Crystal Structure Of Compound Research Articles

Rational Design of Crystalline and Enantiomerically Pure Helicenes with Open‐Shell Singlet Ground States

AbstractHelicene diradical derivatives have attracted widespread attentions because of their unique magnetic and chiroptoelectronic properties, however, crystalline and enantiomerically pure forms of helicene diradicals are extremely rare. Herein, we describe the rational design and synthesis of o‐quinone functionalized helicene diradicals with crystalline enantiomerical purity. Diradical dianion salt Rac‐3K and its enantiomers P/M‐3K were obtained by reduction of corresponding precursors Rac‐3 and P/M‐3 with two equivalent potassium graphite in THF in the presence of (di)benzo‐18‐crown‐6. Neutral dioxoborocyclic helicene diradicals (Rac‐3B and P/M‐3B) were produced by reactions of Rac‐3 or P/M‐3 with chlorobis(perfluorophenyl)borane (B(C6F5)2Cl. Crystal structures of compounds Rac‐3K, Rac‐3B and P/M‐3K were obtained by single crystal X‐ray diffraction. Their open‐shell singlet state ground states were confirmed by electron paramagnetic resonance (EPR) spectroscopy, superconducting quantum interference device (SQUID) measurements and theoretical calculations. Their chiroptical properties were investigated by the electronic circular dichroism (ECD) spectroscopy. This work provides the first examples of enantiopure helicene diradical dianions and boron‐containing helicene diradicals.

Unusual Metal–organic Multicomponent Ni(II) and Mononuclear Zn(II) Compounds Involving Pyridine dicarboxylates: Supramolecular Assemblies and Theoretical Studies

In the present work, we reported the synthesis and characterization [single crystal X-ray diffraction technique, spectroscopic, etc.] of two new Ni(II) and Zn(II) coordination compounds, viz. [Ni(2,6-PDC)2]2[Ni(en)2(H2O)2]2[Ni(en)(H2O)4]·4H2O (1) and [Zn(2,6-PDC)(Hdmpz)2] (2) (where 2,6-PDC = 2,6-pyridinedicarboxylate, en = ethylene-1,2-diamine, and Hdmpz = 3,5-dimethyl pyrazole). Compound 1 is found to crystallize as a multicomponent Ni(II) compound with five discrete complex moieties, whereas compound 2 is isolated as a mononuclear Zn(II) compound. A deep analysis of the crystal structure of 1 unfolds unusual dual enclathration of guest complex cationic moieties within the supramolecular host cavity stabilized by anion–π, π-stacking, N–H⋯O, C–H⋯O, and O–H⋯O hydrogen bonding interactions. Again, the crystal structure of compound 2 is stabilized by the presence of unconventional C–H⋯π(chelate ring) interactions along with C–H⋯O, C–H⋯N hydrogen bonding, π-stacking, and C–H⋯π(pyridyl) interactions. These non-covalent interactions were further studied theoretically using density functional theory (DFT) calculations, molecular electrostatic potential (MEP) surfaces, non-covalent interaction (NCI) plot index, and quantum theory of atoms in molecules (QTAIM) computational tools. The computational study displays that π-stacking or H bonds greatly tune the directionality of compound 1, although non-directional electrostatic forces dominate energetically. For compound 2, a combined QTAIM/NCI plot analysis confirms the presence of unconventional C–H⋯π(chelate ring) interactions along with other weak interactions obtained from the crystal structure analysis. Further, the individual energy contributions of these weak yet significant non-covalent interactions have also been determined computationally.

Synthesis and characterization of novel spiro-(2,2′-dioxybiphenyl)-cyclotriphosphazene derivatives bearing butylated oxyanisole groups and their antioxidant and antimicrobial activities

In this study, novel cyclotriphosphazene derivatives, {[N3P3(biph)(BA)2] (6a/b), [N3P3(biph)(BA)3] (7), [N3P3(biph)2(BA)Cl (8) and [N3P3(biph)2(BA)2 (9)]}, (biph = 2′,2′′-dioxy-1′,1′′- biphenyl, BA = butylated oxyanisole}, were synthesized from the nucleophilic substitution reactions of butylated hydroxyanisole (BHA) (5) with [N3P3(biph)Cl4] (3) and [N3P3(biph)2Cl2] (4), respectively. The structures of all the products (6a/b, 7, 8 and 9) were determined -using elemental analysis, mass and (1H and 31P) NMR spectroscopic techniques. The molecular and crystal structure of compound 9 was also determined by single crystal X-ray crystallography. At the same time, the compounds (3, 4, 7, 8 and 9) were tested for their antimicrobial and antioxidant (free radical scavenging) activities. Of all, compounds 8 and 9 showed relatively significant antimicrobial activity against the control strains Bacillus cereus DSMZ 4312 (16,5 and 18,25 mm) and against Staphylococcus aureus ATCC 29213 (25 and 22,5 mm) compared to their positive controls. The MIC50 values of compounds 8 and 9 against Bacillus cereus were determined at 125 µg/mL and < 325 µg/mL, respectively, and Staphylococcus aureus at 125 µg/ mL for both compounds. While the other compounds (3, 4 and 7) did not possess antimicrobial properties, they showed strong antioxidant activity. In the antioxidant assay based on the EC50 value of BHA used as a control, compound 7 showed antioxidant activity even at low concentrations such as 9,37 µg/ mL (83 %), while compounds 3 and 4 showed antioxidant properties even at relatively low concentrations such as 18,75 µg/mL. Compounds 8 and 9, two antimicrobial compounds, did not exhibit antioxidant properties.

Synthesis, Crystal Structure and Antifungal Activity of (E)-1-(4-Methylbenzylidene)-4-(3-Isopropylphenyl) Thiosemicarbazone: Quantum Chemical and Experimental Studies.

A novel (E)-1-(4-methylbenzylidene)-4-(3-isopropylphenyl) thiosemicarbazone was synthesized in a one-pot four-step synthetic route. Fourier transform infrared spectroscopy (FTIR), 1H and 13C nuclear magnetic resonances (NMR), single-crystal X-ray diffraction, and UV-visible absorption spectroscopy were utilized to confirm the successful preparation of the title compound. Single-crystal data indicated that the intramolecular hydrogen bond N(3)-H(3)···N(1) and intermolecular hydrogen bond N(2)-H(2)···S(1) (1 - x, 1 - y, 1 - z) existed in the crystal structure and packing of the title compound. Besides the covalent interaction, the non-covalent weak intramolecular hydrogen bond N(3)-H(3)···N(1) discussed by atoms in molecules (AIM) theory also functioned in maintaining the title compound's crystal structure. The strong intermolecular hydrogen bond N(2)-H(2)···S(1) (1 - x, 1 - y, 1 - z) discussed by Hirshfeld surface analysis played a major role in maintaining the title compound's crystal packing. The local maximum and minimum electrostatic potential of the title compound was predicted by electrostatic potential (ESP) analysis. The UV-visible spectra and HOMO-LUMO analysis revealed that the title compound has a low ΔEHOMO-LUMO energy gap (3.86 eV), which implied its high chemical reactivity due to the easy occurrence of charge transfer interactions within the molecule. Molecular docking and in vitro antifungal assays evidenced that its antifungal activity is comparable to the reported pyrimethanil, indicating its usage as a potential candidate for future antifungal drugs.

Mononuclear nickel(II) and copper(II) coordination compounds with ligands based on acetyl(benzoyl)acetone S-methylisothiosemicarbazones and 8-quinolinecarboxaldehyde. Synthesis and crystal structure

Template condensation of S-methylisothiosemicarbazones of acetyl- or benzoylacetone with 8-quinolinecarboxaldehyde in the presence of nickel(II) and copper(II) ions gave four new mononuclear coordination compounds [NiL1]I (I), [CuL1I] (II), [NiL2]I (III) и [CuL2I] (IV). The chemical composition of the products was confirmed by elemental analysis, IR spectroscopy, and mass spectrometry, and the crystal structure of compounds I and II was determined by X-ray diffraction analysis (CCDC no. 2266386, 2266387). X-ray diffraction study revealed a square planar coordination environment of the central ion of the cationic Ni(II) complex and square pyramidal geometry for the molecular Cu(II) complex.

Indole-derivative β-diketone samarium and terbium compounds modified by ancillary ligand: Syntheses, crystal structures, and photoluminescence properties

EIFD, LnCl3·6H2O (Ln = Sm, Tb) and ancillary ligand are developed to synthesize a sequence of six new β-diketone Sm-based and Tb-based compounds modified to enhance the photoluminescence property, namely Sm(EIFD)3(H2O)·CH2Cl2 (1), Sm(EIFD)3(bpy) (2), Sm(EIFD)3(phen)·CH2Cl2 (3), Tb(EIFD)3(H2O)·CH2Cl2 (4) and Tb(EIFD)3(bpy) (5), Tb(EIFD)3(phen)·CH2Cl2 (6) (EIFD: 1-(1-ethyl-1H-indol-3-yl)-4,4,4-trifluorobutane-1,3‑dione, bpy = 2,2′-bipyridine, phen = 1,10-phenanthroline). The crystal structures of compounds 1−6 with the lanthanide(III) ions of seven (1, 4)/eight (2, 3, 5, 6) coordinated configuration are determined by single-crystal X-ray diffraction. Different non-covalent interactions (NCIs) and their% contribution to the compounds structures and their roles in stabilizing the structure are determined by Hirshfeld surface analysis. The photoluminescence properties of compounds 1−6 by substituting the solvent H2O with bpy and phen contained nitrogen ancillary ligands are then studied experimentally, leading to a rationalization of their central lanthanide(III) ions emission lifetime.

Single-crystal X-ray structure, theoretical (Hirshfeld, electronic properties, NBO, NLO, RDG), and molecular docking studies of three phthalimidoethanesulfonamide derivatives

The three N-substituted-2-phtalimidoethanesulfonamide derivatives, 2-(1,3-dioxoisoindolin-2- yl)-N-(2-isopropylphenyl)ethane-1-sulfonamide (I), N-(2,6-dimethylphenyl)-2-(1,3-dioxoiso indolin-2-yl)ethane-1-sulfonamide (II) and 2-(2-(morpholinosulfonyl)ethyl) isoindoline-1,3‑dione (III), were analyzed using a combined approach including single-crystal X-ray diffraction (SC-XRD), theoretical calculations with Density Functional Theory (DFT), and molecular docking studies. Phthalimide and sulfonamide compounds have recently attracted attention for their inhibitory properties against AChE and BChE enzymes. In this study, molecular and crystal structures of compounds have been confirmed by the SC-XRD technique. Optimized molecular geometries and vibrational modes have been examined and compared to experimental results. Frontier molecular orbital (HOMO-LUMO) energies, molecular electrostatic potential (MEP), natural bond orbital (NBO) analysis, and non-linear optical (NLO) properties have been investigated by DFT/B3LYP/6–311G++(d,p) method. The reduced density gradient (RDG) analysis has been performed to analyze the non-covalent interactions. The Hirshfeld surfaces and 2D fingerprint analyses have been used to determine the intermolecular interactions of compounds. Moreover, in silico docking studies are performed to investigate the interactions between N-substituted-2-phtalimidoethane sulfonamide derivatives and AChE and BChE enzymes.

Structure of Manganese Chloride and Threonine Crystals Formed by Slow Vaporization Method

Crystals of complex compounds are used in technology, optics, medicine, pharmacy, surface treatment, etc. The study of the crystal structure of complex compounds is important because they are widely used in industry and exhibit mechanical, thermal and a number of other valuable properties. Study of the crystal structure of complex compound of manganese chloride with the amino acid threonine, as well as the study of its physicochemical and biological properties. For the synthesis of complex compound, the method of slow evaporation was used. The composition of the formed crystals of the compound was analyzed by X-ray diffraction and spectroscopic structural analyses. the structure of the complex compound MnСl2×C4H9NO3manganese chloride and the amino acid threonine was studied. As a result of the study, it was established that the crystal structure of the compound MnСl2×C4H9NO3belongs to the orthorhombic system with space symmetry P212121.

Six-coordinated complexes of Co(II), Ni(II) and Cu(II) chlorides with N-propargylimidazoles: Synthesis, structure, antimicrobial activity, AIM analysis and molecular docking

New six-coordinated N-propargylimidazole complexes with cobalt(II), nickel(II) and copper(II) chlorides, [M(N-propargylimidazole)4Cl2], were obtained in good yields by the reaction of N-propargylimidazole with corresponding metal chlorides. Molecular and crystal structures of compounds 1–3 were studied by X-ray analysis. Numerous non-covalent interactions including halogen bonds and π-stacking forms in the crystal were analyzed in the framework of quantum theory Atom in molecules. An evaluation of the antimicrobial activity of N-propargylimidazole complexes with Co(II), Ni(II) and Cu(II) chlorides in relation to E. durans, B. subtilis and E. coli showed that the complexes of nickel exhibit antimicrobial activity comparable to gentamicin in relation to E. coli. To explore the inhibitory activity mechanism the molecular docking was carry out.

A Novel Organic‐Inorganic Hybrid Material (BTTD)MnCl4 with Intelligent Switching Applications Derived from Unusual Wheels‐Like Motion

AbstractIn recent years, phase change materials (PCMs) have received extensive attention because of their applications in many fields, such as construction, semiconductor, energy and intelligent response switch. Organic‐inorganic hybrid materials (OIHMs) are wide applied in the preparation of PCMs due to their controllability of organic and inorganic components. In this study, we successfully synthesized an organic‐inorganic hybrid material (BTTD)MnCl4 (compound 1, BTTD=[(CH3)2NCH2Cl(CH2)3CH2ClN(CH3)2]. The purity of compound 1 was confirmed by PXRD. The crystal structure of compound 1 was analyzed at 300 K, 381 K and 400 K. The three different crystal structures prove the phase change of compound 1. According to the result of differential scanning calorimeter (DSC), the phase transition of compound 1 is reversible. Moreover, the measured bandgap (Eg) of 1 is 2.25 eV. The dielectric constant of compound 1 fluctuates near 370 K, indicating the changes of electrical properties, so compound 1 can be used to cut off circuit. This temperature is close to the boiling point of water under standard ambient conditions. Therefore, this work provides a new direction for the design of intelligent response switch for electric kettle.

Supramolecular assemblies involving unusual N(nitrile)∙∙∙π(fum) and nitrile-nitrile non-covalent contacts in fumarato and succinato bridged polymers of Co(II) and Ni(II): Experimental and theoretical studies

Two new Co(II) and Ni(II) coordination polymers viz. [Co(H2O)2(μ-fum)(3-CNpy)2]n (1) and {[Ni(H2O)2(μ-succ)(4-CNpy)2]·2H2O}n (2) (where, fum= fumarate, CNpy = cyanopyridine, succ = succinate) have been synthesized and characterized using single crystal XRD, elemental analysis, spectroscopic (IR and electronic) techniques and TGA. Compound 1 crystallizes as a fumarato bridged Co(II) polymer; whereas, compound 2 is a succinato bridged Ni(II) polymer. The presence of various non-covalent interactions in the compounds stabilizes the layered assemblies of the compounds. Antiparallel nitrile∙∙∙nitrile interactions are observed in both the crystal structures involving the nitrile moieties of coordinated CNpy which provide rigidity to the compounds. Further analysis reveals that the N-atom of –CN group of 3-CNpy in 1 is involved in unusual N(nitrile)∙∙∙π(fum) interactions with the π-electrons of the C=C bond of fum. Enclathrated (H2O)2 cores within the supramolecular host cavity of compound 2 provides additional reinforcement to the crystal structure. We have also carried out theoretical studies to analyze the π-stacking and H-bonding interactions present in the crystal structure of compound 1 using quantum theory of atoms-in-molecules (QTAIM), non-covalent interaction plot (NCI plot) and molecular electrostatic potential (MEP) surface analysis. The MEP value at the N-atom of the cyano group of 1 is negative and the value is neutral over the double bond of the fum; indicating the possibilities of formation of N(nitrile)∙∙∙π(fum) interactions. Energetic analysis suggests that antiparallel π-stacking observed between the 3-CNpy moieties in 1 is the most dominating force followed by N(nitrile)∙∙∙π(fum) interaction and finally the H-bonds.

Crystal structures, Hirshfeld surface analysis, thermogravimetric, and spectroscopic properties of three Zn(Ⅱ) complexes bridged by 4,4′-bipy with organic sulfonate anions as counterions

Three Zn(Ⅱ) sulfonate compounds: {[Zn3(Ac)4(4,4′-bipy)4]·2(3-pySO3)·H2O}n (1), {[Zn(4,4′-bipy)(H2O)4]·2(Me-phSO3)}n (2), and {[Zn(4,4′-bipy)(H2O)4]·2(NH2-phSO3)}n (3), were synthesized through solvent diffusion method at room temperature (3-pySO3H = Pyridine-3-Sulfonic acid; Me-phSO3H = P-Toluene Sulfonic acid; NH2-phSO3H = Sulfanilic acid). Single-crystal X-ray diffractions reveal that the crystal structure of compound 1 contains a 2D cationic layer with pseudo-square grid motifs formed by trinuclear Zn(II) units which connected by 4,4′-bipy ligands. Water molecule forms hydrogen bonds with free 3-PySO3− anions which are located in the voids of the cationic grids. Compounds 2 and 3 show isostructural 1D [Zn(4,4′-bipy)(H2O)4]2+ chains with sulfonate anions connected to the chain via hydrogen bonding. The weak interactions in the structures of the three compounds have been assessed using Hirshfeld surface analyses and 2D fingerprint plots. The Hirshfeld surface shows that the most important contributions for the crystal packing are from H···H and H··O/O··H interactions, which indicate dominant van der Waals interactions. In addition, the compounds were investigated by powder X-ray diffraction (PXRD), elemental analyses, UV–vis, FT-IR, solid-state fluorescence spectroscopy, and thermal analyses (TG-DSC).

Complexity of the KNa2ZrF7, KNa2HfF7, and KNa2(Hf,Zr)F7 compounds

New mixed-cation fluorides KNa2HfF7 (Pmn21, a = 8.213(2) Å, b = 6.126(2) Å, c = 5.979(2) Å, Z = 2) and KNa2(Hf,Zr)F7 (refined composition KNa2Hf0.44(1)Zr0.56(1)F7; Pmn21, a = 8.2210(8) Å, b = 6.1288(6) Å, c = 5.979(1) Å, Z = 2) together with isostructural KNa2ZrF7 (Pmn21, a = 8.221(2) Å, b = 6.118(2) Å, c = 5.994(2) Å, Z = 2) have been synthesised in aqueous solutions and structurally characterised at room temperature by powder and single-crystal X-ray diffraction. The solid-solid phase transformations have been revealed during the differential scanning calorimetry experiments and further confirmed by temperature-dependent X-ray powder diffraction. It has been found that mixed-cation phases KNa2ZrF7, KNa2HfF7 and KNa2(Hf,Zr)F7 undergo irreversible phase transformations, which can be explained by their decomposition over 673 K. XPS analysis confirmed the presence of exclusively terminated fluorines around the transition metals and the absence of oxygen impurities in the crystal structures of compounds.

Study on the anti-cancer activity of α-phenethylamine ferrocenecarboxylic acid co-crystals.

Ferrocene derivatives show a wide range of pharmacological activities in the medical field, especially in the anti-tumor field, and can be used as candidate drugs or lead compounds for the treatment of tumors and other diseases. And α-phenethylamine is an important intermediate for the preparation of fine chemical products. (R)-(+)-1-Phenethylamine ferrocenecarboxylic acid/(S)-(-)-1-phenethylamine ferrocenecarboxylic acid were prepared, named compounds 1 and 2, respectively. Single crystal X-ray diffraction showed that compounds 1 and 2 crystallized in the orthorhombic system space group P21 21 21 , and the crystal structures of compounds 1 and 2 exhibited mirror symmetry. The inhibitory effect of two compounds on SW480, MDA-MB-231, and H1299 cells was tested by MTT colorimetry. The IC50 values of the compounds against cancer cells were also calculated. The anti-cancer effect was more pronounced for compounds in the S-configuration. Compound 2 made the wild-type cancer cells undergo apoptosis, thus preventing cancer; it also had the function of helping the cell gene repair defects.

5‐Aryl Substituted 2‐(2‐Methoxyphenyl)benzoxazoles with Large Stokes Shifts: Synthesis, Crystal Structures and Optical Properties

Abstract2‐(2‐methoxyphenyl)benzoxazole (MBO) displays similar photophysical properties to 2‐(2‐hydroxyphenyl)benzoxazole (HBO), but it lacks the large Stokes shifts necessary for fluorescence microscopy applications. In this paper, we report the 5‐substitution of MBO with aryl groups to produce 2‐(4‐methoxy‐[1,1’‐biphenyl]‐3‐yl)benzoxazoles (MBBOs) with large Stokes shifts. The synthesis of MBBOs 6–15 was accomplished in moderate to good yields by microwave‐assisted Sonogashira cross couplings. Crystal structures for compounds 6–9 and 15 are provided. MBBOs 6–10, 12, and 14 displayed considerably blue‐shifted absorption maxima and slight bathochromic shifts of their fluorescence maxima relative to the unsubstituted MBO.

New cyclotriphosphazenes with butylated oxyanisole motif; synthesis, characterization and biological properties

In the present work, new cyclotriphosphazene derivatives containing butylated oxyanisole (BA) group (3, 4a/b, 6a/b, 7, 11a/b and 12) were synthesized and characterized with using elemental analysis, mass, and NMR (1H and 31P) spectroscopic techniques in detailed. The molecular and crystal structure of compound 3 was also determined by single-crystal X-ray crystallography. The antimicrobial activities of the compounds (3, 7 and 12) were evaluated against strains of Staphylococcus aureus ATCC 29213 as Gram positive cocci, Bacillus cereus DSMZ 4312 as Gram positive bacilli, Escherichia coli ATCC 8739 as Gram negative bacilli, and Candida albicans ATCC 10231, a dimorphic yeast species representing fungi as well as antioxidant activities of these compounds. In the biological and antioxidant activity tests carried out, compound 3 stood out with both antibacterial and antioxidant activity compared to other compounds.

Synthesis of a novel triptycene-derived protected dithiolene ligand precursor for tri-nuclear mixed ligand metal dithiolene complexes

Abstract We synthesized a novel triptycene analogue, 3,3′,3″,3″′,3″″,3″″′-((triptycene-2,3,6,7,14,15-hexayl)hexakis(sulfanediyl))hexapropanenitrile (3), which served as a valuable precursor for the triptycene-derived tris-bidentate bridging dithiolene ligand, triptycene-2,3,6,7,14,15-hexakis(thiolate) (4), following the removal of the cyanoethyl moiety protection group. We determined the molecular and crystal structures of compound 3 and confirmed its capacity to yield compound 4. By reacting 3 with [NiCl2(BPY)] and [PtCl2(BPY)] (BPY: 2,2′-bipyridine) in methanol, we obtained crude samples of [Ni3(4)(BPY)3] and [Pt3(4)(BPY)3], respectively.

STRUCTURAL INVESTIGATION AND HIRSHFELD SURFACE ANALYSIS OF TWO [ONO]-TYPE SCHIFF BASES

Two novel [ONO]-type tridentate Schiff base compounds namely (E)-2-(((2-hydroxyphenyl)imino)methyl)-4,5-dimethoxyphenol, C15H15NO4 (1), and (E)-2-(((5-chloro-2-hydroxyphenyl)imino)methyl)-4,5-dimethoxyphenol, C15H14ClNO4 (2) were synthesized. These compounds were characterized using various spectroscopic techniques, including single crystal X-ray diffraction (XRD), infrared (IR), proton nuclear magnetic resonance (1H NMR), carbon-13 nuclear magnetic resonance (13C NMR), and UV-Vis spectroscopy. The X-ray crystallographic analysis revealed that both compounds 1 and 2 contain two independent molecules within the asymmetric unit. Compound 1 crystallizes in the orthorhombic system with the Pna21 space group, while compound 2 crystallizes in the monoclinic system with the P21/c space group. An important feature observed in the crystal structure of compound 1 is the presence of O–H···N and O–H···O hydrogen bonds. In compound 2, the hydrogen bonding interactions involve C–H···O, O–H···O and O–H···N. Additionally, both compounds exhibit C–H···π interactions. To further understand the bonding interactions in compounds 1 and 2, Hirshfeld surface analyses and 2D fingerprint graphs were performed. The results indicate that the Hirshfeld surfaces are predominantly influenced by H⋯H, O⋯H, and C⋯H contacts.

Синтез и строение дииододицианоаурата тетрафенилстибония [Ph4Sb][Au(CN)2l2

The reaction of potassium diiododicyanoaurate with tetraphenylstibonium chloride has led to the synthesis of the [Ph4Sb][Au(CN)2I2] (1) complex. The crystal structure of compound 1 has been determined by X-ray diffraction (XRD) analysis for the first time. According to the XRD data, tetraphenylstibonium diiododicyanoaurate (1) [C26H19N2SbI2Au, M = 931.95; triclinic crystal sys-tem, P–1 space group; cell parameters: a = 8.176(5) Å, b = 9.998(6) Å, c = 18.579(15) Å; a = 84.55(3)°, β = 77.37(3)°, g = 67.42(3)°, V = 1368.4(16) Å3, Z = 2; r(calc.) = 2.262 g/cm3; 2qmax: 5.62°–74.5°; –13 ≤ h ≤ 13, –16 ≤ k ≤ 16, –31 ≤ l ≤ 31; 91938 reflections collected; 14033 independent reflec-tions (Rint = 0.0559); GOOF = 1.033; R-factor 5.95%] has the ionic structure and consists of tetra-phenylstibonium cation with practically undistorted tetrahedral coordination of the antimony atom (the CSbC angles vary in the range 102.2(3)–119.8(2)°; the Sb–C distances vary within 2.087(6)–2.099(6) Å) and two types of almost undistorted square-planar diiododicyanoaurate anions (the trans- and cis-angles are close to 180° and 90° respectively; the Au–I and Au–C distances are 2.5863(13), 2.6071(15) Å and 1.986(8), 1.991(7) Å, respectively). The crystal organization in crystal 1 is caused by the interionic С–H∙∙∙N≡C (2.54, 2.55 Å) and С–H∙∙∙I–Au (3.16 Å) hydrogen bonds, as well as by the weak Sb∙∙∙N≡C contacts with the length of 3.30 Å. Complete tables of atomic coordinates, bond lengths, and bond angles for compound 1 have been deposited with the Cambridge Crystallographic Data Centre (CCDC 1900936) and are available, free of charge, at deposit@ccdc.cam.ac.uk and http://www.ccdc.cam.ac.uk.

Two bimetallic compounds with attractive structures and properties

Two new bimetallic lanthanide-mercury isonicotinic acid compounds were successfully synthesized through classical hydrothermal reactions using DyCl3·6H2O or LuCl3·6H2O, HgCl2, isonicotinic acid, and distilled water. The resulting compounds, [Dy2(IA)6(H2O)2(H3O)2(Hg2Cl5)2]n(3nHgCl2) (1; IA refers to isonicotinic acid anions) and [Lu(HIA)(IA)2(H2O)2Hg2Cl5]2n[3n(HgCl2)]·6nH2O (2; HIA refers to isonicotinic acid), exhibit intriguing crystal structures and photophysical properties. The crystal structures of compounds 1 and 2 were determined through single crystal X-ray diffraction, revealing their two-dimensional (2D) nature. Compound 1 displays upconversion yellow photoluminescence, attributed to the 4F9/2 → 6H13/2 electronic transition of the trivalent dysprosium ion. In contrast, compound 2 exhibits blue photoluminescent emission. The Commission Internationale de I'Éclairage (CIE) chromaticity coordinates of (0.4874, 0.5115) for 1 and (0.1225, 0.0678) for 2. The correlated color temperatures (CCT) are 2960 K and 5503 K for compounds 1 and 2, respectively. Furthermore, the semiconductor band gaps for compounds 1 and 2, determined by solid-state diffuse reflectance experiments, are 2.92 eV and 4.75 eV, respectively. Additional insights into their thermal stability are provided via thermogravimetric analysis (TG) results.