The syntheses and crystal structures of the monopotassium salts of difluorinated and tri/perfluorinated trimesic acid (1,3,5-benzenetricarboxylic acid ≡ H 3 BTC) are presented, namely, K(H 2 dF-BTC) (Fdd2, Z = 16) and K(H 2 pF-BTC) (Cc, Z = 4). For the first time, together with already known K(H 2 mF-BTC), all fluorination degrees of trimesic acid are accessible and can be used for a systematic study of the influence of fluorination on the stability of the resulting coordination polymers and metal−organic frameworks (MOFs). The monopotassium salts show a decreasing (chemical) stability in water upon heating, as well as a decreasing thermal stability, as evidenced by differential scanning calorimetry/ thermogravimetric analysis (DSC/TGA). A similar decreasing thermal stability is found for two series of isostructural coordination polymers (UHM-33 topology:• 1 / 2 H 2 O with L 2− = HBTC 2-, HmF-BTC 2− and HdF-BTC 2− ). Remarkably, while the decomposition temperatures decrease with increasing fluorination of the linker, the releasing temperatures for embedded solvent molecules (DMA and H 2 O, respectively) increase. To identify possible candidates for the synthesis of isostructural coordination polymers and MOFs with BTC 3− ligands with different degrees of fluorination, a database-adapted approach was developed, which utilizes the increased torsion angle between the carboxylate groups and the phenyl rings in these materials as a structure-determining parameter.

Abstract. The synthesis of monofluorinated trimesic acid (H 3 mfBTC = 2-fluoro-1,3,5-benzene-tricarboxylic acid) described in the literature leads in fact to its monopotassium salt K(H 2 mfBTC) (1), which was identified by a single crystal structure analysis (Pc, Z = 2). It is obtained as a single-phase product and shows good solubility in water so that from aqueous solutions fourteen new coordination polymers with Ln III cations were synthesized and structurally characterized.

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Starting from the potassium salt of monofluorinated trimesic acid, K[H2mfBTC], and the respective lanthanide nitrates, Ln(NO3)3 · xH2O, 14 new coordination polymers were obtained and characterized by X‐ray single crystal structure analyses. Depending on the size of the Ln3+ cations three different structure types were observed with chain‐like (Ln = La‐Gd and Er‐Lu) or layer‐like (Ln = Tb‐Ho) polymeric units. The Eu3+ and Tb3+ compounds show an intense red and green luminescence. Details are discussed in the article by Uwe Ruschewitz et al. on page http://onlinelibrary.wiley.com/doi/10.1002/zaac.201700108/abstract.

Reaction of Sc(NO3)3·5H2O with K(H2 pF-BTC) – the monopotassium salt of perfluorinated trimesic acid – led to the formation of single crystals of [ Sc ( p F − BTC ) ( H 2 O ) 3 ] ∞ 1 ⋅ 4 H 2 O ${}_{\infty }{}^{1}[\text{Sc}(pF-\text{BTC}){({\text{H}}_{2}\text{O})}_{3}]\cdot 4{\text{H}}_{2}\text{O}$ ( P 1 ‾ $P‾{1}$ , Z = 2). DTA/TGA measurements revealed that all water molecules were released below 200 °C. Using powder synchrotron radiation diffraction data, the crystal structure of the residue of the dehydration was elucidated and the results confirmed the formula [ Sc ( p F − BTC ) ] ∞ 3 ${}_{\infty }{}^{3}[\text{Sc}(pF-\text{BTC})]$ (Fddd, Z = 16). The compound is similar, but not isostructural to the recently published UoC-4 (I41/amd, Z = 8; UoC: University of Cologne) with a difluorinated trimesate (dF-BTC3–) as connecting linker. Both compounds can be classified as metal-organic frameworks (MOFs) consisting of a 3D network of Sc3+ nodes connected by the fluorinated trimesate ligands. They contain small pores, but their opening windows are too small for any guest molecules to pass. Remarkably, UoC-4 with a lower symmetric ligand (dF-BTC3–) crystallizes in a higher symmetry space group (I41/amd) than UoC-6 (Fddd). This can be rationalized by increasing torsion angles of the carboxylate moieties in the pF-BTC3– ligand.