Synthesis and characterization of the Anderson – Evans tungstoantimonate [Na5(H2O)18{(HOCH2)2CHNH3}2][SbW6O24]
A novel tungstoantimonate, [Na5(H2O)18{(HOCH2)2CHNH3}2][SbVWVI6O24] (SbW6), was synthesized from an aqueous solution and structurally characterized by single-crystal X-ray diffraction, which revealed C2/c symmetry. The structure contains two serinol [(HOCH2)2CHNH3]+ and five Na+ cations, which are octahedrally surrounded by 18 water molecules, and one [SbVWVI6O24]7 − anion. The serinol molecules also play a critical role in the synthesis by acting as a mild buffering agent. Each of the WVI and SbV ions is six-coordinated and displays a distorted octahedral motif. A three-dimensional supramolecular framework is formed via...
Source: Acta Crystallographica Section C - June 28, 2021 Category: Chemistry Authors: Sifaki, K. Gumerova, N.I. Giester, G. Rompel, A. Tags: polyoxometalate POM polyoxotungstate POT serinol crystal structure organic-inorganic hybrid research papers Source Type: research
Synthesis, crystal structure determination, and spectroscopic analyses of 1-chloro-2-(2,6-diisopropylphenyl)-4,4-dimethyl-2-azaspiro[5.5]undecane-3,5-dione: an unyielding precursor to a cyclic (alkyl)(amido)carbene
The synthesis, single-crystal X-ray structure, and 1H and 13C NMR spectrocopic analyses of an unyielding precursor molecule to a cyclic (alkyl)(amido)carbene, 1-chloro-2-(2,6-diisopropylphenyl)-4,4-dimethyl-2-azaspiro[5.5]undecane-3,5-dione, C24H34ClNO2 (1), is reported. Despite the use of several bases, 1 could not be deprotonated to afford the corresponding carbene. The crystal structure of 1 was compared to the crystal structures of two structurally similar HCl adducts of stable carbenes (compounds 4 and 5), which revealed no significant differences in the geometries about the `carbene' C atoms. To better understand the...
Source: Acta Crystallographica Section C - June 25, 2021 Category: Chemistry Authors: Hudnall, T.W. Reinheimer, E.W. Dorsey, C.L. Tags: carbene carbene precursor CAAC DAC crystal structure percent buried volume undecanedione research papers Source Type: research
One- and two-dimensional PbII compounds resulting from reaction of PbBr2 and Pb(SCN)2 with pyrimidine-2-thione
Pyrimidine-2-thione (HSpym) reacts with lead(II) thiocyanate and lead(II) bromide in N,N-dimethylformamide (DMF) to form poly[( μ -isothiocyanato- κ 2N:S)( μ 4-pyrimidine-2-thiolato- κ 6N1,S:S:S:S,N3)lead(II)], [Pb(C4H3N2S)(NCS)]n or [Pb(Spym)(NCS)]n, (I), and the polymeric one-dimensional (1D) compound catena-poly[[ μ 4-bromido-di- μ -bromido-( μ -pyrimidine-2-thiolato- κ 3N1,S:S)( μ -pyrimidine-2-thione- κ 3N1,S:S)dilead(II)] N,N-dimethylformamide monosolvate], {[Pb2Br3(C4H3N2S)(C4H4N2S)] · C3H7NO}n or {[Pb2Br3(Spym)(HSpym)] · DMF}n, (IIa), respectively. Poly[ μ 4-bromido-di- μ 3-bromido-( μ -pyrimidine-2-...
Source: Acta Crystallographica Section C - June 25, 2021 Category: Chemistry Authors: Schwade, V.D. Tirloni, B. Tags: pyrimidine-2-thione diffuse reflectance FT-IR crystal structure PXRD one-dimensional coordination polymer research papers Source Type: research
Stabilization of an elusive tautomer by metal coordination
The solid-state isolation of the different tautomers of a chemical compound can be a challenging problem. In many cases, tautomers with an energy very close to the most stable one cannot be isolated (elusive tautomers). In this article, with reference to the 4-methyl-7-(pyrazin-2-yl)-2H-[1,2,4]triazolo[3,2-c][1,2,4]triazole ligand, for which the elusive 3H-tautomer has an energy only 1.4 kcal mol − 1 greater than the most stable 2H form, we show that metal complexation is a successful and reliable way for stabilizing the elusive tautomer. We have prepared two complexes of the neutral ligand with CuBr2 and ZnBr2, ...
Source: Acta Crystallographica Section C - June 22, 2021 Category: Chemistry Authors: Parisi, E. Centore, R. Tags: heterocycle triazole tautomerism elusive tautomer crystal structure zinc copper research papers Source Type: research
Crystal structure and computational study of an oxo-bridged bis-titanium(III) complex
The solid-state structure of the new compound μ -oxido-bis[dichloridotris(tetrahydrofuran- κ O)titanium(III)], [Ti2Cl4O(C4H8O)6], at 150 K has been determined. The crystal has monoclinic (C2/c) symmetry and the complex features C2 symmetry about the bridging O atom. Positional disorder is evident in one of the three tetrahydrofuran environments. A post-Hartree – Fock computational analysis indicates that the complex has nearly degenerate triplet and singlet spin states, with the former favoured slightly by ca 2 kJ mol − 1. (Source: Acta Crystallographica Section C)
Source: Acta Crystallographica Section C - June 19, 2021 Category: Chemistry Authors: Bloomfield, H.R. Hollett, J.W. Ritch, J.S. Tags: titanium(III) bimetallic complex coordination compound crystal structure computational modelling research papers Source Type: research
cis-Bis(l-DOPA- κ 2N,O)copper(II) monohydrate: synthesis, crystal structure, and approaches to the analysis of pseudosymmetry
The crystal structure of the cis isomer of cis-bis(l-DOPA- κ 2N,O)copper(II) monohydrate (l-DOPA is 3,4-dihydroxy-l-phenylalanine) (CuLD), [Cu(C9H10NO4)2] · H2O, is a singular example of a structurally characterized, homoleptic, crystalline metal l-DOPA complex. CuLD crystallizes in the space group P21, with Z ′ = 2. The two independent molecules are square planar, and are interconnected by a linear hydrogen-bonded chain containing 12 independent hydrogen bonds. The copper ions in both molecules have weak apical intermolecular Cu...O interactions [2.739 (2) and 2.973 (2) Å ] with catechol – OH groups. A ...
Source: Acta Crystallographica Section C - June 16, 2021 Category: Chemistry Authors: O'Brien, P. Poyner, E.A. Alraddadi, T.S. Hursthouse, M.B. Foxman, B.M. Tags: Parkinson's disease homolepic complex pseudosymmetry linear packing crystal structure research papers Source Type: research
Molecular structures of the pentaphenylcyclopentadienyl iron complexes [(C5Ph5)Fe(CO)2R] (R = Me, Ph, iPr and Bu)
The PdII-catalysed reaction of [(C5Ph5)Fe(CO)2Br] with Grignard compounds RMgX or butyl lithium gave the iron alkyl/aryl complexes [(C5Ph5)Fe(CO)2R] (R = Me, Ph, iPr and Bu) in 59 – 73% yield, namely, dicarbonylmethyl( η 5-pentaphenylcyclopentadienyl)iron, [Fe(CH3)(C35H25)(CO)2], dicarbonyl( η 5-pentaphenylcyclopentadienyl)phenyliron, [Fe(C6H5)(C35H25)(CO)2], dicarbonyl(isopropyl)( η 5-pentaphenylcyclopentadienyl)iron, [Fe(C3H7)(C35H25)(CO)2], and butyldicarbonyl( η 5-pentaphenylcyclopentadienyl)iron, [Fe(C4H9)(C35H25)(CO)2]. The crystal structure determinations showed the usual `paddle-wheel' orientation of the p...
Source: Acta Crystallographica Section C - June 16, 2021 Category: Chemistry Authors: S ü nkel, K. Klein-He ß ling, C. Tags: pentaphenylcyclopentadienyl iron carbonyl Pd-catalysed crystal structure research papers Source Type: research
Study of naphthopyran derivatives: structure and photochromic properties in solution and in polymer film
Four naphthopyran derivatives, namely, 3,3-bis(naphthalen-1-yl)-3H-naphtho[2,1-b]pyran, C33H22O, NP1, 3,3-bis([1,1 ′ -biphenyl]-4-yl)-3H-naphtho[2,1-b]pyran, C37H26O, NP2, 3,3-bis(4-phenoxyphenyl)-3H-naphtho[2,1-b]pyran, C37H26O2, NP3, and 3,3-bis(4-methoxy-2-methylphenyl)-3H-naphtho[2,1-b]pyran, C29H26O3, NP4, were synthesized and their photochromic properties investigated. NP1 – NP4 exhibited good photochromism in different solutions and in poly(methyl methacrylate) (PMMA) film under UV light irradiation. Solvatochromism and the electronic and steric effects of the substituent group on photochromism were analyzed and...
Source: Acta Crystallographica Section C - June 16, 2021 Category: Chemistry Authors: Shi, L. Sun, Z. Tian, J. Huang, Y. Meng, J. Tags: photochromism single crystal naphthopyran fading speed crystal structure solvatochromism fatigue resistance research papers Source Type: research
Crystal structure and optical properties of a two-sited EuIII compound: an EuIII ion coordinated by two [EuIII(DOTA)] − complexes (DOTA is 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetate)
The structure and solid-state luminescence properties of an EuIII compound with two different lanthanide sites, [Eu( μ -O)5(OH)(H2O)2][Eu(DOTA)(H2O)]2 (DOTA is 1,4,7,10-tetrazacyclododecane-1,4,7,10-tetraacetate, C16H24N4O8), were determined. The compound crystallizes in a laminar structure in the triclinic space group P\overline{1}, where the two sites are a free europium(III) ion and an [Eu(DOTA)(H2O)] − complex. The crystal structure was determined using complex data treatment due to nonmerohedral twinning. Experimental data sets were recorded with large redundancy and separated according to scattering domains in ord...
Source: Acta Crystallographica Section C - June 10, 2021 Category: Chemistry Authors: Thomsen, M.S. Madsen, A. Ø . S ø rensen, T.J. Tags: europium(III) luminescence twinning lanthanide chemistry optical properties crystal structure research papers Source Type: research
Alkali metal salts of 4-hydroxybenzoic acid: a structural and educational study
As part of an educational exercise designed to introduce school students to the technique of single-crystal X-ray diffraction and enhance their understanding of primary and secondary bonding, a group of nine secondary school students was given the opportunity to prepare new compounds and to solve and refine data collected on the crystalline materials they had prepared. Their investigation of the alkali metal salts of 4-hydroxybenzoic acid (H2hba) yielded nine new compounds and their structures are described in this article. Whilst the salts might be expected to have similar atomic arrangements, there are significant differ...
Source: Acta Crystallographica Section C - June 9, 2021 Category: Chemistry Authors: Abrahams, B.F. Commons, C.J. Hudson, T.A. Sanchez Arlt, R. White, K.F. Chang, M. Jackowski, J.J. Lee, M. Lee, S.X. Liu, H.D. Mei, B.M. Meng, J.E. Poon, L. Xu, X. Yu, Z. Tags: crystal structure short strong hydrogen bond SSHB hydrogen-bonded network crystallographic education hydroxybenzoic acid bilayer ionic network crystal engineering research papers Source Type: research
Structural, spectroscopic and DFT theoretical studies of phosphorescent CuIP2S-containing cuprous complexes
Luminescent cuprous complexes are important coordination compounds due to their relative abundance, low cost and ability to display excellent luminescence. The structures of two CuIP2S-type cuprous complexes, namely, iodido(thiourea- κ S)bis(triphenylphosphane- κ P)copper(I), [CuI(CH4N2S)(C18H15P)2] or [CuI(TU)(TPP)2] (I), and (2,3-dihydrobenzimidazole-2-thione- κ S)iodidobis(triphenylphosphane- κ P)copper(I), [CuI(C7H6N2S)(C18H15P)2] or [CuI(DHBIT)(TPP)2] (II), are described. In these two structures, the complex molecules of both are constructed by one copper(I) centre, one iodide ion, two TPP ligands and one thione l...
Source: Acta Crystallographica Section C - June 7, 2021 Category: Chemistry Authors: Liang, Y. Wang, J.-T. Song, L. Dai, D.-Q. Wang, Y.-Y. Chai, W.-X. Tags: CuIP2S-type cuprous complex thione ligand crystal structure phosphorescence TD-DFT wavefunction analysis research papers Source Type: research
Zinc(II) and nickel(II) complexes of 3,5-dimethyl-1-(pyridin-2-yl)-1H-pyrazole: relationship between fluorescence and crystal packing
Two novel coordination complexes, namely, dichlorido[3,5-dimethyl-1-(pyridin-2-yl- κ N)-1H-pyrazole- κ N2]zinc(II), [ZnCl2(C10H11N3)], 1, and aquachloridobis[3,5-dimethyl-1-(pyridin-2-yl- κ N)-1H-pyrazole- κ N2]nickel(II) chloride monohydrate, [NiCl(C10H11N3)(H2O)]Cl · H2O, 2, have been synthesized. The crystal structure analyses revealed that complexes 1 and 2 are mononuclear and have ZnN2Cl2 distorted tetrahedral and NiN4OCl distorted octahedral structures, respectively. Complex 1 displays a dimer in the crystal structure, while complex 2 forms a chain along the [010] direction. The fluorescence properties of both c...
Source: Acta Crystallographica Section C - June 7, 2021 Category: Chemistry Authors: Ma ł ecka, M. Kusz, J. Mayer, P. Sobiesiak, M. Budzisz, E. Tags: fluorescence properties crystal structure hydrogen bonding pyrazole derivatives zinc(II) nickel(II) research papers Source Type: research
Contributions of secondary alcohol – ketone O — H...O=C and furan – acetate Csp2 — H...OOC synthons to the supramolecular packings of two bioactive molecules
The crystal structures of rubescin D (1, C26H30O5) and monadelphin A (2, C30H36O11), bioactive molecules of the vilasinin and gedunin classes of limonoids, respectively, are reported for the first time and the synthons affecting their crystal packings are analyzed on the basis of their occurrences in molecules in the Cambridge Structural Database that share the same moieties. Rubescin D, 1, crystallizes in the space group P21 and its molecular structure consists of three six-membered rings A, C and D having, respectively, envelope, twist-boat and half-chair conformations, and three five-membered rings with half-chair (B an...
Source: Acta Crystallographica Section C - May 27, 2021 Category: Chemistry Authors: Kenfack Tsobnang, P. Tsamo Tontsa, A. Mbiangu é , Y.A. Kemda Nangmo, P. Kenfack Tiofack, S. Mkounga, P. Nkengfack Ephrem, A. Tonl é Kenfack, I. Tags: crystal engineering synthon vilasinin gedunin Cambridge Structural Database CSD crystal structure rubescin D monadelphin A bioactivity research papers Source Type: research
Synthesis, spectroscopic investigation, crystal structure analysis, quantum chemical study, biological activity and molecular docking of three isatin derivatives
Three isatin derivatives, namely, 1-allyl-3-hydroxy-3-(6-oxocyclohex-1-en-1-yl)indolin-2-one, C17H17NO3, 1-ethyl-3-hydroxy-3-(6-oxocyclohex-1-en-1-yl)indolin-2-one, C16H17NO3, and 5-bromo-3-hydroxy-1-methyl-3-(6-oxocyclohex-1-en-1-yl)indolin-2-one, C15H14BrNO3, were synthesized, crystallized by the slow-evaporation technique, characterized by 1H and 13C NMR spectroscopy, and analysed by the single-crystal X-ray diffraction (XRD) method. Quantum chemical parameters, such as the energy of the highest occupied molecular orbital, energy of the lowest unoccupied molecular orbital, energy gap, electronic energy, ionization poten...
Source: Acta Crystallographica Section C - May 26, 2021 Category: Chemistry Authors: Bargavi, S. Gouthaman, S. Sugunalakshmi, M. Lakshmi, S. Tags: isatin derivatives spectroscopy crystal structure quantum chemical calculations druglikeness bioactivity score antimicrobial molecular docking research papers Source Type: research
Novel Ba2+ and Pb2+ metal – organic frameworks based on a semi-rigid tetracarboxylic acid: syntheses, structures, topologies and luminescence properties
Multidentate carboxylate ligands have been widely used in the construction of metal – organic frameworks (MOFs) owing to the rich variety of their coordination modes, which can lead to crystalline products with interesting structures and properties. Two new main-group MOFs, namely, poly[[di- μ -aqua-diaqua(dimethylformamide)[ μ 7-5,5 ′ -methylenebis(2,4,6-trimethylbenzene-1,3-dicarboxylato)]dibarium(II)] trihydrate], {[Ba2(C23H20O8)(C3H7NO)(H2O)4] · 3H2O}n or {[Ba2(BTMIPA)(DMF)(H2O)4] · 3H2O}n (1), and poly[[diaqua[ μ 6-5,5 ′ -methylenebis(2,4,6-trimethylbenzene-1,3-dicarboxylato)]dilead(II)] 2.5-hydrate], {[Pb2...
Source: Acta Crystallographica Section C - May 26, 2021 Category: Chemistry Authors: Sun, Y. Chen, Z. Wang, X. Wang, L. Yang, X. Liang, X. Fan, S. Zhang, P. Tags: crystal structure MOF metal-organic framework semi-rigid tetracarboxylic acid topological analysis fluorescence properties research papers Source Type: research
