Hg2(OH)[BF4], the First Basic Mercurous Tetrafluoroborate

The first basic mercurous tetrafluoroborate, Hg₂(OH)[BF₄], was obtained through a synproportionation reaction of red mercuric oxide, HgO, and elemental mercury in a 35% solution of HBF₄ in water as colourless single crystals. The crystal structure (orthorhombic, Pbca, Z = 8, a = 985.0(1), b = 991.0(1), c = 1141.0(2) pm) contains [(HO)_1/2—Hg—Hg—(OH)_1/2]⁺ zig‐zag chains that are further connected via weak Hg—OH interchain interactions to layers between which the [BF₄]^— are located in an up and down fashion.     

LiTiCl3: Synthesis and thermal behaviour

LiTiCl₃ is obtained as one example within an ample solid solution, Li_24–2nTi_nCl₂₄ (?4?n?10), by synpropotionation of TiCl₃ and Ti in the presence of LiCl (2:1:3 molar ratio) in sealed tantalum tubes at 750°C. It crystallizes with the inverse spinel-type structure according to (Li_0.67)^[4](Li_0.67Ti_1.33)^[4]Cl₄ with, at 25°C, a = 1048.62(4) pm, space group Fd3m. Thermal expansion is linear with α = 4.85 × 10^?5K^?1 up to about 300°C and thereafter, when the migration of Li⁺ from tetrahedral to octahedral interstices becomes increasingly important, it exhibits a relative decrease resulting, finally, in the phase transition to a NaCl-type structure that is observed for the first time at about 575°C.     

Ternäre Lithium-Selten-Erd-Nitrate mit einsamen Nitrationen: Li3[M(NO3)5](NO3) (M = Gd?Lu,Y). Die Kristallstruktur von Li3Er(NO3)6

Ternary Lithium Rare Earth Nitrates with Lonesome Nitrate Ions: Li₃[M(NO₃)₅](NO₃) (M = Gd? Lu, Y). The Crystal Structure of Li₃Er(NO₃)₆ Single crystals of the ternary nitrate Li₃Er(NO₃)₆ are obtained from a solution of “Er(NO₃)₃” in the melt of LiNO₃. In Li₃Er(NO₃)₆ (monoclinic, P2₁/n, Z = 4; a = 776.0(1); b = 748.86(8); c = 2 396(1) pm; β = 90.76(3)°; R1 = 0.0490; wR2 = 0.0792), Er³⁺ is surrounded by five bidentate nitrate ligands yielding the anionic units [Er(NO₃)₅]^2?. These are arranged in the direction of the 2₁ screw axis. Two lonesome NO₃^? ions are in the middle of such a “helix” and are connected by Li⁺ with the anions [Er(NO₃)₅]^2?. The helices are moved against each other by about half of the lattice constant a and are connected by further Li⁺ ions.     

1H-CRAMPS Solid-State NMR and X-Ray Crystal Studies of Inclusion Complexes Formed from 3,3′-bis(9-Hydroxy-9-fluorenyl)-2,2′-binaphthyl Hosts with Acetone

The crystal structures of inclusion compounds of 3,3-bis(9-hydroxy-9-fluorenyl)-2,2-binaphthyl host (1) and its chloro (2) or bromo (3) derivatives substituted in 2,7-positions of the fluorene units with acetone guests (1A–3A) were determined by X-ray studies as well as by ¹H-CRAMPS solid-state NMR. Using this NMR technique allows identification of differently bound guest molecules due to their different chemical shifts caused by the influence of the ring current effects of the host aryl units.     

XRD-Studies of SiC/Si layers on carbon substrates

Structural investigations of thin films of SiC, SiC with free silicon and various titanium suicides (TiSi₂, TiSi and Ti₅Si₃) are described. The crystal phases have been identified using X-ray diffractometry. The growth of reaction products from surface reactions between silicon and deposited titanium can be observed.Dedicated to Professor Dr. rer.nat. Dr. h.c. Hubertus Nickel on the occasion of his 65th birthday     

Phasentransferkatalysatoren auf Basis von Saccharose-Ethylenoxid-Addukten

Sucrose ethyleneoxide adducts have been prepared by reaction of sucrose with various amounts of ethyleneoxide inDMSO. The resulting polypode molecules were found to be efficient phase transfer catalysts in nucleophilic substitutions, oxidation and dichlorcarbene generation. Polymerisable polypodes have been obtained by reaction of sucrose ethyleneoxide adducts with methacrylic anhydride or methacryloylchloride in pyridine. Free radical polymerisation of the resulting mixtures of mono- and polyfunctional methacrylic esters of sucrose ethyleneoxide adducts yielded crosslinked gels. These polymer-supported octopus-molecules were found to be efficient triphase catalysts.

     

Synthesis,Crystal Structure,and Spectral Properties of a Cobalt(II) Complex with N‐Salicylidene‐p‐Toluidine

The complex Co(C₁₄H₁₃NO)₂Cl₂ with the protonated N‐salicylidene‐p‐toluidine ligand was synthesized from an ethanolic solution of CoCl₂·6H₂O and N‐salicylidene‐p‐toluidine. The crystal structure was determined from X‐ray single crystal data (monoclinic, space group Cc, a = 1496.2(3) pm, b = 1257.4(4) pm, c = 1544.6(3) pm, β = 115.01(1)°, Z = 4). Co²⁺ adopts a distorted tetrahedral geometry. The UV‐Vis and IR spectra of the complex are discussed.     

Relative Abundance of Alpha-Amylase/Trypsin Inhibitors in Selected Sorghum Cultivars

Sorghum is of growing interest and considered as a safe food for wheat related disorders. Besides the gluten, α-amylase/trypsin-inhibitors (ATIs) have been identified as probable candidates for these disorders. Several studies focused on wheat-ATIs although there is still a lack of data referring to the relative abundance of sorghum-ATIs. The objective of this work was therefore to contribute to the characterization of sorghum ATI profiles by targeted proteomics tools. Fifteen sorghum cultivars from different regions were investigated with raw proteins ranging from 7.9 to 17.0 g/100 g. Ammonium bicarbonate buffer in combination with urea was applied for protein extraction, with concentration from 0.588 ± 0.047 to 4.140 ± 0.066 mg/mL. Corresponding electrophoresis data showed different protein profiles. UniProtKB data base research reveals two sorghum ATIs, {"type":"entrez-protein","attrs":{"text":"P81367","term_id":"3913899","term_text":"P81367"}}P81367 and {"type":"entrez-protein","attrs":{"text":"P81368","term_id":"3913900","term_text":"P81368"}}P81368; both reviewed and a targeted LC–MS/MS method was developed to analyze these. Quantifier peptides ELAAVPSR ({"type":"entrez-protein","attrs":{"text":"P81367","term_id":"3913899","term_text":"P81367"}}P81367) and TYMVR ({"type":"entrez-protein","attrs":{"text":"P81368","term_id":"3913900","term_text":"P81368"}}P81368) were identified and retained as biomarkers for relative quantification. Different reducing and alkylating agents were assessed and combination of tris (2 carboxyethyl) phosphine/iodoacetamide gave the best response. Linearity was demonstrated for the quantifier peptides with standard recovery between 92.2 and 107.6%. Nine sorghum cultivars presented up to 60 times lower ATI contents as compared to wheat samples. This data suggests that sorghum can effectively be considered as a good alternative to wheat.