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Materials 2021, 14, 1786 3 of 20 2.2. Coordination Polymers’ Preparation The CPs SmCP1, {[Sm(Haip)(aip)(H2O)5]·4H2O}n, and TbCP1, {[Tb(Haip)(aip)(H2O)5]· 4H2O}n, were prepared by two distinct synthetic procedures, namely hydrothermal (HT) synthesis and microwave-assisted synthesis (MWAS), while the CPs TbCP2, {[Tb(Haip)(aip) (H2O)2]·H2O}n, and TbCP3, {[Tb(Haip)(aip)(phen)]·H2O}n, were only prepared by HT syn- thesis. In general, the HT synthesis to obtain SmCP1, TbCP1, TbCP2 and TbCP3 was per- formed by the following procedure (the detailed description is presented in the Supplementary Material: Section 1, coordination polymers preparation): a mixture of 5- aminoisophthalic acid (H2aip, 1.0 equivalent), SmCl3·6H2O or TbCl3·6H2O (ca. 0.65 equiv), NaOH (1.0–1.2 equiv) and water (5 mL) was prepared in a 23 mL reaction vessel. For TbCP1, NaOH (1.3 equiv) was added and the pH was adjusted until 3 < pH < 4, while for TbCP2, NaOH (1.0 equiv) was added without adjustment of pH. In the case of TbCP3, the co-ligand 1,10-phenanthroline (phen, 0.59 equiv) was added to the mixture. For all the materials, the resulting mixture was stirred at room temperature for 30 min and then the reaction vessel was sealed and heated to 110 ◦C for 72 h. After cooling to room temperature, the resulting solid was filtered, washed with water and dried in air. Suitable crystals for single-crystal X-ray diffraction (SCXRD) were collected and analyzed (see more details in Supplementary Material, Figure S1). The MWAS method to obtain SmCP1 and TbCP1 was performed according to the following: a mixture of H2aip (1.0 equiv), SmCl3·6H2O or TbCl3·6H2O (ca. 0.65 equiv), NaOH (1.1–1.2 equiv) and water (5.0 mL) was stirred at room temperature for 30 min in a closed 10 mL microwave vessel. The vessel was then placed in the cavity of the microwave reactor. The reaction mixture was irradiated at 110 ◦C (1 min ramp to 110 ◦C and 2 h at 110 ◦C, using 90 W maximum power, and the mixture was maintained with stirring). After cooling to room temperature, the resulting solid was filtered, and the filtrate was left standing at room temperature to obtain crystalline materials suitable for SCXRD analysis. 2.3. Single Crystal X-Ray Diffraction Suitable single crystals of the material SmCP1, TbCP1, TbCP2 and TbCP3 were collected from the respective crystallization vial, immediately immersed in highly viscous oil and mounted on CryoLoops [44]. Diffraction data were collected on a Bruker X8 APEX II CCD area-detector diffractometer (Mo Kα graphite-monochromated radiation, λ = 0.71073 Å) with the acquisition controlled by the APEX2 software package [45]. The temperature of acquisition, 150(2) or 180(2) K, was set up with a cryosystem by the Oxford Cryosystems Series 700 monitored by the interface Cryopad [46]. Collected images were processed using the software package SAINT+ [47] and the absorption effects correction was carried out by the multi-scan semi-empirical method implemented in SADABS [48]. The structure was solved using the algorithms implemented in SHELXT-2014 [49,50] and the non-H-atoms were located from different Fourier maps calculated from successive full-matrix least squares refinement cycles on F2 using SHELXL-v.2014 [49,51]. All the non-H-atoms were effectively refined by using anisotropic displacement pa- rameters. H-atoms bound to carbon were placed at geometrical positions using suitable HFIX instructions in SHELXL and included in subsequent refinement cycles in riding- motion approximation with isotropic thermal displacements parameters (Uiso) fixed at 1.2 × or 1.5 × Ueq of the carbon atom to which they are attached. H-atoms of the numer- ous coordinated and uncoordinated water molecules were located from different Fourier maps and included in subsequent refinement stages, with the O···H and H···H distances restrained to assure an accurate geometry and using a riding-motion approximation with an isotropic thermal displacement parameter fixed at 1.5 × Ueq of the respective O-atom. Selected crystal and structure refinement data for the CP are summarized in Table 1.PDF Image | Green Chemistry with Supercritical CO2 and Enzymes
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