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Materials 2021, 14, 1786 17 of 20 4. Concluding Remarks A series of multidimensional LnCP (namely, SmCP1, TbCP1, TbCP2 and TbCP3) was prepared using sustainable procedures, namely: (a) water was used as solvent, the use of organic solvents was avoided, and a fast crystallization process was achieved and (b) the MWAS process was found to be a suitable alternative for the preparation of SmCP1 and TbCP1 materials, by reducing the reaction time of 72 h to 2 or 6 h, respectively. A common feature of all the LnCP is the presence of several coordinated and uncoordinated water molecules, except for TbCP3 that only contains one uncoordinated water molecule. In the case of TbCP2 and TbCP3, the use of phen as a co-ligand led to the decrease in the CP dimensionality from 2D (TbCP2) to 1D (TbCP3), associated to eight- or nine-coordinated Tb3+ center, respectively. The PL properties in the solid state were studied, employing two methods: powder and PMMA encapsulation, and the results were similar for both techniques. The PL prop- erties study revealed the influence of the structural differences between the four LnCP. For all cases, the expectable transition bands, for each Ln, were observed. In some cases, like SmCP1, the PL excitation band associated to the H2aip ligand was present, possibly indi- cating a more efficient energy transfer from the ligand-to-Sm3+. Although, for TbCP2, the lower intensity bands and the presence of a small band at ≈325 nm could indicate that the ligand-to-Tb3+ de-activation occurs more efficiently in comparison to TbCP1 and TbCP3. Also, the difference observed in the Tb3+ CP lifetimes may reflect a different environment surrounding the lanthanide ion, associated to the difference in the water content and presence of phen as a co-ligand. This first evaluation of the influence of synthetic methods in the PL properties of Ln-H2aip CP reveals a wide number of possibilities to evaluate and improve the PL properties of the materials. Interesting study approaches can include the modification of the reactions’ temperature and time, the removal by heat/vacuum of the H2O molecules of the CP frameworks (without destroying them) and post-functionalization with ligands containing different functional groups or co-ligands. The potential of these Ln-H2aip CPs can also be extended to other fields, such as heterogeneous catalysis or sensing capability towards solvent molecules, small molecules or metal ions. Supplementary Materials: The following are available online at https://www.mdpi.com/article/ 10.3390/ma14071786/s1: detailed description of the CPs preparation and a figure of the crystalline solids obtained (Figure S1), additional figures and tables related with the crystal structures of all the CPs (Figures S2–S5, and Tables S1–S4), FT-IR spectra for all the CPs isolated by HT and MWAS (Figure S6), other results of the PL studies, particularly the PL excitation spectra (Figure S7) and graphical representation of PL intensity in function of lifetime (Figure S8). Author Contributions: Conceptualization, L.C.-S.; methodology, C.Q. and L.C.-S.; validation, L.C.-S., A.M.G.S. and J.C.-G.; formal analysis, C.Q. and C.S.; investigation, C.Q. and C.S.; writing—original draft preparation, C.Q. and L.C.-S.; writing—review and editing, A.M.G.S., J.C.-G. and L.C.-S.; supervision, A.M.G.S., J.C.-G., B.d.C. and L.C.-S.; project administration, B.d.C. All authors have read and agreed to the published version of the manuscript. Funding: This research work received partial financial support from Portuguese national funds (FCT/MCTES, Fundação para a Ciência e Tecnologia and Ministério da Ciência, Tecnologia e Ensino Superior) through the strategic project UIDB/50006/2020 (for LAQV-REQUIMTE), and it was also funded from the European Union (FEDER funds through COMPETE) and FCT/MCTES by National Funds to the R&D project X-Sensors (PTDC/QUI-QOR/29426/2017). IMDEA Nanociencia acknowl- edges support from the “Severo Ochoa” Programme for Centres of Excellence in R&D (MINECO, grant SEV-2016-0686). J.C.-G. acknowledges financial support from the Spanish Ministry of Science, Innovation and Universities (RTI2018-097508-B-I00), (PCIN-2015-169-C02-01) and from the Regional Government of Madrid (NMAT2D S2018/NMT4511). Institutional Review Board Statement: Not applicable. Informed Consent Statement: Not applicable.PDF Image | Green Chemistry with Supercritical CO2 and Enzymes
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