification.

Microwave Synthesis: Microwave reactions were carried out in 35 ml pressure vials using a CEM Discover SP microwave, equipped with an Explorer 12 Hybrid autosampler. The power was allowed to fluctuate to maintain a constant temperature of 100 °C throughout the course of the reaction. (University of Glasgow)

Powder X-ray Diffraction (PXRD): PXRD measurements were carried out at 298 K using a PANalytical X’Pert PRO diffractometer (λ (CuKα) = 1.4505 Å) on a mounted bracket sample stage. Data were collected over the range 3 – 45 °. PXRD patterns were calculated from single crystal data using Mercury 3.5.1.S1 (University of Glasgow) 

Single Crystal Diffraction (SCXRD): Data for (2) were collected on a Bruker Apex II (λ (MoKα = 0.71073 Å) diffractometer (University of Edinburgh). Data for (etdb-Me2) were collected on a Bruker Apex II (λ (MoKα = 0.71073 Å) diffractometer equipped with an Oxford Cryosystems n-Helix device (University of Glasgow). Data for (2-Br2) were collected using a Rigaku AFC12 goniometer equipped with an enhanced sensitivity (HG) Saturn724+ detector mounted at the window of an FR-E+ SuperBright molybdenum rotating anode generator with VHF Varimax optics (70 µm focus) equipped with an Oxford Cryosystems cryostream device. (EPSRC UK National Crystallography Service)

Thermal Gravimetric Analysis (TGA): Measurements were carried out using a TA Instruments Q500 Thermogravimetric Analyser. Measurements were collected from room temperature to 1000 °C with a heating rate of 10 °C / min under an N2 atmosphere. (University of Glasgow)

Nuclear Magnetic Resonance (NMR): NMR spectra were recorded on either a Bruker AVIII 400 MHz spectrometer or a Bruker AVI 500 MHz Spectrometer and referenced to residual solvent peaks. (University of Glasgow)

Gas Uptake: N2 adsorption isotherms were carried out at 77 K on a Quantachrome Autosorb iQ gas sorption analyser. Samples were degassed under vacuum at 120 °C for 20 h using the internal turbo pump. BET surface areas were calculated using the Micropore BET Assistant and pore size distribution analysis was carried out using QSDFT (N2 on carbon at 77 K, slit/cylindrical pore model) both implemented in the Quantachrome ASiQwin operating software. (University of Glasgow)

Nanoindentation: Nanoindentation was performed under ambient conditions using an MTS Nanoindenter XP. Samples were mounted in an epoxy resin and polished using increasingly fine diamond suspensions. (University of Cambridge)