Ti-based robust MOFs in the combined photocatalytic degradation of emerging organic contaminants.

Photocatalysis process is a promising technology for environmental remediation. In the continuous search of new heterogeneous photocatalysts, metal–organic frameworks (MOFs) have recently emerged as a new type of photoactive materials for water remediation. Particularly, titaniumbased MOFs (Ti-MOFs) are considered one of the most appealing subclass of MOFs due to their promising optoelectronic and photocatalytic properties, high chemical stability, and unique structural features. However, considering the limited information of the reported studies, it is a hard task to determine if real-world water treatment is attainable using Ti-MOF photocatalysts. In this paper, via a screening with seve…

De novo synthesis of mesoporous photoactive titanium(IV)-organic frameworks with MIL-100 topology

[EN] Most developments in the chemistry and applications of metal-organic frameworks (MOFs) have been made possible thanks to the value of reticular chemistry in guiding the unlimited combination of organic connectors and secondary building units (SBUs) into targeted architectures. However, the development of new titanium-frameworks still remains limited by the difficulties in controlling the formation of persistent Ti-SBUs with predetermined directionality amenable to the isoreticular approach. Here we report the synthesis of a mesoporous Ti-MOF displaying a MIL-100 topology. MIL-100(Ti) combines excellent chemical stability and mesoporosity, intrinsic to this archetypical family of porous…

Guest induced reversible on–off switching of elastic frustration in a 3D spin crossover coordination polymer with room temperature hysteretic behaviour

A binary reversible switch between low-temperature multi-step spin crossover (SCO), through the evolution of the population γHS(T) with high-spin (HS)-low-spin (LS) sequence: HS1LS0 (state 1) ↔ HS2/3LS1/3 (state 2) ↔ HS1/2LS1/2 (state 3) ↔ HS1/3LS2/3 (state 4) ↔ HS0LS1 (state 5), and complete one step hysteretic spin transition featuring 20 K wide thermal hysteresis centred at 290 K occurs in the three-dimensional (3D) Hofmann-type porous coordination polymer {FeII(3,8phen)[Au(CN)2]2}·xPhNO2 (3,8phen = 3,8-phenanthroline, PhNO2 = nitrobenzene), made up of two identical interpenetrated pcu-type frameworks. The included PhNO2 guest (x = 1, 1·PhNO2) acts as a molecular wedge between the interp…

Unlocking mixed oxides with unprecedented stoichiometries from heterometallic metalorganic frameworks for the catalytic hydrogenation of CO 2

[EN] Their complex surface chemistry and high oxygen lattice mobilities place mixed-metal oxides among the most important families of materials. Modulation of stoichiometry in mixed-metal oxides has been shown to be a very powerful tool for tuning optical and catalytic properties. However, accessing different stoichiometries is not always synthetically possible. Here, we show that the thermal decomposition of the recently reported metal-organic framework MUV-101(Fe, Ti) results in the formation of carbon-supported titanomaghemite nanoparticles with an unprecedented Fe/Ti ratio close to 2, not achievable by soft-chemistry routes. The resulting titanomaghemite phase displays outstanding catal…

Selective Implantation of Diamines for Cooperative Catalysis in Isoreticular Heterometallic Titanium–Organic Frameworks

[EN] We introduce the first example of isoreticular titanium-organic frameworks, MUV-10 and MUV-12, to show how the different affinity of hard Ti(IV) and soft Ca(II) metal sites can be used to direct selective grafting of amines. This enables the combination of Lewis acid titanium centers and available -NH, sites in two sizeable pores for cooperative cycloaddition of CO2 to epoxides at room temperature and atmospheric pressure. The selective grafting of molecules to heterometallic clusters adds up to the pool of methodologies available for controlling the positioning and distribution of chemical functions in precise positions of the framework required for definitive control of pore chemistr…

Structural reorganization in a hydrogen-bonded organic framework

Self-recognition of 3,3′,5,5′-azobenzenetetracarboxylic acid drives the formation of a grid-like anionic hydrogen-bonded framework with channels occupied by organic cations. This supramolecular solid is capable of reorganizing its connectivity in the presence of specific guests into a different crystalline architecture by sequential dissolution and recrystallization.

Reversible guest-induced gate-opening with multiplex spin crossover responses in two-dimensional Hofmann clathrates.

Spin crossover (SCO) compounds are very attractive types of switchable materials due to their potential applications in memory devices, actuators or chemical sensors. Rational chemical tailoring of these switchable compounds is key for achieving new functionalities in synergy with the spin state change. However, the lack of precise structural information required to understand the chemical principles that control the SCO response with external stimuli may eventually hinder further development of spin switching-based applications. In this work, the functionalization with an amine group in the two-dimensional (2D) SCO compound {Fe(5-NH2Pym)2[MII(CN)4]} (1M, 5-NH2Pym = 5-aminopyrimidine, MII =…

Divergent Adsorption-Dependent Luminescence of Amino-Functionalized Lanthanide Metal-Organic Frameworks for Highly Sensitive NO2 Sensors

International audience; A novel gas sensing mechanism exploiting lanthanide luminescence modulation upon NO2 adsorption is demonstrated here. Two isostructural lanthanide-based metal–organic frameworks (MOFs) are used, including an amino group as the sensitive recognition center for NO2 molecules. The transfer of energy from the organic ligands to Ln is strongly dependent on the presence of NO2, resulting in an unprecedented photoluminescent sensing scheme. Thereby, NO2 exposition triggers either a reversible enhancement or a decrease in the luminescence intensity, depending on the lanthanide ion (Eu or Tb). Our experimental studies combined with density functional theory and complete activ…

Surfactant-assisted synthesis of titanium nanoMOFs for thin film fabrication

We use dodecanoic acid as a modulator to yield titanium MOF nanoparticles with good control of size and colloid stability and minimum impact to the properties of the framework to enable direct fabrication of crystalline, porous thin films. ispartof: CHEMICAL COMMUNICATIONS vol:57 issue:72 pages:9040-9043 ispartof: location:England status: published

Innentitelbild: Selective Implantation of Diamines for Cooperative Catalysis in Isoreticular Heterometallic Titanium–Organic Frameworks (Angew. Chem. 21/2021)

Correction: Effect of nanostructuration on the spin crossover transition in crystalline ultrathin films

Correction for ‘Effect of nanostructuration on the spin crossover transition in crystalline ultrathin films’ by Víctor Rubio-Giménez et al., Chem. Sci., 2019, DOI: 10.1039/c8sc04935a.

Inside Cover: Selective Implantation of Diamines for Cooperative Catalysis in Isoreticular Heterometallic Titanium–Organic Frameworks (Angew. Chem. Int. Ed. 21/2021)

Correction: One-pot synthesis of a new generation of hybrid bisphosphonate polyoxometalate gold nanoparticles as antibiofilm agents

A reduced polyoxovanadate functionalized with bisphosphonate molecules was synthesized and used to prepare in one step hybrid organic–inorganic polyoxometalate decorated gold nanoparticles. These new composites were shown to strongly inhibit P. aeruginosa and S. epidermidis biofilm growth, with the three components constituting the nanoparticles (Au0 core, vanadium and alendronate) acting synergistically.

Heterometallic Titanium–Organic Frameworks by Metal-Induced Dynamic Topological Transformations

Reticular chemistry has boosted the design of thousands of metal and covalent organic frameworks for unlimited chemical compositions, structures, and sizable porosities. The ability to generate porous materials at will on the basis of geometrical design concepts is responsible for the rapid growth of the field and the increasing number of applications derived. Despite their promising features, the synthesis of targeted homo- and heterometallic titanium–organic frameworks amenable to these principles is relentlessly limited by the high reactivity of this metal in solution that impedes the controlled assembly of titanium molecular clusters. We describe an unprecedented methodology for the syn…

Heterometallic Titanium-Organic Frameworks as Dual Metal Catalysts for Synergistic Non-Buffered Hydrolysis of Nerve Agent Simulants

Heterometallic metal-organic frameworks (MOFs) can offer important advantages over their homometallic counterparts to enable targeted modification of their adsorption, structural response, electronic structure, or chemical reactivity. However, controlling metal distribution in these solids still remains a challenge. The family of mesoporous titanium-organic frameworks, MUV-101(M), displays heterometallic TiM2 nodes assembled from direct reaction of Ti(IV) and M(II) salts. We use the degradation of nerve agent simulants to demonstrate that only TiFe2 nodes are capable of catalytic degradation in non-buffered conditions. By using an integrative experimental-computational approach, we rational…

Electronic, Structural and Functional Versatility in Tetrathiafulvalene-Lanthanide Metal-Organic Frameworks

<div>Tetrathiafulvalene-Lanthanide (TTF-Ln) Metal-Organic Frameworks (MOFs) are an interesting class of multifunctional materials in which porosity can be combined with electronic properties such as electrical conductivity, redox activity, luminescence and magnetism. Herein we report a new family of isostructural TTF-Ln MOFs, denoted as <b>MUV-5(Ln)</b> (Ln = Gd, Tb, Dy, Ho, Er), exhibiting semiconducting properties as a consequence of the short intermolecular S···S contacts established along the chain direction between partially oxidised TTF moieties. In addition, this family shows photoluminescence properties and single-molecule magnetic behaviour, finding near-infrared …

Fe-MOF Materials as Precursors for the Catalytic Dehydrogenation of Isobutane.

We investigate the use of a series of iron-based metal–organic frameworks as precursors for the manufacturing of isobutane dehydrogenation catalysts. Both the as-prepared and spent catalysts were characterized by PXRD, XPS, PDF, ICP-OES, and CHNS+O to determine the physicochemical properties of the materials and the active phases responsible for the catalytic activity. In contrast to the previous literature, our results indicate that (i) the formation of metallic Fe under reaction conditions results in secondary cracking and coke formation; (ii) the formation of iron carbide only contributes to coke formation; and (iii) the stabilization of the Fe2+ species is paramount to achieve sta…

Crystalline supramolecular organic frameworksviahydrogen-bonding between nucleobases

We report a crystalline supramolecular framework assembled by H-bonding interactions between covalently fused monomers equipped with two guanine-cytosine nucleobase pairs.

Permanent Porosity in Hydroxamate Titanium-Organic Polyhedra.

Following the synthesis of hydroxamate titanium–organic frameworks, we now extend these siderophore-type linkers to the assembly of the first titanium–organic polyhedra displaying permanent porosity. Mixed-linker versions of this molecular cage (cMUV-11) are also used to demonstrate the effect of pore chemistry in accessing high surface areas of near 1200 m2·g–1.

Effect of nanostructuration on the spin crossover transition in crystalline ultrathin films† †Electronic supplementary information (ESI) available: Materials and methods, supplementary figures and tables. See DOI: 10.1039/c8sc04935a

Film thickness and microstructure critically affect the spin crossover transition of a 2D coordination polymer.

Ultrathin Films of 2D Hofmann-Type Coordination Polymers: Influence of Pillaring Linkers on Structural Flexibility and Vertical Charge Transport

Searching for novel materials and controlling their nanostructuration into electronic devices is a challenging task ahead of chemists and chemical engineers. Even more so when this new application requires an exquisite control over the morphology, crystallinity, roughness and orientation of the films produced. In this context, it is of critical importance to analyze the influence of the chemical composition of perspective materials on their properties at the nanoscale. We report the fabrication of ultrathin films (thickness < 30 nm) of a family of FeII Hofmann-like coordination polymers by using an optimized liquid phase epitaxy (LPE) set-up. The series [Fe(L)2{Pt(CN)4}] (L = pyridine, pyri…

Surface functionalization of metal-organic frameworks for improved moisture resistance

Metal-organic frameworks (MOFs) are a class of porous inorganic materials with promising properties in gas storage and separation, catalysis and sensing. However, the main issue limiting their applicability is their poor stability in humid conditions. The common methods to overcome this problem involve the formation of strong metal-linker bonds by using highly charged metals, which is limited to a number of structures, the introduction of alkylic groups to the framework by post-synthetic modification (PSM) or chemical vapour deposition (CVD) to enhance overall hydrophobicity of the framework. These last two usually provoke a drastic reduction of the porosity of the material. These strategie…

Chemical Engineering of Photoactivity in Heterometallic Titanium–Organic Frameworks by Metal Doping

[EN] We report a new family of titanium-organic frameworks that enlarges the limited number of crystalline, porous materials available for this metal. They are chemically robust and can be prepared as single crystals at multi-gram scale from multiple precursors. Their heterometallic structure enables engineering of their photoactivity by metal doping rather than by linker functionalization. Compared to other methodologies based on the post-synthetic metallation of MOFs, our approach is well-fitted for controlling the positioning of dopants at an atomic level to gain more precise control over the band-gap and electronic properties of the porous solid. Changes in the band-gap are also rationa…

Implementation of slow magnetic relaxation in a SIM-MOF through a structural rearrangement

&lt;p&gt;Here we report the structural flexibility of a Dy-based Single-Ion Magnet MOF in which its magnetic properties can be modified through a ligand substitution process involving an increase of the charge density of the coordination environment.&lt;/p&gt;

A Crystalline 1D Dynamic Covalent Polymer

The synthesis of crystalline one-dimensional polymers provides a fundamental understanding about the structure??? property relationship in polymeric materials and allows the preparation of materials with enhanced thermal, mechanical, and conducting properties. However, the synthesis of crystalline one-dimensional polymers remains a challenge because polymers tend to adopt amorphous or semicrystalline phases. Herein, we report the synthesis of a crystalline one-dimensional polymer in solution by dynamic covalent chemistry. The structure of the polymer has been unambiguously confirmed by microcrystal electron diffraction that together with charge transport studies and theoretical calculations…

Surface Functionalization of Metal–Organic Framework Crystals with Catechol Coatings for Enhanced Moisture Tolerance

Robust catechol coatings for enhanced moisture tolerance were produced in one step by direct reaction of Hong Kong University of Science and Technology (HKUST) with synthetic catechols. We ascribe the rapid formation of homogeneous coatings around the metal–organic framework particles to the biomimetic catalytic activity of Cu(II) dimers in the external surface of the crystals. Use of fluorinated catechols results in hydrophobic, permeable coatings that protect HKUST from water degradation while retaining close to 100% of its original sorption capacity.

Bottom‐Up Fabrication of Semiconductive Metal-Organic Framework Ultrathin Films

Though generally considered insulating, recent progress on the discovery of conductive porous metal-organic frameworks (MOFs) offers new opportunities for their integration as electroactive components in electronic devices. Compared to classical semiconductors, these metal-organic hybrids combine the crystallinity of inorganic materials with easier chemical functionalization and processability. Still, future development depends on the ability to produce high-quality films with fine control over their orientation, crystallinity, homogeneity, and thickness. Here self-assembled monolayer substrate modification and bottom-up techniques are used to produce preferentially oriented, ultrathin, con…

Photoactivity and Chemical Reactivity in Titanium(IV)-Organic Frameworks

La presente tesis doctoral ha sido realizada como compendio de publicaciones y lleva por título “Fotoactividad y reactividad química en redes metal-orgánicas de titanio(IV)” (Photoactivity and Chemical Reactivity in Titanium(IV)-Organic Frameworks). La tesis se encuentra dividida en cinco capítulos además de un capítulo final de conclusiones y un resumen en castellano. El primer capítulo trata de una introducción acerca de las redes metal-orgánicas (del inglés Metal-Organic Frameworks, MOFs) de titanio(IV) existentes hasta la fecha para dar una visión general de su variedad estructural, así como de las estrategias sintéticas empleadas y las propiedades fotocatalíticas de estos materiales. E…

Hydroxamate Titanium–Organic Frameworks and the Effect of Siderophore-Type Linkers over Their Photocatalytic Activity

The chemistry of metal–organic frameworks (MOFs) relies on the controlled linking of organic molecules and inorganic secondary building units to assemble an unlimited number of reticular frameworks. However, the design of porous solids with chemical stability still remains limited to carboxylate or azolate groups. There is a timely opportunity to develop new synthetic platforms that make use of unexplored metal binding groups to produce metal–linker joints with hydrolytic stability. Living organisms use siderophores (iron carriers in Greek) to effectively assimilate iron in soluble form. These compounds make use of hard oxo donors as hydroxamate or catecholate groups to coordinate metal Lew…

CCDC 2018380: Experimental Crystal Structure Determination

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CCDC 2018391: Experimental Crystal Structure Determination

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CCDC 1934948: Experimental Crystal Structure Determination

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CCDC 2016312: Experimental Crystal Structure Determination

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CCDC 2018392: Experimental Crystal Structure Determination

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CCDC 2106824: Experimental Crystal Structure Determination

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CCDC 1576297: Experimental Crystal Structure Determination

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CCDC 2010363: Experimental Crystal Structure Determination

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CCDC 2106822: Experimental Crystal Structure Determination

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CCDC 1576296: Experimental Crystal Structure Determination

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CCDC 2018389: Experimental Crystal Structure Determination

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CCDC 1960226: Experimental Crystal Structure Determination

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CCDC 1855292: Experimental Crystal Structure Determination

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CCDC 2018381: Experimental Crystal Structure Determination

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CCDC 2010365: Experimental Crystal Structure Determination

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CCDC 1934950: Experimental Crystal Structure Determination

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CCDC 1855294: Experimental Crystal Structure Determination

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CCDC 1884457: Experimental Crystal Structure Determination

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CCDC 1965235: Experimental Crystal Structure Determination

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CCDC 2018390: Experimental Crystal Structure Determination

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CCDC 1910991: Experimental Crystal Structure Determination

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CCDC 1934947: Experimental Crystal Structure Determination

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CCDC 2018379: Experimental Crystal Structure Determination

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CCDC 2010361: Experimental Crystal Structure Determination

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CCDC 1934945: Experimental Crystal Structure Determination

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CCDC 2018384: Experimental Crystal Structure Determination

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CCDC 2018386: Experimental Crystal Structure Determination

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CCDC 1910989: Experimental Crystal Structure Determination

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CCDC 1934949: Experimental Crystal Structure Determination

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CCDC 2018388: Experimental Crystal Structure Determination

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CCDC 2010360: Experimental Crystal Structure Determination

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CCDC 1934946: Experimental Crystal Structure Determination

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CCDC 2106823: Experimental Crystal Structure Determination

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CCDC 2010362: Experimental Crystal Structure Determination

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CCDC 2010366: Experimental Crystal Structure Determination

Related Article: Lucía Piñeiro-López, Francisco-Javier Valverde-Muñoz, Elzbieta Trzop, M. Carmen Muñoz, Maksym Seredyuk, Javier Castells-Gil, Iván da Silva, Carlos Martí-Gastaldo, Eric Collet, José Antonio Real|2021|Chemical Science|12|1317|doi:10.1039/D0SC04420B

CCDC 2018382: Experimental Crystal Structure Determination

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CCDC 2018383: Experimental Crystal Structure Determination

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CCDC 2018387: Experimental Crystal Structure Determination

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CCDC 2010364: Experimental Crystal Structure Determination

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CCDC 2018385: Experimental Crystal Structure Determination

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