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To study the implications of highly space-demanding organic moieties on the properties of self-assembled monolayers (SAMs), triptycyl thiolates and selenolates with and without methylene spacers on Au(111) surfaces were comprehensively studied using ultra-high vacuum infrared reflection absorption spectroscopy, X-ray photoelectron spectroscopy, near-edge X-ray absorption fine structure spectroscopy and thermal desorption spectroscopy. Due to packing effects, the molecules in all monolayers are substantially tilted. In the presence of a methylene spacer the tilt is slightly less pronounced. The selenolate monolayers exhibit smaller defect densities and therefore are more densely packed than their thiolate analogues. The Se–Au binding energy in the investigated SAMs was found to be higher than the S–Au binding energy.
The layer‐by‐layer (LbL) method is a well‐established method for the growth of surface‐attached metal–organic frameworks (SURMOFs). Various experimental parameters, such as surface functionalization or temperature, have been identified as essential in the past. In this study, inspired by these recent insights regarding the LbL SURMOF growth mechanism, the impact of reactant solutions concentration on LbL growth of the Cu2(F4bdc)2(dabco) SURMOF (F4bdc2−=tetrafluorobenzene‐1,4‐dicarboxylate and dabco=1,4‐diazabicyclo‐[2.2.2]octane) in situ by using quartz‐crystal microbalance and ex situ with a combination of spectroscopic, diffraction and microscopy techniques was investigated. It was found that number, size, and morphology of MOF crystallites are strongly influenced by the reagent concentration. By adjusting the interplay of nucleation and growth, we were able to produce densely packed, yet thin films, which are highly desired for a variety of SURMOF applications.