Seven nonporous coordination polymers with tetrafluoroterephthalate (tfBDC 2À ) as a bridging ligand were synthesized and structurally characterized. Homoleptic ∞ 3 [Tl 2 (tfBDC)] (P1, Z = 1, 1) contains six-coordinated Tl centers, which are connected by the tfBDC 2À ligand to form a three-dimensional (3D) network. Upon heating it decomposes at approximately 200 °C. Nine-coordinated PbO 9 polyhedra are found in ∞ 2 [Pb(tfBDC)(H 2 O) 3 ] 3 1/2 H 2 O (P1, Z = 1, 2), which forms a layer-like structure. These layers are held together by hydrogen bonds involving water molecules. These water molecules are released by heating to 70À100 °C. ∞ 1 [M II (tfBDC)(H 2 O) 4 ] (P1, Z = 1; M II = Zn (3), Co (4), Ni (5)) contains almost undistorted M II O 6 octahedra with the carboxylate groups of the tfBDC ligands in trans coordination so that a chain-like structural unit is formed. These chains are further connected by hydrogen bonds. Upon heating, these water molecules are released in two steps at 100 and 200 °C. ∞ 3 [Mn 2 (tfBDC) 2 (DMF) 2 (EtOH)] (P2 1 , Z = 2, 7) is isostructural to the known Zn compound (6). Both compounds contain dimeric [M II O 6 ] 2 units, which are connected by tfBDC 2À ligands to form a 3D network.All compounds are unprecedented in the crystal chemistry of coordination polymers with nonfluorinated terephthalate (BDC 2À ) as bridging ligand. This is mainly because the planar conformation found for BDC 2À is energetically less favorable for perfluorinated tfBDC 2À .

Single crystals of anhydrous thallium acetylenedicarboxylate (Tl 2 (C 4 O 4), 1) and thallium acetylenedicarboxylate oxalate (Tl 4 (C 4 O 4)(C 2 O 4), 2) precipitated from aqueous solutions containing thallium(I)-acetate and the respective organic acids. Both compounds crystallize in non-centrosymmetric space groups (1: P 2 1 2 1 2 1 ; 2: C 2), which is probably caused by stereochemically active lone pairs at Tl(I). The crystal structures of 1 and 2 show some similarities. Tl atoms are organized in corrugated layers, which are connected by the respective carboxylate anions. Upon heating 1 decomposes at 195°C to form elemental pyrophorous thallium powder. 2 starts decomposing at approx. 150°C forming elemental thallium next to another compound, which could not be identified up to now. TlHADC was also synthesized, but its crystal structure could not be solved either from powder or single crystal diffraction data. Upon heating it decomposes to form 1.

On the Synthesis of Binary and Ternary Carbides in a Modified Domestic Microwave Oven By modifying a domestic microwave oven binary and ternary carbides were synthesized from the elements in an argon atmosphere. We succeded in preparing CaC2, Ca4Ni3C5 and MgM3Cx (M = Ni, Co) within several minutes. Well crystallized product powders were obtainend with purities as high as 90 % (CaC2, MgNi3Cx). In the case of MgNi3Cx our experiments show that a product with a high carbon content (x ≈ 1) is only synthesized under optimized conditions (magnesium surplus, reaction time). This product exhibits the expected superconductivity with a critical temperature of approx. 6 K. The syntheses and possible structures of MgPdCxHy (x = 0.4‐0.8, y = 0.4‐2.3) and MgPtC0,06H0,32 are briefly discussed.

From an aqueous solution containing ZnCO 3 , Tl(CH 3 COO), and acetylenedicarboxylic acid (H 2 ADC: HOOC-C≡C-COOH) single crystals of 3 ∞ [Tl 2 Zn(ADC) 2 (H 2 O) 2 ] (1) were obtained. Compound 1 crystallizes in triclinic space group P1 with Z = 1. A slightly distorted octahedral ZnO 6 coordination and a very unsymmetric TlO 6 coordination (Tl-O < 321 pm) are found, the latter probably caused by a stereo-* Prof. Dr. U. Ruschewitz

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