Applications for Synthetic Chemistry
IMSERC has a large pool of modern instrumentation for synthetic chemists. Our center is integrated with the Chemistry Department at Northwestern University where scientists run their experiments on a 24/7 basis. From monitoring reactions to full structure elucidation, researchers and students have access to a variety of techniques that can be used for:
Crystallographic atomic structure determination, identification, and refinement of organic and inorganic compounds for extraction of structural information such as:
Determination of unit cell and bonding environment (bond-lengths, bond-angles, cation-anion coordination, site-ordering, etc.)
One of the foremost priorities in materials discovery (both organic and inorganic) is to determine the crystal structure of a material at the atomic scale. The crystallographic determination of the content of the so-called unit cell of a good quality crystal will provide the necessary information for an accurate description of the bonding environment in the crystal structure. Unit cell is essentially the smallest repetitive three-dimensional atomic/molecular building block in a crystal.
After the crystallographic determination of the content of the unit cell in the atomic scale, structural parameters, such as bond-lengths, bond-angles, cation-anion coordination, site-ordering, etc. can be accurately extracted. Crystallographic determination of the content of the unit cell requires collection of diffraction intensity data which is typically collected with X-rays, electrons, and neutrons. After data collection, a series of data reduction, solution, and refinement steps must occur in order to obtain the content of the unit cell.
Determination of packing of molecules and co-crystals
The packing and arrangement of molecules within a crystal structure is important for studying the intermolecular interactions between molecules, e.g. Hydrogen bonding, absolute structure, etc. Crystallographic analyses of single crystal diffraction data could provide information on the absolute structure of a good quality crystal. Hence, for example, it is possible to 1) determine the packing of molecules and co-crystals in new compounds, and/or 2) differentiate between enantiomers in inorganic materials, natural products, etc.
Absolute structure determination by single crystal crystallographic techniques can provide information about the structural chirality, absolute chirality, absolute polarity, absolute morphology, absolute chiral morphology, and absolute polar morphology of a compound.
Determination of Hydrogen bonding
The packing and arrangement of molecules within a crystal structure is important for studying the intermolecular interactions between molecules, e.g. Hydrogen bonding, absolute structure, etc. Crystallographic analyses of single crystal diffraction data could provide information on the absolute structure of a good quality crystal. Hence, for example, it is possible to 1) determine the packing of molecules and co-crystals in new compounds, and/or 2) differentiate between enantiomers in inorganic materials, natural products, etc.
Absolute structure determination by single crystal crystallographic techniques can provide information about the structural chirality, absolute chirality, absolute polarity, absolute morphology, absolute chiral morphology, and absolute polar morphology of a compound.
Determination of enantiomers
The packing and arrangement of molecules within a crystal structure is important for studying the intermolecular interactions between molecules, e.g. Hydrogen bonding, absolute structure, etc. Crystallographic analyses of single crystal diffraction data could provide information on the absolute structure of a good quality crystal. Hence, for example, it is possible to 1) determine the packing of molecules and co-crystals in new compounds, and/or 2) differentiate between enantiomers in inorganic materials, natural products, etc.
Absolute structure determination by single crystal crystallographic techniques can provide information about the structural chirality, absolute chirality, absolute polarity, absolute morphology, absolute chiral morphology, and absolute polar morphology of a compound.
Refinement of modulated and twinned structures (incommensurate, commensurate, composite superstructures)
A modulated crystal structure, in simple terms, is quasi-periodic, i.e., its periodicity cannot be defined by traditional three-dimensional lattice parameters and requires additional vectors to define its periodicity. Modulation vectors and structure solution of modulated structures can be determined crystallographically. If the components of the modulation vector are all rational numbers, the structure is called commensurately modulated. In case one of the components of the vector is an irrational number, the structure is called incommensurately modulated.
Twinning occurs when a crystal possesses domains in different orientations and can be related by a translation, rotation, inversion, or reflection. Depending on the degree of twinning in a material, either single crystal or powder crystallographic techniques can be utilized for a proper structure elucidation.
High resolution data for charge density measurement and precise assignment of atoms with similar chemical environment
One of the foremost priorities in materials discovery (both organic and inorganic) is to determine the crystal structure of a material at the atomic scale. The crystallographic determination of the content of the so-called unit cell of a good quality crystal will provide the necessary information for an accurate description of the bonding environment in the crystal structure. Unit cell is essentially the smallest repetitive three-dimensional atomic/molecular building block in a crystal.
After the crystallographic determination of the content of the unit cell in the atomic scale, structural parameters, such as bond-lengths, bond-angles, cation-anion coordination, site-ordering, etc. can be accurately extracted. Crystallographic determination of the content of the unit cell requires collection of diffraction intensity data which is typically collected with X-rays, electrons, and neutrons. After data collection, a series of data reduction, solution, and refinement steps must occur in order to obtain the content of the unit cell.
Powder evaluation of sample purity (sensitivity of ~2% by weight)
Quantitative determination of individual crystalline phases and impurities in mixtures of powder
Monitor reactions in real time as a function of time, temperature, pressure, and gas flow/pressure
Probe catalytic changes to substrates
Investigate decomposition mechanism
Thermal or chemical decomposition mechanism in a material can be monitored in real time using in-situ/operando X-ray diffraction measurements that can be performed as a function of time and/or under non-ambient conditions, such as heating, cooling, oxidizing, reducing, etc.
Additionally, Thermal Analysis coupled with GC-MS and/or IR might yield information regarding the decomposition temperature and identification of generated gas molecules (e.g., water, ammonia, carbon dioxide, etc.) during the decomposition thermal event.