hatcher content part 5

what are the challenges associated with forming a complex network of metals and ligands into a highly ordered and defined structure?

find synthesis conditions that create defined SBUs without decomposition of the organic linker

same starting reaction mixtures can lead to different mofs depending on the reaction conditions

thermodynamics plays a crucial role in mof synthesis

what is the direct precipitation method of mof synthesis?

simple mixing of starting materials in solvent at room temperature

known to access some prominent mofs

slow reaction rates, small crystals/powders of low crystal quality

what is the non-solvothermal synthesis method of mof synthesis?

reaction below boiling point of solvent (no pressure in system)

simpler synthetic requirements

slow reaction rates, small crystals/powders and low crystal quality

what is the solvothermal synthesis method for making mofs?

reactants and solvent are placed in a steel autoclave vessel

vessel is heated in an oven to above the solvent boiling point

autogenous pressure generated inside vessel

what is the definition of solvothermal synthesis?

a chemical reaction taking place in a solvent at temps above the boiling point and pressures above 1 bar

what types of vessel can be used for solvothermal synthesis?

Parr bombs - max temp 250, max pressure 124 bar

schott bottle - max temp 180, max pressure 1.5 bar

what is the antoine equation?

log10P = A - B/(C + T)

P = vapour pressure

T = temp in K

A B and C are antoine coefficients

what are some solid state snalysis methods that can be used to analyse mofs?

vibrational spectroscopy (FT-IR and Raman)

solid state absorption spectroscopy

solid state nmr

powder x ray diffraction

single crystal x ray diffraction

what non-solid state analysis methods can be used to snalyse mofs?

solution nmr digestion

absorption isotherms (porosity measurements)

what is needed to analyse a mof with powder x ray diffraction?

requires only powder/small crystallites

fast, visual way to confirm crystallinity

usually fingerprint method but full 3D structure determination possible from high quality data

what is needed to analyse a mof by single crystal xrd?

require high quality large crystals (0.1-0.5 mm³)

full 3D structure can be determined

unambiguously describes full connectivity

gold standard of solid state analysis