the major phases within the residual glass matrix in some formulations of the glass-ceramic waste form for treatment of raffinate high-level waste (Crum et al., 2012, 2014, 2016). Studies on the crystal chemistry and crystallization mechanism of lanthanide borosilicates are important in understanding the formation and durability of crystalline phases in the glass- ceramic waste forms (Crum et al., 2012, 2014, 2016). In this work, we report the synthesis method and crystalstructure of Nd 3 BSi 2 O 10 solved by powder XRD and EPMA analysis.
We report the synthesis and characterization of a meso-meso directly linked bisporphyrin 6 bearing both alkyl and aryl residues. Oxidative fusing results in a meso- meso, β−β,β−β -linked bisporphyrin. The first crystalstructure analysis of a meso-meso directly linked porphyrin dimer 6 shows the inequivalency of the two porphyrin units with regard to the macrocycle conformation. Quite distinct mixings of distortion modes were observed for the two aromatic macrocycles.
Phenols and cyclic aminals are known to form a variety of supramolecular aggregates via O—H N hydrogen bonds, and complexes of phenols with various nitrogen bases are model systems often applied in the study of the nature of the hydrogen bond (Majerz et al. 2007). Previously, hydrogen bonding between the hydroxyl group of acidic groups such as phenols and heterocyclic nitrogen atoms has proved to be a useful and powerful organizing force for the formation of supramolecules (Jin et al., 2014). In a continuation of our previously published work in this area (Rivera et al., 2007, 2015) and as a part of our research on compounds in which a cyclic aminal acts as a central host and organizes guest mol- ecules around it via hydrogen bonding, we report herein the synthesis and crystalstructure of title compound. This was assembled through hydrogen-bonding interactions between the cyclic aminal 1,3,6,8-tetraazatricyclo[126.96.36.199 3,8 ]undecane (TATU) and 4-chloro-3,5-dimethylphenol.
The crystal and molecular structure of salicylaldehyde N(4)- morpholinothiosemicarbazone was published previously (Koo et al., 1977) based on multiple-film equi-inclination Weissen- berg data using Cu K radiation and refined to an R value of 0.11. In this study, we present the synthesis of salicylaldehyde N(4)-morpholinothiosemicarbazone (3) together with its structural characteristics and crystalstructure redetermination using present-day technology.
Herein, we report the synthesis of a new class of metacyclophane “thiametacyclophane” in which sulfur atoms are introduced into the bridges due to giving the flexibility to the molecule and two rigid biphenyl parts are also introduced. When a mixture of precursors was reacted under basic conditions, they are successfully cyc- lized to the metacyclophane as a thiacalix  arene analogue, which is readily separated using simple column chromatography. A crystalstructure analysis is performed to determine the exact structure of the molecule.
Synthesis, single-crystal X-ray diffraction studies and reducing power assay of 2-(4-chlorophenyl)-2-oxoethyl 2- aminobenzoate (2a), 2-(4-chlorophenyl)-2-oxoethyl 3-aminobenzoate (2b) and 2-(4-chlorophenyl)-2-oxoethyl 4- aminobenzoate (2c) have been described. The reaction offered convenient, mild conditions, high purity and good yield. The crystalstructure stability is consolidated by C ― H… π interactions and weak π − π stacking interactions in compound 2b whereas the stability is mainly due to Van der Waals interactions in compounds 2a and 2c.
is 6-methyl-2,2'-bipyridine). Herein the synthesis, characterization and crystalstructure of a new indium(III) complex containing 5,5’-Dimethyl-2,2’- bipyridine ligand by the formula of [In(5,5’-DiMeBiPy) Cl 3 (DMSO)].2(DMSO) have been reported.
Geometry . All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.
A single crystal with dimensions of 0.15mm × 0.11mm × 0.06mm was mounted on a Bruker Apex CCD diffractometer equipped with a graphite-mono- chromatic MoKα radiation at 295(2) K. Crystallo- graphic data for the title compound are summarized in Table 1. A total of 892 reflections were taken from 3.91<θ<28.10º, yielding 370 unique reflections (R int
hedra generates a dense three-dimensional network in which each calcium cation is surrounded by five others linked via edges with Ca Ca separations clustered in the narrow range of 3.6938 (5)–3.8712 (5) A ˚ . There appear to be small voids in the structure but these correspond to the P—H vertices and a PLATON (Spek, 2009) analysis did not reveal any free space in the structure.
different synthesis route involving refluxing in concentrated phosphorous acid and using HF to precipitate the desired compound (Millini et al., 1993). The structure was elucidated from powder X-ray diffraction data and has many similarities to the title structure shown above (Table 1). The main difference between the two is the metal–oxygen bond length, where the Ce—O bond length is unsurprisingly slightly longer. The zirconium coordination appears to be a bit closer to being octahedral than the cerium, but they are nearly the same after comparing the error of refinement.
The starting material SrAs was synthesized by heating stoi- chiometric amounts of Sr (Sigma–Aldrich, 99.95%) and As (Alfa Aesar, 99.99999+%) in alumina crucibles, sealed in silica ampules under an atmosphere of purified argon for 20 h at 1223 K. The title compound was obtained via high-pressure synthesis using a modified Walker-type multianvil set-up driven by a 1000 t hydraulic press (Voggenreiter, Mainleus, Germany). A Cr 2 O 3 -substituted (6%) MgO octahedron
The result of elemental analysis indicated that the composition of Ni (II) complex conforms to a 1:3 metal-to-ligand stoichiometry, and is accorded with the result of single crystal X-ray diffraction analysis. The Ni (II) complex is soluble in DMF, DMSO, methanol, a little soluble in ethanol and acetone, insoluble in benzene, diethyl and THF. The molar conductance value of the Ni (II) complex measured in CH 3 OH solution (1×10 -3 mol L -1 ) at 25 °C is 8.8 scm 2
been synthesized using branched tube method. Compound 1 was structurally characterized by single crystal X-ray diffraction, IR spectroscopy and Thermal gravimetric (TG) and differential thermal analysis (DTA). The crystalstructure of compound 1 consists of a 3D supramolecular compound and shows the coordination number in the Pb(II) ions is six. Calcination of the compound 1 at 500, 550 and 600ᵒC under air atmosphere yields mixture of orthorhombic and tetragonal PbO nanoparticles and nanorods.
In the title structure, all atoms are located in general posi- tions. The three crystallographically different molybdenum atoms have a tetrahedral coordination with Mo—O distances between 1.715 (3) and 1.801 (2) A ˚ . The mean distances (Mo1—O = 1.762, Mo2—O = 1.766 and Mo3—O = 1.760 A ˚ ) are in good accordance with those usually observed in molybdates (Abrahams et al., 1967; Harrison & Cheetham, 1989; Smit et al., 2006). The [Mg,Fe]—O distances and the cis O—[Mg,Fe]—O angles in the [Mg,Fe] 2 O 10 units range from
Crystal data, data collection and structure refinement details are summarized in Table 1. The (001) reflection, affected by the beamstop, has been removed from the refinement. Another reflection (201), flagged as potentially affected by the beamstop, was in fact not and was kept in the refinement. After positioning and refining all the atom positions except Ni2b, the difference Fourier map revealed residual density (’8 e A ˚ 3 ) near Ni2a (at ’0.6 A ˚ ). It was refined introducing a second position Ni2b with complementary occupation. The occupancy ratio was refined to 0.80 (4):0.20 (4) for the Ni2a/ Ni2b site, constraining the sum to be equal to 1.
The X-ray diffraction measurements were made on a STOE IPDS-II diffractometer with graphite monochromated Mo-K α radiation. For 1, a blue needle crystal of 0.30 × 0.10 × 0.05 mm and for 2, a blue plate crystal of 0.45 × 0.35 × 0.15 mm were mounted on a glass fiber and used for data collection. Cell constants and an orientation matrix for data collection were obtained by least-squares refinement of the diffraction data from 6370 for 1 and 23117 for 2 unique reflections. Data were collected at 298(2) and 120(2) K t o a maximum 2θ value of 58.34° for 1 and 58.32° for 2 and in a series of ω scans in 1° oscillations and integrated using the Stoe X-AREA  software package. The numerical absorption coefficient, μ, for Mo-K α radiation is 1.647 mm -1
O(1)#1-Co(1)-O(1)#3=89.35(7) Å; total = 360.02(8) Å].It is seen from Fig.2a, each simpleunit linked with six adjacent units through hydrogen bonding interactionsof R 1 2 (6) patterns. On one hand, the four O-atoms of the coordinated water in each chain are engaged in eight hydrogen bondings with the non-coordinating carboxylate groups of nicotinic acid ligands of the six adjacent units ,on the other hand, in each unit, the four O-atoms of the two nicotinic acid ligands are also engaged in eight hydrogen bondings with six O-atoms of the coordinated water in the same six adjacent units. For example, Co2 and Co5 units are connected to the center Co unit through four O-H…O hydrogen bondsrespectively ; while the other four cobalt units (Co1, Co3, Co4 and Co6 units) are also linked with center Co unit with two O-H…O hydrogen bonds respectively. In this way, the adjacent molecules recognize eachother to generate a 2D supramolecular chain between the uncoordinated carboxylate oxygen atoms (O2, O3) and aquae oxygen atoms (O1)[O(1)-H(1A)...O(2) vi ,2.7099(15)Å;O(1)-H(2A)...O(3) vii , 2.6936(19)Å; symmetry code (vi): x+1/2,y+1/2,z+1; (vii):-x+1,-y,-z+1 ](Fig. 2b). Such strong hydrogen bonds in the crystal lattice of 1 make the crystals more stable. It is worthwhile to note that a 3D hydrogen bonding network were formed if thehydrogen bonding interactions between O1 atoms of carboxylate groups and H atoms of the pyridyl group with C3 and C4 [C3–H3…O1, 3.585 Å; C4-H4…O1, 3.983Å] are all taken into account, which contributes to the additional stability of thestructure (Fig. 3a). Need to add that in the solid state, π … π interactions are observed as illustrated in Fig. 3b. and the two coordinated pyridyl rings of nicotinic acid ligands in one molecule unit are interact with other pyridyl rings from adjacent units (3.744 Å for centroid-centroid distance), which consolidate the 3D network structure of the supramolecular.
The title compound was synthesized following Claisen-Schmidt condensation reaction and the structure of this compound was confirmed by IR, 1 H NMR, UV-Vis spectroscopy and single crystal X-ray diffraction. The structure was optimized by DFT using B3LYP/6-311G basis set and geometrical parameters are in good agreements with XRD results. The vibrational wave numbers were examined theoretically and the normal modes were assigned by potential energy distribution calculation. The UV-Vis spectrum studied by TD-DFT/CAM-B3LYP was reasonably capable of predicting the excitation energies and the absorption spectra of the molecule. The molecular orbital coefficients analyses suggest that the electronic transitions are mainly π → π*. The calculated HOMO-LUMO band gap shows the chemical reactivity of the molecule. Using NBO analysis the stability of the molecule arising from hyper-conjugative interaction and charge delocalization through π-conjugated bridge has been analyzed. A computation of the first hyperpolarizability indicates that compound may be a good candidate as a NLO material. The calculated relative value of local reactivity descriptors ( , , ) at C-5 indicate that this site is more prone to nucleophilic attack. Thus, synthesized molecule 3 may be used as intermediate for the synthesis of new heterocyclic compounds such as pyrazoline and oxazoline. Intramolecular interactions and ellipticity studied by AIM approach confirms the presence of resonance assisted intramolecular hydrogen bond of medium strength between O1… H37.
units were drawn as Hirshfeld surfaces (Hirshfeld, 1977) and some others as ‘ball-and-stick’ models for clarity. The selected contributions to the crystal packing are shown as two-dimensional Hirshfeld surface fingerprint plots with cyan dots (Wolff et al., 2012). The analysis of the complete asymmetric units of the three crys- talline modifications suggests that the contribution of the H H and H I contacts for the crystal cohesion are 43.30% and 17.40% for the modification (Fig. 7a and 7b). For the modification, the values for the H H and H I contacts amount to 29.20% and 33.90% (Fig. 7c and 7d). Finally, for the modification the values for the selected contacts amount to 23.00% and 39.70% (Fig. 7e and 7f). The H H and H I contacts were selected for comparison and analysis of the four crystalline modifications because they are the most frequent (in percentage terms) for all structures, but still show clear differences between the polymorphs.