Structural Diversities of a Series of Cd(II) Coordination Complexes Based on a Flexible Tripodal N-donor Ligand

Three Cd(II) coordination complexes with unique structures and topologies, namely, {[Cd(tttmb)(Hbtc)]·5H2O}n (1), {[Cd(tttmb)(m-phda)(H2O)]·2H2O}n (2), and {[Cd(tttmb)(o-cpla)]·(CH3CN)·(H2O)1.5}n (3), have been successfully synthesized under hydro(solvo)thermally condition based on a flexible tripodal N-contained ligand 1,3,5-tris(1,2,4-triazol-1-ylmethyl)-2,4,6-trimethylbenzene (tttmb) and aromatic polycarboxylate acids (H3btc = 1,2,4-benzenetricarboxylic acid, m-H2phda = 1,3-phenylenediacetic acid and o-H2cpla = Homophthalic acid). Complexes 1–3 were characterized by elemental analysis, IR spectroscopy, X-ray single-crystal diffraction and thermogravimetric analyses. 1 crystallize in the orthorhombic chiral space group P212121 and feature 3D coordination networks. 2 reveals a 2D ladder-like structure with (4,4) topology containing alternating Cd(II)/m-phda2− left- and right-handed helical motifs. 3 exhibits a 3D net with (63)(66)(7·82) topology. The structural and dimensional diversity of these complexes not only indicates that the flexible ligand tttmb exhibits strong coordination ability and diverse coordination modes, but also shows that aromatic polycarboxylates play important roles in constructing the frameworks of complexes. Moreover, the different photoluminescence behaviors of 1–3 have been studied in the solid state.

Synthesis, crystal structure, vibrational study, optical properties and Hirshfeld surface analysis of a new centrosymmetric hybrid material, bis(3-aminoquinolium) tetrachloridocobaltate (II)

Background: The title compound (C9H9N2)2[CoCl4] belongs to a large compound’s family, enriching the new technologies materials range. Objective: The chemical synthesis and the crystal structure are the main goals to reach in this study. In addition, the optoelectronic properties and the material behavior are investigated. Methods: The single-crystal diffraction, photoluminescence, infrared spectroscopy, and several computations are applied in this work to characterize the studied compound. Results: At room temperature, the synthesized (C9H9N2)2[CoCl4] crystallizes in the monoclinic C2/c space group. The cohesion of the 0-D crystal structure is ensured by hydrogen interactions and confirmed by the Hirshfeld surface analysis. Conclusion: A new hybrid compound is discovered and added to the structural database ICDD. The structural study, the spectroscopic investigations, particularly the photoluminescence, indicate that the newly obtained material is promising for interesting application as a non-linear optical material.

Synthesis and Crystal Structure of New Zn(II) Complex with N-[bis(benzylamino)phosphoryl]-2,2,2-trichloroacetamide

The novel binuclear Zn(II) complex of general formula Zn2(L)4(CH3OH)2 where HL is N-[bis(benzylamino)phosphoryl]-2,2,2-trichloroacetamide has been synthesized from non-aqueous solution and characterized by elemental analysis, FTIR and NMR spectroscopy as well by X-ray single crystal diffraction. This complex represents the third example of binuclear complexes with this ligand within four known for today.

BN-Embedded Perylenes

Transition metal catalyzed coupling reaction strategy has been utilized in the synthesis of two novel BN-perylenes starting from halogenated BN-naphthalene derivatives. The molecular structures and packing modes of BN-perylenes were confirmed by NMR spectroscopy and X-ray single-crystal diffraction experiments. Their photophysical properties were further investigated using UV-vis and fluorescence spectroscopy and DFT calculations. Interestingly, the isosteric BN-insertion in perylene system resulted in stronger π-π stacking interaction both in solid and solution phases. The synthesized BN-perylenes are proved to be highly stable and thus provide a new valuable platform for novel organic materials applications which is otherwise inaccessible to date.

Tautomerism troubles: proton transfer modifies the stereochemical assignments in diastereoisomeric structures of spirocyclic 5-methyl-2H-imidazol-4-amine dimers

During the racemization of a novel pharmaceutical spirocyclic imidazole–amine compound, namely, 6′-bromo-N-(6′-bromo-4-methoxy-4′′-methyl-3′H-dispiro[cyclohexane-1,2′-indene-1′,2′′-imidazol]-5′′-yl)-4-methoxy-4′′-methyl-3′H-dispiro[cyclohexane-1,2′-indene-1′,2′′-imidazol]-5′′-imine, C36H41Br2N5O2, two impurities were isolated. These impurities were clearly dimers from mass spectroscopic analysis, however single-crystal diffraction characterization was required for the assignment of stereochemistry. The single-crystal diffraction results revealed subtly different structures to those proposed, due to an unexpected proton transfer. The dimers contain four stereocentres, but two of primary interest, and are centrosymmetric, so after careful structure refinement and close inspection it was possible to unambiguously assign the stereochemistry of both the homochiral [(S),(S)- and (R),(R)-] and the heterochiral [(S),(R)- and (R),(S)-] compounds.

4,5-Dicyano-1,2,3-Triazole—A Promising Precursor for a New Family of Energetic Compounds and Its Nitrogen-Rich Derivatives: Synthesis and Crystal Structures

The nitrogen-rich compounds and intermediates with structure of monocyclic, bicyclic, and fused rings based on 1,2,3-triazole were synthesized and prepared by using a promising precursor named 4,5-dicyano-1,2,3-triazole, which was obtained by the cyclization reaction of diaminomaleonitrile. Their structure and configurational integrity were assessed by Fourier transform-infrared spectroscopy (FT-IR), mass spectrometry (MS), and elemental analysis (EA). Additionally, fourteen compounds were further confirmed by X-ray single crystal diffraction. Meanwhile, the physical properties of four selected compounds (3·H2O, 6·H2O, 10·H2O, and 16) including thermal stability, detonation parameters, and sensitivity were also estimated. All these compounds could be considered to construct more abundant 1,2,3-triazole-based neutral energetic molecules, salts, and complex compounds, which need to continue study in the future in the field of energetic materials.

Hidden and apparent twins in uranyl-oxide minerals agrinierite and rameauite: a demonstration of metric and reticular merohedry

In this work, the structures of chemically related uranyl-oxide minerals agrinierite and rameauite have been revisited and some corrections to the available structure data are provided. Both structures were found to be twinned. The two minerals are chemically similar, and though their structures differ considerably, their unit-cell metrics are similar. Agrinierite was found to be twinned by metric merohedry (diffraction type I), whereas the structure of rameauite is twinned by reticular merohedry (diffraction type II). The twinning of the monoclinic unit cells (true cells) leads to pseudo-orthorhombic or pseudo-tetragonal supercells in the single-crystal diffraction patterns of both minerals. According to the new data and refinement, agrinierite is monoclinic (space group Cm), with a = 14.069 (3), b = 14.220 (3), c = 13.967 (3) Å, β = 120.24 (12)° and V = 2414.2 (12) Å3 (Z = 2). The twinning can be expressed as a mirror in (101) (apart from the inversion twin), which leads to a supercell with a = 14.121, b = 14.276, c = 24.221 Å and V = 2 × 2441 Å3, which is F centered. The new structure refinement converged to R = 3.54% for 6545 unique observed reflections with I > 3σ(I) and GOF = 1.07. Rameauite is also monoclinic (space group Cc), with a = 13.947 (3), b = 14.300 (3), c = 13.888 (3) Å, β = 118.50 (3)° and V = 2434.3 (11) Å3 (Z = 2). The twinning can be expressed as a mirror in (101) (apart from the inversion twin), which leads to a supercell with a = 14.223, b = 14.300, c = 23.921 Å and V = 2 × 2434 Å3, which is C centered. The new structure refinement of rameauite converged to R = 4.23% for 2344 unique observed reflections with I > 3σ(I) and GOF = 1.48. The current investigation documented how peculiar twinning can be, not only for this group of minerals, and how care must be taken in handling the data biased by twinning.

A remark on ab initio indexing of electron backscatter diffraction patterns

There is a growing interest in ab initio indexing of electron backscatter diffraction (EBSD) patterns. The methods of solving the problem are presented as innovative. The purpose of this note is to point out that ab initio EBSD indexing belongs to the field of indexing single-crystal diffraction data, and it is solved on the same principles as indexing of patterns of other types. It is shown that reasonably accurate EBSD-based data can be indexed by programs designed for X-ray data.

Cyclopeptide Derivatives from the Sponge-Derived Fungus Acremonium persicinum F10

Cyclopeptides usually play a pivotal role, either in the viability or virulence of fungi. Two types of cyclopeptides, six new hydroxamate siderophore cyclohexapeptides (1–6), including acremonpeptides E and F, and their complexes with aluminum and ferric ions; one new cyclic pentapeptolide, aselacin D (9); together with a known compound, aselacin C (10), were isolated and characterized from the sponge-derived fungus Acremonium persicinum F10. In addition, two new siderophore analogues chelating gallium ions (Ga3+), Ga (Ⅲ)-acremonpeptide E (7) and Ga (Ⅲ)-acremonpeptide F (8), using isolated acremonpeptides E and F, were prepared. The planar structures of 1–10 were elucidated by HRESIMS and (1D and 2D) NMR. The absolute configurations of amino acids were determined by means of the advanced Marfey’s method and X-ray single-crystal diffraction analysis. X-ray fluorescence (XRF) spectrometer was performed to disclose the elements of compound 1, indicating the existence of aluminum (Al). Al (Ⅲ)-acremonpeptides E (1), Ga (Ⅲ)-acremonpeptides E (5), Al (Ⅲ)-acremonpeptide F (7), and Ga (Ⅲ)-acremonpeptide F (8) displayed high in vitro anti-fungal activities, which are comparable to amphotericin B, against Aspergillus fumigatus and Aspergillus niger.

Two supramolecular compounds constructed by polyacid anion clusters: Synthesis, characterization and performance research

In this paper, two novel organic-inorganic hybrid supramolecule compounds {[Cu·L1’·H2O]·(α-Mo8O26)0.5}n 1 and compound {[Cu·L2’·H2O]·(α-Mo8O26)0.5}n 2 have been synthesized [L1’ = 1, 3-bis (4-carboxylpyridine) propane dibromide, L2’ = 1, 4-bis (4-carboxylpyridine) butane dibromide]. Compounds 1 and 2 have been expressly confirmed by PXRD, IR, X-ray single crystal diffraction and TG. Last, the study found that compounds 1 and 2 have obvious adsorption effects on MB and RhB organic dyes, and compound 2 has high adsorption capacity for MB.