Space Group C2 Research Articles

Purification, crystallization, and X‐ray diffraction analysis of succinyl‐diaminopimelate desuccinylase from Wolbachia endosymbiont of Brugia malayi

AbstractLymphatic filariasis (LF) is a debilitating mosquito‐borne parasitic disease caused by Brugia malayi in humans in the lymphatic system. Although limited drugs are available to treat this disease, these drugs are only effective against the larvae of Brugia malayi. As resistance has been reported to the available drugs, a new antifilarial drug is needed with better prognostic features, a short period of time of use, and efficiency at preventing adult worm survival. In this study, we have targeted succinyl‐diaminopimelate desuccinylase (DapE) from the Wolbachia endosymbiont of Brugia malayi (WBm), which is involved in the production of lysine and meso‐diaminopimelic acid, an essential component for the formation of bacterial cell walls, and plays a vital role in pathogen survival. Deletion of DapE gene is lethal to WBm since the organism has no alternative pathway for lysine biosynthesis. Here, the expression, purification, and crystallization of DapE are reported. The crystals of DapE, with an estimated solvent content of 50.76%, diffract synchrotron X‐rays to a resolution of 2.3 Å and belong to the space group C2221, with unit‐cell parameters of a = 51.78, b = 78.83, and c = 216.20 Å. The X‐ray absorption spectroscopy further confirms that zinc atoms are incorporated in DapE.

Growth and characterization of D-Alanine DL-Mandelic acid single crystals for antibacterial activity and optical limiting applications

A promising optically prospective D-Alanine DL-Mandelic acid (DADLMA) an organic single crystal was successfully grown at room temperature by a slow solvent evaporation approach. The monoclinic crystal structure of the title crystal with space group C2 has been verified. The existence of multiple operational groups and linkages in the DADLMA crystal was ensured with the FTIR spectrum. The grown crystal was investigated to determine optical absorption cut-off wavelength (274 nm), energy band gap and linear refractive index by the UV–Visible absorption spectrum. The luminescence response has been observed to probe the compatibility of the material for the production of optical devices and the grown crystal shows a peak at 570 nm. The major focus of our work was to determine NLO properties of the sample and the DADLMA crystal was investigated for the first attempt by Z-scan measurement to bring out third-order nonlinear optical properties. The determined values are β (0.0149 × 10-4 cm/W), n2 (3.351 × 10-10 cm2/W) and χ(3) (1.674 × 10-7esu). The antibacterial activity of the title compound was investigated against a few foodborne pathogens (Streptococcus aureus, Klebsiella pneumoniae, Streptococcus pneumoniae and Escherichia coli) by measuring the zone of inhibition. Existing data indicate that the synthesized crystals are potential candidates for opto-electronic devices, optical limiting devices and biological applications.

Synthesis and Structure of COE-11, a New Borosilicate Zeolite with a Two-Dimensional Pore System of 12-Ring Channels

The new zeolite, COE-11, was synthesized at 155 °C to 168 °C by hydrothermal synthesis from a reaction mixture of SiO2/tetraethylammonium hydroxide/H3BO3/NaOH/H2O. Because tetraethylammonium is an unspecific structure directing agent, COE-11 crystallizes in all cases together with at least one impurity phase from a selection of phases: zeolite types *BEA, CHA, FER, MFI, MOR, MTW; the layered silicates magadiite and kenyaite; and searlsite and silica polymorph quartz. The crystal structure was solved from 3D electron diffraction (3D ED) data. Subsequent structure refinements of X-ray powder diffraction (PXRD) data and single crystal electron diffraction data converged to residual values of RF = 0.039, chi2 = 3.6 (PXRD) and RF = 21.81% (3D ED) confirming the structure model. COE-11 crystallizes in space group C2 with unit cell dimensions of a0 = 17.3494(11) Å, b0 = 17.3409(11) Å, c0 = 14.2789(4) Å and β = 113.762(2) °. The structure of COE-11 is characterized by a microporous borosilicate framework with intersecting, highly elliptical 12-ring channels running parallel (110) and (1–10) and forming a two-dimensional pore system. The Rietveld refinement provided a hint that boron partly substitutes silicon on three specific T sites of the framework. The idealized chemical composition of as-made COE-11 is [(CH3CH2)4N]4[B4Si62O132] per unit cell. Physico-chemical characterization using solid-state NMR spectroscopy, SEM, TG-DTA, and ATR-FTIR spectroscopy confirmed that COE-11 is a microporous borosilicate zeolite. COE-11 is structurally closely related to zeolite beta polymorph B but differs concerning the dimensionality of the pore system, which is 2D instead of 3D.

Synthesis and crystal structures of halogenated oxathiazolones and an unexpected propanamide.

The known 1,3,4-oxathiazol-2-ones with crystal structures reported in the Cambridge Structural Database are limited (13 to date) and this article expands the library to 15. In addition, convenient starting materials for the future exploration of 1,3,4-oxathiazol-2-ones are detailed. An unexpected halogenated propanamide has also been identified as a by-product of one reaction, presumably reacting with HCl generated in situ. The space group of 5-[(E)-2-chloroethenyl]-1,3,4-oxathiazol-2-one, C4H2ClNO2S, (1), is P21, with a high Z' value of 6; the space group of rac-2,3-dibromo-3-chloropropanamide, C3H4Br2ClNO, (2), is P21, with Z'= 4; and the structure of rac-5-(1,2-dibromo-2-phenylethyl)-1,3,4-oxathiazol-2-one, C10H7Br2NO2S, (3), crystallizes in the space group Pca21, with Z'= 1. Both of the structures of compounds 2 and 3 are modeled with two-component disorder and each molecular site hosts both of the enantiomers of the racemic pairs (S,S)/(R,R) and (R,S)/(S,R), respectively.

Crystal structure and spectral properties of the heterometallic 3d-4f complex of gadolinium (III) – cobalt (II) with ethylenediamine-N,N,N′,N′-tetraacetic acid

The 4f-3d heteronuclear complex Co3Gd2(EDTA)11∙9·5H2O was synthesized by the "block" synthesis method using protonated ethylenediaminetetraacetate Co(II) and Gd(III) nitrate. The complex was fully characterized by means of elemental, thermal and X-ray structural analyses, as well as by the methods of diffuse reflection spectroscopy and IR spectroscopy. The complex crystallizes in monoclinic system (space group C2) with lattice parameters a = 15.8142(3) Å, b = 14.5875(3) Å, c = 14.6808(3) Å, α = γ = 90°, β = 116.5009(10)°.The complex is a 2D coordination polymer in which each Gd(III) ion is connected to with three atoms Co(II) atoms through tridentate bridging carboxylate groups of EDTA, and each Co atom has two neighboring Gd(III) atoms. The polymer layers are packed in parallel, outer-sphere water molecules are located between the layers, forming a branched system of hydrogen bonds.

An Interesting Conversion Route of Mononuclear Zinc Complex to Zinc Mixed Carboxylate Coordination Polymer.

A complex [Zn(bpy)(acr)2]·H2O (1) was converted in a DMF medium (DMF = N,N'-dimethylformamide) into a coordination polymer [Zn(bpy)(acr)(HCOO)]n (1a) (bpy = 2,2'-bipyridine, and Hacr = acrylic acid), and the species was fully characterized through a single crystal X-ray diffraction. Additional data were obtained by IR and thermogravimetric analysis. Complex (1a) crystalized the coordination polymer in the space group Pca21 of an orthorhombic system. Structural characterization revealed that Zn(II) adopted a square pyramidal stereochemistry generated by bpy molecules, coordinated by chelate, acrylate, and formate ions as unidentate and bridged, respectively. The presence of both the formate and the acrylate with different coordination modes generated two bands in ranges that were characteristic for the carboxylate vibration modes. Thermal decomposition occurs in two complex steps: it first happens via a bpy release, which is followed by an overlapped process that is associated with acrylate and formate decomposition. The obtained complex is of present interest due to the presence of two different carboxylates in its composition and situation, which is rarely reported in the literature.

Diisopropyl 2-[(4-nitro-benzo-yl)amino]-propane-dioate.

The title compound, C16H20N2O7, crystallizes in the space group C2 with two mol-ecules in the asymmetric unit. The crystal packing shows O⋯π inter-actions between the two mol-ecules.

Prevalence and Significance of Approximate Symmetry in Organic Pc Structures

AbstractA survey has been made of the well determined (R≤0.050) organic crystal structures that have only a single glide plane (e. g., are in space group Pc) and that have more than one crystallographically independent formula unit (Z′>1); the goal was to discover what fraction have additional approximate symmetry. Of the 377 unique structures examined 8 % should almost certainly been refined in a higher‐symmetry unit cell; 86 % of the remaining 347 have approximate symmetry that is periodic in at least one dimension. While these percentages are similar to those found for P1 structures (C. P. Brock, Acta Crystallogr., Sect. B 2022, 78, 576–588), the types of approximate symmetry differ because 89 % of the P1, Z′>1 structures were composed of enantiopure material. The 347 reliable Pc structures include 118 that are slightly distorted or mimicked Cc and P21/c structures, 15 of which were reported as having been determined at room temperature. The distortions in another 72 are so large that the approximate symmetry must be seen as periodic in two dimensions only. These results suggest that symmetry lowering may accompany transformation of a crystal nucleus to a macroscopic crystal.

Noncentrosymmetric Supramolecular Hydrogen-Bonded Assemblies Based on Achiral Pyrazine-Bridged Zinc(II) Coordination Polymers with Pyrazinedione Derivatives

Reaction of M(OAc)2·xH2O (M, x = Zn, 2 and Co, 4), 1,4-dihydro-5,6-dicyano-2,3-pyrazinedione (H2CN2pyzdione), and pyrazine (pyz) affords two compounds of the same molecular formula {[M(H2O)6][M(CN2pyzdione)2(pyz)]·6H2O}n (M = Zn for 1 and Co for 2) in which discrete units of [M(H2O)6]2+ are linked to one-dimensional chains of [M(CN2pyzdione)2(pyz)]2– via multiple O–H···O hydrogen-bonding interactions and M2+-bound H2O molecules in [M(H2O)6]2+ also serve as linkers of hydrogen-bonded interstitial H2O molecules. Remarkably, 1 crystallizes in the monoclinic crystal system, the similar crystal system and unit cell parameters as 2, but with a space group distinct from 1 and 2, i.e., 1 is the noncentrosymmetric space group C2, whereas 2 is the centrosymmetric space group C2/m. This polar structure for 1 is induced by the presence of alternating arrangements of distinguishable two axial Zn–N bonds within [Zn(CN2pyzdione)2(pyz)]2– chains. Indeed, solid-state circular dichroism spectra of 1 exhibit significant Cotton effects, as evidenced by the polar space group C2. Moreover, these Cotton effects show clear temperature-dependence depending on contents of H2O molecules of 1.

Silesiaite, ideally Ca2Fe3+Sn(Si2O7)(Si2O6OH), a new species in the kristiansenite group: crystal chemistry and structure of holotype silesiaite from Szklarska Poręba, Poland, and Sc-free silesiaite from Häiviäntien, Finland

AbstractTwo silesiaite crystals, one from Szklarska Poręba, Poland (type locality), and the other from Häiviäntien, Finland, were studied with electron-probe microanalysis, Raman spectroscopy and single-crystal X-ray diffraction. The crystals have the following compositions normalised to 13 O2– + 1 (OH)– anions: Ca2.001(2)[(Sn1.105(6)Zr0.009(1))Σ1.114(Fe3+0.523(78)Sc0.185(62)Al0.070(14))Σ0.779(Fe2+0.065(12)Mn2+0.041(5)Mg0.003(3))Σ0.110]Σ2.003(Si3.997(2)O13OH), and Ca2.006(8)[(Sn1.110(18)Ti0.006(3))Σ1.107(Fe3+0.648(50)Al0.063(11))Σ0.710(Fe2+0.140(30)Mn2+0.011(3)Mg0.005(2))Σ0.155(Nb0.020(6)Ta0.011(3))Σ0.040]Σ2.009(Si3.991(14)O13OH), respectively. The structure of the crystals was refined in the triclinic system with unconventional space-group symmetry C1 to R1 = 2.02% and 3.56%, respectively. The unit cells were found to be a = 10.0080(2), b = 8.3622(1), c = 13.2994(2) Å, α = 89.987(1), β = 109.095(2), γ = 89.978(1)° and V = 1051.77(3) Å3 for silesiaite from Szklarska Poręba, and a = 9.9985(3), b = 8.3446(2), c = 13.2760(4) Å, α = 89.986(3), β = 109.122(2), γ = 90.020(2)° and V = 1046.55(5) Å3 for silesiaite from Häiviäntien. In both crystals, the Ca sites are occupied solely by calcium and Si sites by silicon atoms. Optimised occupancies of the four M sites indicated slightly different site fillings. In the Szklarska Poręba silesiaite, the M1 site is predominantly occupied by trivalent Fe + Sc and the M2–M4 sites by Sn. In contrast, in the Häiviäntien silesiaite, the M1–M3 sites are Sn-dominant, while Fe3+ predominantly occupies the M4 site. The differences can be considered a result of an evolution of the M1–M4 site occupancies following a decrease of the <M–O> distance. Among the minerals of the kristiansenite group, Sc-free silesiaite from the Häiviäntien pegmatite has the smallest average radius of M-site cations and a unit-cell volume that increases proportionally to the (Fe2+ ± Sc) content. The hydrogen atoms form moderate hydrogen bonds between disilicate groups (Si2O7 and Si2O6OH) linked in rows along [101], indicating the presence of one hydroxyl in the formula calculated for Z = 4. All three kristiansenite-group species, i.e. silesiaite, kozłowskiite and kristiansenite, are isostructural.

Structure of Y0.75La0.25PO4·0.67H2O rhabdophane nanoparticles synthesized by the hydrothermal microwave method

Nanopowders with a rhabdophane structure of nominal composition Y0.75La0.25PO4·0.67H2O were obtained by hydrothermal-microwave synthesis. The monoclinic structure of rhabdophane was refined by the Rietveld method within the C2 (5) space group. The nanopowders were studied by X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron microdiffraction (selected area electron diffraction, SAED), small angle X-ray scattering (SAXS), thermal analysis, low-temperature nitrogen adsorption-desorption measurements for analysis of surface area and porosity (ASAP) and pycnometric density measurements. These methods showed the formation of rod-like single-crystal rhabdophane nanoparticles with isolated pores inside the nanoparticles. To describe the formation of such nanoparticles, a mechanism of coherent-accommodative intergrowth of nanoscale clusters with rhabdophane structure is proposed.

CHARACTERIZATION, CRYSTAL STRUCTURE, ANTICANCER AND ANTIOXIDANT ACTIVITY OF NOVEL N-(2-OXO-2-(10H-PHENOTHIAZIN-10-YL) ETHYL)PIPERIDINE-1-CARBOXAMIDE

A new compound, N-(2-oxo-2-(10H-phenothiazin-10-yl)ethyl)piperidine-1-carboxamide (PTZ-PIP) was synthesized and characterized by Fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy (1H and 13C NMR) and mass spectrometry. The molecular structure of the compound (PTZ-PIP) was confirmed by single-crystal X-ray crystallographic studies. The compound (PTZ-PIP) was crystallized in a monoclinic crystal system with a space group of C2. The anticancer and antioxidant activity of the compound was investigated.

Comprehensive study on the origin of orthorhombic phase stabilization in Gd-doped HfO2 and DFT calculations.

In recent times, ultra-thin films of hafnium oxide (HfO2) have shown ferroelectricity (FE) attributed to the orthorhombic (o) phase of HfO2 with space group Pca21. This polar o-phase could be stabilized in the doped thin film of the oxide. In the present work, both polar and non-polar o-phases of HfO2 could be stabilized in Gd-doped bulk polycrystalline HfO2. Rietveld analysis of XRD data shows that the relative population of o-phases in the presence of the monoclinic (m) phase of HfO2 increases with increasing Gd-content. The local environment around the host atom has been investigated by time differential perturbed angular correlation (TDPAC) spectroscopy, synchrotron based X-ray near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) measurements. Field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) measurements showed a reduction in grain size with increasing Gd-dopant indicating a solute drag effect. It could be established that the segregation of the Gd-dopant in the grain boundary is a thermodynamically favorable process and the solute drag effect plays an important role in nucleation of the o-phase in bulk HfO2. Stabilization of Gd in both Pbca and Pca21 phases of HfO2 was supported by defect formation energy calculations using density functional theory (DFT). The present study has important implications in future applications of HfO2 in ferroelectric devices and in understanding the role of dopants in stabilizing the o-phase of HfO2 in the bulk.

New layered nonlinear optical iodate Cs3Ta(IO3)8: topology-symmetry analysis and structure prediction

New polar iodate Cs3Ta(IO3)8, space group P31c, has been obtained under mild hydrothermal conditions and its structural determination was carried out with a single crystal. Two structural variants are predicted based on OD topology-symmetry approach.

Synthesis, Crystal structure, DFT investigation and Antimicrobial, Molecular docking studies of (E)-3-methoxy-N'-(1-phenylethylidene) benzohydrazide

Hydrazone derivatives have drawn much attention because of their large pharmacological applications. In the present work, the compound (E)-3-methoxy-N'-(1-phenylethylidene) benzohydrazide (3-MAPHN), noted was synthesized, and its 3D structure was determined by X-ray crystallography. Structural characterization by X-ray crystallography was supported by Density Functional Theory (DFT) calculations. Intermolecular interactions in the crystal network were determined using Hirshfeld surface analyses. The optimized geometry analysis and HOMO-LUMO of the molecule were computed using the DFT-B3LYP method and 6-311++G (d,p) basis set. The compound has a Orthorhombic system and Pca21space group with the parameters of a = 8.1494(4) A˚, b = 10.5844(6) A˚,c = 16.3976(9) A˚, α = 90 °, β = 90 °, γ = 90 °.and Z = 4, V = 1414.40(13)˚A3. It forms an S(6) ring motif with an intermolecular N-H/O and C-H/O hydrogen bonds. Hirshfeld surface analysis and 2D fingerprint plots signify meaningful interactions in crystal packing [H-H (49.8%), C-H (24%), O-H (16.4%), N-H (3.9%), C-N (3.0%), C-O (2.4%) and C-C (0.5%) contacts]. Atomic charges were predicted using the Mulliken population analysis. The molecular electrostatic potential (MEP) picture was drawn using the same level of theory to visualize the chemical reactivity and charge distribution on the molecule. Antimicrobial activity and docking studies of 3-MAPHN revealed that the molecule posses antibacterial and fungal activity and the ability of drug resistance, respectively.

Synthesis of Na3SbS4 solid electrolyte from aqueous solution and its application in solid state rechargeable batteries

The tetragonal Na3SbS4 solid electrolyte was synthesized from aqueous solution in this study. The XRD results showed that the peak separation at 2θ = 30.1 and 35.1 º might from a defect in the crystal structure of t-Na3SbS4. The results of Rietveld analysis showed that the crystal structure of the Na3SbS4 sample after heat treatment belongs to the space group P-421c with the reliability coefficients Rwp=14.959%, Rp=11.690%. The lattice parameters are a = b = 7.1554(13) Å and c = 7.2829(13) Å. The pressure dependence in the pelletizing process of the ionic conductivity of the solid electrolyte t-Na3SbS4 was investigated and the pellets made at a pressure of 550 MPa had the highest ionic conductivity among the prepared samples, reaching a value of 6.0x10-4 Scm-1 at 25 ºC. The activation energies for the transport of Na⁺ ions in the prepared samples were 23, 24, 26 and 24 kJ mol-1 for pellets formed at pressures of 330, 403, 477 and 550 Mpa, respectively. These results demonstrate that the ion conduction mechanism is independent of the pellet forming pressure but the ionic conductivity at 25 ºC is directly proportional to those values. In addition, the electrochemical stability of Na3SbS4 was also evaluated through the discharge-charge characteristics of the battery cell TiS2−Na3SbS4|Na3SbS4| Na15Sn4. In the first discharge - charge cycle, the Coulomb efficiency was about 92.7% and higher than 99% from the second cycle onwards.

New Room-Temperature Molecular Ferroelectric (C6H16N2O)CdBr4·H2O with Preferable Luminescent Properties

Organic–inorganic hybrid materials are easy to modify, which makes it possible to construct multifunctional ferroelectrics directionally and apply the built-in electric field and switching properties of ferroelectrics to multidisciplinary fields. Particularly, the coupling of photoluminescence and ferroelectricity in a single hybrid material facilitates its novel applications in lighting sensors, memory devices, and other multifunctional applications. Based on the photoluminescent molecule 4-(2-aminoethyl) morpholine (AEM), here, a room-temperature ferroelectric (C6H16N2O)CdBr4·H2O (AEM-CdBr4) is designed and obtained, which crystallizes in a polar orthorhombic space group of Pca21. A reversible ferroelectric–paraelectric phase transition was confirmed at 353 K through experimental results, such as differential scanning calorimetry (DSC) curves, variable-temperature Raman spectroscopy, and photoluminescence (PL) spectroscopy. The crystal exhibits ferroelectricity at room temperature with a saturation polarization of approximately 8 μC/cm2. The photoluminescence of compound AEM-CdBr4 is mainly derived from the monomeric fluorescence emission of the AEM molecule and is not directly related to the energy band structure of the crystal. This room-temperature molecular-type ferroelectric AEM-CdBr4 with photoluminescence will provide new ideas for the design of new multifunctional ferroelectrics.

Purification and Crystallisation of a Novel Two-Domain Lectin from Scilla Campanulata

Abstract: In the last decade a number of single-domain mannose-binding lectins (11-14 kDa) have l:ieen characterised from different monocot plants and shown to belong to a superfamily of evolutionary related proteins. We have isolated and crystallized a novel two-domain, multivalent lectin, with 26.2 kDa subunits, from Scilla campanulata bulbs. The native agglutinin crystallizes in space group C2 and 3.3A resolution data set has been recorded.

Pyrazine-2-carboxylate copper(II) complexes

A pyrazine-2-carboxylate (pzCO2) complex of copper(II) has been synthesized, studied structurally and magnetically, and compared with structurally similar compounds. The structure of [CuCl(pzCO2)] (1) is reported and compared with the known structures of [Cu(pzCO2)2] (2) and [Cu(pzCO2)2(H2O)2] (3). Single-crystal X-ray diffraction measurements show that 1 crystallizes in the monoclinic space group Pc, with two crystallographically independent five-coordinate Cu(II) ions in a geometry close to square-pyramidal. It has a bilayer structure in the packing. Magnetic susceptibility data of 1 show that it exhibits weak ferromagnetic interactions (2 J = 2.26(7) K). In contrast, magnetic susceptibility data of 2 and 3 show weak antiferromagnetic interactions.

Synthesis, growth and characterization of magnesium chloride doped L-alanine cadmium chloride single crystal: For nonlinear optical application

The aim of this research was to synthesize and characterize pure and magnesium chloride (MgCl2) doped L–alanine cadmium chloride (LACC) single crystals. Pure and MgCl2 doped LACC single crystals were synthesized by solution method with slow evaporation solution growth technique at room temperature. The single crystal X-ray diffraction studies of pure, 1 and 2 mol% MgCl2 doped LACC single crystals revealed monoclinic crystal structure with C2 space group. The optical properties of pure and MgCl2 doped LACC single crystals investigated by UV–VIS/NIR spectrometer confirmed that the crystals were transparent in the wavelength range of 230-1100 nm. The optical band gap energy of pure and doped LACC single crystals were found to have the same value of 5.4 eV. The energy-dispersive X-ray analysis indicated the incorporation of magnesium and chlorine atoms in LACC single crystal. The second harmonic generation efficiency of 1 and 2 mol% MgCl2 doped LACC crystals were analyzed by Kurtz-Perry powder technique and found to be 1.75 and 2 times greater than that of the standard potassium dihydrogen phosphate crystal, respectively.