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Journal articles on the topic 'Sodium. X-ray crystallography'

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Published: 4 June 2021

Last updated: 28 January 2023

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1

Tirkkonen, B., A. Aukrust, E. Couture, et al. "Physicochemical characterisation of mangafodipir trisodium." Acta Radiologica 38, no. 5 (1997): 780–89. http://dx.doi.org/10.1080/02841859709172411.

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Purpose: To determine the structure and various physicochemical properties of man-gafodipir (MnDPDP) trisodium, the active ingredient of Teslascan, a new organ-specific contrast medium for MR imaging. Material and Methods: The structure of MnDPDP trisodium crystals was determined by X-ray crystallography. The possible existence of polymorphism in MnDPDP trisodium was evaluated by powder X-ray diffraction, optical microscopy, thermal analysis and IR spectroscopy. In addition, various spectroscopic techniques and physicochemical measurements were used for characterisation of MnDPDP trisodium. Re

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2

Chu, De-Qing, Ji-Qing Xu та Ao-Qing Tang. "The Synthesis and Structural Characterization of a Two-Dimensional Coordination Polymer [Co(H2O)(phen)(μ4-bta)1/2]n (H4bta = Benzenetetracarboxylic Acid)". Collection of Czechoslovak Chemical Communications 66, № 6 (2001): 870–76. http://dx.doi.org/10.1135/cccc20010870.

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Complex [Co(H2O)(phen)(μ4-bta)1/2]n was hydrothermally synthesized from sodium benzene-1,2,4,5-tetracarboxylate, 1,10-phenanthroline and CoCl2·6H2O, and structurally characterized by single-crystal X-ray crystallography, showing that it possesses a novel two-dimensional polymeric structure.

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3

Hu, Jiaxin, Leonard J. Barbour та George W. Gokel. "Cation-π Interactions Between Alkali Metal Cations and Neutral Double Bonds". Collection of Czechoslovak Chemical Communications 69, № 5 (2004): 1050–62. http://dx.doi.org/10.1135/cccc20041050.

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Two-armed lariat ethers having double bonds present in their side arms form stable complexes with sodium and potassium cations. When the double bonds are positioned appropriately, cation-π interactions are observed between the neutral double bonds and the macroring- bound cation as demonstrated by X-ray crystallography.

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4

Tagg, S. L., J. C. Huffman, and J. W. Zwanziger. "Crystal Structure and Sodium Environments in Sodium Tetratellurite, Na2Te4O9, and Sodium Tellurite, Na2TeO3, by X-ray Crystallography and Sodium-23 NMR." Chemistry of Materials 6, no. 10 (1994): 1884–89. http://dx.doi.org/10.1021/cm00046a052.

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5

Pressprich, Mark R., Mark A. White, Yanina Vekhter, and Philip Coppens. "Analysis of a metastable electronic excited state of sodium nitroprusside by X-ray crystallography." Journal of the American Chemical Society 116, no. 12 (1994): 5233–38. http://dx.doi.org/10.1021/ja00091a030.

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6

Tabba, Hani D., Nidal M. Yousef, and Mohammad M. Al-Arab. "Michael-Michael Aldol Reaction of Chalcones with Cyanoacetylurea and Cyanoacetylpiperidine." Collection of Czechoslovak Chemical Communications 60, no. 4 (1995): 594–604. http://dx.doi.org/10.1135/cccc19950594.

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Several highly substituted cyclohexane derivatives were synthesized by the one-pot condensation of chalcones and cyanoacetylurea (2 : 1) using sodium alkoxide in anhydrous alcohol at room temperature. The structure of the reaction products was established by infrared, 1H and 13C NMR spectroscopy as well as by their elemental analysis. Single crystal X-ray crystallography shows the presence of the cyclohexane moiety.

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7

Wieber, Markus, and Ralph Habersack. "Bis(triorganotelluronium)hexasulfide / Bis(triorganotelluronium)hexasulfides." Zeitschrift für Naturforschung B 49, no. 10 (1994): 1314–18. http://dx.doi.org/10.1515/znb-1994-1002.

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AbstractThe reaction of triorganolelluronium chlorides R3TeCl (R = Me, Ph, 4-tBu-C6H4) with Na2Sx, (x = 4 - 6) yields the corresponding bis(triorganotelluronium) hexasulfides (R3Te)2S6 regardless of the employed sodium polysulfide or the size of the lelluronium cation. All compounds are thermally stable and insensitive to moisture or air. (Ph3Te)2S6 was structurally characterized by X-ray crystallography (monoclinic, space group P21/c). Each tellurium atom is connected to both ends of the hexasulfide chain.

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8

TAGG, S. L., J. C. HUFFMAN, and J. W. ZWANZIGER. "ChemInform Abstract: Crystal Structure and Sodium Environments in Sodium Tetratellurite, Na2Te4O9, and Sodium Tellurite, Na2TeO3, by X-Ray Crystallography and Sodium-23 NMR." ChemInform 26, no. 18 (2010): no. http://dx.doi.org/10.1002/chin.199518001.

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9

Kovácsová, Gabriela, Marie Luise Grünbein, Marco Kloos, et al. "Viscous hydrophilic injection matrices for serial crystallography." IUCrJ 4, no. 4 (2017): 400–410. http://dx.doi.org/10.1107/s2052252517005140.

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Serial (femtosecond) crystallography at synchrotron and X-ray free-electron laser (XFEL) sources distributes the absorbed radiation dose over all crystals used for data collection and therefore allows measurement of radiation damage prone systems, including the use of microcrystals for room-temperature measurements. Serial crystallography relies on fast and efficient exchange of crystals upon X-ray exposure, which can be achieved using a variety of methods, including various injection techniques. The latter vary significantly in their flow rates – gas dynamic virtual nozzle based injectors pro

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10

Field, LD, TW Hambley, BD Jacobs, K. Wilson, and RK Norris. "1H D.N.M.R. and X-Ray Structure of 2,2-Dimethyl-1-(Para-nitrophenyl)propyl Mesityl Sulfone." Australian Journal of Chemistry 41, no. 4 (1988): 443. http://dx.doi.org/10.1071/ch9880443.

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2,2-Dimethyl-1-(p- nitrophenyl ) propyl mesityl sulfone (3), formed by an SRN1 reaction between sodium mesitylenesulfinate and p-(1-chloro-2,2- dimethylpropyl )nitrobenzene displays a number of conformational interconversions in solution. The activation parameters for the rotation of the mesityl ring about the aryl-sulfur bond and the rotation of the p- nitrophenyl ring about the aryl-carbon bond were determined by 1H d.n.m.r .spectroscopy. The conformation of (3) in the solid state, determined by X-ray crystallography, is very similar to the preferred ground-state conformation of the molecule

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11

Buchanan, G. W., S. Mathias, C. Bensimon, and J. P. Charland. "Stereochemistry of crown ethers, X-ray crystallographic structures, solid phase 13C NMR, and solution conformational equilibria in cis-syn-cis dicyclohexano-15-crown-5 ether and its sodium thiocyanate complex." Canadian Journal of Chemistry 70, no. 3 (1992): 981–91. http://dx.doi.org/10.1139/v92-900.

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The structures of the title materials have been determined via X-ray crystallography. In the free crown ether, there is effectively a plane of symmetry that bisects the molecule. In the NaNCS complex, ring inversion of one of the cyclo-hexane moieties has occurred, giving a distorted pentagonal pyramidal coordination geometry about the sodium ion. For the free crown, two conformers, whose free energies differ by ca. 0.5 kJ / mol in solution can be detected via 13C NMR at 168 K. Limiting low-temperature solution spectra are compared to those which have been obtained in the solid phase using the

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12

Black, DS, N. Chaichit, BM Gatehouse, and GI Moss. "Metal Template Reactions. XXV. N-Acyl Isatin Precursors for the Synthesis of Malonamido Macrocyclic Metal Complexes." Australian Journal of Chemistry 40, no. 10 (1987): 1745. http://dx.doi.org/10.1071/ch9871745.

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Reaction of sodium isatide with dimethylmalonyl dichloride yielded the oxazinoindole (6) rather than the expected product (4). The glyoxylamide (8), which served as a precursor to the macrocyclic complex (15), was therefore prepared by a sequence involving compounds (9), (10) and (7). Such a route makes use of the reactivity of N-acyl isatins and the protecting capacity of the benzyloxycarbonyl group. The structure of compound (6) was established by X-ray crystallography.

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13

Arnold, AP, KJ Cavell, AJ Edwards, BF Hoskins, and EJ Peacock. "Preparation and X-Ray Crystal-Structure of 4,4'-Triselenobis(pent-3-en-2-one)." Australian Journal of Chemistry 41, no. 10 (1988): 1601. http://dx.doi.org/10.1071/ch9881601.

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The title compound was prepared by the reaction of sodium hydrogen selenide with 4-chloropent-3-en-2-one. The compound appears unstable with respect to higher oligomers of the SeC (CH3)CHC(CH3)O ( seacac ) unit. X-ray crystallography reveals the unusual structure in which a central 'complexed' selenium atom is coordinated to the two selenium atoms of the seacac ligands which are in their normal cis conformations. The oxygen atoms are uncoordinated and as far removed from the coordination environment of the central selenium atom as possible. Crystals of Se( seacac )2 are orthorhombic with space

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14

Casaretto, Nicolas, Dominik Schaniel, Paul Alle, et al. "In-house time-resolved photocrystallography on the millisecond timescale using a gated X-ray hybrid pixel area detector." Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials 73, no. 4 (2017): 696–707. http://dx.doi.org/10.1107/s2052520617009234.

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With the remarkable progress of accelerator-based X-ray sources in terms of intensity and brightness, the investigation of structural dynamics from time-resolved X-ray diffraction methods is becoming widespread in chemistry, biochemistry and materials science applications. Diffraction patterns can now be measured down to the femtosecond time-scale using X-ray free electron lasers or table-top laser plasma X-ray sources. On the other hand, the recent developments in photon counting X-ray area detectors offer new opportunities for time-resolved crystallography. Taking advantage of the fast read-

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15

Maksin, V. I., R. V. Lavrik, T. I. Ushchapivska, and O. V. Petrenko. "Growing of single-crystals of double sodium-manganese(II) pyrophosphate." Voprosy Khimii i Khimicheskoi Tekhnologii, no. 1 (January 2022): 76–82. http://dx.doi.org/10.32434/0321-4095-2022-140-1-76-82.

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Single crystals of Na2Mn3(P2O7)2 compound have been first obtained during the examination of interaction in the Na2O–P2O5–Mn2O3–NaF (10 wt.%.) system in the fluxes with Na2O:P2O5 molar ratios ranging from 0.52 to 0.76 (saturated with manganese(III) oxide 25.0–32.0 wt.%) at the temperatures of 960–8800С. Optimum conditions for the synthesis and growing of single crystals of Na2Mn3(P2O7)2 compound have been determined. Complete X-ray diffraction analysis of the synthesized phosphate Na2Mn3(P2O7)2 has been performed. According to its structure, the double phosphate Na2Mn3(P2O7)2 belongs to the tr

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16

Pérez, Diego, Pankaj Sharma, Ana M. Ortiz, et al. "Synthesis, Characterization and Crystal Structures of 1,2-Disubstituted Ferrocenyl Stibines." Zeitschrift für Naturforschung B 67, no. 1 (2012): 36–40. http://dx.doi.org/10.1515/znb-2012-0107.

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New 1,2-disubstituted ferrocenyl stibines containing a -CH2OR pendant arm were synthesized and characterized by various spectral and analytical methods. Nucleophilic substitution of rac-diphenyl[( 2-trimethylammoniomethylferrocen-1-yl)]stibine iodide by methanol produces compound Fc(CH2OMe)SbPh2 (1). The acetylation of diphenyl(2-dimethylaminomethylferrocen-1-yl)stibine by acetic anhydride affords compound Fc(CH2OCOCH3)SbPh2 (2), which on further reaction with sodium hydroxide affords the alcohol Fc(CH2OH)SbPh2 (3). The molecular structures of the stibines 1, 2 and 3 were determined by X-ray c

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17

Voronin, Alexey A., Sofya P. Balabanova, Ivan V. Fedyanin, et al. "Anions Containing Tripoid Conjugated N4− System: Salts of 5-(Substituted Amino)-[1,2,3]triazolo[4,5-c][1,2,5]oxadiazol-5-ium-4-ides, as well as Their Synthesis, Structure, and Thermal Stability." Molecules 27, no. 19 (2022): 6287. http://dx.doi.org/10.3390/molecules27196287.

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A strategy for the synthesis of 5-((2-cyanoethyl)-X-amino)-[1,2,3]triazolo[4,5-c][1,2,5]oxadiazol-5-ium-4-ides (X = H; CH2CH2CN; NO2 (4a); CN (4b); CO2Et (4c)) starting from 3-amino-4-azido-1,2,5-oxadiazole was developed. The key step in this strategy is the intramolecular thermolytic cyclization of the azido group and the bis(2-cyanoethyl)triazene group. Removal of the 2-cyanoethyl protecting group from amides 4a–c gave potassium salt of the corresponding nitramide and sodium salts of cyano- and ethoxycarbonylamide. The structure and thermal stability of the synthesized compounds were studied

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18

Armstrong, David R., Liam Balloch, Eva Hevia, et al. "Meta-metallation of N,N-dimethylaniline: Contrasting direct sodium-mediated zincation with indirect sodiation-dialkylzinc co-complexation." Beilstein Journal of Organic Chemistry 7 (September 6, 2011): 1234–48. http://dx.doi.org/10.3762/bjoc.7.144.

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Previously we reported that direct zincation of N,N-dimethylaniline by the mixed-metal zincate reagent 1 ((TMEDA)Na(TMP)(t-Bu)Zn(t-Bu)) surprisingly led to meta-metallation (zincation) of the aniline, as manifested in the crystalline complex 2 ((TMEDA)Na(TMP)(m-C6H4-NMe2)Zn(t-Bu)), and that iodination of these isolated crystals produced the meta-isomer N,N-dimethyl-3-iodoaniline quantitatively. Completing the study here we find that treating the reaction solution with iodine produces a 72% conversion and results in a mixture of regioisomers of N,N-dimethyliodoaniline, with the meta-isomer stil

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19

McKague, A. Bruce, Douglas W. Reeve, Steven J. Rettig, and James Trotter. "Reactions of lignin model compounds with pulp bleaching chemicals. Cannizzaro-type reaction of tetrachloro-o-benzoquinone with alkali." Canadian Journal of Chemistry 70, no. 6 (1992): 1706–10. http://dx.doi.org/10.1139/v92-214.

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Reaction of tetrachloro-o-benzoquinone 1 with aqueous sodium hydroxide resulted in a Cannizzaro-type disproportionation into tetrachloromuconic acid and tetrachlorocatechol. The tetrachloromuconic acid was isolated and identified by X-ray crystallography as the methyl ester of the cyclized lactone 3. Crystals of C7H3Cl3O4, 4, are orthorhombic, a = 9.991 (2), b = 7.981 (1), c = 24.626(2) Å, Z = 8, space group Pna21. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.033 for 1609 reflections with I ≥ 3σ(I).

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20

Penkova, Anita, Pascal Retailleau, and Ilia Manolov. "Crystal Structure of Poly[(acetone-O)-3-((3,4-dimethoxyphenyl)(4-hydroxy-2-oxo-2H-chromen-3-yl)methyl)-(2-oxo-2H-chromen-4-olate)sodium]." Organic Chemistry International 2010 (June 28, 2010): 1–7. http://dx.doi.org/10.1155/2010/564256.

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The structure of Poly[(acetone-O)-3-((3,4-dimethoxyphenyl)(4-hydroxy-2-oxo-2H-chromen-3-yl)methyl)-(2-oxo-2H-chromen-4-olate)sodium] was determined by X-ray crystallography. The compound crystallizes in an orthorhombic system and was characterized thus P 21 21 21, a=9.967(2) Å, b=11.473(3) Å, c=22.176(5) Å. Z=4, V=2535.9(10) Å3. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F2 to final values of R1=0.0601 and wR2=0.1515.

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21

Dilsky, Stefan, and Wolfdieter A. Schenk. "Anionic Tungsten Carbonyl Complexes Containing Dithiocarboxylate, Dithiocarbamate, and Xanthate Ligands." Zeitschrift für Naturforschung B 61, no. 5 (2006): 570–76. http://dx.doi.org/10.1515/znb-2006-0511.

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The reaction of Et4N[W(CO)5Cl] with sodium dithiobenzoate, ethylxanthate, or various dithiocarbamates gave the corresponding salts Et4N[W(CO)4(SSCX)] (X = Ph, NEt2, N(H)t-Bu, NPh2, OEt) which contain the dithio ligand in a chelating bonding mode. Two of them (X = N(H)t-Bu, NPh2) were characterized by X-ray crystallography. The tungsten atom resides in the center of a slightly distorted octahedron surrounded by a symmetrically bidentate planar dithio ligand and four CO groups. Reaction with PPh3 or PMe3 at elevated temperature gave the tricarbonyl complexes Et4N[W(CO)3(PR3)(SSCX)] and in one ca

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22

Catterall, William A., Michael J. Lenaeus, and Tamer M. Gamal El-Din. "Structure and Pharmacology of Voltage-Gated Sodium and Calcium Channels." Annual Review of Pharmacology and Toxicology 60, no. 1 (2020): 133–54. http://dx.doi.org/10.1146/annurev-pharmtox-010818-021757.

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Voltage-gated sodium and calcium channels are evolutionarily related transmembrane signaling proteins that initiate action potentials, neurotransmission, excitation-contraction coupling, and other physiological processes. Genetic or acquired dysfunction of these proteins causes numerous diseases, termed channelopathies, and sodium and calcium channels are the molecular targets for several major classes of drugs. Recent advances in the structural biology of these proteins using X-ray crystallography and cryo-electron microscopy have given new insights into the molecular basis for their function

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23

Yamada, Yohei, Shota Toyama, and Tomoki Yabutani. "Effects of solvents on the crystal structure of cross-linked lysozyme crystals." International Journal of Modern Physics B 32, no. 19 (2018): 1840041. http://dx.doi.org/10.1142/s0217979218400416.

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The effects of solvents on the structural stability of cross-linked lysozyme crystals were investigated by an immersion test using alkaline (0.1 M ammonia [NH3] and 0.1 M sodium hydroxide [NaOH]), acidic (0.1 M acetic acid [CH3COOH] and 0.1 M hydrochloric acid [HCl]) and organic (50% [v/v] and undiluted ethanol, acetone, 2-propanol and dimethyl sulfoxide [DMSO]) solvents. The morphology and lattice constants were monitored by optical microscopy and X-ray crystallography. The cross-linked crystals exhibited good stability against NH3, CH3COOH, HCl, ethanol, acetone and 2-propanol. However, samp

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24

Carr, Jenny M., Peter J. Duggan, David G. Humphrey, and Edward M. Tyndall. "Enhanced Anti-Fungal Activity of the Organo-Soluble Borate Ester, Tetra-n-butylammonium Bis(ortho-hydroxymethylphenolato)borate." Australian Journal of Chemistry 58, no. 1 (2005): 21. http://dx.doi.org/10.1071/ch04247.

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The borate ester, tetra-n-butylammonium bis(ortho-hydroxymethylphenolato)borate, NBu4[B(o-hmp)2], was synthesized and characterized by NMR spectroscopy (1H, 13C, 11B), ES-MS, and X-ray crystallography. The anti-fungal activity of this compound, as well as its sodium salt, the parent phenol, tetra-n-butylammonium bromide, and boric acid were evaluated against two wood decay fungi. The tetraalkylammonium borate NBu4[B(o-hmp)2] shows the highest activity out of the compounds examined. This finding suggests that the formation of lipophilic borate esters is a promising approach for the development

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25

Maltezou, Elena, Marios Stylianou, Sudeshna Roy, Chryssoula Drouza, and Anastasios D. Keramidas. "Synthesis, Solution, and Structural Characterization of Tetrahydrofuranyl-2,2-Bisphosphonic Acid Disodium Salt." Bioinorganic Chemistry and Applications 2010 (2010): 1–7. http://dx.doi.org/10.1155/2010/563875.

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Bisphosphonates are biologically relevant therapeutics for bone disorders and cancer. Reaction ofγ-chlorobutyric acid, phosphorus acid, and phosphorus trichloride without the use of solvent gave the tetrahydrofuranyl-2,2-bisphosphonate sodium salt (Na2H2L). TheNa2H2Lwas isolated, characterized in solution byH,C, andPNMR spectroscopy and in solid state by single X-Ray crystallography. The crystal structure showed that theNa2H2Lforms in the crystal infinite two-dimensional sheets stacked one parallel to the other. A comparison of the chelating properties ofH2L2−with similar hydroxyl bisphosphona

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26

Levason, William, J. Steven Ogden, Mark D. Spicer, Michael Webster, and Nigel A. Young. "Characterization of sodium bromite by x-ray crystallography and bromine K-edge EXAFS, IR, Raman, and NMR spectroscopies." Journal of the American Chemical Society 111, no. 16 (1989): 6210–12. http://dx.doi.org/10.1021/ja00198a035.

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27

Bennett, B. A., M. R. Shahbandeh, and M. Streat. "Sorption of caesium by complex hexacyanoferrates: II. X-ray crystallography and mössbauer spectroscopy of sodium-copper cyanoferrates (II)." Journal of Chemical Technology and Biotechnology 32, no. 5 (2007): 586–93. http://dx.doi.org/10.1002/jctb.5030320506.

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28

Ma, Chunlin, Junhong Zhang, and Rufen Zhang. "Syntheses, characterization, and X-ray crystal structures of diorganotin(IV) derivatives of 2-pyridinethiolato-N-oxide." Canadian Journal of Chemistry 81, no. 10 (2003): 1070–75. http://dx.doi.org/10.1139/v03-134.

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The diorganotin(IV) dichloride reacts with sodium 2-pyridinethiolato-N-oxide in a 1:1 ratio to produce [Me2SnCl(2-SpyO)] (1), [Et2SnCl(2-SpyO)] (2), [Bu2SnCl(2-SpyO)] (3), [Ph2SnCl(2-SpyO)] (4), and [(PhCH2)2SnCl(2- SpyO)] (5). The new complexes have been characterized by elemental analysis and IR and NMR (1H, 119Sn, and 13C) spectroscopy. On the basis of 119Sn NMR data the effective coordination number in solution is five. The structures 1 and 4 have been confirmed by X-ray crystallography. Crystals of 1 are triclinic with space group P[Formula: see text] and those of 4 are monoclinic, P21/n.

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29

Fewings, Kym R., and Peter C. Junk. "The Syntheses and Structural Characterizations of Some Monoaza- and Diaza-crown Ethers." Australian Journal of Chemistry 52, no. 12 (1999): 1109. http://dx.doi.org/10.1071/ch99103.

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Several aza-crown ethers have been synthesized and their structures determined by X-ray crystallography. In a modified synthesis of diaza-18-crown-6 we isolated two of the intermediates, viz. the NaI salt (1) of N,N′-dibenzyldiaza- 18-crown-6 and the salt-free macrocycle (2), and determined their stuctures. In compound (1) a hydrated crown-encapsulated sodium cation was revealed with both benzyl groups folded down and away from the water molecule while in compound (2) a centrosymmetric crown with the benzyl groups splayed out from the ring was found. In addition, we have determined the X-ray c

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30

Venkatachalam, Taracad K., Paul V. Bernhardt, Damion H. R. Stimson, Gregory K. Pierens, Rajiv Bhalla, and David C. Reutens. "A Novel Strategy to Introduce 18F, a Positron Emitting Radionuclide, into a Gallium Nitrate Complex: Synthesis, NMR, X-Ray Crystal Structure, and Preliminary Studies on Radiolabelling with 18F." Australian Journal of Chemistry 71, no. 3 (2018): 81. http://dx.doi.org/10.1071/ch17334.

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A hexan-3,4-dione bis(4N-phenylthiosemicarbazone) gallium nitrate complex was synthesised and the structure was confirmed by NMR studies. The complex was prepared using an appropriately substituted dithiosemicarbazone and sodium methoxide in anhydrous methanol. The structure was further confirmed using single crystal X-ray crystallography. The crystal structure of gallium nitrate complex of diphenylthiosemicarbazone comprise a planar configuration of the tetradentate coordinated thiosemicarbazone with the Ga3+ ion, with the nitrate ligand occupying the apical coordination site. The X-ray struc

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31

Jumina, Jumina. "ALDOL CONDENSATION OF N-ALKYLATED-3-ARYL-4,6-DIMETHOXY-7-FORMYLINDOLES AS A GOOD METHOD FOR THE SYNTHESIS OF 1-ARYL-6,8-DIMETHOXYPYRROLO[3,2,1-hi]INDOLE-4-CARBOXYLATES." Indonesian Journal of Chemistry 6, no. 3 (2010): 297–303. http://dx.doi.org/10.22146/ijc.21735.

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Alkylation of 3-aryl-4,6-dimethoxyindole 3a and 3b with methyl and ethyl a-bromoacetates afforded good yields of indol-1-ylacetates 4. Treatment of these indoles 4 with the Vilsmeier formylation reagent gave formylindoles 5 in 54-81 % yield. These formylindole 5 underwent intramolecular aldol condensation when treated with sodium hydride in tetrahydrofuran to give pyrroloindole-4-carboxylates 6 in 30-60 % yield. Structural assignment based on spectroscopic data confirmed the structure of the synthesized pyrroloindoles. In the case of pyrroloindole 6c, the structure of this molecule was also pr

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32

Tamasi, A. L., C. L. Barnes, and J. R. Walensky. "Structure and spectroscopy of uranyl salicylaldiminate complexes." Radiochimica Acta 101, no. 10 (2013): 631–36. http://dx.doi.org/10.1524/ract.2013.2071.

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Summary The synthesis of uranyl complexes coordinated to tridentate, monoanionic salicylaldiminate (Schiff base) ligands was achieved by the reaction of UO2Cl2(THF)3, 1, with one equivalent of the corresponding sodium salicylaldiminate salts affording [(C9H6N)N=C(H)C6H2t Bu2O]UO2Cl(THF), 2, [(NC5H4)N=C(H)C6H2 t Bu2O]UO2Cl(THF), 3, and [(C6H4SCH3)N=C(H)C6H2tBu2O]UO2Cl(THF), 4. These are uncommon examples of uranyl complexes with a monoanionic ancillary ligand to stabilize the coordination sphere and one chloride ligand. Compounds 2-4 have been characterized by 1H and 13C NMR spectroscopy as wel

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Mackay,, Maureen F., Michael J. McTigue, and Maruse Sadek. "Conformation of a Fluorochrome from Aniline Blue." Australian Journal of Chemistry 50, no. 10 (1997): 987. http://dx.doi.org/10.1071/c97066.

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The solid-state conformation of the fluorochrome sodium 4,4′-[carbonylbis(benzene-4,1-diyl)bis(imino)]-bisbenzenesulfonate has been defined by single-crystal X-ray crystallography. Monoclinic crystals belong to the space group C 2/c with a 11·732(1), b 6·185(1), c 37·179(3) Å, β 94·40(1)° and Z 8. The structure was refined to a final R0·042 for all 2271 unique terms. In the crystal six oxygen atoms form an octahedral grouping around the sodium ion and these octahedra are linked into layers sandwiched between the layers of organic anions which adopt an extended conformation. The n.m.r. spectra

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34

Zahra, Asmat, Tariq Mahmud, Hazoor Ahmad Shad, et al. "Synthesis, Characterization and Magnetic Studies of Cobalt (II), Manganese (II) and Copper (II) Complexes containing Nitrogen-Oxygen Donor Ligands." Revista de Chimie 69, no. 7 (2018): 1722–27. http://dx.doi.org/10.37358/rc.18.7.6404.

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Transition metal complexes, [M(COOPh)2(TMEDA)�(OH2)], (where M=Co+2 and Mn+2) and [Cu3(COOPh)2(TEA)2(CH3COO)2] have been synthesized by using sodium benzoate, tetramethyl-ethylenediamine and triethanolamine. The bonding nature and structure of complexes (1), (2) and (3) were explored through X-ray crystallography, IR, elemental analysis and magnetic studies. Single crystal X-ray analysis showed that in (1) and (2) complexes, each M (II) is bridged by two benzoate ions, one TMEDA and one water molecule while in (3) complex, Cu1 is coordinated by four oxygen atoms, two from TEA and two from carb

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35

Szarek, Walter A., George W. Hay, Ramesh K. Sood, Konia Trouton, and Suzanne Fortier. "X-Ray structure determination of 1,2-anhydro-3,4:5,6-di-O-isopropylidene-1-C-nitro-D-mannitol." Canadian Journal of Chemistry 66, no. 7 (1988): 1600–1604. http://dx.doi.org/10.1139/v88-259.

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The structure of the major product of the reaction of 1,2-dideoxy-3,4:5,6-di-O-isopropylidene-1-C-nitro-D-arabino-hex-1-enitol with 30% hydrogen peroxide and aqueous sodium hydrogencarbonate has been confirmed by X-ray crystallography to be that of 1,2-anhydro-3,4:5,6-di-O-isopropylidene-1-C-nitro-D-mannitol (2). The crystal structure of 2, C12H19NO7, is orthorhombic, P212121, with cell dimensions a = 10.269(3), b = 15.115(7), c = 9.295(8) Å, and Z = 4. The calculated density is Dx = 1.336 gcm−3. The structure was solved by direct methods and refined to a residual R = 0.052. The molecule has a

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36

Jagleniec, Damian, Krzysztof Ziach, Kajetan Dąbrowa, and Jan Romański. "The Effect of Substitution Pattern on Binding Ability in Regioisomeric Ion Pair Receptors Based on an Aminobenzoic Platform." Molecules 24, no. 16 (2019): 2990. http://dx.doi.org/10.3390/molecules24162990.

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A series of ditopic ion pair receptors equipped with 4-nitrophenylurea and 1-aza-18-crown-6-ether linked by ortho-(1), meta-(2), and para-(3) substituted benzoic acid were readily synthesized in three steps from commercially available materials. The binding properties of these regioisomeric receptors were determined using UV-vis and 1H NMR spectroscopy in MeCN and in the solid state by single-crystal X-ray diffraction crystallography. The solution studies revealed that, apart from carboxylates, all the anions tested formed stronger complexes in the presence of sodium cations. Receptors 2 and 3

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Resende, Diana I. S. P., Amalia M. Estévez, Andre M. Alker, Rainer E. Martin, and Hans Peter Wessel. "A carbohydrate-derived trifunctional scaffold for medicinal chemistry library synthesis." Mediterranean Journal of Chemistry 7, no. 2 (2018): 135–44. http://dx.doi.org/10.13171/mjc72/01809051415-wessel.

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For the generation of compound libraries for drug discovery a central scaffold containing three exit vectors with defined chirality was devised starting from commercially available tri-O-acetyl-glucal. Surprisingly, the reaction of a 4-O-mesylate with sodium azide did not lead to the expected 4-azido-4-deoxy derivative but to a 3-azido-3-deoxy regioisomer via intermediate epoxide formation. The absolute stereochemical configuration of the final tetrahydropyran building block was proven by X-ray crystallography. This scaffold endowed with a carboxylic acid, a secondary alcohol, and an azide fun

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38

Deslongchamps, Ghislain, Daniel Mink, Paul D. Boyle, and Nina Singh. "Unusual Weiss–Cook condensation of dimethyl 2,3-dioxobutanedioate and dimethyl 3-oxoglutarate." Canadian Journal of Chemistry 72, no. 4 (1994): 1162–64. http://dx.doi.org/10.1139/v94-148.

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The Weiss–Cook condensation of dimethyl 2,3-dioxobutanedioate with two equivalents of dimethyl 3-oxoglutarate in aqueous bicarbonate produces an "abnormal" product, pentamethyl cis-3-(carbomethoxymethyl)-3,7-dihydroxy-2-oxabicyclo-[3.3.0]oct-7-ene-1,4,5,6,8-pentacarboxylate 7, whose structure has been determined by X-ray crystallography. Rrapcho decarbomethoxylation (sodium chloride, aqueous dimethyl sulfoxide, 140 °C) of this compound produces dimethyl cis-3,7-dioxobi-cyclo[3.3.0]octane-1,5-dicarboxylate 4 in quantitative yield. These results suggest that compound 7 may be the product of a ki

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39

Amiel, Pascale, Abdallah Mahamoud, Pierre Brouant, et al. "Tautomérie du 2,5-dimercapto-1,3,4-thiadiazole et synthèse de thiadiazoloacridiniques." Canadian Journal of Chemistry 73, no. 8 (1995): 1258–66. http://dx.doi.org/10.1139/v95-154.

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Some 2(3H)-thione-5-alkylthio-1,3,4-thiadiazoles were prepared with a view to arylating these compounds with 9-chloroacridines. Using pyridine as solvent and base, this arylation led to the 2-thione-(N)3-acridinyl-5-alkylthio-1,3,4-thiadiazoles. Molecular structures of the latter were determined either by NMR spectroscopy or by referring to X-ray crystallography of the 5-(diethylaminoethylthio)-1,3,4-thiadiazole-2-thione. Thus, with respect to the tautomeric equilibrium of the compound investigated, the thione group was detected either in the solid state or in solution. In contrast, 2-acridiny

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40

Wang, Xue-Mei, Jia-Yan Qiang, Ai-Quan Jia, Bihai Tong, and Qian-Feng Zhang. "Syntheses, crystal structures and phosphorescence properties of cyclometalated iridium(III) bis(pyridylbenzaldehyde) complexes with dithiolate ligands." Zeitschrift für Naturforschung B 72, no. 12 (2017): 941–46. http://dx.doi.org/10.1515/znb-2017-0105.

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AbstractThe synthesis of three neutral bis-cyclometalated iridium(III) complexes [Ir(pba)2(S^S)] (pbaH=4-(2-pyridyl)benzaldehyde; S^S=Et2NCS2− (1), iPrOCS2− (2), (nPrO)2PS2− (3)) from [{Ir(μ-Cl)(pba)2}2] and the corresponding sodium or potassium dithiolates in methanol-dichloromethane is described. The composition of complexes 1–3 is discussed on the basis of 1H NMR, 13C NMR, IR, and mass spectroscopy, and the crystal structures of 1 and 3 were determined by X-ray crystallography. The absorption and emission spectra show that the [Ir(pba)2(S^S)] complexes may be effective candidates as green-e

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41

Bruno, Andrew, Amanda Ruby, Joseph Luft, et al. "Chemical clustering and visualization applied to macromolecular crystallography." Acta Crystallographica Section A Foundations and Advances 70, a1 (2014): C1145. http://dx.doi.org/10.1107/s2053273314088548.

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Many bioscience fields employ high-throughput methods to screen multiple biochemical conditions. The analysis of these becomes tedious without a degree of automation. Crystallization, a rate limiting step in biological X-ray crystallography, is one of these fields. Screening of multiple potential crystallization conditions (cocktails) is the most effective method of probing a proteins phase diagram and guiding crystallization but the interpretation of results can be consuming. To aid this empirical approach a cocktail distance coefficient was developed to quantitatively compare macromolecule c

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Karetsi, V. A., C. N. Banti, N. Kourkoumelis, et al. "An Efficient Disinfectant, Composite Material {SLS@[Zn3(CitH)2]} as Ingredient for Development of Sterilized and Non Infectious Contact Lens." Antibiotics 8, no. 4 (2019): 213. http://dx.doi.org/10.3390/antibiotics8040213.

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The [Zn3(CitH)2] (1) (CitH4= citric acid), was dispersed in sodium lauryl sulphate (SLS) to form the micelle of SLS@[Zn3(CitH)2] (2). This material 2 was incorporated in hydrogel made by hydroxyethyl-methacrylate (HEMA), an ingredient of contact lenses, toward the formation of pHEMA@(SLS@[Zn3(CitH)2]) (3). Samples of 1 and 2 were characterized by UV-Vis, 1H-NMR, FT-IR, FT-Raman, single crystal X-ray crystallography, X-ray fluorescence analysis, atomic absorption and TG/DTA/DSC. The antibacterial activity of 1–3 as well as of SLS against Gram-positive (Staphylococcus epidermidis (St. epidermidi

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Mishra, Manish Kumar, Upadrasta Ramamurty, and Gautam R. Desiraju. "Bimodal nanoindentation response of the (001) face in crystalline sodium saccharin dihydrate." Macedonian Journal of Chemistry and Chemical Engineering 34, no. 1 (2015): 51. http://dx.doi.org/10.20450/mjcce.2015.649.

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<p>The nanoindentation response of the (001) face of sodium saccharin dihydrate is examined. The structure can be demarcated into regular and irregular regions or domains. The regular domains have solid-like and the irregular ones have liquid-like characteristics. Therefore, these domains impart a microstructure to the crystal. The indent face (001) is prominently developed in this crystal and unambiguously presents the regular and irregular regions to nanoindention. Average values of elastic modulus and hardness show a distinct bimodal mechanical response. Such a response has been obser

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Kariuki, Benson M., Bakr F. Abdel-Wahab, Hanan A. Mohamed, Mohamed S. Bekheit, and Gamal A. El-Hiti. "Synthesis and Characterization of Novel 2-(1,2,3-Triazol-4-yl)-4,5-dihydro-1H-pyrazol-1-yl)thiazoles and 2-(4,5-Dihydro-1H-pyrazol-1-yl)-4-(1H-1,2,3-triazol-4-yl)thiazoles." Molecules 27, no. 24 (2022): 8904. http://dx.doi.org/10.3390/molecules27248904.

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Reactions of 1-(5-methyl)-1H-1,2,3-triazol-4-yl)ethan-1-ones and benzaldehydes in ethanol under basic conditions gave the corresponding chalcones. Reactions of the chalcones combined with thiosemicarbazide in dry ethanol containing sodium hydroxide afforded the corresponding pyrazolin-N-thioamides. Reactions of the synthesized pyrazolin-N-thioamides and several ketones (namely, ethyl 2-chloro-3-oxobutanoate, 2-bromoacetylbenzofuran, and hydrazonoyl chloride) gave the corresponding novel 2-(1,2,3-triazol-4-yl)-4,5-dihydro-1H-pyrazol-1-yl)thiazoles in high yields (77–90%). Additionally, 2-(4,5-d

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Crosas, Eva, Albert Castellvi, Isidro Crespo, et al. "Uridine as a new scavenger for synchrotron-based structural biology techniques." Journal of Synchrotron Radiation 24, no. 1 (2017): 53–62. http://dx.doi.org/10.1107/s1600577516018452.

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Macromolecular crystallography (MX) and small-angle X-ray scattering (SAXS) studies on proteins at synchrotron light sources are commonly limited by the structural damage produced by the intense X-ray beam. Several effects, such as aggregation in protein solutions and global and site-specific damage in crystals, reduce the data quality or even introduce artefacts that can result in a biologically misguiding structure. One strategy to reduce these negative effects is the inclusion of an additive in the buffer solution to act as a free radical scavenger. Here the properties of uridine as a scave

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46

Xiao, Y. H., H. Y. Wu, C. B. Sun, and J. L. Hou. "Synthesis, crystal structures and biological activity of trinuclear nickel(II) and copper(II) complexes derived from N,N'-bis(4-bromosalicylidene)-1,3-pentanediamine." Журнал структурной химии 63, no. 4 (2022): 521–23. http://dx.doi.org/10.26902/jsc_id91980.

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The self-assembly reaction of the bis-Schiff base N,N'-bis(4-Bromosalicylidene)-1,3-pentanediamine (H2L) with nickel chloride and sodium azide in methanol afforded a new phenolate and end-on azide bridged trinuclear nickel complex [Ni3L2(μ1,1-N3)2(CH3OH)2]2CH3OH (1). The reaction of H2L with copper acetate produced a new phenolate and acetate bridged trinuclear copper complex [Cu3L2(CH3COO)2] (2). The complexes were characterized by elemental analysis, IR and UV-Vis spectroscopy. The crystal structures of the complexes have been determined by X-ray crystallography. In complex 1, the Ni atoms a

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47

Apblett, A. W., G. D. Georgieva, and J. T. Mague. "Spectroscopic and thermochemical investigation of alkaline earth metal salts of 2-oximinopropionate." Canadian Journal of Chemistry 75, no. 5 (1997): 483–90. http://dx.doi.org/10.1139/v97-056.

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Alkaline earth metal 2-oximinopropionates were prepared by the reaction of sodium 2-oximinopropionate with the respective metal nitrates or chlorides in water at room temperature. These compounds were characterized by infrared and multinuclear NMR spectroscopy and thermogravimetric analysis. The thermal decomposition of the salts occurs in the range 144-188°C and exhibits a trend towards lower temperature with increasing size of the cation. In all cases, the decomposition yields a metal carbonate. The molecular structure of calcium 2-oximinopropionate hydrate was determined by single-crystal X

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48

Bujacz, Grzegorz, Blanka Wrzesniewska, and Anna Bujacz. "Cryoprotection properties of salts of organic acids: a case study for a tetragonal crystal of HEW lysozyme." Acta Crystallographica Section D Biological Crystallography 66, no. 7 (2010): 789–96. http://dx.doi.org/10.1107/s0907444910015416.

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Currently, the great majority of the data that are used for solving macromolecular structures by X-ray crystallography are collected at cryogenic temperatures. Selection of a suitable cryoprotectant, which ensures crystal stability at low temperatures, is critical for the success of a particular diffraction experiment. The effectiveness of salts of organic acids as potential cryoprotective agents is presented in the following work. Sodium formate, acetate, malonate and citrate were tested, as were sodium potassium tartrate and acetate in the form of potassium and ammonium salts. For each salt

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49

Sudagar, Alcina Johnson, Slávka Andrejkovičová, Fernando Rocha, et al. "Combined Influence of Low-Grade Metakaolins and Natural Zeolite on Compressive Strength and Heavy Metal Adsorption of Geopolymers." Minerals 11, no. 5 (2021): 486. http://dx.doi.org/10.3390/min11050486.

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Metakaolins (MKs) prepared from low-grade kaolins located in the Alvarães (A) and Barqueiros (B) regions of Portugal were used as the aluminosilicate source to compare their effect on the compressive strength and heavy metal adsorption of geopolymers. Natural zeolite, an inexpensive, efficient adsorbent, was used as an additive in formulations to enhance geopolymers’ adsorption capacities and reduce MK utilization’s environmental footprint. Geopolymers were synthesized with the replacement of MK by zeolite up to 75 wt.% (A25, B25—25% MK 75% zeolite; A50, B50—50% MK 50% zeolite; A75, B75—75% MK

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50

Goher, Mohamed A. S., Morsy A. M. Abu-Youssef та Franz A. Mautner. "Crystal Structures of mer-Cr(pyridine)3(N3)3 and Polymeric NaCr(pyridine)4(N3)4. A Structure Containing μ(1,3) Bridging Azido Ligands between Chromium-and Sodium-Centered Polyhedra". Zeitschrift für Naturforschung B 47, № 1 (1992): 139–43. http://dx.doi.org/10.1515/znb-1992-0124.

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The structures of mer-Cr(py)3(N3)3 (1) and polymeric NaCr(py)4(N3)4 (2) were determined by X-ray crystallography. Crystal data; 1, C15H15N12Cr, triclinic, space group P1̄, a = 895.3(2), b = 999.1(3), c = 1269.9(5) pm , α = 106.76(3), β = 96.69(3), γ = 116.30(2)°, V = 943.8(6) · 106 pm3, Z = 2 and Rw = 0.038 for 1736 observed MoKα diffractometer data; 2, C20H20N16CrNa, monoclinic, space group C2/c, a = 1561.2(3), b = 1028.8(2), c = 1573.6(4) pm, β = 90.70(2)°, V = 2 527.3(9) · 106 pm3, Z = 4 and = 0.033 for 1272 MoKα diffractometer data.The coordination around the chromium (III) ion in the disc

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