Post-Synthetic Shaping of Porosity and Crystal Structure of Ln-Bipy-MOFs by Thermal Treatment
Abstract
:1. Introduction
2. Results and Discussion
2.1. Post-Synthetic Surface Modification and Morphology Control
2.2. Thermal Conversion Processes
2.3. Synthesis of Single Crystalline High-Temperature Phases via a Solvothermal Approach
2.4. Crystal Structures of[LaCl3(bipy)] (2),[Ln3Cl9(bipy)3], Ln = Pr (8), Sm (9),[Ho2Cl6(bipy)2] (11), and[Gd2Cl6(qtpy)2(bipy)2]·bipy (12)
[LaCl3(bipy)] (2) | [Pr3Cl9(bipy)3] (8) | [Sm3Cl9(bipy)3] (9) | [Ho2Cl6(bipy)2] (11) | [Gd2Cl6(qtpy)2 (bipy)2]·bipy (12) | |
---|---|---|---|---|---|
Formula weight/g·mol−1 | 401.44 | 1210.36 | 1238.65 | 854.95 | 1608.40 |
Crystal system | orthorhombic | orthorhombic | orthorhombic | monoclinic | monoclinic |
Space group | Pcca | Cmcm | Cmcm | P21/c | C2/m |
a/pm | 2387.4(5) | 1213.49(14) | 1206.99(5) | 988.4(2) | 1177.53(13) |
b/pm | 744.9(2) | 2015.5(2) | 2015.93(9) | 2463.1(6) | 2351.7(2) |
c/pm | 717.8(2) | 1606.2(2) | 1590.81(7) | 1137.2(3) | 1687.2 (2) |
β/° | - | - | - | 112.142(7) | 107.710(3) |
Volume/pm3 | 1276.6(4) | 3928.5(8)·106 | 3870.8(3)·106 | 2564.4(11)·106 | 4450.8(8)·106 |
Z | 4 | ||||
dc/g/cm3 | 2.089 | 2.0463 | 2.126 | 2.214 | 2.400 |
Diffractometer | Bruker Apex II | SMART Bruker Apex | Bruker Apex II | Bruker Apex II | Bruker Apex II |
Monochromator | Helios-mirror | Graphite | Helios-mirror | Helios-mirror | Helios-mirror |
Radiation | 70.93 pm (Mo-Kα) | ||||
Temperature/K | 100(3) | 168(5) | 100(3) | 100(3) | 100(3) |
2θ range | 3.42 ≤ 2θ ≤ 60.7° | 3.92 ≤ 2θ ≤ 60.08° | 3.94 ≤ 2θ ≤ 60.22° | 4.2 ≤ 2θ ≤ 61.82° | 2.54 ≤ 2θ ≤ 60.18° |
μ/mm−1 | 3.946 | 4.305 | 5.144 | 6.768 | 1.697 |
F000 | 761.5 | 2308.8 | 2340.0 | 1604.0 | 1584.0 |
Reflections collected | 17347 | 22073 | 28523 | 39177 | 33891 |
Independent reflections | 1834 | 3091 | 3023 | 7326 | 6484 |
[R(int) = 0.0355] | [R(int) = 0.1876] | [R(int) = 0.0768] | [R(int) = 0.1042] | [R(int) = 0.2972] | |
Data/restraints/parameters | 1834/0/74 | 3091/0/122 | 3023/0/123 | 7326/0/288 | 6484/0/225 |
S | 1.143 | 1.001 | 1.077 | 1.018 | 1.083 |
R1 for n reflections > [I ≥ 2σ (I)] [a] | 0.0255 | 0.0580 | 0.0356 | 0.0432 | 0.1241 [a] |
R1[all data] [a] | 0.0372 | 0.0993 | 0.0541 | 0.0915 | 0.3063 [a] |
wR2[all data] [b] | 0.0458 | 0.1341 | 0.0700 | 0.0789 | 0.3879 [b] |
Largest diff. peak/hole/(e pm−3)·10−6 | 1.02/−1.33 | 2.78/−3.25 | 2.53/−1.08 | 3.69/−4.07 | 2.00/−2.05 |
2.5. Photoluminescence and Vibrational Spectroscopy
3. Experimental Section
3.1. Synthesis
3.1.1. Synthesis of[La2Cl6(bipy)5]·4(bipy) (1),[Ln2Cl6(bipy)3]·2(bipy), Ln = Pr (4), Sm (5), and[Ln2Cl6(bipy)3], Ln = Pr (6), Sm (7), Eu (13), Eu/Tb (14)
3.1.2. Synthesis of[LaCl3(bipy)] (2)
3.1.3. Synthesis of[Pr3Cl9(bipy)3] (8)
3.1.4. Synthesis of[Sm3Cl9(bipy)3] (9)
3.1.5. Synthesis of[Ho2Cl6(bipy)2] (11)
3.1.6. Synthesis of[Gd2Cl6(qpy)2(bipy)2]·bipy (12)
3.2. Crystal Structure Determination
3.3. Powder X-ray Diffraction
3.4. Photoluminescence- and Vibrational Spectroscopy
3.5. Thermal and Elemental Analysis
3.6. Gas Adsorption Experiments
3.7. SEM and EDX Analysis
4. Conclusions
Supplementary Materials
Acknowledgments
Author Contributions
Conflicts of Interest
References
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Matthes, P.R.; Schönfeld, F.; Zottnick, S.H.; Müller-Buschbaum, K. Post-Synthetic Shaping of Porosity and Crystal Structure of Ln-Bipy-MOFs by Thermal Treatment. Molecules 2015, 20, 12125-12153. https://doi.org/10.3390/molecules200712125
Matthes PR, Schönfeld F, Zottnick SH, Müller-Buschbaum K. Post-Synthetic Shaping of Porosity and Crystal Structure of Ln-Bipy-MOFs by Thermal Treatment. Molecules. 2015; 20(7):12125-12153. https://doi.org/10.3390/molecules200712125
Chicago/Turabian StyleMatthes, Philipp R., Fabian Schönfeld, Sven H. Zottnick, and Klaus Müller-Buschbaum. 2015. "Post-Synthetic Shaping of Porosity and Crystal Structure of Ln-Bipy-MOFs by Thermal Treatment" Molecules 20, no. 7: 12125-12153. https://doi.org/10.3390/molecules200712125