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1 Supplementary Information Zeolitic Polyoxometalates Metal Organic Frameworks (Z- POMOF) with Imidazole Ligands and ε-keggin ions as Building Blocks; Computational Evaluation of Hypothetical Polymorphs and a Synthesis Approach L. Marleny Rodriguez Albelo, a A. Rabdel Ruiz-Salvador,*,a Dewi L. Lewis, b Ariel Gómez, c Pierre Mialane, d Jérome Marrot, d Anne Dolbecq,*,d Alvaro Sampieri b,e and Caroline Mellot-Draznieks*,b a Zeolites Engineering Laboratory, Institute of Materials Research and Engineering (IMRE), University of Havana, Havana, Cuba rabdel@imre.oc.uh.cu (A.R.R.-S.) b Department of Chemistry, University College London, 20 Gordon St., London, WC1H 0AJ, UK c.mellot-draznieks@ucl.ac.uk (C.M.-D.) c Department of Physics, University of Guelph, ON, N1G 2W1 Canada. d Institut Lavoisier de Versailles, UMR 8180, Université de Versailles Saint-Quentin en Yvelines, 45 Avenue des Etats-Unis, Versailles cedex, France. dolbecq@chimie.uvsq.fr (A.D.) e Present address: Benemérita Universidad Autónmoma de Puebla, Facultad de Ingeniería Química, 18 Sur y Av. San Claudio s/n, C.P , Puebla, PUE, Mexico.
2 O38 O18 Mo11 O35 O39 O21 O16 Mo5 O20 Zn4 O19 Zn3 O33 O37 Mo10 O9 O34 Mo12 O36 O40 O22 Mo6 O15 O14 O23 Mo4 O17 O13 O27 P1 O28 O6 Mo9 O8 O31 O32 Mo2 O10 Zn2 O7 O24 O25 Mo7 O12 O11 Mo3 O30 O2 O5 Zn1 O26 O3 Mo8 O4 Mo1 O29 O1 Figure S1. Atom labeling scheme of the POM unit; blue spheres = Mo(VI) ions, yellow spheres = Mo(V) ions, grey spheres = protonated oxygen atoms.
3
4 Table S1. Valence bond calculations. Mo(1)-O(1) (18) Mo(7)-O(25) 1.688(2) Mo(1)-O(2) (17) Mo(7)-O(26) (18) Mo(1)-O(3) (16) Mo(7)-O(27) (18) Mo(1)-O(4) (15) Mo(7)-O(23) (19) Mo(1)-O(5) (17) Mo(7)-O(24) (17) Mo(1)-O(6) (16) Mo(7)-O(28) (18) Mo(1)-Mo(8) (4) Σ (Mo(1)) = 5.3 Σ (Mo(7)) = 6.0 Mo(2)-O(7) 1.700(2) Mo(8)-O(29) (19) Mo(2)-O(8) (18) Mo(8)-O(3) (16) Mo(2)-O(5) (18) Mo(8)-O(2) (17) Mo(2)-O(9) (17) Mo(8)-O(26) (18) Mo(2)-O(10) (17) Mo(8)-O(30) (18) Mo(2)-O(6) (17) Mo(8)-O(28) (17) Mo(2)-Mo(12) (4) Σ (Mo(2)) = 5.9 Σ (Mo(8)) = 5.2 Mo(3)-O(11) (19) Mo(9)-O(31) 1.680(2) Mo(3)-O(12) (16) Mo(9)-O(32) (19) Mo(3)-O(13) (17) Mo(9)-O(33) (19) Mo(3)-O(8) (18) Mo(9)-O(27) (19) Mo(3)-O(4) (15) Mo(9)-O(30) (18) Mo(3)-O(6) (16) Mo(9)-O(28) (16) Mo(3)-Mo(4) (3) Mo(9)-Mo(10) (4) Σ (Mo(3)) = 5.2 Σ (Mo(9)) = 5.2 Mo(4)-O(14) (19) Mo(10)-O(34) (19) Mo(4)-O(12) (16) Mo(10)-O(35) (19) Mo(4)-O(13) (18) Mo(10)-O(33) 1.971(2) Mo(4)-O(15) (18) Mo(10)-O(32) (17) Mo(4)-O(16) (18) Mo(10)-O(36) (19) Mo(4)-O(17) (17) Mo(10)-O(37) (16) Σ (Mo(4)) = 5.3 Σ (Mo(10)) = 5.3 Mo(5)-O(18) 1.691(2) Mo(11)-O(38) (19) Mo(5)-O(19) (19) Mo(11)-O(35) (19) Mo(5)-O(20) (18) Mo(11)-O(19) (17) Mo(5)-O(21) 2.006(2) Mo(11)-O(20) (19) Mo(5)-O(16) (19) Mo(11)-O(39) (19) Mo(5)-O(17) (17) Mo(11)-O(37) (17 Mo(5)-Mo(11) (4) Σ (Mo(5)) = 5.1 Σ (Mo(11)) = 5.3 Mo(6)-O(22) 1.685(2) Mo(12)-O(40) 1.677(2) Mo(6)-O(15) (18) Mo(12)-O(39) (18) Mo(6)-O(21) (18) Mo(12)-O(36) (18) Mo(6)-O(23) (18) Mo(12)-O(9) (17) Mo(6)-O(24) (17) Mo(12)-O(10) (17) Mo(6)-O(17) (17) Mo(12)-O(37) (18) Mo(6)-Mo(7) (5) Σ (Mo(6)) = 5.9 Σ (Mo(12)) = 6.0
5 Σ (O(16)) = 1.3 Σ (O(30)) = 1.3
6 c b a double POM layer TBA + Figure S2. View of the unit-cell; hydrogen atoms have been omitted for clarity except on the protonated imidazole. A ball and stick representation of the POM has been used and the TBA + have been omitted on the left side of the unit-cell in order to show more clearly the H-bond interactions between double POM layers.
7 In the simulations, only rigid body motions were considered for the imidizolate and ε-keggin subunits. It is possible that a non-constant contribution to the total lattice energy throughout the whole set of structural models studied here might arise from the relaxation of the building blocks which is omitted here by the use of rigid imidizolate and ε-keggin ions. However, as shown further in our experimental crystal structure, these units may be considered as rigid in practice, with only small deviations expected. Considering the above approximations used and the general character of the forcefield, we tend to analyse the results in terms of relative trends rather than quantitative ones All contributions of the UFF force field were considered, including bond stretching, bond bending, torsion, van der Waals and electrostatic interactions, therefore accounting for both intramolecular (imidazole, Keggin) and inter-molecular interactions. It is noteworthy that the link between the N atoms of the imidazolate ligands and the Zn metal centres of the ε-keggin were described with Zn-N bonds. The advantage of using rigid bodies for the organic ligand and on the ε-keggin is that the energy contributions emanating from each single subunits are constant for all the studied structures, while the differences in lattice energies result solely from the differences in the orientation of the building-units to each other. This includes bonded and non-bonded interactions. Table S2: Partial charges used in the lattice energy minimizations Atom label Force Field Charge C2 C_R H2 H_ N N_R C1 C_R H1 H_ Atom label Force Field Charge Zn Zn Mo Mo
8 O O_
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