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Techniques

Overview

We are a synthetic inorganic chemistry group with an interest in a broad range of research topics (rigid ligands in f-element chemistry, Lewis acid appended transition metal complexes, and ALD-focused research). Students in the group are therefore exposed (through their own research or the research of others in the group) to various aspects of ligand design/synthesis and actinide, lanthanide, transition metal and main group chemistry.The majority of this work is highly air sensitive, so the laboratory is set up to handle complexes at the extreme of air sensitivity.

Complexes prepared in the group are investigated using a array of techniques. NMR spectroscopy, single crystal X-ray crystallography and elemental analysis are used in almost all cases. Powder X-ray diffraction, cyclic voltammetry (CV), NIR, IR and UV-Visible spectroscopy, and DFT calculations are also used routinely, where applicable. A more complete list of techniques (with more details) is provided below:

Synthesis
Vacuum line techniques for air-sensitive inorganic synthesis.
Glove box techniques for handling air sensitive complexes. 
For information on some specialized glove box applications, see here.
Organic synthesis (ligand and reagent synthesis, catalysis).

Crystallography
Single crystal X-ray crystallography (most graduate students learn to mount their own crystals and solve their own structures)

PXRD (powder X-ray diffraction) 

Spectroscopy and Analytical Techniques
NMR spectroscopy: Multinuclear (
1H, 2H, 11B, 13C, 19F, 29Si, 31P, 195Pt etc.), VT, and 2D (COSY, HSQC, HMBC, ROSY, EXSY).
EPR spectroscopy (for selected paramagnetic compounds; currently only available via collaboration).

Magnetic measurements: (a) SQUID magnetometry in the McMaster Cryogenic Characterization Facility of the BIMR at McMaster, and (b)xEvans solution magnetic measurements. 
UV-Visiblenear-IRIR spectroscopy.

Solution Electrochemistry (primarily cyclic voltammetry) conducted under inert-atmosphere conditions.

Thin Film Deposition
Atomic Layer Deposition (ALD): our home-built ALD reactor was completed in 2016.

Chemical Vapor Deposition (CVD):xthe ALD reactor can carry out CVD reactions, although it is configured to test the chemistry, not to produce films of uniform thickness.

Computational Studies
DFT calculations (e.g. geometry optimization, fragment calculations, Atoms in Molecules). We generally only run fairly simple calculations aimed
x at better understanding the bonding involved in unique metal complexes. If students or PDFs are interested in running their own calculations they are encouraged to do so; if not, D. Emslie will run them (currently only Kris Kolpin in the group runs his own calculations). Some calculations (especially those involving uranium, which are particularly challenging) are carried out by academic collaborators.

Other Techniques (typically not hands-on)
TGA and DSC; studies are currently performed by collaborators who have this equipment housed within an inert-atmosphere glovebox.
SEM and XPS: these techniques are used to characterize thin films prepared in the ALD project. Typically students and PDFs do not run theirxown samples; we simply submit our samples for testing by staff of the appropriate facility.
Analytical f-Element Separation Studies: these studies (to determine the effectiveness of new ligands prepared in the group for selective
f-element complexation and separation) are conducted by academic collaborators.


Major equipment in the Emslie group

Single-station MBraun glove box with a large -35 oC freezer (MBraun)

2 x Double-station glove boxes with -35 oC freezers

Double manifold argon/vacuum lines (10 on benches, 4 in fume hoods) with Chemglass valves and associated glassware

Inert atmosphere electrochemistry setup (with the capability to perform low temperature and high scan rate measurements): 283 PAR Potentiostat Galvanostat (EG&G), various electrochemistry cells, removable low temperature cold well in the glove box, Pt, GCE and Au electrodes, and Faraday cage (BASi)

Photochemical Reaction Assembly (ACE Glassware) with Quartz glassware, 450 W Power supply, Medium pressure mercury vapour lamp (450 W) with water-cooled quartz immersion well, and Photochemical reaction safety cabinet

4 Point Probe for Resistivity Measurement (Jandel Engineering)


Departmental and BIMR Facilities

The departmental facilities at McMaster are essential to our research.
McMaster has a wide array of NMR spectrometers (2 x 200 MHz, 300 MHz, 2 x 500 MHz, 600 MHz, 700 MHz). Two of these are routinely used to peform solution multinuclear, 2D and VT solution experiments. Our X-Ray facility is well equiped with a Mo diffractometer (Bruker Smart-Apex II CCD- typically used for inorganic compounds), a Cu diffractometer (Bruker Smart 2000 RA/CCD - typically used for organic compounds), and a powder diffractometer capable of running small angle X-ray scattering experiments.

The Brockhouse Institute for Materials Research (BIMR) is also a valuable resource which is located in the same building as the Department of Chemistry. The BIMR was one of the first materials research institutes in North America and is equiped with a range of instrumentation (e.g. TGA, DSC, SQUID magnetometer, scanning probe microscopes etc.) to which researchers in chemistry have access.

For additional information, click on the links below:

NMR Spectroscopy X-Ray Crystallography
Mass Spectrometry BIMR

Emslie Laboratory Pictures

Emslie Group ALD Reactor (2015)
ald
Brad Cowie using a swivel frit
BC vac line
Metal Deposition in Solution Screening Reaction
metal
Kelly Motolko using the large glove box
Kelly GB
Synthesis of PtCl2(COD) via H2PtCl6
Pt Aqua Regia
Kris Kolpin using the lab 'super computer'
computer
Quenching 50g Scale 9,9-Dimethylxanthene Prep
rxn
Carlos Cruz working at his Vac Line
James Blackwell using one of the Vac Lines
Vac lines 2
Emslie working in the Electrochemistry Glove Box
Carlos doing Air-Free Electrochemistry
Carlos Cruz running our GC-MS
Synthesis Glove Box with assorted N2(l) Dewars
View down the lab towards the 2 glove boxes
Carlos purifying a starting material in a swivel frit