Multifunctionality of Nano-Sized Metal-Oxide Materials and Phenomena under Confined Conditions

Abstract in keywords
Processes under confined conditions, especially in capsules with stepwise closable pores and tunable internal functionalities; coordination chemistry in the cavity and pores of nano-containers; sphere surface supramolecular chemistry; tuning the hydrophobicity of nano-container interiors to influence, for example, encapsulated water structures; cation transport/separation under confined conditions; molecular porosity; designed synthesis of nanosized clusters based on constitutional dynamic libraries; chemical adaptability.

     Structurally well-defined spherical porous metal-oxide based nanocapsules of the type {Pentagon}12{Linker}301-3 allow unprecedented chemistry including catalytic(!) reactions4 which can be performed in the cavities, in the pores and at the surfaces;3 interestingly, the size of the capsules and their 20 pores can be varied.3 As the pores have crown ether function they can - based on sphere surface supramolecular chemistry - be stepwise opened and closed with appropriate corks/guests3 (Fig. 1 top right) while according to their flexibilities uptake of compounds larger than the pores is possible (see below). The internal cavities' shells can get differently functionalized which influences the structures of encapsulates, e.g. in case of the (inverse micelle type) butyrate-24 aggregate5 (Fig. 1 bottom right) and of higher and lower density water molecule assemblies (see below).

Figure 1


Figure 1


     The capsules interact specifically with their environment, e.g. with cations (Fig. 1 top left) - allowing after their uptake their nanoscaled separations corresponding to a nano-ionchromatograph principle and to model transmembrane cation transport3 - but also with themselves in aqueous solution leading to giant spherical supramolecular aggregates (Fig. 1 bottom left - here shown for molybdenum-oxide wheels6). A comparable scenario can, remarkably, lead to a new type of self-recognition process: the two spherical {Pentagon}12M30 (M = FeIII, CrIII) type capsules - both having the same surface like a nano drop of water - assemble in solution to two separate spherical structures without interference.7

     Present investigations refer especially to the study of hydrophobic effects which play a major role in a variety of important phenomena, for example in protein folding and formation of lipid bilayers as well as the insertion of proteins into biological membranes. Investigations were performed within the porous capsules of the type {Pentagon}12{Linker}30 ≡ {(M) M5}12{MoV2 (Ligand)}30 (M = Mo, W), which can be constructed with varying hydrophobic interiors, i.e. "ligands" and therefore, with different amounts and structures of encapsulated water (see below) or hydrophobic materials. In a special case, it could be shown that capsules containing 30 hydrophobic propionate ligands allow the removal of (toxic) hydrophobic species like n-hexanol molecules from water solutions corresponding to their uptake and appropriate internal interactions, i.e. hydrophobic clustering. The latter could be studied by NMR spectroscopy.8a (This effect leads - in the presence of butyrate ligands - to the formation of an encapsulated unique butyrate-24 micelle-like aggregate containing a hydrophobic cavity5 already mentioned above; Fig. 1 bottom right.) The mentioned processes were considered as a paradigmatic shift with respect to molecular recognition and clustering of hydrophobic materials in water. Remarkably, it was also possible to study - with EXSY-NMR spectroscopy - uptake-release guest exchange processes simultaneously with the exchange between guests like acetate positioned on different sites inside a capsule - an interesting artificial cell scenario.8b

     One important result/aspect refers to considering "water" in hydrophobic cavities (like in protein pockets). In a remarkable scenario within a nanocapsule an unprecedented segregation between the mostly hydrophobic internal capsule wall - spanned by the acetate/water ligand arrangement - and an encapsulated "water molecule collection"9a forming an unprecedented spherical shell with strongly interacting molecules can be observed (Fig. 2). We can refer to a molecular Lotus effect or to "Water's response to the fear of water".9b Importantly, one can influence the type of "water assembly" by changing the ratio of acetate and water ligands, that is, the hydrophobicity.

Figure 2


Figure 2


     In a special case - only considered here for completeness - a highly symmetrical (H2O)100 cluster is formed3,10 (Fig. 3 left) in a special hydrophilic capsule while it is remarkably even template driven3,10 (Fig. 3 right). The Figure shows correspondingly three O5 (water) pentagons extracted from the water cluster of Figure 3 left, while the yellow pentagon is formed by the template effect of the O5 (water ligand) pentagon (red) of the capsule skeleton.3,10 By changing the internal hydrophilic ligands regarding their sizes also "higher and lower density water" can be generated/encapsulated10a (Fig. 4).



Figure 3
Figure 3


Figure 3



Figure 4


Figure 4


     Our interest in the future will focus especially on the high reactivity (including related catalysis) of the 60 unsaturated MoV Lewis acid centers within the capsule interior3,11 (which can easily be generated), furthermore on molecular porosity12 (Fig. 5), and chemical adaptability13 (Fig. 6).
Figure 5

Figure 5
Figure 6

Figure 6

     The mentioned metal-oxide nano-objects were used by several groups because of their easy preparation14 in context with experiments of importance for materials science (for examples see ref. 3).

  1. A. Müller, P. Kögerler, C. Kuhlmann
    "A variety of combinatorially linkable units as disposition: from a giant icosahedral Keplerate to multi-functional metal-oxide based network structures"
    Chem. Comm., 1347-1358 (1999)
  2. A. Müller, S. Roy
    In: "The Chemistry of Nanomaterials: Synthesis, Properties and Applications" (Eds.: C. N. R. Rao, A. Müller, A. K. Cheetham)
    Wiley-VCH, Weinheim, 452-475 (2004)
  3. A. Müller, P. Gouzerh
    "From linking of metal-oxide building blocks in a dynamic library to giant clusters with unique properties and towards adaptive chemistry"
    Chem. Soc. Rev. 41, 7431-7463 (2012)
  4. S. Kopilevich, A. Gil, M. Garcia-Ratés, J. B. Avalos, C. Bo, A. Müller, I. A. Weinstock
    "Catalysis in a porous molecular capsule: activation by regulated access to sixty metal centers spanning a truncated icosahedrons"
    J. Am. Chem. Soc. 134, 13082-13088 (2012)
  5. C. Schäffer, H. Bögge, A. Merca, I. A. Weinstock, D. Rehder, E. T. K. Haupt, A. Müller
    "A Spherical 24 Butyrate Aggregate with a Hydrophobic Cavity in a Capsule with Flexible Pores: Confinement Effects and Uptake-Release Equilibria at Elevated Temperatures"
    Angew. Chem. 121, 8195-8200 (2009)
    Angew. Chem. Int. Ed. 48, 8051-8056 (2009)
  6. T. Liu, E. Diemann, H. Li, A. W. M. Dress, A. Müller
    "Self-assembly in aqueous solution of wheel-shaped Mo154 oxide clusters into vesicles"
    Nature 426, 59-62 (2003)
  7. T. Liu, M. L. K. Langston, D. Li, J. M. Pigga, C. Pichon, A. M. Todea, A. Müller
    "Self-Recognition Among Different Polyprotic Macroions During Assembly Processes in Dilute Solution"
    Science 331, 1590-1592 (2011)
  8. (a) C. Schäffer, A. M. Todea, H. Bögge, O. A. Petina, D. Rehder, E. T. K. Haupt, A. Müller
    "Hydrophobic Interactions and Clustering in a Porous Capsule: Option to Remove Hydrophobic Materials from Water"
    Chem. Eur. J. 17, 9634-9639 (2011)
    (b) O. Petina, D. Rehder, E. T. K. Haupt, A. Grego, I. A. Weinstock, A. Merca, H. Bögge, J. Szakács, A. Müller
    "Guests on Different Internal Capsule Sites Exchange with Each Other and with the Outside"
    Angew. Chem. 123, 430-434 (2011)
    Angew. Chem. Int. Ed. 50, 410-414 (2011)
  9. (a) C. Schäffer, A. M. Todea, H. Bögge, E. Cadot, P. Gouzerh, S. Kopilevich, I. A. Weinstock, A. Müller
    "Softening of Pore and Interior Properties of a Metal-Oxide-Based Capsule: Substituting 60 Oxide by 60 Sulfide Ligands"
    Angew. Chem. 123, 12534-12537 (2011)
    Angew. Chem. Int. Ed. 50, 12326-12329 (2011)
    (b) H. J. Bakker "Water's response to the fear of water"
    Nature 491, 533-535 (2012)
  10. (a) T. Mitra, P. Miró, A.-R. Tomsa, A. Merca, H. Bögge, J. B. Ávalos, J. M. Poblet, C. Bo, A. Müller
    "Gated and Differently Functionalized (New) Porous Capsules Direct Encapsulates' Structures: Higher and Lower Density Water"
    Chem. Eur. J. 15, 1844-1852 (2009) (cover picture)
    (b) A. Oleinikova, H. Weingärtner, M. Chaplin, E. Diemann, H. Bögge, A. Müller
    "Self-Association Based on Interfacial Structured Water Leads to {Mo154}ca. 1165 Super Clusters: A Dielectric Study"
    ChemPhysChem 8, 646-649 (2007)
  11. S. Garai, E. T. K. Haupt, H. Bögge, A. Merca, A. Müller
    "Picking up 30 CO2 Molecules by a Porous Metal Oxide Capsule Based on the Same Number of Receptors"
    Angew. Chem. 124, 10680-10683 (2012)
    Angew. Chem. Int. Ed. 51, 10528-10531 (2012)
  12. A. Ziv, A. Grego, S. Kopilevich, L. Zeiri, P. Miro, C. Bo, A. Müller, I. A. Weinstock
    "Flexible Pores of a Metal Oxide-Based Capsule Permit Entry of Comparatively Larger Organic Guests"
    J. Am. Chem. Soc. 131, 6380-6382 (2009) (cover picture)
  13. A. Müller, A. Merca, A. J. M. Al-Karawi, S. Garai, H. Bögge, G. Hou, L. Wu, E. T. K. Haupt, D. Rehder, F. Haso, T. Liu
    "Chemical Adaptability: The Integration of Different Kinds of Matter into Giant Molecular Metal Oxides"
    Chem. Eur. J. 18, 16310-16318 (2012) (VIP paper, cover picture)
  14. (a) A. Müller, S. K. Das, E. Krickemeyer, C. Kuhlmann
    "Polyoxomolybdate Clusters: Giant Wheels and Balls"
    Checked by: M. Sadakane, M. H. Dickman, M. T. Pope
    Inorganic Syntheses 34 (Ed.: J. R. Shapley), Wiley, New York (2004), pp. 191-200
    (b) L. Cronin, E. Diemann, A. Müller
    "Polyoxomolybdate Clusters: Nanoscopic Wheels and Balls"
    In: "Inorganic Experiments" (Ed.: J. D. Woollins)
    Wiley-VCH, Weinheim (2003), pp. 340-346