A novel cadmium(II) complex, [CdCl3(HAEP)H2O]& sdot;H2O (HAEP = 1-(2-aminoethyl)piperazinium), was synthesized and characterized. Single-crystal X-ray diffraction reveals a slightly distorted octahedral geometry around the Cd(II) center, stabilized by a three-dimensional hydrogen-bonding network. DFT calculations indicate high electronic stability and charge-transfer potential. Molecular docking suggests moderate binding affinity to Alzheimer's-related enzymes (AChE, BChE, GR). Impedance spectroscopy reveals non-Debye dielectric relaxation and thermally activated localized conduction regimes associated with the heterogeneous hydrogen-bonded framework formed by protonated HAEP cations, chloride ligands, and coordinated/lattice water molecules. The combined structural, electronic, and in silico analyses highlight the complex's potential in coordination chemistry and bioinorganic applications.

The most challenging aspect of the structural elucidation of novel metal-organic frameworks (MOFs) is presumably the small crystal size of the obtained compounds, since nanocrystallites cannot be analysed by X-ray single crystal diffraction without special equipment. In this paper, we present a new method based on the example of the well-known MIL-88A with which the size of the MOF crystals can be significantly increased by varying the reactants. It was shown that by replacing the originally used fumaric acid with fumaric acid esters, the fumarate ions are successively added to the reaction mixture because of the required ester hydrolysis, which results in a controlled growth of large MIL-88A crystals. In addition to the previously existing Rietveld refinements, it was thereby possible to obtain the first single crystal structure analysis of MIL-88A. This new method for growing large MOF crystals may thus provide access to the structural elucidation of further MOFs and offers a field of applications, such as the investigation of chemical reactions on defined MOF crystal surfaces.

A new, less hazardous synthetic pathway to chloropentaphenyldisilane, ClSi2Ph5, has been developed. Starting from this compound and lithium diorganophosphides, the two previously unknown diorganophosphanyldisilanes (diphenylphosphanyl)pentaphenyldisilane, Ph2PSi2Ph5, and (di-iso-propylphosphanyl)pentaphenyldisilane, (i-Pr)2PSi2Ph5, were prepared. To compare these compounds with the corresponding monosilanes, the known (diphenylphosphanyl)triphenylsilane, Ph2PSiPh3, and the unknown (di-iso-propylphosphanyl)triphenylsilane, (i-Pr)2PSiPh3, were prepared, too. The former was prepared via new synthetic routes. The compounds were characterized with IR-, Raman-, 31P-, 29Si-, and 1H-NMR spectroscopy and melting point determination. Single crystal structure analyses of ClSi2Ph5 and (i-Pr)2PSiPh3 were carried out and confirm the results presented.

[1,4,7,10-Tetraazacyclododecano-κ4N1,4,7,10(3-)]silicon(IV) chloride was synthesized from 1,4,7,10-tetraazacyclododecane (cyclen), n-butyl lithium, and silicon tetrachloride. The crystal structure analysis reveals that this cationic compound is a dimer in the solid state with pentacoordinate silicon atoms. The compound was characterized by melting point, IR, and NMR spectroscopy. The quantum chemical analysis shows that this compound might be an interesting precursor to generate a mononuclear silicon (IV) complex with unusual reactivity due to nearly planar tetracoordinate coordination geometry at the silicon atom.

Thiocyameluric acid C 6 N 7 S 3 H 3 was reacted with various aqueous solutions of metal hydroxides and other metal salts, as well as ammonia. Crystalline products were obtained from reaction mixtures containing main group metal hydroxides. Only in the case of strontium hydroxide single crystals of Sr[HC 6 N 7 S 3 ]·6H 2 O suitable for an X-ray structure analysis were formed. Similar to other cyamelurates containing anions like [C 6 N 7 O 3 ] 3– , [HC 6 N 7 O 3 ] 2– or [H 2 C 6 N 7 O 3 ] – , or analogous melonates [C 6 N 7 (NCN) 3 ] 3– , the anion [HC 6 N 7 S 3 ] 2– in the title salt is completely planar. The hydrogen atom is located at a terminal N atom, which indicates that mono- and di-hydrogen thiocyamelurates and thiocyameluric acid preferably occur as thioketone tautomeric isomers, and are not encountered in the thiol form, at least in the solid state. Since all water molecules coordinate the strontium atoms and the anions do not act as ligands the salt may be described as [Sr(H 2 O) 6 ][HC 6 N 7 S 3 ].

XRD, FT-IR, Hirshfeld surface, TG-DTA, and ultimately a DFT calculation using Gaussian software were used to describe the novel perovskite based on chloromercurate(II) compound, bis(3-amino-2-chloropyridinium) tetrachloromercurate(II), (C5H6ClN2)2HgCl4. The material's overall structure can be described as an alternation of tetrachloromercurate(II) anions and 3-amino-2-chloropyridinium cations. H-bonding and pi-pi interactions contribute to the harmony and stability of the crystalline structure. The investigation of Hirshfeld's surface allows us to calculate the percentages of intermolecular interactions in the structure of the title compound. FT-IR spectroscopy was used to identify the functional groups. Thermal study reveals three endothermic peaks recorded at 406, 435, and 575 K, and just one exothermic peak detected at 735 K. The experimental results were validated following DFT calculations. The title compound expected antibacterial action was investigated in silico utilizing molecular docking analysis.

The title SiIV complex, C16H21NO3Si, is built up by a tridentate dinegative Schiff base ligand bound to a sila-cyclo-hexane unit. The coordination geometry of the penta-coordinated SiIV atom is a distorted trigonal bipyramid. The presence of the sila-cyclo-hexane ring in the complex leads to an unusual coordination geometry of the SiIV atom with the N atom from the Schiff base ligand and an alkyl-C atom in apical positions of the trigonal bipyramid. There is a disorder of the methyl group at the imine bond with two orientations resolved for the H atoms [major orientation = 0.55 (3)]. In the crystal, C-H⋯O inter-actions are found within corrugated layers of mol-ecules parallel to the ab plane.

[C3H10N][C12H24BO4]·B(OH)3, orthorhombic, Fdd2 (no. 43), a = 30.3986(6) Å, b = 40.4094(13) Å, c = 7.0603(2) Å, V = 8672.8(4) Å3, Z = 16, R gt(F) = 0.0324, wR ref(F 2) = 0.0828, T = 153 K.

Liquid hydrosilanes are required for the production of silicon films. The silicon layers can be processed for electronic devices like transistors or thin-film solar cells. Hydrosilanes are highly reactive and pyrophoric. Therefore, the synthesis of these compounds is challenging and dangerous. The available synthesis methods for hydrosilanes are reviewed and compared.Hydrosilanes are highly attractive compounds, which can be processed as liquids with printing technology to amorphous silicon films on nearly any solid substrate. The silicon layers can be processed for electronic devices like transistors or thin-film solar cells. The endothermic character of hydrosilanes with their positive enthalpies of formation results in favorable properties for processing. The larger the molecules, the lower their decomposition temperature and the higher their photoactivity. Cyclic hydrosilanes such as cyclopentasilane and cyclohexasilane can be easily deposited. The branched neopentasilane is more difficult to deposit but yields better-quality films after processing.The key challenge is the complex synthesis of the precursors and the hydrosilanes. The available preparative methods are presented in this review and their advantages and disadvantages are evaluated. The following synthesis methods are presented and discussed in this article: Wurtz coupling and other reductive coupling processes, dehydrogenative coupling of silanes, plasma synthesis of chlorinated polysilanes, amine- or chloride-induced disproportionations, and transformation of monosilane to higher silanes.Plasma synthesis is already carried out today as a continuous industrial process. The most effective synthesis methods in the laboratory are currently amine- and chloride-induced disproportionations. There is a great need to further optimize the syntheses of hydrosilanes and to develop new simple synthesis variants. image

[SbCl3(C9H11N3S2)(2)], monoclinic, P2(1)/n (no. 14), a = 13.8069(4) & Aring;, b = 13.5739(6) & Aring;, c = 14.0182(5) & Aring;, beta = 94.231(3)degrees, V = 2,620.04(17) & Aring;(3), Z = 4, R- gt (F) = 0.0329, wR(ref)(F-2) = 0.0726, T = 153 K.

The coordination geometry of the penta­coordinated SiIV atom in the title complex is a distorted trigonal bipyramid.

The title SiIV complex, C16H21NO3Si, is built up by a tridentate dinegative Schiff base ligand bound to a silacyclohexane unit. The coordination geometry of the pentacoordinated SiIV atom is a distorted trigonal bipyramid. The presence of the silacyclohexane ring in the complex leads to an unusual coordination geometry of the SiIV atom with the N atom from the Schiff base ligand and an alkyl-C atom in apical positions of the trigonal bipyramid. There is a disorder of the methyl group at the imine bond with two orientations resolved for the H atoms [major orientation = 0.55 (3)]. In the crystal, C—H...O interactions are found within corrugated layers of molecules parallel to the ab plane.

The literature on aluminum coordination networks so far contains data on COO-bridged derivatives exclusively. This paper addresses the question whether or not aluminum complexes, especially carbamate-bridged {Al3(μ3−O)}7+ units, can also form networks via the neutral ligand positions. Our findings show that a highly unexpected polymerization of the aluminum carbamates can occur during the isolation of the initially targeted compound. Although bidentate ligands bind to the neutral ligand coordination sites as expected, they do not act as linker molecules but cause an uncontrolled networking via the carbamate ligands. One- and two-dimensional solution and solid-state NMR experiments were primarily used to investigate the coordination behavior of the ligands and to elucidate the actual obtained product.

C23H19NO3Si, monoclinic, P21/n (no. 14), a = 8.5543(3) Å, b = 24.0927(8) Å, c = 9.7971(4) Å, β = 113.265(3)°, V = 1854.96(12) Å3, Z = 4, Rgt (F) = 0.0355, wRref (F 2) = 0.0932, T = 153 K.

Two polymorphs of the title compound, C20H23N3O2, have been isolated. Polymorph (I) crystallizes in the monoclinic space group P2 1/n and polymorph (II) in the tetra-gonal space group I4 1/a. The main difference between the two polymorphs on the mol-ecular level is the orientation of the n-propyl group. This group is anti-periplanar in (I) and synclinal in (II). The core of the mol-ecule consists of two carbamoyl units bound to an enamine unit. The most prominent features are intra-molecular N-H⋯O hydrogen bonds in both polymorphs. Both polymorphs form dimers with graph set R 2 2(12) via inter-molecular N-H⋯O hydrogen bonds. Adjacent dimers of (I) are connected via a weak C-H⋯O inter-action, resulting in a chain parallel to the crystallographic a-axis. The dimers of (II) are connected by weak C-H⋯π inter-actions, forming inter-molecular chains along the c-axis direction.

In this work, the synthesis and structure of an antimony complex with an aromatic, asymmetric tridentate ligand without an Sb-C bond were studied. Ethoxy(2-salicylidenaminophenolato)antimony(III) was studied with NMR, UV-Vis, and IR spectroscopy and the molecular structure was determined by single crystal X-ray diffraction. The antimony atom is formally tetracoordinate in this molecule. Coordinative unsaturation becomes visible in the solid-state structure where intermolecular Sb…O interactions supplement the coordination sphere of the antimony atom to be hexacoordinated. Quantum chemical calculations were performed in order to obtain a better understanding of the bond properties in the antimony complex. These show a spherical distribution of the lone pair at antimony and polar shared bonds from antimony to the heteroatoms of the tridentate ligand.

We synthesized a series of new antimony(III) compounds by reaction of Sb(OEt)3 with organic ligands of the type E(CH2-CH2-OH)2, with E = NH, NMe, O, S, Se, and Te. The synthesized compounds have the general composition [E(CH2-CH2-O)2]Sb(OEt). For comparison, the compound (O-CH2-CH2-S)Sb(OEt) was prepared. All compounds are characterized using NMR, IR, and Raman spectroscopy. The molecular structures of the products reveal the formation of chelate complexes, wherein the ligand molecules coordinate as tridentate O,E,O-ligands to the antimony atom. Dimer formation in the solid state allows the antimony atoms to reach pentacoordination. Quantum chemical calculations including topological analysis of electron density reveal that there are polar shared bonds between antimony and the oxygen atoms bound to antimony. The interactions between the donor atom E and the Sb atom and the interactions in the dimers can be characterized as Van der Waals interactions. The reactivity of [MeN(CH2-CH2-O)2]Sb(OEt) was investigated as an example. For this purpose, the compound reacted with a range of organic compounds such as carboxylic acids and carboxylic anhydrides and small molecules like CO2 and NH3. This study establishes a new and easy accessible class of antimony(III) compounds, provides new insights into the chemistry of antimony compounds and opens up new opportunities for further research in this field.

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

The title compound, C12H24BN, is an adduct formed from 9-borabi­cyclo­[3.3.1]nonane (9-BBN) and pyrrolidine. It crystallizes in the triclinic space group PUnlabelled Image with three mol­ecules in the asymmetric unit, one of which has disorder of the pyrrolidine ring. The B—N bond lengths are between 1.631 (2) and 1.641 (2) Å. The boron and nitro­gen atoms are bound to one hydrogen atom each. These hydrogen atoms are in anti­periplanar orientation. Both six-membered rings of the 9-BBN unit are in a chair conformation in all three mol­ecules. Differences between the three crystallographic independent mol­ecules are found in the five-membered rings of the pyrrolidine unit. These adopt different twisted and envelope conformations.Unlabelled Image

The title compound was prepared by reaction of the Schiff base ligand N-(2-hydroxy-1-naphthylidene)leucine with dichlorodimethylsilane in the presence of triethylamine as base. The resulting pentacoordinate silicon complex was characterized by NMR, IR, UV-Vis spectroscopy and melting point. The structure was confirmed by single-crystal X-ray diffraction data. It crystallizes in the monoclinic space group Ic with unit cell dimensions a = 7.2030(6), b = 22.9842(14), c = 10.8946(12) Å, β = 96.141(7)°, V = 1793.3(3) Å3, Z = 4.