Search

A new azaphthalide derivative, (S)-3-hydroxy-2,7-dimethylfuro [3,4-b]pyridin-5(7H)-one (1), and a new phthalide derivative, (S)-7-hydroxy-3-((S)-1-hydroxyethyl)isobenzofuran-1(3H)-one (2), were isolated from the coral-derived fungus Aspergillus sp. SCSIO41405, together with eight known compounds (3–10). Their structures, including absolute configurations, were determined by NMR and MS spectroscopic analyses, optical rotation, calculated electronic circular dichroism (ECD) and X-ray crystal data. The isolated compounds were examined for antibacterial and enzyme inhibition activities. Compounds 7 and 8 exhibited weak antibacterial activities, and 10 displayed moderate inhibition on pancreatic lipase with an IC50 value of 15.6 μg/mL.

The crystal structures of salts (DienH3)4[IrCl6]5Cl2 (I), (DienH3)[IrCl6]Cl (II), and (DienH3)2[IrCl6]3 (III) $$\text{(DienH}_{3}^{3+}$$ is triple protonated diethylenetriamine). Crystal data for I: a = 26.891(2) A, b = 6.9379(3) A, c = 35.031(3) A, β = 100.758(2)°, space group C2/c, Z = 8, V = 6420.8(8) A3, ρcalc = 2.607 g/cm3; II: a = 6.8598(3) A, b = 23.2075(11) A, c = 9.5730(4) A, β = 90.240(2)°, space group P21/n, Z = 4, V = 1524.00(12) A3, ρcalc = 2.382 g/cm3; III: a = 12.4277(3) A, b = 19.6134(5) A, c = 14.3613(3) A, β = 98.260(1)°, space group P21/n, Z = 4, V = 3464.25(14) A3, ρcalc = 2.736 g/cm3.

2-Chloro-3-tosyl-5,5-dimethyl-2-cyclohexenone was subjected to a series of regiospecific Suzuki-Miyaura cross-coupling reactions in suspensions of nine different substituted boronic acids, Pd(OAc) 2 , P(Ph 3 ) 3 , K 3 PO 4 and 1,4-dioxane solvent, under sealed tube conditions. The regiospecific substitution of the tosyl-group by the aryl group in preference over the chloride- group was observed. A comparison between the bromo- and tosylate group’s reactivities is highlighted. Using the methodology, the products: 2-chloro-3-aryl-5,5-dimethyl-2-cyclohexenones were isolated in greater than 85% yields. Good quality crystals of three representative compounds were obtained by slow evaporation technique and subjected to single crystal XRD studies, Hirshfeld surface analysis, 3-D energy framework, and molecular docking studies. Crystal data for compound 3; C 15 H 17 ClO 4 S: monoclinic, space group P 2 1 / c (no. 14), a = 8.8687(3) A, b = 10.5537(4) A, c = 16.6862(7) A, β = 89.807(3)°, V = 1561.78(10) A 3 , Z = 4, T = 290 K, μ(MoKα) = 0.390 mm -1 , Dcalc = 1.398 g/cm 3 , 13623 reflections measured (6.716° ≤ 2Θ ≤ 54.962°), 3570 unique ( R int = 0.0467, R sigma = 0.0512) which were used in all calculations. The final R 1 was 0.0452 (I > 2σ(I)) and wR 2 was 0.1019 (all data). Crystal data for compound 5e; C 20 H 18 O 2 FCl: monoclinic, space group P 2 1 / c (no. 14), a = 6.4900(5) A, b = 18.6070(13) A, c = 14.2146(11) A, β = 102.324(2)°, V = 1677.0(2) A 3 , Z = 4, T = 296(2) K, μ(MoKα) = 0.239 mm -1 , Dcalc = 1.309 g/cm 3 , 25575 reflections measured (6.262° ≤ 2Θ ≤ 52.224°), 3283 unique ( R int = 0.0494, R sigma = 0.0307) which were used in all calculations. The final R 1 was 0.0875 (I > 2σ(I)) and wR 2 was 0.2056 (all data). Crystal data for compound 5h; C 12 H 13 OSCl: triclinic, space group P -1 (no. 2), a = 6.7517(6) A, b = 8.8376(9) A, c = 12.6049(12) A, α = 109.538(3)°, β = 98.597(3)°, γ = 90.417(3)°, V = 699.52(12) A 3 , Z = 2, T = 290 K, μ(MoKα) = 0.410 mm -1 , Dcalc = 1.376 g/cm 3 , 28754 reflections measured (6.114° ≤ 2Θ ≤ 59.288°), 3898 unique ( R int = 0.0544, R sigma = 0.0349) which were used in all calculations. The final R 1 was 0.1101 (I > 2σ(I)) and wR 2 was 0.2481 (all data).

Two investigated DNA 18-mers indicate a dynamic equilibrium of conformations in solution and crystallize as duplexes with two consecutive T–T mismatches. Neither these mismatched nucleotides nor others found in the PDB exhibit unique structural features compared with Watson–Crick paired nucleotides., Solution and crystal data are reported for DNA 18-mers with sequences related to those of bacterial noncoding single-stranded DNA segments called repetitive extragenic palindromes (REPs). Solution CD and melting data showed that the CG-rich, near-palindromic REPs from various bacterial species exhibit dynamic temperature-dependent and concentration-dependent equilibria, including architectures compatible with not only hairpins, which are expected to be biologically relevant, but also antiparallel duplexes and bimolecular tetraplexes. Three 18-mer oligonucleotides named Hpar-18 (PDB entry 6rou), Chom-18 (PDB entry 6ros) and its brominated variant Chom-18Br (PDB entry 6ror) crystallized as isomorphic right-handed A-like duplexes. The low-resolution crystal structures were solved with the help of experimental phases for Chom-18Br. The center of the duplexes is formed by two successive T–T noncanonical base pairs (mismatches). They do not deform the double-helical geometry. The presence of T–T mismatches prompted an analysis of the geometries of these and other noncanonical pairs in other DNA crystals in terms of their fit to the experimental electron densities (RSCC) and their geometric fit to the NtC (dinucleotide conformational) classes (https://dnatco.datmos.org/). Throughout this work, knowledge of the NtC classes was used to refine and validate the crystal structures, and to analyze the mismatches.

Multi-crystal data collection using synchrotron radiation was successfully applied to determine the three-dimensional structure of a triclinic crystal form of Dps from Escherichia coli at 2.0 Å resolution. The final data set was obtained by combining 261 partial diffraction data sets measured from crystals with an average size of approximately 5 µm. The most important features of diffraction data measurement and processing for low-symmetry crystals are discussed.

A series of antipyrinyl-pyrazolo[1,5- a ]pyrimidines have been synthesized by reactions of aminopyrazole (4) with various formylated active proton compounds in the presence of KHSO 4 (aqueous media), under ultrasound irradiation. The structures of the compounds have been established with the help of spectral and analytical data. N -(1,5-Dimethyl-3-oxo-2-phenyl-2,3-dihydro-1 H -pyrazol-4-yl)-7-phenylpyrazolo[1,5- a ]pyrimidine-3-carboxamide (6a) was further subjected to X-ray crystallographic studies to avoid any ambiguity of the derived structures. Crystal data for compound 6a, C 51 H 46 N 12 O 5 ( M =907.00 g/mol): triclinic, space group P-1 (no. 2), a = 9.9554(3) A, b = 14.0875(4) A, c = 17.4572(4) A, α = 79.676(2)°, β = 85.283(2)°, γ = 72.647(2)°, V = 2297.97(11) A 3 , Z = 2, T = 296.15 K, μ(MoKα) = 0.088 mm -1 , Dcalc = 1.311 g/cm 3 , 29732 reflections measured (4.174° ≤ 2Θ ≤ 57.068°), 10681 unique ( R int = 0.0400, R sigma = 0.0533) which were used in all calculations. The final R 1 was 0.0566 (I > 2σ(I)) and wR 2 was 0.1663 (all data). The novel compounds were also screened for their biological activities.

The organisation of the p-xylylenebis(triphenylphosphonium) dication in the solid state, in crystals formed under a variety of conditions, at different pH values and in the presence of THF and other potential building moieties including p-sulfonatocalix[4]arene, 1-methyl-3-butylimidazolium and aquated gadolinium(III) has been investigated using single crystal X-ray diffraction studies. Striking changes in the dication conformations (cis- and trans-) that contribute to the different crystal packings of the dication (two-dimensional layerings and three-dimensional scaffoldings) have been established for five different compounds. The interplay and the self-assembled arrays of the dication with other incorporated components and the overall non-covalent interactions have been quantified using Hirshfeld surface analyses.

A new enaminone was synthesized by reacting 3,5- bis -(trifluoromethyl)acetophenones and N , N -dimethylformamide dimethyl acetal and its detailed structural and crystalline properties were studied. The crystal data were found to be as C 13 H 11 F 6 NO, monoclinic, space group P2 1 /c (no. 14), a = 8.1556(8) A, b = 24.877(3) A, c = 7.6067(7) A, β = 116.745(6)°, V = 1378.2(3) A 3 , Z = 4, T = 293(2) K, μ(MoKα) = 0.150 mm -1 , Dcalc = 1.500 g/cm 3 , 40777 reflections measured (5.594° ≤ 2Θ ≤ 56.786°), 3413 unique ( R int = 0.1040, R sigma = 0.0584) which were used in all calculations. The final R 1 was 0.0771 (I > 2σ(I)) and wR 2 was 0.2541 (all data).

We report herein the fabrication and structural characterization of two new coordination complexes [Cu3(μ3-O)(pz)3(Hpz)(Hpdc)(H2O)2](H2O)4 (1, H2pdc = pyridine-3,5-dicarboxylic acid, Hpz = pyrazol) and [Cd(phen)(bdc)](H2O) (2, phen = 1,10-phenanthroline, H2bdc = 1,2- acidic benzenedicarboxylic) through the application of acidic carboxylic and the N-containing linkers as the co-ligands. The molecular arrangement for the constructed CPs were probed by the structural solution and refinement based on the singe crystal X-ray data and their phase purities was confirmed via a comparison between the simulated profile from the crystal data with the measured profile using the powder X-ray diffraction. Furthermore, an ultrasonic treatment method was used to produce the nano particles of CPs 1 and 2 with good water dispersibility and framework integrality. Moreover, the in vitro 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) method were administered on the breast cancer cell line BT474 with rising aggregations of the nanostructures 1 and 2, the cell apoptosis and ROS production level was also performed on BT474 cell line. This study suggested both nanostructures 1 and 2 have promising anticancer properties.

The Inorganic Crystal Structure Database (ICSD) is the world's largest database of fully evaluated and published crystal structure data, mostly obtained from experimental results. However, the purely experimental approach is no longer the only route to discover new compounds and structures. In the past few decades, numerous computational methods for simulating and predicting structures of inorganic solids have emerged, creating large numbers of theoretical crystal data. In order to take account of these new developments the scope of the ICSD was extended in 2017 to include theoretical structures which are published in peer‐reviewed journals. Each theoretical structure has been carefully evaluated, and the resulting CIF has been extended and standardized. Furthermore, a first classification of theoretical data in the ICSD is presented, including additional categories used for comparison of experimental and theoretical information., The article discusses how theoretical crystal data are supplementing experimental data for simulation and prediction of structures of inorganic solids in the Inorganic Crystal Structure Database.

The reaction between an atropoisomeric diphosphine, Bitianp and [Ni(CO) 4 ] was achieved by direct condensation in CH 3 Cl to afford complexes of general formula [Ni(CO) 2 (Bitianp)]. This compound was characterized by elemental analysis, IR, 1 H-, 13 C- and 31 P-NMR spectroscopies. The structure of nickel complex has been determined by X-ray crystal-lography. Crystal data for C 42 H 28 NiO 2 P 2 S 2 ( M = 749.41 g/mol): triclinic, space group P -1 (no. 2), a = 10.539(2) A, b = 11.811(2) A, c = 15.994(3) A, α = 83.93(3)°, β = 88.18(3)°, γ = 65.24(3)°, V = 1797.6(7) A 3 , Z = 2, T = 294(2) K, μ(MoKα) = 0.781 mm -1 , Dcalc =1.385 g/cm 3 , 22744 reflections measured (2.56° ≤ 2Θ ≤ 64.726°), 11837 unique ( R int = 0.0157, R sigma = 0.0215) which were used in all calculations. The final R 1 was 0.0360 (I > 2σ(I)) and wR 2 was 0.1088 (all data). The coordination sphere of the Ni center is best described as a tetrahedral geometry.

All primary data files related to the publication. Procedures, recation conditions and used analytical equipment is discussed in detail in the experimental section or the supporting information of the paper. Productivities in olefin metathesis reactions were examined via gas-chromatography / mass spectrometry (GC-MS) analysis and can be found in the GC-MS folder. Furthermore, the GC-MS folder contains an Excel-file in which the names of the data files are listed and assigned to table entries in the publication. Novel complexes were examined via nuclear magnetic resonance (NMR) spectroscopy and the spectra can be found in NMR folder. The NMR folder also contains NMR experiments mentioned in the paper and shown in the Supplementary Information. NMR Spectra are named according to the numbering in the publication. All crystal data mentioned in the paper can be found in the related datasets.

A new compound, (H2L)2SO4 (1) (HL = β-alanine), was synthesized and studied based on X-ray single crystal diffraction analysis. β-alanine molecular displays two kinds of molecule torsion geometries (I and II) in compound 1, which construct supramolecular Z-shaped chains and supramolecular helical chains respectively. Based on our understanding of the helical packing mechanism of β-alanine in compound 1, we predicted and found supramolecular helical chains in another compound H2LClO4 (2) for the first time, although the crystal data of compound 2 has been reported previously. The way of simple β-alanine self-organizing into supramolecular helical chains was discussed in detail by comparing the structure of the compound 1 and compound 2, which may be important for understanding the way of simple molecules self-organizing into supramolecular helical structure and offers a good case for achiral ligands to construct supramolecular helical chains.

A series of new polynuclear complexes of divalent Ni and Cu with 2-cyano-2-oximino-acetic acid (later AACO2-) were obtained as the result of the ligand modification reaction in the process of complexation, using 2-cyano-2-oximino-acetates such as methyl- (later as MeCO), and ethyl- (as ECO later on). Synthesized compounds were characterized by spectroscopic methods, thermal analysis, magnetochemistry, and X-ray crystallography. Crystal data revealed the formation of the dimeric [Ni(AACO)(H2O)3]2·H2O (1), trimeric K2[Ni3(AACO)4(H2O)4]·4H2O (2), and K2[Cu3(AACO)4(H2O)4]·4H2O (3) complexes, with bridging NO-groups cyanoxime dianions. In the latter two compounds, the AACO2– anions adopt cis-arrangements around metal centers. One mononuclear complex of K2[Cu(AACO)2(H2O)]·2H2O (4) composition was isolated and characterized as well, where the cyanoxime forms the trans-complex 4. There is moderate-to-strong antiferromagnetic coupling between metal centers in polynuclear complexes. Data of thermal analysis studies...

SPIND is an auto-indexing algorithm developed for sparse-pattern diffraction data. It is generally applicable to multiple crystallographic data types including serial crystallographic data collected from X-ray free-electron lasers (XFEL), synchrotron light sources or transmission electron diffraction data collected on a transmission electron microscope (TEM), and can also be extended to ultrafast electron diffraction data. The algorithm and comparative studies on experimental serial femtosecond protein crystallography data sets demonstrate its ability to maximize data efficiency by making use of sparse patterns that are discarded by other indexing programs., SPIND (sparse-pattern indexing) is an auto-indexing algorithm for sparse snapshot diffraction patterns (‘stills’) that requires the positions of only five Bragg peaks in a single pattern, when provided with unit-cell parameters. The capability of SPIND is demonstrated for the orientation determination of sparse diffraction patterns using simulated data from microcrystals of a small inorganic molecule containing three iodines, 5-amino-2,4,6-triiodoisophthalic acid monohydrate (I3C) [Beck & Sheldrick (2008 ▸), Acta Cryst. E64, o1286], which is challenging for commonly used indexing algorithms. SPIND, integrated with CrystFEL [White et al. (2012 ▸), J. Appl. Cryst. 45, 335–341], is then shown to improve the indexing rate and quality of merged serial femtosecond crystallography data from two membrane proteins, the human δ-opioid receptor in complex with a bi-functional peptide ligand DIPP-NH2 and the NTQ chloride-pumping rhodopsin (CIR). The study demonstrates the suitability of SPIND for indexing sparse inorganic crystal data with smaller unit cells, and for improving the quality of serial femtosecond protein crystallography data, significantly reducing the amount of sample and beam time required by making better use of limited data sets. SPIND is written in Python and is publicly available under the GNU General Public License from https://github.com/LiuLab-CSRC/SPIND.

To conduct a comparative study on proton conductivities of a hydrogen-bonded organic framework (HOF) and its related metal–organic framework (MOF), we selected and fabricated a 3D HOF (HOF-H3L) (H3L = [3-(4-methyl-benzoyl)-thioureido]-acetic acid; CH3C6H4C(O)NHC(S)NHCH2COOH) and its related 3D copper MOF, {[CuI3CuII3L3(DMF)2(CH3OH)(H2O)]·3CH3OH}n (1). Both HOF-H3L and MOF 1 exhibit high water stability. Their proton conductivities under different relative humidities (RHs) were fully investigated. Note that the MOF 1 exhibited the optimized conductivity of 3.78 × 10−4 S cm−1 that was nearly one order of magnitude larger than that of HOF-H3L (6.91 × 10−5 S cm−1) at 100 °C and 98% RH. Based on the crystal data, Ea calculations, water vapor absorptions and PXRD patterns, the proton-conducting mechanisms were suggested. This comparative investigation provides a new inspiration to researchers to design new proton-conductive materials in the future.

The title complex, [{Os2(CO)4(C21H21P)2}2(C12H14O4)2], is a centrosymmetric molecular loop consisting of two Os—Os sawhorse units linked by two adamantane dicarboxylato bridges. It was synthesized by the microwave-mediated reaction between Os3(CO)12 and adamantane-1,3-dicarboxylic acid. In contrast to the related complex [{Os2(CO)6}2(μ4-adamantane-1,3-diacetate)2], the metal–metal axes within each molecule are oriented parallel rather than perpendicular to one another. The crystal structure exhibits cavities that contain residual electron density peaks, but it was not possible to unambiguously identify the solvent therein. The contribution of the disordered solvent molecules to the scattering was removed using the SQUEEZE (Spek (2015). Acta Cryst. C71, 9–18) routine in PLATON [Spek (2020). Acta Cryst. E76, 1–11]. These solvent molecules are not considered in the given chemical formula and other crystal data.

Fatty liver disease (FLD) has become an increasing global health risk. However, an accurate diagnosis of FLD at an early stage remains a great challenge due to lack of suitable imaging tools. To this end, we developed the first fluorescent two-photon aggregationinduced emission (AIE) luminogen ABCXF for high-contrast imaging of FLD tissue. ABCXF has a large Stokes shift, good two-photon absorption cross-section, bright red emission, high fluorescence quantum yield in solid state, and excellent photostability. It shows abnormal intramolecular charge transfer effect instead of twisted intramolecular charge transfer effect in polar solvents. Photophysical and crystal data demonstrated that it exhibits nonaromatic rotors - trifluoromethyto contribute to its AIE effect. Biocompatible lipid droplet-targeting ABCXF can selectively light up lesions in the FLD tissue with a high signal-to-noise ratio. It shows superior imaging performances compared to Oil Red O. Thus, ABCXF can be a powerful tool for the diagnosis and evaluation of FLD from a liver biopsy.

Liquid crystal-based technologies have evolved explosively over these last few decades in other than display applications. One of the examples is 4-Cyano-4′-alkylbiphenyl (nCB), which is a well-known thermotropic liquid crystal (LC) material, commonly used in numerous advanced photonic materials and electro-optical devices. Owing to their uncomplicated method of synthesis and high optical birefringence, these molecules have been very well characterised by noticeable and efficient use in optical instruments. The present review emphasizes on the molecular structure, synthesis, crystal data and LC properties of the various nCB materials. Further, their latest applications in the fields of sensors, smart windows, liquid crystal lenses, PV cells, supercapacitors and drug delivery have been covered in detail beyond their regular display applications. This review will encourage researchers to carry out further research into the diverse applications of LC molecules.

The crystal structure of the title compound, bis{μ-1,3-bis[2-(diphenylphosphanyl)ethyl]-1H-imidazole-κ2 P:P′}bis[trichloridoiron(III)], [Fe2Cl6(C31H31N2P2)2] or [{FeCl3}2(μ-PCHP)2] (PCHP = C31H31N2P2), consists of dinuclear complexes that are located about centres of inversion. The FeIII cation is in a distorted trigonal–bipyramidal coordination with three chloride ligands located in the trigonal plane and two P atoms of symmetry-related PCHP ligands occupying the axial positions. Within the centrosymmetric complex, a pair of intramolecular C—H...Cl hydrogen bonds between aromatic CH groups and chloride ligands are found. Individual complexes are linked into layers parallel to (\overline{1}01) by intermolecular C—H...Cl hydrogen bonds. No pronounced intermolecular interactions occur between these layers. This arrangement leaves space for disordered solvent molecules. Electron density associated with these additional solvent molecules was removed with the SQUEEZE procedure in PLATON [Spek (2015). Acta Cryst. C71, 9–18]. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s).

Modern force fields are accurate enough to describe thermal effects in molecular crystals. Here, we have extended our earlier approach to discrete force fields for various temperatures to a force field with a continuous function. For the parametrisation of the force field, we used data mining on experimental structures with the temperature as an additional descriptor. The obtained force field can be used to minimise energy at a finite temperature and for molecular dynamics with zero-K potentials. The applicability of the method has been demonstrated for the prediction of crystal density, temperature density gradients and transition temperature.

A method is presented to simultaneously resolve the crystal symmetry and indexing ambiguity from sparse data sets., Combining X-ray diffraction data from multiple samples requires determination of the symmetry and resolution of any indexing ambiguity. For the partial data sets typical of in situ room-temperature experiments, determination of the correct symmetry is often not straightforward. The potential for indexing ambiguity in polar space groups is also an issue, although methods to resolve this are available if the true symmetry is known. Here, a method is presented to simultaneously resolve the determination of the Patterson symmetry and the indexing ambiguity for partial data sets.

Rheumatoid arthritis (RA) is one of the inflammatory joint diseases in a heterogeneous group of disorders that share features of the destruction of the extracellular matrices of articular cartilage and bone. Matrix metalloproteinase (MMP) enzymes (in particular MMP9), are crucial for RA. Given the limited investigation of the MMP9 inhibition by coumarin derivatives, the present study was taken up. A coumarin derivative (ethyl 6-[(4-methyl-2-oxo-2H-chromen-7-yl)oxy]hexanoate) was synthesized, characterized by spectral analysis (1HNMR, 13CNMR, IR, and MS), single crystal XRD and molecular docking was carried out. The title compound C18H22O5 crystallizes in the monoclinic crystal system in P21/c space group. The glide docking score for the title compound is -6.8, compared with -6.6 for co-crystal compound (LT4). The synthesis, characterization and crystal data are discussed.

A ETS-10-like topological vanadoarsenate [NH4VO(AsO4)]n 1 has been hydrothermally synthesized and structurally characterized by X-ray diffraction. The molecule structural analysis reveals that 1 is constructed by helical [–V–O–]n chains and AsO4 tetrahedra. Crystal data for 1: Orthorhombic, with space group Pnna, a = 13.212(3) A, b = 10.753(2) A, c = 6.6266(13) A, V = 941.4(3) A3, Z = 8, R1 = 0.0515 and wR2 = 0.1144.

Chiral drug naftopidil (NAF), a specific α1D-adrenoceptor (AR) antagonist for the treatment of benign prostatic hyperplasia, was used in racemic form for several decades. Our recent work declared that NAF enantiomers showed the same antagonistic effects on the α1D-AR, but the binding mechanism of these two stereochemical NAF isomers to the α1D receptor remained unclear. Herein, we reported the crystallographic structures of optically pure NAF stereoisomers for the first time and unambiguously determined their absolute configurations. The crystal data of R and S enantiomers matched satisfactorily the pharmacophore model for α1D-selective antagonists. Based on the constructed α1D homology model, molecular docking studies shed light on the molecular mechanism of NAF enantiomers binding to α1D-AR. The results indicated that NAF enantiomers exhibited the very similar binding poses and occupied the same binding pocket., Graphical abstract In this work, the crystallographic structures of optically pure NAF stereoisomers were reported for the first time and provided insight into the molecular mechanism of NAF enantiomers binding to α1D-adrenoceptor.fx1

Crystallographic information files (CIFs) are now widely used for recording crystal-structure data in the authorized manner. Two macros, cif2pdf and E2J, have recently been added to integrated assistance environments for the RIETAN-FP–VENUS system. Cif2pdf is used to convert CIFs, which are obtained by lst2cif and refln macros from output files of RIETAN-FP, into reports with the portable document format (PDF). The resulting PDF files may include (a) graphs such as Rietveld-refinement patterns, and Williamson–Hall and Halder–Wagner plots output by gnuplot and (b) images such as structural models and three-dimensional electron- and nuclear-density distributions drawn by VESTA. E2J practically translates LaTeX text files, *.tex, output by cif2pdf into Japanese by means of a stream editor, sed. A set of files input by cif2pdf and procedures to execute cif2pdf and E2J are described in detail. These two documentation utilities must enhance the value of the assistance environments greatly.

A series of 10-substituted-3,3,6,6-tetramethyl-9-aryl-3,4,6,7,9,10-hexahydroacridine-1,8(2H,5 H)-dione derivatives 2 were synthesized by reaction of compounds 1 with amines. The compounds 1 were effectively prepared by 5,5-dimethylcyclohexane-1,3-dione and aldehydes in the presence of a little amount of L-proline as catalyst at room temperature. All the compounds were characterized by IR, MS, and 1H NMR. The crystal data of 1b and 2d were collected by X-ray single-crystal diffraction, and compounds 2b and 2d exhibited better inhibitory activity against HepG2 cells.

The centrosymmetric binuclear complex, [Zn 2 (C 8 H 7 O 2 ) 4 (C 7 H 7 NO) 2 ], has been synthesized and characterized by FT-IR and NMR methods. The obtained Zn(II) metal complex has been also characterized by a single crystal X-ray diffraction study. Crystal data for C 46 H 42 N 2 O 10 Zn 2 : Monoclinic, Space group P2 1 /c (no. 14), a = 10.4827(3) A, b = 8.6141(2) A, c = 24.7582(6) A, β = 101.066(1) °, V = 2194.07(10) A 3 , Z = 4, D calc = 1.383 g/cm 3 , 22545 reflections measured (3.96° ≤ 2Θ ≤ 52.74°), 4465 unique ( R int = 0.0388, R sigma = 0.0333) which were used in all calculations. The final R 1 was 0.0489 (I ≥ 2s(I)) and wR 2 was 0.1533 (all data). The four nearest oxygen atoms around each zinc ion form a distorted square-planar arrangement, and the distorted square-pyramidal coordination is completed by the nitrogen atom of the 1-(pyridin-4-yl)ethanone compound.

We present new constraints on the dark matter-induced annual modulation signal using 1.7 years, of COSINE-100 data with a total exposure of 97.7 kg$\cdot$years. The COSINE-100 experiment, consisting of 106 kg of NaI(Tl) target material, is designed to carry out a model-independent test of DAMA/LIBRA's claim of WIMP discovery by searching for the same annual modulation signal using the same NaI(Tl) target. The crystal data show a 2.7 cpd/kg/keV background rate on average in the 2--6 keV energy region of interest. Using a $\chi$-squared minimization method we observe best fit values for modulation amplitude and phase of 0.0092$\pm$0.0067 cpd/kg/keV and 127.2$\pm$45 d, respectively., Comment: 6 pages, 5 figures, revised version as published in PRL

Background Cross validation of internal COD obtainable from carbon rule of law that govern human body to function are crucial for future application is concerned Verification leads to identification of all sick cells to cure to outperform better tomorrow Cross validation of bond of all atoms is necessary for checking and arriving at conclusion that whether disease can be cured or not Importantly rule of carbon based law interpret that incoming probe can be altering internal COD value obtainable from carbon value alone Cross checking of these internal COD obtained from crystal data are to be the focus of this work Verification can also be done from internal COD of protein in native form and alternative one obtained via complex formed using probe protein interaction Results are in agreement with cross validation of protein in two different states via internal COD obtained from crystal data of bound and unbound protein Fantastic results are in agreement with changes of internal COD and bond of changes at that point One of the mini tests of internal COD identification obtainable from sequence alone is demonstrated here in addition to original work All are in accordance with rule of law obtainable from carbon value Results are promising that futuristic application that leads to disease free world of human nature

Some symboles could not be reproduce. For the full abstract, please consult the original article C-Allyl –D-mannopyranosideswere preparedvia a variety of routesto determine an optimal route to the -anomers. The relative conformational energies of the key intermediate was evaluated by molecular modelingwhich showed the conventional 4C1chair conformation to be the lowest energy conformer. This finding was also confirmed by NMR and X-ray crystallography. The perbenzoylated C-allyl mannoside was also converted into 1,1’-biphenyl analogues using a palladium-catalyzed Heck reaction. Two of the resulting minor reaction products were co-crystallized with the uropathogenic E. coliFimH. Alternatively, the KDof the major and expected Heck product was in the low nM range as measured by SPR. Crystal data showed that the C-linked derivatives efficiently bind in the FimH binding cavity near the so-called hydrophobic tyrosine gate.

The present work showcases, first time, the synthesis of tri-palladium substituted sandwich type phosphotungstate, [Pd3(PW9O34)2]11−, from its individual salts in super acidic medium as well as the single crystal structure of the same. Further, various spectral analysis carried out to support the crystal data. A preliminary study for the hydrogenation of nitrobenzene has been carried out to evaluate the catalytic activity of the complex.

Two ytterbium(III) complexes comprising alkynylamidinate ligands, Cp2Yb[(iPr2N)2C—C≡C—c-C3H5] (1) and Yb[(CyN)2C—C≡C—Ph]3 (Cy = cyclo­hex­yl) (2) have been synthesized and structurally characterized. Both complexes are monomers without any coordinated solvent in the solid state., Two ytterbium(III) complexes comprising alkynylamidinate ligands, namely bis­(η5-cyclo­penta­dien­yl)(3-cyclo­propyl-N,N′-diiso­propyl­propynamidinato-κ2 N,N′)ytterbium(III), [Yb(C5H5)2(C12H19N2)] or Cp2Yb[(iPr2N)2C—C≡C—c-C3H5] (1) and tris­(3-phenyl-N,N′-di­cyclo­hexyl­propynamidinato-κ2 N,N′)ytterbium(III), [Yb(C21H27N2)3] or Yb[(CyN)2C—C≡C—Ph]3 (Cy = cyclo­hex­yl) (2) have been synthesized and structurally characterized. Both complexes are monomers; for complex 2, the contribution to the scattering from highly disordered toluene solvent molecules in these voids was removed with the SQUEEZE routine [Spek (2015). Acta Cryst. C71, 9–18] in PLATON. The stated crystal data for Mr, μ etc. do not take these into account.

The chemical and physical properties of inorganic compounds predicted from density functional theory (DFT) calculations depend on their crystal structures, with the underlying assumption being made that the computed lattice parameters are accurate. This assumption is evaluated by comparing the lattice parameters computed in the Materials Project using PBE-GGA with the experimental values reported for 10,033 compounds in Pearson's Crystal Data. On average, the computed lattice parameters are overestimated relative to the experimental parameters by 1–2% for the cell lengths and 4% for the cell volumes. The discrepancy can largely be traced to the neglect of corrections due to London dispersion forces in many DFT calculations, and is especially severe for layered crystal structures in trigonal systems. Within the experimental crystal data alone, the uncertainty in unit cell volumes for multiple entries of the same compound can range between 0.1 and 1%, which is at least an order of magnitude greater than the stated uncertainties for individual entries. The stability of 36,857 compounds computed in the Materials Project was also assessed by comparing to experimental structures reported in Pearson's Crystal Data. This analysis suggests that predicted compounds having a formation energy of > 200 meV atom-1 above the convex Hull should not necessarily be ruled out as synthetically inaccessible.

Eight new flavonoids daemoflavans A-H, including two dimeric proanthocyanidins (1 and 2), four flavans (3–6), two 2-arylbenzofurans (7 and 8), along with nine known compounds (9–17), were isolated from the fruit of Daemonorops draco. Their structures, including the absolute configurations, were elucidated by extensive spectroscopic data, ECD analysis, and X-ray crystal diffraction. Besides, the X-ray crystal data of a known compound dracoflavan B1 (9) was firstly reported. Daemoflavan G (7) represents a rare example of C-5 methylated 2-arylbenzofuran in natural products. Among the known compounds, 15, 16, 17 were reported from this species for the first time. All the compounds were evaluated for their cytotoxicity against HepG2 cell line. Among them, compounds 1, 9 and 10 exhibited modest cytotoxic activity with IC50 values of 12.4, 12.0 and 13.2 μM, respectively.

The crystal structure of 2-amino-4-hydroxy-6-methylpyrimidine-trihydrate was characterized by single crystal X-ray diffraction. The crystal data: C10H20O5N6, triclinic, P-1, a = 6.8770 (14) Å, b = 10.486 (2) Å, c = 11.320 (2) Å, V = 778.9 (3) Å3, Z = 2, Rgt = 0.0646, wRref (F2) = 0.2144, T = 293 (2) K. The title compound molecules form 1D chained structure by the interaction of hydrogen bonds. And the one-dimensional chains further form three-dimensional network structure by interactions of hydrogen bonds and pyrimidine rings.

The advent at 3rd generation synchrotron sources of extremely brilliant beamlines for macromolecular crystallography (MX) has meant that for systems which produce only small crystals, the practice of multi-crystal data collection, in which partial data sets collected from a series of crystals of the same target are merged to produce a final, complete data set, is enjoying a renaissance. In principle such experiments are straightforward. All that is needed is to mount all the crystals required on the sample support, to collect the partial data sets in series and then to merge them to produce the final data set. However, multi-crystal data collection is actually fraught with difficultly. The positions of the crystals on the sample support must be determined; individual partial data sets should be collected without inducing too much radiation damage; and the correct choice of partial data sets to merge in order to produce the best final data set must be made. Here, we describe an automatic pipeline, Mesh&Collect, which facilitates multi-crystal experiments, present newer developments designed to improve the quality of the final data sets obtained, give examples of the successes that can be obtained and describe the pitfalls to be avoided in such experiments.

In this work, a force field for molecular dynamics and Monte Carlo simulations of ionic liquids containing imidazolium and halo-imidazolium derivatives is presented. This force field is an extension of the well-known CL&P and OPLS-AA models and was validated by comparing predicted crystalline structures for 22 ionic liquid compounds with the corresponding data deposited at the Cambridge Structural Database. The obtained results indicate that the proposed force field extension allows the reproduction of the crystal data with an absolute average deviation lower than 2.4%. Finally, it was also established that the halogen atoms covalently bound to the studied imidazolium cations are positively charged and do not exhibit a so-called σ-hole feature. For this reason, the formation of halogen bonds in the proposed force field appears naturally from the parametrized atomic point-charge distribution, without the necessity of any extra interaction sites.

In the title compound a distorted Ag4N4-heterocubane core is set up by AgI cations and N atoms of cyanate anions. The core is decorated by four tri­phenyl­phosphine ligands bonded to the AgI cations. Ag⋯Ag distances as short as 3.133 (9) Å suggest the presence of argentophilic (d 10⋯d 10) inter­actions., In the title compound, [{[(C6H5)3P]Ag}4{NCO}4], a distorted Ag4N4-heterocubane core is set up by four AgI ions being coordinated by the N atoms of the cyanato anions in a μ 3-bridging mode. In addition, a tri­phenyl­phosphine ligand is datively bonded to each of the AgI ions. Intra­molecular Ag⋯Ag distances as short as 3.133 (9) Å suggest the presence of argentophilic (d 10⋯d 10) inter­actions. Five moderate-to-weak C—H⋯O hydrogen-bonding inter­actions are observed in the crystal structure, spanning a three-dimensional network. A region of electron density was treated with the SQUEEZE procedure in PLATON [Spek (2015). Acta Cryst. C71, 9–18] following unsuccessful attempts to model it as being part of disordered tetra­hydro­furan solvent mol­ecules. The given chemical formula and other crystal data do not take into account these solvent mol­ecules.

This review highlights some structural features and luminescent properties of homo- and hetero-multinuclear silver(I)–pyridinyl complexes. It focuses on the coordination and geometry of the silver(I) ions to the pyridinyl-nitrogen. For this reason, we have considered only pyridinyl-N–Ag(I) complexes whose crystal data are available. In addition, this review does not consider mononuclear silver(I)–pyridinyl complexes as these have been reviewed elsewhere. This is motivated by the fact that multinuclear silver(I)–pyridinyl complexes have been shown to be more stable in solution, possess enhanced properties, and have fascinating structures compared to their mononuclear counterparts. The introduction highlights pyridinyl ligands used in complexation of silver(I) ions. The main body highlights complexation of silver(I) through pyridinyl nitrogen and the interactions found in the multinuclear silver(I)–pyridinyl complexes as well as the coordination number and geometry of silver(I) centers. Though silver(I) has...